FINAL REPORT

6 May 2009

70000 metric ton Acrylic

Acid Production Plant

Prepared by:
Jackson Toh
Lee Sin Wei
Lee Yu Wee
Lim Yee Chiat
Mohd Izham bin Ibrahim

KEK 050019
KEK 050035
KEK 050036
KEK 050039
KEK 050042

Department of Chemical Engineering University of Malaya

50603 Kuala Lumpur

TABLE OF CONTENT
Content
Chapter 1:

Pages

Introduction

1.1

Biodiesel Production

1-1

1.2

Glycerol Produced from Biodiesel Plant

1-1

1.3

Potential Product of Glycerol

1.3.1 Process Route
1.3.1.1 Acrylic Acid via Acrolein
1.3.1.2 Propylene Glycol
1.3.1.3 Hydrogen
1.3.1.4 Epichlorohydrin
1.3.2 Comparison of the Products

1.4

1-2
1-2
1-2
1-3
1-3

Introduction of Acrylic Acid

1.4.1 Description
1.4.2 Chemical Identification
1.4.3 Potential Usage of Acrylic Acid
1.4.4 Physical Properties of Acrylic Acid

1.5 References
Chapter 2:

1-4
1-4
1-4
1-5
1-6

Process Description of Acrylic Acid Production

2.1

Process Principle

2-1

2.2

Unit Operation Description

2.2.1 Reactor 1, CRV-100
2.2.2 Separator, V-100
2.2.3 Reactor 2, CRV-101
2.2.4 Quenching Tower, T-100
2.2.5 Extractive Distillation Column, T-101
2.2.6 Decanter, X-100
2.2.7 Solvent Recovery Distillation Column, T-102

2-1
2-2
2-2
2-2
2-3
2-3
2-3

2.3

Process Description

2-3

2.4

Process Flow Diagram

2.4.1 Flow Description

2-6
2-7

2.5

References

2-10
i

TABLE OF CONTENT
Content
Chapter 3:
3.1

Plant Economic & Feasibility Study

Market Analysis
3.1.1 Global Demand
3.1.2 Local Demand
3.1.3 Forecasted Future Demand
3.1.4 Production of Acrylic Acid
3.1.5 Major Manufacturer of Acrylic Acid

3.2

3.3

3.4

3.5

Pages

3-1
3-2
3-2
3-2
3-3

Location of Acrylic Acid Plant

3.2.1 Site Selection
3.2.2 Plant location

3-3
3-5

Government Policy-Taxation
3.3.1 Company Tax
3.3.2 Real Property Gain Tax
3.3.3 Sales Tax
3.3.4 Import Tax

3-6
3-7
3-7
3-7

Economic Evaluation

3-7

3.4.1 Purchased Equipment

3.4.2 Total Capital Investment
3.4.3 Total Product Cost
3.4.4 Profitable Analysis

3-8
3-9
3-10
3-11

References

3-13

ii

TABLE OF CONTENT
Content

Pages

Chapter 4: Environmental, Safety and Health

4.1

4.2

Environment
4.1.1 Law and Regulation
4.1.2 Waste Water Treatment
4.1.3. Gas Emmision and Treatment

4-1
4-1
4-3

Health
4.2.1 Effect to Human
4.2.1.1 Acetic Acid
4.2.1.1.1 Health Hazard

4-5

4.2.1.1.2. Exposure Limits

4-5

4.2.1.2 Acetol
4.2.1.2.1 Health Hazard

4-5

4.2.1.2.2 Exposure Limits

4-5

4.2.1.3 Acrolein
4.2.1.3.1 Health Hazard

4-5

4.2.1.3.2 Exposure Limits

4-6

4.2.1.4 Acrylic Acid

4.2.1.4.1 Health Hazard

4-6

4.2.1.4.2 Exposure Limits

4-6

4.2.1.5 Carbon Dioxide

4.2.1.5.1 Health Hazard

4-6

4.2.1.5.2 Exposure Limits

4-7

4.1.1.6 Glycerol
4.2.1.6.1 Health Hazard

4-7

4.2.1.6.2 Exposure Limits

4-7

iii

TABLE OF CONTENT
Content

Pages

Chapter 4: Environmental, Safety and Health

4.2.2 Effect to Environment

4.3

4.2.2.1 Acetic Acid

4-7

4.2.2.2 Acrolein

4-7

4.2.2.3 Acrylic Acid

4-7

4.2.2.4 Glycerol

4-8

Safety
4.3.1 Hazard Introduction

4-8

4.3.2 Handling and Storage of Hazardous Chemical

4.4

4.3.2.1 Acetic acid

4-9

4.3.2.2 Acetol

4-9

4.3.2.3 Acrolein

4-9

4.3.2.4 Acrylic Acid

4-10

4.3.2.5 Glycerol

4-10

4.3.2.6 Isopropyl Acetate

4-10

4.3.2.7 Thermal Oil

4-11

References

4-11

iv

TABLE OF CONTENT
Content

Pages

Chapter 5: Mass and Energy Balances

5.1

Introduction

5-1

5.2

Comparison between Manual Calculations and HYSIS Result

5.2.1 Approach of Manual Calculation
5.2.2 Approach to HYSIS Simulation

5-1
5-1

Mass Balance Results

5.3.1 Feed rate calculation
5.3.2 Mixture of Stream 4 and 16
5.3.3 CRV-100
5.3.4 V-100
5.3.5 Purge Stream from Stream 10
5.3.6 Mixture of Stream 14, 15 and 16
5.3.7 Mixture of Stream 20, 21 and 22
5.3.8 CRV-101
5.3.9 Mixture of Stream 26 and 34
5.3.10 T-100
5.3.11 MIX-100
5.3.12 T-101
5.3.13 X-100
5.3.14 T-103

5-1
5-2
5-2
5-2
5-3
5-4
5-4
5-4
5-5
5-5
5-5
5-6
5-6
5-7

5.3

5.4

Comparison of Mass Balance Results between Hand Calculations with HYSIS

5-7

5.5

Energy Balance Results

5.6

Comparison Energy Balance Result between Hand Calculation and HYSIS

5-8

5-9

TABLE OF CONTENT
Content

Pages

Chapter 6: Packed Bed Reactor 1

6.1

CHEMICAL ENGINEERING DESIGN

6.1.1 Introduction

6-1

6.1.2

6-2

Type of Catalyst

6.1.3 Type of Reactor

6-2
6.1.3.1 Packed Bed Reactor
6-2
6.1.3.1.1 Type of Heat Transfer Fluid
6-3
6.1.3.1.2 Packed Bed Reactor Dimension
6-4
6.1.3.1.3 Equation Involved in Packed Bed Reactor Design
6-5
6.1.3.1.3.1 Rate Law
6-5
6.1.3.1.3.2 Mole Balance
6-6
6.1.3.1.3.3 Ergun Equation for Pressure Drop
6-6
6.1.3.1.3.4 Simultaneous Ordinary Differential Equations
6-7
6.1.3.1.4 Packed Bed Reactor Optimization
6-8
6.1.3.1.4.1 Shell Diameter Analysis
6-9
6.1.3.1.4.2 Pressure Analysis
6-10
6.1.3.1.4.3 Temperature Analysis
6-12
6.1.3.1.4.4 Result of Packed Bed Reactor Optimization Analysis 6-12
6.1.3.2 Fluidized Bed Reactor
6-13
6.1.3.2.1 Equation Involved in Fluidized Bed Reactor Design
6-14
6.1.3.2.1.1 Conversion of Glycerol in Fluidized Bed Reactor
6-14
6.1.3.2.2 Fluidized Bed Reactor Optimization
6-15
6.1.3.2.2.1 Temperature Analysis
6-15
6.1.3.2.2.2 Reactor Diameter Analysis
6-16
6.1.3.2.2.3 Result of Fluidized Bed Reactor Optimization Analysis 6-17
6.1.3.3 Comparison of Packed Bed and Fluidized Bed Reactor
6-17
6.1.4 Heat Duty of Heating Jacket

6-18

vi

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Content

Pages

Chapter 6: Packed Bed Reactor 1

6.1.5

Clean Overall Heat Transfer Coefficient

6.1.5.1 Tube-side Film Coefficient, hio
6.1.5.2 Shell-side Film Coefficient, ho

6-19
6-19
6-19

6.1.6

Fouling Factor

6-20

6.1.7 Summary of Specification of Reactor 1

6-21

6.2

MECHANICAL ENGINEERING DESIGN

6.2.1

Design Pressure

6-22

6.2.2

Design Temperature

6-22

6.2.3

Material of Construction

6-22

6.2.4

Design Stress

6-22

6.2.5

Welded Joint Efficiency

6-23

6.2.6

Corrosion Allowance

6-23

6.2.7

Minimum Practical Wall Thickness

6-23

6.2.8 Head and Closure

6-24

6.2.9

6-24

Connection

6.2.10 Manhole

6-24

6.2.11 Compensation for Openings

6-25
vii

TABLE OF CONTENT
Content

Pages

Chapter 6: Packed Bed Reactor 1

6.2.11.1 Compensate Opening for Feed
6.2.11.2 Compensate Opening for Molten Salt (Heater)

6-25
6-25

6.2.12 Dead Weight Load

6.2.12.1 Cylindrical Vessel
6.2.12.2 Tubes
6.2.12.3 Catalyst
6.2.12.4 Baffles
6.2.12.5 Feed
6.2.12.6 Molten Salt
6.2.12.7 Insulation
6.2.12.8 Total Dead Weight

6-26
6-26
6-27
6-27
6-27
6-28
6-28
6-28
6-29

6.2.13 Winds Load

6-29

6.2.14 Analysis Stress

6.2.14.1 Pressure Stress
6.2.14.2 Dead Weight Stress
6.2.14.3 Bending Stress
6.2.14.4 Resultant Longitudinal Stresses

6-29
6-29
6-30
6-30
6-30

6.2.15 Vessel Support

6.2.15.1 Skirt Supports
6.2.15.2 Total Weight
6.2.15.3 Bending Stress
6.2.15.4 Dead Weight Stress
6.2.15.5 Tensile Stress
6.2.15.6 Compressive Stress

6-31
6-31
6-31
6-31
6-32
6-32
6-32

6.2.16 Criteria for Design

6-32

6.2.17 Summary of Mechanical Design of Reactor 1

6-33

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TABLE OF CONTENT
Content

Pages

Chapter 6: Packed Bed Reactor 1

6.3

SAFETY AND PROCESS CONTROL

6.3.1

Safety Consideration
6.3.1.1 Safety Review
6.3.1.2 Reactor Potential Hazards
6.3.1.3 Reactor Safety Practices

6-36
6-36
6-37
6-37

6.3.2

Hazard and Operability Studies (HAZOP) Analysis

6.3.2.1 Objectives of HAZOP
6.3.2.2 HAZOP Procedures

6-38
6-38
6-38

6.3.3

Process Control and Instrumentation

6.3.3.1 Description of Instruments
6.3.3.2 Description of Control System
6.3.3.2.1 Inlet Feed Temperature Control
6.3.3.2.2 Inlet Feed Flow and Pressure Control
6.3.3.2.3 Molten Salt (Heating Stream) Temperature Control

6-45
6-45
6-45
6-45
6-48
6-48

6.4

Reference

6-48

ix

TABLE OF CONTENT
Content

Pages

Chapter 7: Packed Bed Reactor 2

7.1.0. CHEMICAL ENGINEERING DESIGN

7.1.0.1 Vapour Phase Oxidation of Propylene and Acrolein
7.1.0.2 Objective
7.1.0.3 Reactor Selection

7-1
7-1
7-1

7.1.1. Process Description

7.1.1.1. Feed Stream Condition
7.1.1.2. Properties of Feed Stream and Cooling Stream
7.1.1.3. Properties of Catalyst

7-2
7-2
7-3

7.1.2. Process Principle

7.1.2.1. Proposed Reaction Scheme for Oxidation of Acrylic Acid

7-4

7.1.3. Chemical Design

7.1.3.1. Kinetic Parameter
7.1.3.2. Assumptions
7.1.3.3. Catalyst Weight and Pressure Drop
7.1.3.4. Reactor Sizes
7.1.3.5. Tube Size Selection
7.1.3.6. Number of Tubes
7.1.3.7. Number of Tubes Passes
7.1.3.8. Tube Pitch and Buddle Diameter
7.1.3.9. Shell Inside Diameter
7.1.3.10. Baffles

7-4
7-5
7-5
7-7
7-7
7-7
7-8
7-8
7-8
7-8

7.1.4. Cooling Stream Requirement

7.1.4.1.Log Mean Temperature Difference
7.1.4.2.Cooling Water Flow
7.1.4.3.Tube Side Heat Transfer Coefficient
7.1.4.4.Shell Side Heat Transfer Coefficient
7.1.4.5.Overall Heat Transfer Coefficient
7.1.4.6.Heat Transfer Area Required

7-9
7-9
7-10
7-10
7-11
7-12

Content

Pages

Chapter 7: Packed Bed Reactor 2

7.1.5. Pressure Drop

7.1.5.1. Tube Side Pressure Drop
7.1.5.2. Shell Side Pressure Drop

7-12
7-12

7.1.6. Fluidized Bed Reactor

7.6.1.1.Minimum Fluidization Superficial Velocity, vsfm
7.6.1.2.Minimum Bubbling Velocity, vmb
7.6.1.3.Terminal Velocity, ut
7.6.1.4.Superficial velocity, vsf
7.6.1.5.Actual Velocity, v
7.6.1.6.Diameter of reactor, D
7.6.1.7.Minimum Reactor Wall Thickness, tm
7.6.1.8.Outer Diameter, OD
7.6.1.9.Bubble Velocity, vB
7.6.1.10. Slugging Problem & Reactor Height at Minimum Fluidization, Hmf
7.6.1.11. Reactor Height
7.6.1.12. Pressure Drop
7.6.1.13. Comparison between FBR and PBR

7-13
7-13
7-14
7-14
7-14
7-14
7-15
7-15
7-15
7-16
7-16
7-17
7-18

7.1.7. Summary of Chemical Engineering Design

7-19

7.1.8. Cost Analysis

7-20

7.1.9. Comparison of the Conversion

7-20

7.1.10. Comparison of the Molar Flow of the Components in Reactor Product Stream
7-21
7.1.11. Case study
7.1.11.1. Optimization of Temperature
7.1.11.2. Optimization of Pressure
7.1.11.3. Summary Optimization Analysis

7-22
7-22
7-23

xi

Content

Pages

Chapter 7: Packed Bed Reactor 2

7.2.0. MECHANICAL ENGINEERING DESIGN

7.2.0.1. Codes and Standards
7.2.1. General Design Considerations
7.2.1.1. Design Pressure
7.2.1.2. Design Temperature
7.2.1.3. Material of Construction
7.2.1.4. Design Stress (Nominal Design Strength)
7.2.1.5.Welded Joint Efficiency and Construction Categories
7.2.1.6.Corrosion Allowance

7-24

7-24
7-24
7-25
7-25
7-26
7-26

7.2.2. Shell and Tube Wall Thickness Design

7.2.2.1.Shell Wall Thickness and Outer Diameter
7.2.2.2.Tube Wall Thickness
7.2.2.3.Head and Closure
7.2.2.4.Tube Sheet Thickness

7-26
7-27
7-27
7-27

7.2.3. Design Loads

7.2.3.1.Dead Weight Load
7.2.3.2.Weight of Vessel
7.2.3.3. Total Dead Weight
7.2.3.4. Wind Load

7-28
7-28
7-30
7-30

7.2.4. Stress Analysis

7-31

7.2.5. Vessel Support

7.2.5.1.Design of Skirt Support
7.2.5.2.Pipe Sizing for Nozzles and Flanges
7.2.5.3.Manholes
7.2.5.4.Base Ring and Anchor Bolt

7-32
7-33
7-34
7-35

7.2.6. Summary of Mechanical Engineering Design

7-36

xii

Content

Pages

Chapter 7: Packed Bed Reactor 2

7.3.0. SAFETY, CONTROL AND INSTRUMENTATION

7.3.1. The Importance of Safety
7.3.1.1. Safety Considerations
7.3.1.1.1. Pressure Relief Systems
7.3.1.1.2. Effects of Fouling
7.3.1.1.3. Corrosion Failure
7.3.1.1.4. Stress Failure

7-38
7-39
7-39
7-39
7-39

7.3.2. Process Safety Design

7-40

7.3.3. Process Hazard Analysis (HAZOP Analysis)

7-40

7.3.4. The Importance of Control System

7-46

7.3.4.1. Types of Controller

7.3.4.1.1. Temperature Control
7.3.4.1.2. Pressure Control
7.3.4.1.3. Level Control
7.3.4.1.4. Feed Flow Control
7.3.4.1.5. Feed Composition Control
7.3.4.2. Control System Loop
7.3.4.2.1. Feed Flow Control (Control System Loop 1)
7.3.4.2.2. Reactor Pressure Control (Control System Loop 2)
7.3.4.2.3. Cooling Stream and Reactor Temperature Control
(Control System Loop 3)

7-46
7-47
7-47
7-47
7-47

7-48
7-48
7-48

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Pages

Chapter 8: Quenching Tower

8.1

CHEMICAL ENGINEERING DESIGN

8.1.1 Objective

8-1

8.1.2

Introduction
8.1.2.1 The Mechanism of Absorption

8-1
8-1

8.1.3

General Design Decisions

8.1.4

8.1.3.1 Choices of Solvent

8-3

8.1.3.2 Determination of Operating Pressure and Temperature

8-3

8.1.3.3 Selection of the Type of Quenching Tower

8-4

8.1.3.4 Simulation of Design Problem

8-4

8.1.3.5 Physical Properties Data

8-5

8.1.3.6 Prediction of Overall Column Efficiency

8-6

8.1.3.7 Number of Stage

8-7

Plate Specifications and Configurations

8.1.4.1 Plate Contactors

8-8

8.1.4.2 Choice of Plate Type

8-9

8.1.4.3 Plate Design Algorithm

8-10

8.1.4.4 Physical Properties

8-12

8.1.4.5 Plate Spacing

8-12

8.1.4.6 Column Diameter

8-13

8.1.4.7 Flow Arrangements

8-14

8.1.4.8 Provisional Plate Design

8-15

8.1.4.9 Weep Point

8-17

8.1.4.10 Pressure Drop

8-19

8.1.4.10.1 Column Pressure Drop Estimation

8-20
xiv

TABLE OF CONTENT
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Pages

Chapter 8: Quenching Tower

8.1.4.10.2 Dry Plate Drop

8-20

8.1.4.10.3 Residual Head

8-22

8.1.4.11 Downcomer Liquid Back-up

8-22

8.1.4.12 Residence Time

8-24

8.1.4.13 Entrainment

8-24

8.1.4.14 Trial Layout

8-25

8.1.4.14.1 Perforated Area

8-26

8.1.4.15 Hole Pitch

8-27

8.1.4.16 Height of Column

8-29

8.1.5

Summary of Chemical Design Parameter

8-30

8.2

MECHANICAL ENGINEERING DESIGN

8.2.1

Introduction

8-31

8.2.2

Vessel Function

8-31

8.2.3

Operating Design Pressure and Temperature

8.2.3.1 Design Pressure
8.2.3.2 Design Temperature

8-31
8-31
8-31

8.2.4

Material of Construction

8-32

8.2.5

Maximum Allowable Stress Value

8-32

8.2.6

Welded Joint Efficiency

8-33

8.2.7

Corrosion Allowance

8-33

8.2.8

Design of Thin Walled Vessel

8-33

8.2.9

Torispherical Head Design

8-34

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Chapter 8: Quenching Tower

8.2.10 Design of Vessel Subject to Combined Loading
Dead Weight of Vessel
8.2.10.1
8.2.10.1.1
Shell
8.2.10.1.2
Plates
8.2.10.1.3
Insulation
8.2.10.2
Wind Loading
8.2.10.3
Analysis of Stress
8.2.10.1.3.1 Pressure Stresses
8.2.10.1.3.2 Longitudinal and Circumferential Stresses due to Pressure
8.2.10.1.3.3 Dead Weight Stress
8.2.10.1.3.4 Bending Stress
8.2.10.1.3.5 Check Elastic Stability (Bucking)

8-35
8-35
8-35
8-35
8-36
8-36
8-37
8-37
8-37
8-37
8-37
8-38

8.2.11 Design of Skirt Support

8.2.11.1 Operating Weight
8.2.11.1.1 Weight of Full Liquid
8.2.11.1.2 Weight of Skirt
8.2.11.2 Thickness of Skirt

8-39
8-39
8-39
8-40
8-40

8.2.12 Opening

8-41

8.2.13 Design of Manhole

8-42

8.2.14 Design of Anchor Bolt

8.2.14.1 Design Anchor Bolt
8.2.14.2 Checking Stress in Anchor Bolt

8-43
8-43
8-44

8.2.15 Design of Base Ring

8.2.15.1 Design Base Ring
8.2.15.2 Checking Stress

8-44
8-44
8-45

8.2.16 Design Parameters

8-46

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Chapter 8: Quenching Tower

8.3 SAFETY, CONTROL & INSTRUMENTATION

8.3.1 Safety Analysis
8.3.1.1 Introduction
8.3.1.2 Hazardous and Operability Study
8.3.1.3 Conclusion

8-48
8-48
8-48
8-49

8.3.2

Control and Instrumentation

8.3.2.1 Introduction
8.3.2.2 Control of Quenching Tower
8.3.2.3 Control Variable and Parameter

8-50
8-50
8-50
8-51

8.4

Nomenclatures

8-53

8.5

References

8-57

xvii

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Pages

Chapter 9: Extractive Distillation Column

9.1.0. CHEMICAL ENGINEERING DESIGN

9.1.1Introduction

9-1

9.1.2 Objective

9-1

9.1.3 Process Description

9-2

9.1.4. Selection of Column

9.1.4.1. Selection of Internal Column
9.1.4.2. Packing Selection
9.1.4.3. Random Packing selection

9-3
9-3
9-3
9-3

9.1.5

9-4
9-4
9-4
9-5
9-5
9-6
9-6
9-8
9-8
9-9
9-9

Packed Column Design

9.1.5.1. Selection of solvent
9.1.5.2. Composition and condition of feed stream, distillate and bottom
9.1.5.3. Number of theoretical stages
9.1.5.4. Optimum Feed Location
9.1.5.5. Optimum reflux ratio
9.1.5.6. Column Diameter
9.1.5.7. Height of Packed Zone
9.1.5.8. Wetting rate
9.1.5.9. Liquid Hold-up
9.1.5.10. Operating Void Space

9.2.0. MECHANICAL ENGINEERING DESIGN

9.2.1Introduction

9-11

9.2.2 Material of Construction

9.2.2.1. Design Pressure
9.2.2.2. Design temperature
9.2.2.3. Material of construction
9.2.2.4. Material of construction
9.2.2.5. Welded joint factor
9.2.2.6. Corrosion Allowance

9-11
9-11
9-11
9-11
9-11
9-12

9.2.3 Internal Fitting

9.2.3.1. Packing support

9-12
9-12
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Chapter 9: Extractive Distillation Column

9.2.4

9.2.3.2. Vapor distributor

9.2.3.3. Hold down plate
9.2.3.4. Liquid distributors
9.2.3.5. Liquid redistributors
9.2.3.6. Mist eliminator (Demister)
9.2.3.7. Support ledges
9.2.3.8. Manhole

9-12
9-12
9-12
9-13
9-13
9-13
9-13

Column Design
9.2.4.1. Cylindrical Shell Thickness
9.2.4.2. Vessel Head
9.2.4.3. Vessel Height
9.2.4.4. Flange
9.2.4.5. Load Analysis
9.2.4.5.1. Dead Weight loads
9.2.4.5.2. Wind load
9.2.4.6. Stress analysis
9.2.4.7. Support
9.2.4.8. Pipe Sizing for Nozzles
9.2.4.9. Reinforcement of Openings

9-14
9-14
9-14
9-14
9-15
9-15
9-15
9-15
9-15
9-15
9-16
9-16

9.3.0. SAFETY, CONTROL AND INSTRUMENTATION

9.3.1.Introduction

9-17

9.3.2 Control

9-17

9.3.3 Safety
9.3.3.1. HAZOP analysis

9-19
9-19

xix

TABLE OF CONTENT
Content

Pages

Chapter 10: Distillation Column

10.1. CHEMICAL ENGINEERING DESIGN

10.1.1. Introduction

10-1

10.1.2. Distillation Column Design

10.1.2.1. Schematic Diagram of T-102
10.1.2.2. Type of Column of T-102

10-1
10-2
10-3

10.1.3. Key Components

10-3

10.1.4. Number of Stages

10.1.4.1. Relative Volatility
10.1.4.2. Number of Stages and Operating Reflux Ratio
10.1.4.2.1. Minimum Number of Stages
10.1.4.2.2. Minimum Operating Reflux Ratio
10.1.4.3. Number of Theoretical Stages
10.1.4.4. Overall Column Efficiency
10.1.4.5. Actual Number of Stages

10-3
10-3
10-4
10-4
10-4
10-5
10-6
10-7

10.1.5. Feed Point Location

10-7

10.1.6. Plate Specification

10.1.6.1. Plate Spacing
10.1.6.2. Types of Plate
10.1.6.3. Liquid and Vapour Flow in a Plate Colum

10-7
10-7
10-8
10-8

10.1.7. Plate Design Procedure

10.1.7.1. Vapour and Liquid Flow Rates
10.1.7.2. Physical Properties
10.1.7.3. Column Diameter
10.1.7.3.1. Liquid Vapour Flow Factor
10.1.7.3.2. Flooding Velocity
10.1.7.3.3. Maximum Velocity Flow Rate
10.1.7.4. Liquid Flow Pattern

10-9
10-10
10-11
10-11
10-11
10-12
10-12
10-13
xx

TABLE OF CONTENT
Content

Pages

Chapter 10: Distillation Column

10.1.7.5. Provisional Plate Design
10.1.7.6. Check Weeping
10.1.7.6.1. Weir Liquid Crest
10.1.7.7. Plate Pressure Drop
10.1.7.7.1. Dry Plate Drop
10.1.7.7.2. Residual Head
10.1.7.7.3. Total Pressure Drop
10.1.7.8. Check Entrainment

10-14
10-14
10-15
10-16
10-16
10-17
10-17
10-17

10.1.8. Trial Layout

10-18

10.1.9. Perforated Area

10.1.9.1. Number of Holes

10-18
10-19

10.1.10. Column Height

10-19

10.1.11. Simulation by HYSYS

10.1.11.1. Approach by Manual Calculation
10.1.11.2. Approach by HYSYS

10-20
10-20
10-20

10.1 MECHANICAL ENGINEERING DESIGN

10.2.1. Introduction

10-21

10.2.2. General Design Consideration of Pressure Vessel

10.2.2.1. Design Pressure
10.2.2.2. Design Pressure
10.2.2.3. Materials of Construction
10.2.2.4. Design Stress
10.2.2.5. Welded Joint Efficiency
10.2.2.6. Corrosion Allowance

10-21
10-22
10-22
10-23
10-23
10-23
10-24

xxi

TABLE OF CONTENT
Content

Pages

Chapter 10: Distillation Column

10.2.3 Design Column
10.2.3.1 Wall Thickness
10.2.3.2 Design of Vessel Head
10.2.0.3.2.1 Choice of Closure
10.2.0.3.2.2 Design of Torispherical Head

10-24
10-24
10-25
10-25
10-25

10.2.4 Design of Vessel Loads

10.2.4.1 Weight Loads
10.2.4.2 Vessel Weight
10.2.4.3 Plate Weight
10.2.4.4 Cage Ladder Weight
10.2.4.5 Platform Stells Weight
10.2.4.6 Total Load Weight

10-26
10-26
10-26
10-27
10-27
10-27
10-27

10.2.5 Wind Loads

10.2.5.1 Load per Unit Length
10.2.5.2 Bending Moment at Colum Height

10-28
10-28
10-28

10.2.6 Analysis of Stress

10.2.6.1 Pressure Stress
10.2.6.2 Dead Weight Stress
10.2.6.3 Bending Stress
10.2.6.4 Principal Stress
10.2.6.5 Critical Buckling Stress

10-28
10-28
10-28
10-29
10-29
10-30

10.2.7 Vessel Support

10.2.7.1 Skirt Thickness
10.2.7.2 Bending Moment at Base of Skirt
10.2.7.3 Design Criteria

10-30
10-30
10-31
10-31

10.2.8 Manhole

10-32

10.2.9 Summary

10-33

xxii

TABLE OF CONTENT
Content

Pages

Chapter 10: Distillation Column

10.3 SAFETY, CONTROL AND INSTRUMENTATION

10.3.1 Introduction
10.3.1.1 Safety
10.3.1.2 Environment Protection
10.3.1.3 Equipment Protection
10.3.1.4 Smooth Plant Operation
10.3.1.5 Product Quality
10.3.1.6 Profit
10.3.1.7 Monitoring and Diagnosis

10-35
10-35
10-35
10-36
10-36
10-36
10-36
10-36

10.3.2 Distillation Control Objective

10-37

10.3.3 Column Control

10.3.3.1 Feed Stream Control
10.3.3.2 Product Quality Control
10.3. 3.3 Top Stream Control
10.3. 3.4 Bottom Stream Control

10-38
10-39
10-39
10-39
10-40

10.3.4 Instruments Notation

10-40

10.3.5 Instrumentations
10.3.5.1 Pressure Measurements
10.3.5.2 Flow Measurements
10.3.5.3 Level Measurements
10.3.5.4 Temperature Measurements

10-41
10-41
10-41
10-41
10-41

10.3.6 Hazards and Operability Study

10-43

xxiii

LIST OF TABLES
Table 1.1: Comparison the Economic for Different Products of Glycerol

1-3

Table 1.2: Physical Properties of Acrylic Acid

1-5

Table 3.1: Forecasted Global Growth of the Usage of Acrylic Acid up to Year 2011

3-2

Table 3.2: Forecasted Annual Production of Acrylic Acid up to Year 2011

3-2

Table 3.3: Major Manufacturer of Acrylic Acid

3-3

Table 3.4: Price of Acrylic Acid at Asia and USA

3-3

Table 3.5: Petrochemical Plant in Gebeng

3-6

Table 3.6: Estimation of Equipment Cost

3-8

Table 3.7: Estimation of Total Capital Investment

3-9

Table 3.8: Estimation of Total Product Cost

3-10

Table 3.9: Estimation of Payback Period

3-11

Table 4.1: Waste Water Composition

4-1

Table 4.2: Waste Water Discharge Target

4-3

Table 4.3: Gas Emission Target

4-4

Table 5.1: Molar Flow Rate at Stream 5 and its Comparison with HYSIS

5-2

Table 5.2: Molar Flow Rate of Stream 6 at CRV-100 and its Comparison with HYSIS

5-2

Table 5.3: Molar Flow Rate of Stream 10 at V-100 and its Comparison with HYSIS

5-2

Table 5.4: Molar Flow Rate of Stream 20 at V-100 and its Comparison with HYSIS

5-3

Table 5.5: Molar Flow Rate of Stream 11 of and its Comparison with HYSIS

5-3

Table 5.6: Molar Flow Rate of Stream 12 and its Comparison with HYSIS

5-3

Table 5.7: Molar Flow Rate of Stream 17 and its Comparison with HYSIS

5-4

Table 5.8: Molar Flow Rate of Stream 23 and its Comparison with HYSIS

5-4

Table 5.9: Molar Flow Rate of Stream 24 at CRV-101 and its Comparison with HYSIS

5-4

Table 5.10: Molar Flow Rate of Stream 27 and its Comparison with HYSIS

5-5

Table 5.11: Molar Flow Rate of Stream 28 at T-100 and its Comparison with HYSIS

5-5

Table 5.12: Molar Flow Rate of Stream 29 at T-100 and its Comparison with HYSIS

5-5

Table 5.13: Molar Flow Rate of Stream 31 at MIX-100 and its Comparison with HYSIS 5-5
Table 5.14: Molar Flow Rate of Stream 33 at T-101 and its Comparison with HYSIS

5-6

Table 5.15: Molar Flow Rate of Stream 32 at T-101 and its Comparison with HYSIS

5-6

LIST OF TABLES
Table 5.16: Molar Flow Rate of Stream 34 at X-100 and its Comparison with HYSIS

5-6

Table 5.17: Molar Flow Rate of Stream 35 at X-100 and its Comparison with HYSIS

5-6

Table 5.18: Molar Flow Rate of Stream 36 at T-103 and its Comparison with HYSIS

5-7

Table 5.19: Molar Flow Rate of Stream 37 at T-103 and its Comparison with HYSIS

5-7

Table 5.20: Summary of Energy Balance and the Comparison

5-8

Table 6.1: Property of Catalyst

6-2

Table 6.2: Property of Hot Molten Salt (HITEC)

6-4

Table 6.3: Dimension of Packed Bed Reactor

6-4

Table 6.4: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length
to Diameter, L/D at Different Number of Tube per Reactor

6-10

Table 6.5: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length
to Diameter, L/D at Different Inlet Pressure, Po

6-11

Table 6.6: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length
to Diameter, L/D at Different Inlet Temperature, To

6-13

Table 6.7: Results of Packed Bed Reactor Optimization Analysis

6-13

Table 6.8: Length of Reactor, L and Ratio of Length to Diameter, L/D at Different Inlet
Temperature, To

6-16

Table 6.9: Length of Reactor, L and Ratio of Length to Diameter, L/D for Different Shell
Diameter, IDs

6-17

Table 6.10: Results of Packed Bed Reactor Optimization Analysis

6-17

Table 6.11: Variables to Calculate Heat Duty

6-18

Table 6.12: Variables to Tube-side Film Coefficient

6-19

Table 6.13: Variables to Shell-side Film Coefficient

6-19

Table 6.14: Variables to Calculate Fouling Factor

6-20

Table 6.15: Summary of Specification of Reactor 1

6-21

Table 6.16: Variables to Calculate Optimum Diameter in Feed Opening

6-25

Table 6.17: Variables to Calculate Optimum Diameter in Molten Salt Opening

6-26

Table 6.18: Variables to Calculate Total Weight of Shell

6-26

Table 6.19: Variables to Calculate Total Weight of Tube

6-27

LIST OF TABLES
Table 6.20: Variables to Calculate Total Weight of Baffles

6-27

Table 6.21: Variables to Calculate Total Weight of Feed

6-28

Table 6.22: Variables to Calculate Total Weight of Molten Salt

6-28

Table 6.23: Variables to Calculate Total Weight of Insulation

6-29

Table 6.24: Criteria for Design

6-32

Table 6.25: Summary of Mechanical Design of Reactor 1

6-33

Table 6.26: HAZOP Analysis on Packed Bed Reactor 1 Streamline 5

6-39

Table 6.27: HAZOP Analysis on Packed Bed Reactor 1 Streamline 6

6-41

Table 6.28: HAZOP Analysis on Packed Bed Reactor 1 Streamline H_1

6-42

Table 6.29: HAZOP Analysis on Packed Bed Reactor 1 Streamline H_2

6-43

Table 6.30: Description of Instrument

6-45

Table 6.31: Description of Inlet Feed Temperature Control

6-45

Table 6.32: Description of Inlet Feed Flow and Temperature Control

6-46

Table 6.33: Description of Molten Salt Temperature Control

6-46

Table 7.1: Initial Condition of Feed Stream Reactant

7-2

Table 7.2: Properties of Feed Stream and Cooling Stream

7-3

Table 7.3: Properties of Catalyst

7-3

Table 7.4: Kinetic Parameter for Oxidation of Acrolein

7-5

Table 7.5: Determination of Catalyst Weight and Pressure Drop

7-6

Table 7.6: Determination of Reactor Sizes

7-7

Table 7.7: Properties of Pipe

7-7

Table 7.8: Specifications of Baffles

7-9

Table 7.9: Determination of Tube Side Heat Transfer Coefficient

7-10

Table 7.10: Determination of Shell Side Heat Transfer Coefficient

7-10

Table 7.11: Determination of Overall Heat Transfer Coefficient

7-11

Table 7.12: Inner Diameter of Reactor for Various

vsf
vsfm

Ratios

7-15

Table 7.13: Determination of Height of Reactor

7-17

Table 7.14: Comparison between FBR and PBR

7-18

LIST OF TABLES
Table 7.15: Summary of Chemical Engineering Design of Reactor

7-19

Table 7.16: Comparison of the Conversion Value with the HYSYS Simulation

7-20

Table 7.17: Comparison of the Component Molar Flow with the HYSYS Simulation

7-21

Table 7.18: Design Pressure for Tube Side and Shell Side

7-24

Table 7.19: Design Temperature for Tube Side and Shell Side

7-25

Table 7.20: Design Stress for Tube Side and Shell Side

7-25

Table 7.21: Optimum Diameter for Inlet Streams and Outlet Streams

7-34

Table 7.22: HAZOP Analysis on Feed Stream of the Reactor

7-41

Table 7.23: HAZOP Analysis on Outlet Stream of Reactor

7-43

Table 7.24: HAZOP Analysis on Cooling Water Supply of Reactor

7-44

Table 7.25: Control Variables for Packed Bed Reactor

7-50

Table8.1:ComparisonbetweenDifferentTrays

89

Table8.2:SummaryofChemicalDesignParameterfortheQuenchingTower

831

Table8.3:PipingSystem

843

Table8.4:MechanicalDesignParameterforQuenchingTower

847

Table8.5:ControlVariableandParameter

851

Table 9.1: Comparison between Plate Column and Packed Column

9-3

Table 9.2: Comparison between Random Packing and Structured Packing

9-3

Table9.3: Molar Flow Rate of the Inlet Streams and Outlet Streams of Extractive Distillation

Column

9-4

Table 9.4: Operating Condition of the Inlet Streams and Outlet Streams of Extractive Distillation
Column

9-4

Table 9.5: Equilibrium Data for Raffinate Phase

9-5

Table 9.6: Equilibrium Data for Extracted Phase

9-5

Table 9.7: Purify of Product with vary Reflux Ratio

9-6

Table 9.8: Extractive Distillation Column Design Summary

9-10

Table 9.9: Control System for Extractive Distillation Column

9-18

Table 9.10: HAZOP Analysis

9-19

10-2

Table 10.1: Stream Description for Distillation Column T-102

LIST OF TABLES
Table 10.2: Stage Requirement at Different Reflux Ratio

10-6

Table 10.3: Vapor and Liquid Flow Rates

10-10

Table 10.4: Physical Properties

10-11

Table 10.5: Provisional Design

10-15

Table 10.6: Molar Flow Rate of Feed Stream and its Comparison with Hysys

10-21

Table 10.7: Molar flow rate of Top stream and its Comparison with Hysys

10-21

Table 10.8: Molar flow rate of Bottom Stream and its Comparison with Hysys

10-21

Table 10.9: Summary of Chemical Engineering Design

10-34

LIST OF FIGURES
Figure 4.1: Schematic of Water Treatment System

4-2

Figure 4.2: Schematic of Gas Treatment System

4-3

Figure 6.1: Schematic Diagram of Reactor 1

6-1

Figure 6.2: Shell-and-tube Packed-bed Reactor with Co-current Heating

6-3

Figure 6.3: Plot of Conversion and Pressure Ratio Obtained from Matlab

6-8

Figure 6.4: Data of Conversion and Pressure Ratio Obtained from Matlab

6-9

Figure 6.5: Schematic Diagram of Fluidized Bed Reactor

6-14

Figure 6.6: Ellipsoidal Head

6-24

Figure 6.7: Schematic Diagram of Opening

6-25

Figure 6.8: Mechanical Drawing of Reactor 1

6-34

Figure 6.9: Detail A of Mechanical Drawing

6-35

Figure 6.10: Process and Instrumentation Diagram (PID) of Reactor 1

6-47

Figure 7.1: Fluidized Bed Reactor

7-13

Figure 7.2: Ratio of Length and Diameter, L/D vs. Inlet Temperature, To

7-22

Figure 7.3: Ratio of Length and Diameter, L/D vs. Inlet Pressure, Po

7-23

Figure 7.4: Control System for Packed Bed Reactor

7-49

Figure 8.1 Schematic Diagram of Quenching Tower

8-5

Figure 8.2: Absorber Column Efficiency

8-6

Figure8.3: Typical Cross Flow Plate (Sieve)

8-8

Figure 8.4: Column Operation Regimes

8-8

Figure 8.5: Plate Design Algorithm

8-11

Figure 8.6: Flooding Velocity, Sieve Plate

8-13

Figure 8.7: Selection of Liquid Flow Arrangement

8-15

Figure 8.8: Relationship between the Weir Length and Downcomer Area

8-17

Figure 8.9: Weep Point Correlation

8-20

Figure 8.10: Discharge Coefficient, Sieve Plates (Liebson et al., 1957)

8-22

Figure 8.11: Entrainment Correlation for Sieve Plates

8-26

Figure 8.12: Trial Layout of the Plate Design

8-27

Figure 8.13: Relation between Downcomer Area and Weir Length

8-28

LIST OF FIGURES
Figure 8.14: Relation between Hole Area and Pitch

8-30

Figure 8.15: Torispherical Head

8-36

Figure 8.16: Analysis of Stresses

8-39

Figure 8.18: Feedback Control Loop in Quenching Tower

8-53

Figure 8.19: Ratio Control Loop in Absorbed

8-53

Figure 9.1: Flow Diagram for Extractive Distillation Column

9-2

Figure 9.2: Flooding and Pressure Drop in Packed Column

9-6

Figure 9.3: Table Constant for TETP Correlation

9-8

Figure 9.4: Flow Diagram with Controller

9-17

Figure 10.1: Schematic Diagram of Distillation Column T-102

10-2

Figure 10.2: Flow of Vapor and Liquid across Each Plate

10-9

Figure 10.3: Trial Plate Layout

10-18

Figure 10.4: Complete Process Control and Instrumentation Diagram of Distillation Column
10-43

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

CHAPTER 1: INTRODUCTION
1.1 Biodiesel Production
Biodiesel can be produced from vegetable oil, animal oil/fats, tallow and waste oils.
There are three basic routes for biodiesel production from oils and fats.

Base catalyzed transesterification of the oil

Direct acid catalyzed transesterification of the oil

Conversion of the oil to its fatty acids and then to biodiesel.

Almost all biodiesel is produced by base catalyzed transesterification as it is the most

economical process requiring only low temperatures and pressures and producing a 98%
conversion yield.[1] The production of biodiesel by using oil and fats and shown below.

The oil or fats is reacted with alcohol under proper catalyst and condition will produce
biodiesel as main product and glycerol as by product for process. For every 1 tonne of
biodiesel that is manufactured, 100 kg of glycerol are produced. [2] After neutralization
treatment, crude Glycerol with 80-88% purity containing water and catalyst residual can
be obtained. [1]

1.2 Glycerol Produced from Biodiesel Plant

In year 1999 biodiesel glycerol accounted for just 7% of the glycerol market and in year
2004 that figure had grown to 19%. This has lead to oversupply in the market and new
investments in oleochemical as well as biodiesel industries are expected to make the
situation worse in the next couple of years. 450 million gallons of biodiesel were
produced in 2007, which left with 45 million gallons of glycerol. Considering that the
National Biodiesel Board is expecting 60 new plants with a production capacity of 1.2
billion gallons of biodiesel to come online by 2010, over 100 million gallons of glycerol
is expected to be produced annually.[3] Due to the overcapacity of glycerol, the price

1-1

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

decreased drastically over recent years. Hence researches have been made to develop
technologies to utilize the glycerol produced from biodiesel plant.

1.3 Potential Product of Glycerol

By research there are several useful products that can be manufactured by using glycerol.

Acrylic acid via acrolein

Propylene glycol

Hydrogen

Epichlorohydrin

1.3.1 Process Route

1.3.1.1 Acrylic Acid via Acrolein
The production of acrylic acid is by two reaction routes. Glycerol (C3H8O3) is dehydrated
to form acrolein (C3H4O), which acts as an intermediate (refer to Equation 1.1). Then the
acrolein is oxidized to form acrylic acid (C3H4O2). (refer to Equation 1.2).

C3 H 8O3
C3 H 4O + 2 H 2O

(Equation 1.1)

1
C3 H 4O + O2
C3 H 4O2
2

(Equation 1.2)

1.3.1.2 Propylene Glycol

The production of propylene glycol is by dehydration of glycerol (C3H8O3) to produce an

intermediate product, acetol (C3H6O2) (refer to Equation 1.3). Then it is further
hydrogenated to produce propylene glycol (C3H8O2) (refer to Equation 1.4).
C3 H 8O3
C3 H 6O2 + H 2O

(Equation 1.3)

C3 H 6O2 + H 2
C3 H 8O2

(Equation 1.4)

1.3.1.3 Hydrogen

The production of hydrogen from glycerol is by steam reforming (refer to Equation 1.5),
followed by the water-gas shift reaction (refer to Equation 1.6). The overall reaction is
summarized in Equation 1.7.

1-2

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

H 2O
C3 H 8O3
3CO + 4 H 2

(Equation 1.5)

CO + H 2O
CO2 + H 2

(Equation 1.6)

C3 H 8O3 + 3H 2O
3CO2 + 7 H 2

(Equation 1.7)

1.3.1.4 Epichlorohydrin

Dichloropropanol

is

synthesized

from

glycerol

and

hydrochloric

acid.

Dehydrochlorination of the intermediates then produces epichlorohydrin.

1.3.2 Comparison of the Products

Table 1.1: Comparison the economic for different products of glycerol [4, 5, 6, 7, 8, 9, 10, 11]

Acrylic acid

PG

Hydrogen

Epichlorohydrin

Annual Global

3.75 million

1.4 million ton/

675 billions

Demand

ton/ year

year

SCF/year

3.5

4.5

4.0

5.0

1650

1800

510.5

1650

Competition from

Propylene via

Propylene

Industries

Acrolein

Oxide

Methane

Propylene

1000

1410

122

1000

1.3 million ton/year

Forecasted
Average Global
Growth (%)
Price per ton
(USD)

Raw materials
price of competitor
(USD/ton)

From the table above, all the potential products are considered profitable by using
glycerol as raw material without consider the capital cost. However acrylic acid is chosen
to be produced based on the following criteria:

The annual global demand of acrylic acid is the highest.

The forecasted annual global growth is high that is 3.5%.

Price of glycerol is cheaper than the current raw material, propylene.

Storage and handling of acrylic acid is easier compared to hydrogen.

1-3

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

Acrylic acid is less toxic compared to epichlorohydrin.

The usage of acrylic acid is more and the potential market is wide.

1.4 Introduction of Acrylic Acid

1.4.1 Description

Acrylic acid or prop-2-enoic acid is a chemical compound that can be easily polymerized.
Pure acrylic acid is a clear, colorless liquid with a characteristic acrid odor. It is miscible
in water, alcohols, ethers and chloroform. Acrylic acid is used as monomer for acrylate
resins and forms crystalline needle in solid state.

1.4.2 Chemical Identification

Structure formula:

H 2C = CHCOOH

Chemical structure:

H H OH
| | |
C=CC=O
|
H

IUPAC name: Propenoic acid

CAS number: [79-10-7]
RTECS number: AS4375000
Synonyms: Ethylenecarboxylic acid, Propene acid, Propenoic acid, Vinylformic acid

1.4.3 Potential Usage of Acrylic Acid

Acrylic acid is most often been polymerize to form acrylic acid polymer. The most
common product is superabsorbent polymers (SAP) that account for 32% of the global
demand for acrylic acid. SAPs are cross-linked polyarcylates with the ability to absorb
and retain more than 100 times their own weight in liquid. Acrylic acid also can be used
to produce detergent polymer. It can be used with zeolites or phosphates in washing
powder formulation. Besides that acrylic acid is also the raw material for various acrylic
ester productions.

1-4

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

1.4.4 Physical Properties of Acrylic Acid

Important physical properties of acrylic acid are summarized in Table 1.2.

Table 1.2: Physical properties of acrylic acid

Properties

Data

Molecular Weight

72.06 g/mol

Specific Gravity

1.050 (20/4 oC)

Melting Point

13 oC

Boiling Point (101.3 kPa)

141 oC

Flash Point

54 oC (Cleveland open cup)

Critical Temperature

380 oC

Critical Pressure

5.06 Mpa

Viscosity (25 oC)

1.149 mPa.s

Refractive Index (25 oC)

1.4185

Solubility

> 10g/L

Dissociation Constant (25 oC)

5.5 x 10 -5

pKa

4.26

Vapor Density (air =1)

2.5

Vapor Pressure (20 oC)

0.4133 kPa

Auto-ignition Temperature

360 oC

Explosive Limit

2.4 8.0 vol % in air

Heat of Vaporization (101.3 kPa)

45.6 kJ/mol

Heat of Combustion

1376 kJ/mol

Heat of Melting (13 oC)

11.1 kJ/mol

Heat of neutralization

58.2 kJ/mol

Heat of polymerization

77.5 kJ/mol

1-5

KKEK 4281 Design Project

Chapter 1: Introduction

Group 6
Acrylic Acid Project

1.5 References
1. http://www.esru.strath.ac.uk/EandE/Web_sites/02-03/biofuels/what_biodiesel.htm
2. http://en.wikipedia.org/wiki/Biodiesel#Production
3. Frost & Sullivan - What is the Global Market Outlook for Glycerine in 2006, 19th
Oct 2008.
4. http://www.alibaba.com/trade/search?Type=&ssk=y&year=&month=&industry=
&location=&keyword=&SearchText=crude+glycerine&Country=MY&srchLocat
ion=&srchYearMonth=&IndexArea=product_en&CatId=0
5. http://www.dow.com/productsafety/finder/prog.htm
6. http://www.icis.com/v2/chemicals/9076442/propylene-glycol/pricing.html
7. http://www.the-innovation-group.com/ChemProfiles/Propylene%20Glycol.htm
8. http://en.wikipedia.org/wiki/Ethanol#Production
9. http://www.the-innovation-group.com/ChemProfiles/Ethanol.htm
10. http://en.wikipedia.org/wiki/Hydrogen#Applications
11. http://www.the-innovation-group.com/ChemProfiles/Hydrogen.htm

1-6

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Chapter 2: Process Description

Group 6
Acrylic Acid Project

CHAPTER 2: PROCESS DESCRIPTION OF ACRYLIC

ACID PRODUCTION
2.1 Process Principle
The raw material used is crude glycerol obtained from biodiesel plant. The purity of
crude glycerol obtained is 88% purity. [1] The production of acrylic acid from glycerol is
by two process routes. First, crude glycerol (C3H8O3) is dehydrated to acrolein (C3H4O)
via acetol (C3H6O2) as intermediate (refer to Equation 2.1 and Equation 2.2) under
heterogeneous catalytic reaction. The reaction is endothermic.

C3 H 8O3
C3 H 6O2 + H 2O

(Equation 2.1)

C3 H 6O2
C3 H 4O + H 2O

(Equation 2.2)

Acrolein is then oxidized to form acrylic acid in Reactor 2 (refer to Equation 2.3) via
heterogeneous catalytic reaction. The reaction is exothermic. Acetic acid will form as the
major by product for the process refer to Equation 2.4)

1
C3 H 4O + O2
C3 H 4O2
2

3
C3 H 4O + O2
C2 H 4O2 + CO2
2

(Equation 2.3)

(Equation 2.4)

2.2 Unit Operation Description

2.2.1 Reactor 1, CRV-100

In the first reactor, crude glycerol is dehydrated to acrolein via heterogeneous catalytic
endothermic reaction. The catalyst used is aluminasilicates supported silicotungstic acid
which by research gives a higher conversion of glycerol and higher yield of acrolein. The
temperature of the reactor is maintained at 275oC by control the temperature of the inlet
air-steam stream temperature. The pressure of the reactor is set at 1 atm. Under these
conditions, the conversion of glycerol is 98.3% and selectivity of acrolein is 86.2%.[2, 3]
Steam and air are added into Reactor 1 along with glycerol. The mass ratio of steam to
glycerol is 4 to 1 while the proportion of oxygen to the total mass is 0.07. [3] Steam is
added as inert gas to control the rate of the reaction. Air which consists of oxygen and
nitrogen is added to increase the lifetime of the catalyst by reducing coke formation or

2-1

KKEK 4281 Design Project

Chapter 2: Process Description

Group 6
Acrylic Acid Project

any undesired adsorption. [4] The gaseous phase products of this reaction consist of air,
water vapour, acrolein, acetol, and some other minor by product. [3]

2.2.2 Separator, V-100

The separator separated the gaseous product stream from Reactor 1 to liquid stream and
gas stream by an internal cooler. The cooling fluid used is cooling water. The purpose of
the separation is to recycle back the huge quantity of water in the product stream to avoid
wastage. The liquid stream which consists of major proportion of water and acetol will
recycle back to Reactor 1 while gas stream consist of major proportion of acrolein and air
will proceed to Reactor 2 for oxidation reaction.

2.2.3 Reactor 2, CRV-101

In the second reactor, acrolein is oxidized to form acrylic acid via heterogeneous catalytic
exothermic reaction. The catalyst used is Mo10 W2 V3.5 Cu2 Sr

0.8. The

temperature of the

reactor is maintained at 260 C by using molten salt cooling jacket. The pressure of the
reactor is set at 2 bar. The volume percentage of acrolein, oxygen, nitrogen and water
vapour fed to Reactor 2 is 10%, 16%, 64% and 10% respectively. Under these conditions,
the conversion of acrolein is 98% and yield of acrylic acid is 94.1%.[5] Steam is added as
inert gas to control the rate of the reaction. Air is supplied to provide the oxygen required
for the oxidation reaction. The nitrogen consists in air will act as an inert to control the
reaction. The gaseous product stream consists of air, water vapour, acrylic acid and acetic
acid which is a by product of the reaction, air and water vapour.

2.2.4 Quenching Tower, T-100

The product stream from Reactor 2 is fed into quenching tower to separate out the air and
form aqueous solution. Water is fed from the top of the tower and the product stream
from the bottom of the tower. Water will wash the product stream in counter current
flow. Air, water vapour and other minor component exited the tower at the top. Acrylic
acid and acetic acid will dissolve in water and form aqueous solution.

2-2

KKEK 4281 Design Project

Chapter 2: Process Description

Group 6
Acrylic Acid Project

2.2.5 Extractive Distillation Column, T-101

The aqueous acrylic acid and acetic acid solution is entering extractive distillation
column. Due to close volatility between acrylic acid and acetic acid, the mixture cannot
be separated by conventional distillation column. The solvent used for the extraction of
acetic acid is the mixture of cyclohexane and isopropyl acetate. Polymer inhibitor,
diphenylamine with benzoquinone and hydroquinone mono-methyl-ether is also fed to
the column to prevent acrylic acid polymerization.

[6]

The solvent and polymer inhibitor

feed from the top while the mixture feed from bottom. The solvent extracted out acetic
acid from the mixture and exit at the top of the column. The bottom exit stream consists
of acrylic acid with purity 99.7% which is the process final product.

2.2.6 Decanter, X-100

Amount of water will exit along with the extracted stream from extractive distillation
column and form two phase liquid, water phase and solvent phase. The water can be
separated from the two phase liquid by using a decanter and is recycled back to
quenching tower as solvent.

2.2.7 Solvent Recovery Distillation Column, T-102

After the water is separated, the extracted stream entered a distillation column to recover
the solvent. The solvent with lower boiling point will exit as distillate while acetic acid
and other residual with higher boiling point will exit as bottom product. The distillate
solvent has the purity of 99.8% and is recycled back to extractive distillation column. The
bottom stream is treated as residual and sent to waste water treatment plant.

2.3 Process Description

Glycerol feed is preheated by E-100 and E-101 by heat exchanged with the product
stream from Reactor 2, CRV-101 and molten salt from cooling jacket of CRV-101. The
glycerol is then vaporized by using thermal oil in E-102. Steam feed is mix with the
recycle stream and air feed from air compressor. The mixture is preheated by E-103 by
heat exchanged with the product stream of Reactor 1, CRV-100. It is further heated by
E104 by thermal oil to a temperature controlled by the temperature transmitter of CRV-

2-3

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Chapter 2: Process Description

Group 6
Acrylic Acid Project

100 so that CRV-100 temperature always maintain at optimum reaction temperature of

275 oC.

Both gaseous glycerol and steam-air mixture is fed into CRV-100 by feed nozzle. The
feeds undergo catalytic endothermic reaction under 1 atm absolute pressure at CRV-100.
It produced acrolein, acetol and some other minor by-product. The product stream is
compressed to 2.4 bar by a compressor, K-100 and cooled down by E-103 and E-105 by
air-water mixture feed and recycled stream from separator, V-100 respectively.

The cooled acrolein stream is fed to V-100 and separated to liquid stream and gas stream.
Liquid stream consist of higher proportion of water. A small portion of liquid stream is
purged out to waste treatment plant. The remaining liquid streams pressure is reduced by
a pressure relief valve to 1 atm and heated up by Reactor 1 product stream via E-105. It is
then vaporized by E-106 by using molten salt from Reactor 2 cooling jacket. The
vaporized stream is mixed with feed steam and recycled back to CRV-100.

The gas stream from V-100 consists of higher proportion of acrolein. It is fed into
Reactor 2, CRV-101 along with make up air from air compressor and make up steam.
The feeds undergo catalytic exothermic reaction under 2 bar to from gaseous acrylic Acid,
acetic acid and some minor by-product. The reactor temperature is maintained at
optimum reaction temperature, 260 oC by using molten salt cooling jacket. The hot
molten salt is cooled down by heat exchange with glycerol feed and recycled liquid
stream via E-101 and E-106. The acrylic acid product stream is cooled down at E-100 by
heat exchanged with glycerol feed and fed into quenching tower, T-100.

In quenching tower water is fed from top stage and acrylic acid product stream is fed
from bottom. Acrylic acid stream will cool by the water and exit as liquid stream at
bottom while air and some volatile components are discharged as gaseous stream from
the top of the tower. The gas stream will eventually treated at waste treatment plant
before discharged.

2-4

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Chapter 2: Process Description

Group 6
Acrylic Acid Project

The liquid stream consists of acrylic acid, acetic acid and water is fed into extractive
distillation column T-101. The solvent used is a mixture of cyclohexane and isoprpyl
acetate. Polymer inhibitor, diphenylamine with benzoquinone and hydroquinone monomethyl-ether is also added into T-101 to prevent acrylic acid polymerize in the column.
The solvent and polymer inhibitor with higher density is fed from top while the liquid
stream is fed from bottom. Under solvent extraction acetic acid will be extracted by the
solvent and leave at the top of T-101 along with water. Acrylic acid discharged at the
bottom of the column as raffinate is pure acrylic acid with 99.7% purity.

The solvent along with the extracted acetic acid and water is a two phases liquid with
water phase and solvent phase. The mixture is fed into decanter, X-100 with water is
separated and recycled back to quenching tower, T-100.

The solvent and acetic acid is then fed into solvent recovery distillation column, T-102.
The bottom product will become residual of the process and sent to waste treatment plant.
The solvent with 99.8% is recovered and recycle back to extraction distillation column,
T-101.

2-5

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Chapter 2

Group 6
Acrylic Acid Project

2.4 Process Flow Diagram

Figure 2.1: Process Flow Diagram

2-6

KKEK 4281 Design Project

Chapter 2

2.4.1 Flow Description

Stream
Unit
Phase
Pressure

10

L
160

L
140

L
120

G
101.3

G
101.3

G
101.3

G
240

G
220

G
200

L
200

25
135

157.1
135

230
135

300
135

135.00
0.00
0.00
0.00
0.00
0.00

135.00
0.00
0.00
0.00
0.00
0.00

135.00
0.00
0.00
0.00
0.00
0.00

Unit

11

12

13

14

15

atm

L
200

L
140

L
120

G
101.3

G
300

kPa

o
C
Temperature
kmol/hr
Mole Flow
Component kmol/hr
Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein

Stream
Phase
Pressure

Group 6
Acrylic Acid Project

o
C
Temperature
kmol/hr
Mole Flow
Component kmol/hr
Glycerin
Water
Oxygen
Nitrogen
Acetol

303.8
275
407.7
284.3
101.2
66
3932.41 4201.39 4201.39 4201.39 4201.39 2921.16

135.00 137.22
2.33
0.00 2780.90 3049.90
0.00
205.91 205.91
0.00
774.55 774.55
0.00
12.31
13.10
0.00
21.52 155.61

2.33
3049.90
205.91
774.55
13.10
155.61

2.33
3049.90
205.91
774.55
13.10
155.61

2.33
2.33
3049.90 2884.40
205.91
0.02
774.55
0.03
13.10
12.97
155.61 21.44

16

17

18

19

20

G
300

G
140

G
120

G
101.3

G
200

66
66
105
180
146.06 2775.11 2775.11 2775.11

133.6
50.95

25
144.3
295
304.5
66
980.40 3797.41 3797.41 3797.41 1280.23

0.12
2.21
2.21
2.21
144.22 2740.20 2740.20 2740.20
0.00
0.16
0.16
0.16
0.00
0.03
0.03
0.03
0.65
12.31
12.31
12.31

0.00
50.95
0.00
0.00
0.00

0.00
2.22
2.22
2.22
0.00
0.00 2780.90 2780.90 2780.90 165.52
205.89 205.91 205.91 205.91 205.89
774.52 774.55 774.55 774.55 774.52
0.00
12.31
12.31
12.31
0.13

2-7

KKEK 4281 Design Project

Chapter 2
Acrolein
Stream
Phase
Pressure

Group 6
Acrylic Acid Project

Unit

1.07
21

20.37
22

20.37
23

20.37
24

0.00
25

0.00
26

21.52
27

21.52
28

21.52
29

134.17
30

kPa

G
300

G
300

G
200

G
200

G
180

L
101.3

L
101.3

G
101.3

L
101.3

L
101.3

133.6
0.00

25
45.52

65.15
260
170
29
1325.75 1260.00 1260.00 245.90

42.17
69.07
72.88
400.00 1367.05 292.96

51.3
15.49

0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

0.00
9.52
36.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

165.52
215.41
810.52
0.13
134.17
0.00
0.00
0.00
0.00
0.00

400.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.18
15.44

o
C
Temperature
kmol/hr
Mole Flow
Component kmol/hr
Water
Oxygen
Nitrogen
Acetol
Acrolein
Acrylic acid
CO2
Acetic acid
Cyclohexane
I-P-acetate

165.52
144.42
810.52
0.14
2.69
126.25
5.23
5.23
0.00
0.00

165.52
144.42
810.52
0.14
2.69
126.25
5.23
5.23
0.00
0.00

245.90
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

402.94
144.43
810.51
0.00
2.54
0.58
5.23
0.81
0.00
0.00

162.58
0.15
0.01
0.13
0.14
125.67
0.00
4.42
0.00
0.00

2-8

KKEK 4281 Design Project

Chapter 2

Stream
Phase
Pressure

Unit

31

32

33

34

35

36

37

38

39

40

kPa

L
101.3

L
15

L
15

L
15

L
101.3

L
15

L
15

L
15

L
101.3

L
101.3

32
425.51

87.97
124.70

35.68
593.80

53.97
154.50

63.2
154.50

31.87
439.30

45.66
29.28

31.26
410.00

31.34
410.00

240
619.16

0.19
0.32
0.00
0.00
191.25
233.75
0.00

0.15
124.36
0.06
0.13
0.00
0.00
0.00
0.00

162.62
1.32
4.69
0.00
0.14
191.25
233.75
0.00

154.50
0.00
0.00
0.00
0.00
0.00
0.00
0.00

154.50
0.00
0.00
0.00
0.00
0.00
0.00
0.00

8.13
1.32
4.69
0.00
0.14
191.25
233.75
0.00

8.00
1.32
4.38
0.00
0.00
0.17
15.42
0.00

0.14
0.00
0.30
0.00
0.14
191.08
218.33
0.00

0.14
0.00
0.30
0.00
0.14
191.08
218.33
0.00

0.00
0.00
0.00
0.00
0.00
0.00
0.00
619.16

Unit

41

42

43

44

45

46

47

kPa

L
101.3

L
101.3

L
101.3

L
101.3

L
101.3

L
101.3

L
101.3

236.14
619.16

330
558.66

300
558.66

330
65.70

300
65.70

236.14
619.16

200
619.16

619.16
0.00

0.00
558.66

0.00
558.66

0.00
65.70

0.00
65.70

0.00
619.16

0.00
619.16

o
C
Temperature
kmol/hr
Mole Flow
Component kmol/hr
Water
Acrylic acid
Acetic acid
Acetol
Acrolein
Cyclohexane
I-P-acetate
Molten Salt

Stream
Phase
Pressure

Group 6
Acrylic Acid Project

o
C
Temperature
kmol/hr
Mole Flow
Component kmol/hr
Molten Salt
Thermal Oil

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Chapter 2

Group 6
Acrylic Acid Project

2.5 References
1. http://www.esru.strath.ac.uk/EandE/Web_sites/02-03/biofuels/what_biodiesel.htm
2. Hanan Atia, Udo Armbruster, Andreas Martin, Dehydration of glycerol in gas
phase using heteropolyacid catalysts as active compounds, 29 May 2008
3. Eriko Tsukuda, Satoshi Sato, Ryoji Takahashi, Toshiaki Sodesawa, Production of
acrolein from glycerol over silica-supported heteropoly acids, 27 July 2006
4. Jean-Luc Dubois, Millery (FR); Christophe Duquenne, Zickau (DE); Wolfgang
Holderich, Frankenthal (DE), Process For Dehydrating Glycerol To Acrolein, Jul.
8, 2008
5. Won-Ho Lee, Kyung-Hwa Kang; Dong-Hyun Ko; Young-Chang Byun, Method
Of Producing Acrylic Acid Using A Catalyst For Acrolein Oxidation, May 7,
2002
6. Otsuki et al., Polymerization Inhibition of Acrylic Acid, July 4, 1972

2-10

KKEK 4281 Design Project

Chapter 3: Plant Economy and Feasibility Study

Group 6
Acrylic Acid Project

CHAPTER 3: PLANT ECONOMIC AND FEASIBILITY STUDY

3.1

Market Analysis

3.1.1 Global Demand

The current global demand capacity for acrylic acid is about 7.5 billion pound/ year at year 2007
[1]

and global demand for raw acrylic acid is forecast to rise by 3.7% per annum in the coming 5

years (2007-2011). [2] The growth is especially high at Asia and China which shown amount of
8% annual growth.

[3]

This is partly due to demand competition for acrylic acid supply with

acrylic ester producers. Acrylic esters make the main product derived from acrylic acid and
account for 55% of global demand. [2]

About half of the crude acrylic acid is processed to purified (glacial) acrylic acid, which is
further processed both on-site (captive use) and by external downstream users. The other half of
crude acrylic acid is transformed into various acrylate esters at the production sites. Identical to
glacial acrylic acid, these acrylic esters serve as commercial products, which are further
processed both on-site and by external downstream users. Glacial acrylic acid is used in the
manufacture of superabsorbing polymers (SAP), which account for 32% of the global demand
for acrylic acid. Acrylic acid and basic alkyl esters (methyl, ethyl, butyl and 2-ethylhexyl esters)
are used for the manufacture of polymer dispersions, adhesives, super absorbent polymers,
flocculants, detergents, varnishes, fibres and plastics as well as chemical intermediates. [4]

Besides, there are number of factors drive demand for acrylic acid. Typically, acrylic acid trends
align with the economy; as the economy improves, so does demand for acrylic acid. Products
made from acrylic acid have continued at their normal, constant growth rates in spite of
economic slowdowns. There has not been a lot of additional acrylic acid capacity added in the
recent years.

3-1

KKEK 4281 Design Project

Chapter 3: Plant Economy and Feasibility Study
3.1.2

Group 6
Acrylic Acid Project

Local Demand

Malaysia has the demand of acrylic acid in producing polyacrylates and acrylic ester thus the
local market of acrylic acid in different local sectors of industry has good prospect. Currently
there is only one manufacturer of acrylic acid in Malaysia which is BASF Petronas Sdn Bhd
located at Gebeng, Pahang. [5]

3.1.3

Forecasted Future Demand

The demand for Acrylic Acid to produce polyacylates and acrylic ester is increasing steadily.
Table 3.1: Forecasted global growth of the usage of acrylic acid up to year 2011 [6]

3.1.4

Area

Growth (%)

United State

Europe

1.6

Asia (China)

Average Global Growth

3.5

Production of Acrylic Acid

Based on the average global growth of 3.7% and take the basis of year 2007 Acrylic Acid
production, the future production of acrylic acid is forecasted.
Table 3.2: Forecasted annual production of acrylic acid up to year 2011 [6], [9]

Year

Forecasted Demand (billion pound per year)

2007

7.50

2008

7.78

2009

8.07

2010

8.37

2011

8.68

3-2

KKEK 4281 Design Project

Chapter 3: Plant Economy and Feasibility Study
3.1.5

Group 6
Acrylic Acid Project

Major Manufacturer of Acrylic Acid

Table 3.3: Major manufacturer of acrylic acid [6]

Company

Based

Rohm and Haas

USA

BASF

Germany

Dow Chemical

USA

American Acryl

USA

LG Chemical

Korea

3.1.6 Price of Acrylic Acid

The market price of Acrylic Acid at different area
Table 3.4: Price of acrylic acid at Asia and USA [7]

3.2

Area

Price (per Metric Ton)

Asia

USD 1800 1850

USA

USD 1490

Location of Acrylic Acid Plant

Country Malaysia
Through the harnessing of its oil and gas reserves and the forging of smart partnerships with
some of the worlds largest petroleum companies, Malaysia has established the ideal
infrastructure to support a vibrant petrochemical industry.
(i) Criteria of Chosen: [11]

Strategic location in the heart of South-East Asia.

Gateway to ASEAN and AFTA.

(AFTA is a free trade zone in Southeast Asia where member countries include
Malaysia, Singapore, Thailand, Philippines, Indonesia, Vietnam, Laos, Myanmar,
Cambodia and Brunei. The AFTA agreement supports the effort to relax trade
barriers amongst member countries in order to achieve direct trade benefits)

Rich reserves of natural gas.

3-3

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Chapter 3: Plant Economy and Feasibility Study

Group 6
Acrylic Acid Project

Political and Economic stability.

Developed infrastructure.

Governments commitment

Quantity of life.

World-class facilities.

Integrated infrastructure.

Availability of capable workforce and skilled technical manpower.

The fast development of China had become a net importer of petrochemical

products; her entry into World Trade Organization will also open up new business
opportunities for petrochemical manufacturers in Malaysia.

(ii) The GDP of Malaysia as shown as following: [12]

Year

Growth Rate %

2003

4.2

2004

5.2

2005

7.1

2006

5.2

2007

5.9

2008

5.7

(iii) Petrochemical industry in Malaysia

The petrochemical industry is an important sector in Malaysia with investments totaling RM6.9
billion as at the end of 2007. [13] Malaysia is an exporter of major petrochemicals products such
as ethylene oxides, glycols, oxo-alcohols, styrene monomers and so on.
Petrochemical zones in Malaysia: [14]

Kertih, Terengganu

Gebeng, Pahang

Pasir Gudang port

Tanjung Langsat port

3-4

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Chapter 3: Plant Economy and Feasibility Study

Group 6
Acrylic Acid Project

Bintulu, Sarawak

(iv) Export of Acrylic Acid Product

With the full implementation of AFTA, petrochemical manufacturers in Malaysia will benefit
from a single market. Manufacturers based in Malaysia will also benefit from the access to a
much larger Asia Pacific market. With China being a net importer of petrochemicals, Malaysia's
'early harvest' Free Trade Agreement with China will open up new business opportunities for
petrochemicals manufacturers in Malaysia. [14]

3.2.2

Plant location

Location: Gebeng, Pahang

The development of petrochemicals zones where petrochemical plants are clustered together has
created a value chain which ensures the progressive development of petrochemicals activities.
Gebeng is another petrochemical hub for multinational players like BASF, Amoco, Kaneka,
Eastman and Polyplastics.

[11]

The petrochemical zone provides an integrated environment that

meets specific needs of the petrochemical industry.

(i) Factors: [11]

Availability of land.

Strategic location for import of raw material and export of products.

Logistics gateway for the East Coast Economic Region (ECER) to the Asean and the
Asia-Pacific regions

Eastern Corridor Incentives

Penisular Gas Utilisation (PGU) project which trans-peninsular gas transmission pipeline
channels sales gas to industries around the country.

Centralised Utility Facilities (CUF) which provides sufficient supply of utilities such as
power, industrial gases, water and steam.

Kuantan Port
9 Centralised tankage facilities.
9 Pipeline and piperack system connecting Gebeng to Kuantan Port.
9 Container and bulk liquid port.

3-5

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Chapter 3: Plant Economy and Feasibility Study

Group 6
Acrylic Acid Project

9 Railway linking Kerteh, Gebeng and Kuantan Port.

East Coast Highway.

Environment Technology Part which incorporating a training centre, a waste collection

and processing centre as well as raw material management and storage facilities,
maintenance and servicing facilities.

(ii) Petrochemical Plant in Gebeng

Table 3.5: Petrochemical plant in Gebeng [11]

Petrochemical Plants

Products
Acrylic Acid and Esters, Syngas, Butyl
Acrylate, Oxo-alcohols, Phthalic Anhydride

BASF Petronas Chemical (M) Sdn Bhd

and Plasticizers,
Butanediol, Tetrahydrofurane and
Gamma-butyrolactone

Eastman Chemicals (M) Sdn Bhd

Polyester Copolymers

Amoco Chemicals (M) Sdn Bhd

Purified Terephthalic Acid

Kaneka Paste Polymers Sdn Bhd

Dispersion Polyvinyl Chloride

Kaneka Malaysia Sdn Bhd

Methyl Methacrylates Copolymers

Polypropylene (M) Sdn Bhd

Polypropylene

3.3

Government Policy-Taxation [16]

3.3.1

Company Tax

A company, whether resident or not, is assessable on income accrued in or derived from

Malaysia. Income derived from sources outside Malaysia and remitted by a resident company is
exempted from tax, except in the case of the banking and insurance business, and sea and air
transport undertakings. A company is considered a resident in Malaysia if the control and
management of its affairs are exercised in Malaysia. Effective from the year assessment of 2007,
the company income tax rate be reduced to 27%, including for SMEs.

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3.3.2

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Acrylic Acid Project

Real Property Gain Tax

Capital gains are generally not subject to tax in Malaysia. Real property gains tax is charged on
gains arising from the disposal of real property situated in Malaysia or of interest, options or
other rights in or over such land as well as the disposal of shares in real property companies. The
tax rates for Malaysian citizens and permanent residents are as follows:
Disposal within 2 years 30%
Disposal in the 3rd year 20%
Disposal in the 4th year 15%
Disposal in the 5th year 5%
Disposal in the 6th year and thereafter - Company 5%
- Individual nil

Citizens and permanent residents also enjoy an exemption of RM5, 000 or 10% of the gains
whichever is the greater, besides a one-time tax exemption on the gains arising from the disposal
of one private residence. For non-citizens and non-permanent resident individuals, gains from the
disposal of real property within five years are taxed at a flat rate of 30%, after which the tax rate
will be 5%.

3.3.3

Sales Tax

Sales tax is generally at 10%. However, raw materials and machinery for use in the manufacture
of taxable goods are eligible for exemption from the tax, while inputs for selected non-taxable
products are also exempted.

3.3.4 Import Tax

Malaysia is committed to the ASEAN Common Effective Preferential Tariffs (CEPT) scheme
under which all industrial goods traded within ASEAN are imposed import duties of 0% to 5%.

3.4

Economic Evaluation

The main purpose of this study is to calculate the profit which could be generated if the product
is selling at the current market value. With the profit, we can determine the period where the
generated income can be compensate with the investment made throughout the project.

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The cost measurement can be divided into few elements:

I. Total Capital Investment
II. Total Product Cost
III. Profitability Analysis

3.4.1

Purchased Equipment
Table 3.6: Estimation of equipment cost [17], [18]

No.

Equipment Type

Quantity

Unit Price

Total

Storage Tank 1

71521

357605

Storage Tank 2

77629

388145

Storage Tank 3

70781

353905

Distillation Column

408697

817394

Quenching Tower

123301

123301

Reactor 1

473200

473200

Reactor 2

139700

139700

E-101 & E-100

13346

26692

E-104

63000

63000

10

E105

50600

50600

11

E-103

81400

81400

12

Separator

27800

27800

13

Compressor

1900000

1900000

14

Pump

30

4500

135000

15

Cooling Tower

11

520100

5721100

16

Treatment Cost

2500000

1769500

17

Reboiler

947000

2841000

Total (USD)

15269342

Total (MYR)

50388828.6

Total Capital Cost (After Index Factor)

57415993.1

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3.4.2

Group 6
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Total Capital Investment

Total capital investment can be defined as the sum of the fixed-capital investment and the
working capital. Total capital investment is evaluated by using fraction of delivered equipment
method.
Table 3.7: Estimation of Total Capital Investment [19]

Fraction of
Delivered

Cost (MYR)

Equipment
Direct Cost
Cost of Purchased Equipment, E'

60895750.00

Delivery, 10% E'

6089575.00

Subtotal: Delivery Equipment

66985325.00

Purchased Equipment Installation

0.47

31483102.75

Instrumentation & Controls (Installation)

0.36

24114717.00

Piping (Installed)

0.66

44210314.5

Electrical System (Installed)

0.11

7368385.75

Building (Including Services)

0.18

12057358.5

Yard Improvements

0.1

6698532.5

Service Facilities (Installed)

0.7

46889727.5

Land

0.06

4019119.5
176841258

Total Direct Cost, A

Indirect Cost
Engineering and Supervision

0.33

22105157.25

Construction Expenses

0.41

27463983.25

Legal Expenses

0.04

2679413

Contractor's Fees

0.22

14736771.5

Contingency

0.44

29473543

Total Indirect Cost, B

96458868

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273300126

Fixed Capital Investment (FCI) = A+B

3.4.3

Working Capital (15% of FCI), C

40995018.90

Total Capital Investment (TCI) = A+B+C

314295144.9

Total Product Cost

Product: Acrylic Acid

Targeted Operating Time, day/ year: 330 day/ year
Targeted Capacity, tonne/ day: 215.448 tonne/ day
Table 3.8: Estimation of Total Product Cost [19]

Suggested Factor

Calculated Value

Manufacturing Cost
A. Direct Production Cost
Raw Material (Glycerol)

74652732.00

Catalyst

526694.00

Utilities

30585365.00

Opearating Labor

0.10 of TPC

26514140.00

Laboratory Charges

0.10 of OL

2651414.00

Operating Supervision

0.10 of OL

2651414.00

Maintenance and Repairs

0.05 of FCI

13665006.30

Operating Suppliers

0.10 of FCI

27330012.60

Insurance

0.01 of FCI

2733001.26

Local Taxes

0.02 of FCI

5466002.52

Financing

0.03 of TCI

9428854.35

C. Plant Overhead Cost

0.10 of TPC

26514140.00

B. Fixed Charges

General Expenses

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Administrative Costs

0.03 of TPC

7954242.00

Distribution and Marketing Costs

0.08 of TPC

21211312.00

Research and Development Costs

0.05 of TPC

13257070.00

Total Product Cost

265141400.04

Revenue

410590026.00

Gross Profit (Before Tax)

145448625.96

Tax

0.28

Net Profit After Tax

104723010.69

Depreciation

0.05 of FCI

13665006.30
91058004.39

Annual Income (Including Depreciation)

3.4.4

40725615.27

Profitable Analysis

(i) Simple Payback Period

Payback period is defined as the minimum length of time for the total return to equal the capital
investment.
Payback Period =

(ii) Compounded Payback Period

Table 3.9: Estimation of payback period [19]

End

Cumulative PW

Present worth

Cumulative PW

at i=0%/year

of cash flow at

at MARR =

through year k

i=10%/year

10%/year

-314295144.9

-314295144.9

-314295144.9

-314295144.9

0.9091

91058004.39

-223237140.5

82780831.79

-231514313.1

0.8264

91058004.39

-132179136.1

75250334.83

-156263978.3

0.7513

91058004.39

-41121131.73

68411878.7

-87852099.58

0.683

91058004.39

49936872.66

62192617

-25659482.58

0.6209

91058004.39

140994877.1

56537914.93

30878432.34

Present Worth

Net cash

Factor (P/F)

flow

-314295144.9

of
year

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0.5645

91058004.39

232052881.4

51402243.48

82280675.82

0.5132

91058004.39

323110885.8

46730967.85

129011643.7

0.4665

91058004.39

414168890.2

42478559.05

171490202.7

0.4241

91058004.39

505226894.6

38617699.66

210107902.4

By using the compounded payback period,

Payback Period =

(iii) Rate of Return

Rate of Return = (Net Profit/ Total Investment) x 100
Rate of Return = 28.97%

(iv) Internal Rate of Return (IRR)

Internal Rate of Return = 28.28%

3.5 Conclusion
Since the Internal Rate of Return (IRR) is greater than the Minimum Attractive Rate of Return
(MARR), the plant is worth to invest. Furthermore the payback period is around 4-5 years
according to the calculation. Hence from the economic evaluation, it can be concluded that our
project is economical feasible and relatively good future.

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3.5 References
1. http://www.freedoniagroup.com/Acrylic-Acid-And-Derivatives.html
2. http://mcgroup.co.uk/researches/A/03/Acrylic%20Acid%20Market%20Research.html
3. http://www.icis.com/v2/chemicals/9074869/acrylic-acid/pricing.html
4. http://mcgroup.co.uk/researches/A/03/Acrylic%20Acid%20Market%20Research.html
5. http://www.chemicals-technology.com/projects/gebeng/
6. http://www.icis.com/v2/chemicals/9074870/acrylic-acid/uses.html
7. http://www.icispricing.com/il_shared/Samples/SubPage219.asp
8. http://www.chemicals-technology.com/projects/gebeng/
9. http://www.icis.com/v2/chemicals/9074870/acrylic-acid/uses.html
10. http://www.icispricing.com/il_shared/Samples/SubPage219.asp
11. http://www.mida.gov.my/beta/pdf/MIDA%20Petrochemical%202007.pdf
12. http://www.indexmundi.com/malaysia/gdp_real_growth_rate.html
13. http://www.aseansources.com/jsp/malaysia_petrochemical_polymer.jsp
14. http://www.mida.gov.my/en/view.php?cat=5&scat=9&pg=641
15. http://www.ktak.gov.my/template01.asp?contentid=306
16. http://e-directory.com.my/doc/taxation.htm
17. http://www.mhhe.com/engcs/chemical/peters/data/ce.html
18. www.matche.com
19. Peter, M. S., Timmerhaus, K. D.; Plant Design and Economics for Chemical Engineers,
5th Edition, McGraw-Hill Inc: New York, 2003.

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Chapter 4: Safety, Health and Environment

Group 6
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CHAPTER 4: ENVIRONMENT, SAFETY AND HEALTH

4.1 Environment
4.1.1

Law and Regulation

In Malaysia, the environmental matter is handled by the Department of Environment

(DOE), a department constituted under the Ministry of Science, Technology and
Environment. The pollution control and strategy or remedial approach is implemented
through the enforcement of the Environmental Quality Act, 1974. This act provides for
the prevention, abatement, and control of pollution through licensing, and mandates the
conducting of an Environmental Assessment Report.

The enforcement of this act and the accompanying 16 sets of Regulations and Orders
have played a significant role in the management of the environment, and in particular,
with respect to pollution control. Examples of the regulations have to be concern under
Environment Quality Act, 1974 are:

Environment Quality (Clean Air): Regulation 1978

Environmental Quality (Sewage and Industrial Effluents): Regulations 1979

Environmental Quality (Schedule wastes): Regulation 1989

4.1.2 Waste Water Treatment

The waste water stream from production mainly contaminate by following contaminants.
Table 4.1: Waste water composition

Mass flow

Mole flow

Concentration

Waste water

(kg/hr)

(kgmole /hr)

(ppm)

Glycerol

10.741

0.11663

3952.228846

Water

2599.2

144.28

Acetol

48.042

0.64853

17677.40231

Acrolein

59.724

1.0653

21975.87893

Total

2717.707

146.11046

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1,2-Ethanedithiol
Waste Water

meta-xylylenediamine

Flocculants

Flocculant tank
Reactor

Reactor

Clarifier

Filter press

Sludge

halophilic
bacteria

NaCl, Mg2+, K+,

NH4+, PO43-

Discharge

Carbon Filter

Biological treatment system

Membrane Bioreactor

Figure 4.1: Schematic of water treatment system

The flow rate of water is estimated 2717.7liter per hour. The waste water stream is stored
in a stabilizer tank. The waste water stream is treated by chemical precipitation method as
primary treatment and biological treatment as secondary treatment.

In primary treatment, the waste water stream is dosing with 1,2-Ethanedithiol and metaxylylenediamine in a reactor to remove acrolein and acetol. Dosing 1,2-Ethanedithiol at a
pH of between 3.0 and 7.0 to form an acrolein derivative in a process stream to remove
acrolein.[1] The polyamine interacts with or binds the carbonyl bearing impurities
including acetol. Dosing meta-xylylenediamine can reduce the concentration of acetol. [2]

After the chemical precipitation process, the waste water then is dosing with flocculants
for flocculation before flow into the clarifier. The bottom outlet is then pumped through

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the filter press for dewatering process. Sludge generated is sent for disposal and the
effluence water is pump to biological treatment system.

The biological treatment system used is membrane bioreactor. By adding halophilic

bacteria into the solution and addition of ions NaCl, Mg2+, K+, NH4+, PO43- to enhance
growth can remove the glycerol inside the waste water.

The treated water is filter by carbon filter to remove the remaining organic matter and
reduce the COD before discharge out. The discharge waste water have following target.
Table 4.2: Waste water discharge target

Concentration

After chemical

After biological

Waste stream

(ppm)

precipitation (ppm)

treatment

Glycerol

3952.228846

3952.228846

Acetol

17677.40231

Acrolein

21975.87893

The sludge / precipitate are then destroyed by controlled burning in an incinerator.

4.1.3 Gas Emmision and Treatment

Purge

Discharge

Scrubber System

Carbon Filter
Figure 4.2: Schematic of gas treatment system

The gas emission from the plant mainly containing acrylic acid, acetic acid, acrolein and
carbon dioxide.

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Acrylic acid and acetic acid in gas phase can be neutralized by wet scrubber with caustic
solution as scrubbing fluid.

[3]

Emissions of acrolein and other odorous components in

vents can be controlled with water scrubbers. [4]

Hence the purge gas is flow through scrubber system to remove the acrylic acid, acetic
acid and acrolein. The concentration of carbon dioxide discharge is 0.6% which is
insignificant which do not need addition treatment. Before the gas discharge to
environment, the gas is flow through the carbon filter to filter out the remaining organic
compounds. Removal of air pollutants by adsorption onto granules of activated carbon is
an extremely effective technology for volatile organic compounds (VOCs) and other
organic pollutants. [3]

The target of the gas treatment plant can simply in following table:
Table 4.3: Gas emission target

Concentration

After Scubber

After Carbon

Waste stream

(ppm)

(ppm)

Filter(ppm)

Acrylic Acid

1022.686871

10

Acetic Acid

1282.029479

10

Acrolein

4059.200779

0.1

0.05

The water used for absorb the acrolein is sent to waste water treatment plant before
discharge out. The granular activated carbon can be regenerated by controlled burning in
the incinerator too. [5]

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4.2 Health
4.2.1 Effect to Human
4.2.1.1 Acetic Acid
4.2.1.1.1 Health Hazard
Glacial acetic acid is a highly corrosive liquid. Contact with the eyes can produce mild to
moderate irritation in humans. Contact with the skin may produce burns. Ingestion of this
acid may cause corrosion of the mouth and gastrointestinal tract. Death may occur from a
high dose (2030 mL), and toxic effects in humans may be felt from ingestion of 0.10.2
mL. An oral LD50 value in rats is 3530 mg/kg. Glacial acetic acid is toxic to humans and
animals by inhalation and skin contact. In humans, exposure to 1000 ppm for a few
minutes may cause eye and respiratory tract irritation. Rabbits died from 4-hour exposure
to a concentration of 16,000 ppm in air.

4.2.1.1.2 Exposure Limits

TLV-TWA 10 ppm (25 mg/m3) (ACGIH, OSHA, and MSHA); TLV-STEL 15 ppm (37.5
mg/m3) (ACGIH).

4.2.1.2 Acetol
4.2.1.2.1 Health Hazard
Acetol is flammable liquid and vapor. It may cause eye and skin irritation. Ingestion of
acetol may cause irritation of the digestive tract. Inhalation may cause respiratory tract
irritation. Vapors may cause dizziness or suffocation. An oral LD50 value in rats is 2200
mg/kg.

4.2.1.2.2 Exposure Limits

Not listed in ACGIH, OSHA and NIOSH.

4.2.1.3 Acrolein
4.2.1.3.1 Health Hazard
Acrolein is one of the EPA Classified Acute Hazardous Waste. It is a highly toxic
compound that can severely damage the eyes and respiratory system and burn the skin.

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Ingestion can cause acute gastrointestinal pain with pulmonary congestion. An oral LD50
value in mice is 40 mg/kg.

Inhalation can result in severe irritation of the eyes and nose. A concentration of 0.5 ppm
for 12 minutes can cause intolerable eye irritation in humans. In rats, exposure to a
concentration of 16 ppm acrolein in air for 4 hours was lethal. Acrolein can be absorbed
through the skin. The spillage of liquid can cause severe chemical burns. Skin contact
may lead to chronic respiratory disease and produce delayed pulmonary edema. In a
study on inhalation toxicity in rats, the exposure to 1 atm of acrolein vapors caused
physical incapacitation. The animals lost the ability to walk and expired.

4.2.1.3.2 Exposure Limits

TLV-TWA 0.25 mg/m3 (0.1 ppm) (ACGIH and OSHA); STEL 0.8 mg/m3 (0.3 ppm);
IDLH 5 ppm (NIOSH).

4.2.1.4 Acrylic Acid

4.2.1.4.1 Health Hazard
Acrylic acid is a corrosive liquid that can cause skin burns. Spill into the eyes can
damage vision. The vapors are an irritant to the eyes. The inhalation hazard is of low
order. An exposure to 4000 ppm for 4 hours was lethal to rats. The dermal LD50 value in
rabbits is 280 mg/kg.

4.2.1.4.2 Exposure Limits

TLV-TWA 10 ppm (30 mg/m3) (ACGIH).

4.2.1.5 Carbon Dioxide

4.2.1.5.1 Health Hazard
Carbon dioxide is an asphyxiant. Exposure to about 910% concentration can cause
unconsciousness in 5 minutes. Inhalation of 3% CO2 can produce weak narcotic effects.
Exposure to 2% concentration for several hours can produce headache, increased blood
pressure, and deep respiration.

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4.2.1.5.2 Exposure Limits

TLV-TWA 5000 ppm (9000 mg/m3) (ACGIH, MSHA, and OSHA); STEL 30,000 ppm
(ACGIH).

4.1.1.6 Glycerol
4.2.1.6.1 Health Hazard
Glycerol is a clear, colorless solution with a faint to slight odor. It may cause eye and
skin irritation. Ingestion of large amounts may cause gastrointestinal irritation. It is low
hazard for usual industrial handling. Inhalation of a mist of this material may cause
respiratory tract irritation.

4.2.1.6.2 Exposure Limits

TLV-TWA: 10 mg/m3 (ACGIH), 15mg/m3 (OSHA), TLV-STEL: 20mg/m3

4.2.2 Effect to Environment

4.2.2.1 Acetic Acid
Environmental effects depend on the concentration and duration of exposure to acetic
acid. In high concentrations it can be harmful to plants, animals and aquatic life. Acetic
acid degrades rapidly to harmless substances in the environment.

4.2.2.2 Acrolein
In view of the high toxicity of acrolein for aquatic organisms, it presents a risk to aquatic
life at, or near, sites of industrial discharges or spills, and during biocidal use.
Contamination of soil, water, and the atmosphere can be avoided by the use of proper
methods of storage, transport, and waste disposal.

4.2.2.3 Acrylic Acid

Acrylic acid emitted into the atmosphere will react with photochemically produced
hydroxyl radicals and ozone, resulting in rapid degradation. There is no potential for
long-range atmospheric transport of acrylic acid because it has an atmospheric lifetime of
less than one month. When released into water, acrylic acid readily biodegrades. The fate

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of acrylic acid in water depends on chemical and microbial degradation. When added to
water acrylic acid is rapidly oxidized, and so it can potentially deplete oxygen if
discharged in large quantities into a body of water. Acrylic acid has been shown to be
degraded under both aerobic and anaerobic conditions. The toxicity of acrylic acid to
bacteria and soil microorganisms is low.

4.2.2.4 Glycerol
Acute toxicity of glycerol to fish, daphnia, algae and microorganisms has been test. The
studies show that glycerol is of low acute toxicity to fish and aquatic invertebrates.
LC/EC50 values are all in excess of 5000 mg/L.

4.3 Safety
4.3.1 Hazard Introduction
The term hazardous properties may be broadly classified into two principal categories:
namely toxicity, and flammability and explosivity.

The term toxicity refers to substances that produce poisoning or adverse health effects
upon acute or chronic exposure. It includes mutagenicity and carcinogenic potential,
teratogenicity and corrosivity or irritant actions.

Animal data on the median lethal dose (LD50) by various routes of administration is good
indicator of the degree of toxicity of a substance. Substances that exhibit acute oral LD50
values of <100 mg/kg in rats or mice are termed highly toxic compounds. Those that have
LD50 values of 100500 mg/kg and >500 mg/kg are termed moderate and low toxicants,
respectively.

The flammable properties of substances in air include their flash point, vapor pressure,
autoignition temperatures, and flammability range. Liquids that have a flash point of
<100F (37.8C) are termed flammable, whereas liquids that have a flash point of 100
200F (37.893.3C) are termed combustible. A violent reaction that produces flame can
cause an explosion under more severe conditions.

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Hazardous substances can be disposed of in an approved landfill disposal site, although

such disposal of highly toxic compounds can lead to groundwater contamination.
Incineration in a chemical incinerator equipped with an afterburner and scrubber is a
widely used practice for the destruction of toxic wastes. Biodegradation of toxic
compounds to nontoxic products in soils, waters, treatment plants, and bioreactors has
become treatment for toxic waste in recent years. Other processes that are used include
treatment with molten metals, wet oxidation, ultraviolet (UV) light-catalyzed oxidation
using hydrogen peroxide or ozone, and dechlorination or desulfurization.

4.3.2 Handling and Storage of Hazardous Chemical

4.3.2.1 Acetic acid
Acetic acid is a combustible liquid and the vapor of acetic acid forms explosive mixtures
with air. Acetic acid may react explosively with the fluorides of chlorine and bromine.
When it reacts with metals, it will produce flammable hydrogen gas. The dilute acetic
acid and dilute hydrogen also can undergo an exothermic reaction if heated, forming
peracetic acid which is explosive at 110 C. So it needed to be stored in a segregated and
approved area and keep container in a cool, well-ventilated area.

Splash goggles, synthetic apron and vapor respirator is used as personal protective
equipment when handling acetic acid since it is irritant and corrosive chemical.

4.3.2.2 Acetol
Acetol is flammable liquid and incompatible with strong oxidizing agents. Safety glasses
and adequate ventilation is used when handling the acetol. The storage area should keep
away from any source of ignition. It also should protect from moisture or called as
hygroscopic.

4.3.2.3 Acrolein
Acrolein is highly flammable in presence of open flames and sparks, of heat. The vapors
of acrolein may form explosive mixtures with air. When heated to decomposition it emits
toxic fumes of carbon monoxide, peroxides. Hence it needed to be stored in a segregated

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and approved area and keep container in a cool, well-ventilated area and do not store
above 8C (46.4F).

Since acrolein is highly toxic, irritant and corrosive, eyewash stations and safety showers
are ensure proximal to the work-station location. Personal protection such as vapor
respirator, face shield, gloves and boots is put on when handling the chemical.

4.3.2.4 Acrylic Acid

Acrylic acid is a flammable liquid. Its extremely flammable in presence of open flames
and sparks. The storage tank of acrylic acid should keep dry and the area keep locked up
and dry. It should always keep away from all possible sources of ignition (spark or flame).
The container should tightly close and sealed until ready for use. Hand gloves and vapor
respirator is used when handling the chemical.

4.3.2.5 Glycerol
Glycerol is slightly flammable to flammable in presence of open flames and sparks, of
heat, of oxidizing materials. It is incompatible with strong oxidizers such as chromium
trioxide, potassium chlorate, or potassium permanganate and may explode on contact
with these compounds. Glycerol and chlorine may explode if heated and confined.

The container should keep container tightly closed and at cool, well-ventilated area.
Safety glasses, lab coat, vapor respirator and hand gloves should be used when handling
glycerol.

4.3.2.6 Isopropyl Acetate

Isopropyl acetate is flammable liquid. It slightly flammable to flammable and explosive
to explosive in presence of oxidizing materials, of acids, of alkalis. It should keep away
from heat and ground all equipment containing material.
Since it is flammable materials and should be stored in a separate safety storage cabinet
or room. The container should keep away from sources of ignition and tightly closed. A
refrigerated room would be preferable for materials with a flash point lower than 37.8C

4-10

KKEK 4281 Design Project

Chapter 4: Safety, Health and Environment

Group 6
Acrylic Acid Project

(100F). Splash goggles, lab coat and vapor respirator is used when handling the
chemical.

4.3.2.7 Thermal Oil

When handling the thermal oil, avoid contact with eyes, skin and clothing. The container
should always closed and avoid breathing vapour or mist. It use with adequate ventilation
and wash thoroughly after handling. The heat transfer fluids are intended for indirect
heating purposes only.

4.4 References
1. Gregory J. Ward, Process For Removal of Acrolein from Acrylonitrile Product
Streams, 2003.
2. Zafarullah K. Cheema, Purification of Phenol, 1969.
3. Frank Woodard, Industrial Waste Treatment Handbook, 2001.
4. Van Nostrand Reinhold, Air and Waste Management Association, 1992.
5. Pradyot Patnaik, A Comprehensive Guide To The Hazardous Properties Of
Chemical Substances, 2007.

4-11

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance

Group 6
Acrylic Acid Project

CHAPTER 5: MASS AND ENERGY BALANCE

5.1

Introduction

The objective of this project is to design a plant with production of 70,000 tonnes/year of acrylic
acid from the dehydration of glycerol. In this chapter, mass and energy balance hand calculation
was done based on the HYSIS simulation input values to calculate the output results in each unit
operation. After that, the output results of HYSIS were compared with hand calculation and
hence calculate the deviation between them.

5.2

Comparison between Manual Calculations and HYSIS Result

5.2.1

Approach of Manual Calculation

The manual calculation for this plant was calculated by making several assumptions for the
purpose to simplify the equation. Since there is lack of literature values of date such as
equilibrium constant, some of the thermodynamics data were obtained from HYSIS whenever it
was necessary. In order to simplify the whole manual calculation, the input values of every unit
operations are taken from the HYSIS results which the recycle streams were already considered.
Assumption such as ideal mixing, and constant heat capacity with a wide range of pressure were
made for the energy calculation.

5.2.2

Approach to HYSIS Simulation

Simulation was carried out using HYSIS 3.2 software. The package was used: NRTL for the
acrylic acid production. Below are the tables that presented the mass and energy balance of each
stream and its deviations with the HYSIS.

5.3

Mass Balance Results

5.3.1

Feed rate calculation

Acrylic Acid Rate Desire

= 70000ton/ year = 107.38kmol/h

Given:

Conversion rate for the reactor 2 is 98%, Yield is 94.1%

107.38
So, the acrolein fed to Reactor 2 =
x 100 = 114.12kmol / h
94.1

Given:

Conversion rate for the reactor 1 is 98.3%, Selectivity is 86.2%

5-1

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance
So, the glycerol fed to Reactor 1 =

Group 6
Acrylic Acid Project
114.12
x 100 = 134.68kmol / h
( 98.3x86.2 )

Given: In order to achieve high conversion and selectivity, we need to feed in water and oxygen
together with the crude glycerol. From the sources that we found, the weight ratio of crude
glycerol to water is 20:80. On the other hand, the oxygen needed for the mixture of glycerol and
water is 0.07%.
5.3.2

Mixture of Stream 4 and 16

Table 5.1: Molar flow rate at stream 5 and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total

Stream 5
HYSIS

Hand Calculation

% Deviation

137.22
2780.90
205.91
774.55
12.31
21.52
3932.41

137.22
2780.90
205.91
774.55
12.31
21.52
3932.41

0.0
0.0
0.0
0.0
0.0
0.0
0.0

5.3.3 CRV-100
Table 5.2: Molar flow rate of stream 6 at CRV-100 and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total
5.3.4

Stream 6
HYSIS

Hand Calculation

% Deviation

2.33
3049.90
205.91
774.55
13.10
155.61
4201.39

2.33
3049.87
205.91
774.55
13.10
155.61
4201.37

0.0
0.0
0.0
0.0
0.0
0.0
0.0

V-100
Table 5.3: Molar flow rate of stream 10 at V-100 and its comparison with HYSIS

Component

Glycerin
Water

Stream 10
HYSIS

Hand Calculation

% Deviation

2.33
2884.40

2.33
2904.95

0.0
1.9
5-2

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance
Oxygen
Nitrogen
Acetol
Acrolein
Total

0.02
0.03
12.97
21.44
2921.16

Group 6
Acrylic Acid Project
0.16
0.03
12.98
120.63
3041.07

87.5
0.0
0.1
82.2
3.9

Table 5.4: Molar flow rate of stream 20 at V-100 and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total
5.3.5

Stream 20
HYSIS

Hand Calculation

% Deviation

0.00
165.52
205.89
774.52
0.13
134.17
1280.23

0.00
144.95
205.04
774.52
0.12
34.98
1159.60

0.0
14.2
0.4
0.0
8.3
283.6
10.4

Purge Stream from Stream 10

Table 5.5: Molar flow rate of stream 11 of and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total

Stream 11
HYSIS

Hand Calculation

% Deviation

0.12
144.22
0.00
0.00
0.65
1.07
146.06

0.12
144.22
0.01
0.00
0.65
1.07
146.06

0.0
0.0
100
0.0
0.0
0.0
0.0

Table 5.6: Molar flow rate of stream 12 and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total

Stream 12
HYSIS

Hand Calculation

% Deviation

2.21
2740.2
0.16
0.03
12.31
20.37
2775.11

2.21
2740.18
0.15
0.03
12.33
20.37
2775.10

0.0
0.0
6.7
0.0
0.2
0
0.0

5-3

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance
5.3.6

Group 6
Acrylic Acid Project

Mixture of Stream 14, 15 and 16

Table 5.7: Molar flow rate of stream 17 and its comparison with HYSIS

Component

Glycerin
Water
Oxygen
Nitrogen
Acetol
Acrolein
Total

Stream 17
HYSIS

Hand Calculation

% Deviation

2.22
2780.90
205.91
774.55
12.31
21.52
3797.41

2.22
2780.90
205.91
774.55
12.31
21.52
3797.41

0.0
0.0
0.0
0.0
0.0
0.0
0.0

5.3.7 Mixture of Stream 20, 21 and 22

Table 5.8: Molar flow rate of stream 23 and its comparison with HYSIS

Component

Water
Oxygen
Nitrogen
Acetol
Acrolein
Total

Stream 23
HYSIS

Hand Calculation

% Deviation

165.52
215.41
810.52
0.13
134.17
1325.75

165.52
215.41
810.53
0.13
134.17
1325.76

0.0
0.0
0.0
0.0
0.0
0.0

5.3.8 CRV-101
Table 5.9: Molar flow rate of stream 24 at CRV-101 and its comparison with HYSIS

Component

Water
Oxygen
Nitrogen
Acetol
Acrolein
Acrylic acid
Carbon dioxide
Acetic acid
Total

Stream 24
HYSIS

Hand Calculation

% Deviation

165.52
144.42
810.52
0.14
2.69
126.25
5.23
5.23
1260.00

165.52
144.43
810.52
0.13
2.69
126.25
5.23
5.23
1260.00

0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0

5-4

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance
5.3.9

Group 6
Acrylic Acid Project

Mixture of Stream 26 and 34

Table 5.10: Molar flow rate of stream 27 and its comparison with HYSIS

Component

Water

Stream 27
HYSIS

Hand Calculation

% Deviation

400.00

400.00

0.0

5.3.10 T-100
Table 5.11: Molar flow rate of stream 28 at T-100 and its comparison with HYSIS

Component

Water
Oxygen
Nitrogen
Acrolein
Acrylic acid
CO2
Acetic acid
Total

Stream 28
HYSIS

Hand Calculation

% Deviation

402.94
144.43
810.51
2.54
0.58
5.23
0.81
1367.05

405.52
144.43
810.52
2.69
0.00
5.23
0.00
1368.39

0.6
0.0
0.0
5.6
0.0
0.1

Table 5.12: Molar flow rate of stream 29 at T-100 and its comparison with HYSIS

Component

Water
Oxygen
Nitrogen
Acetol
Acrolein
Acrylic acid
CO2
Acetic acid
Total

Stream 29
HYSIS

Hand Calculation

% Deviation

162.58
0.15
0.01
0.13
0.14
125.67
0.00
4.42
292.96

160.00
0.00
0.00
0.13
0.14
126.25
0.00
5.23
291.62

1.6
0.0
0.0
0.5
0
15.5
0.5

5.3.11 MIX-100
Table 5.13: Molar flow rate of stream 31 at MIX-100 and its comparison with HYSIS

Component

Water

Stream 31
HYSIS

Hand Calculation

% Deviation

0.19

0.19

0.0
5-5

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance
Acetic acid
Acetol
Acrolein
Cyclohexane
I-P-acetate
Total

0.32
0.00
0.00
191.25
233.75
425.51

Group 6
Acrylic Acid Project
0.32
0.01
0.16
191.25
233.75
425.86

0.0
100.0
100.0
0.0
0.0
0.08

5.3.12 T-101
Table 5.14: Molar flow rate of stream 33 at T-101 and its comparison with HYSIS

Component

Acrylic acid
Others
Total

Stream 33
HYSIS

Hand Calculation

% Deviation

1.32
592.45
593.77

1.26
593.81
595.07

4.8
0.2
0.2

Table 5.15: Molar flow rate of stream 32 at T-101 and its comparison with HYSIS

Component

Acrylic acid
Others
Total

Stream 32
HYSIS

Hand Calculation

% Deviation

124.36
0.34
124.7

124.41
0.25
124.66

0.04
36.0
0.03

5.3.13 X-100
Table 5.16: Molar flow rate of stream 34 at X-100 and its comparison with HYSIS

Component

Water
Total

Stream 34
HYSIS

Hand Calculation

% Deviation

154.49
154.49

154.49
154.49

0.0
0.0

Table 5.17: Molar flow rate of stream 35 at X-100 and its comparison with HYSIS

Component

Water
Others
Total

Stream 35
HYSIS

Hand Calculation

% Deviation

8.13
431.15
439.28

8.13
431.15
439.28

0.0
0.0
0.0

5-6

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance

Group 6
Acrylic Acid Project

5.3.14 T-103
Table 5.18: Molar flow rate of stream 36 at T-103 and its comparison with HYSIS

Component

Cyclohexane
IP-acetate
Others
Total

Stream 36
HYSIS

Hand Calculation

% Deviation

0.17
15.42
13.69
29.28

7.65
9.35
14.28
31.28

97.7
64.9
4.1
6.4

Table 5.19: Molar flow rate of stream 37 at T-103 and its comparison with HYSIS

Component

Cyclohexane
IP-acetate
Others
Total
5.4

Stream 37
HYSIS

Hand Calculation

% Deviation

191.08
218.33
0.59
410.00

183.60
224.40
0.41
408.41

4.1
2.7
43.9
0.4

Comparison of mass balance results between Hand Calculations with HYSIS

In the mass balance, the deviations of results are mostly 0%. This is due to the formula and data
we used in hand calculation are same with the HYSIS. Some of the small deviation results in
HYSIS have fewer decimal points which also contribute to the deviation. However, high
deviation of acetol and acrolein at MIX-103 is due to the value is relatively small. Thus a small
change in amount of acetol or acrolein will cause a big deviation. This effect of the deviation
also can be seen from others in Stream 32 and Stream 36. Besides that, the deviations in Stream
10, Stream 20 and Stream 37 are due to those assumptions made during manual calculation. This
means the interaction between components, for example binary coefficient is neglected during
hand calculation.

5-7

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance

5.5

Group 6
Acrylic Acid Project

Energy Balance Results

Table 5.20: Summary of Energy Balance and the Comparison

Hand

HYSIS

Calculation

Simulation

Temperature (K)

420.90

417.49

0.8

Mixer MIX-101

Temperature (K)

422.35

452.15

7.1

Mixer MIX-102

Temperature (K)

338.02

338.30

0.1

Mixer MIX-103

Temperature (K)

305.29

305.15

0.05

Mixer MIX-104

Temperature (K)

577.05

576.95

0.02

Mixer MIX-105

Temperature (K)

315.36

315.32

0.01

Heat Exchanger E-100

Temperature (K)

478.13

443.15

7.3

Heater E-101

Heat Flow (kJ/hr)

2.869x106

2.688x106

6.3

Heater E-102

Heat Flow (kJ/hr)

9.876 x 106

1.085x107

9.9

Heater E-103

Heat Flow (kJ/hr)

552.1

560.45

1.5

Heater E-104

Heat Flow (kJ/hr)

1.148 x 106

1.276x106

10.0

Heat Exchanger E-105

Temperature (K)

382.15

374.35

2.0

Heater E-106

Heat Flow (kJ/hr)

2.323x107

2.529x107

8.9

Reactor CRV-100

Heat Flow (kJ/hr)

-357.0

-323.8

9.3

Reactor CRV-101

Heat Flow (kJ/hr)

-2.91x x107

-2.809x107

3.5

Compressor K-100

Power (kW)

5767

5905

2.4

Pump P-100

Power (kW)

1.513

1.497

1.1

Pump P-101

Power (kW)

9.886

9.921

0.4

Separator V-100

Power (kW)

1.569x104

1.492x104

4.9

Quenching Tower T-100

Heat Flow (kJ/hr)

3.74x104

4.0x104

8.1

Condenser T-101

Heat Flow (kJ/hr)

8.74x107

8.85x107

1.3

Reboiler T-101

Heat Flow (kJ/hr)

8.80 x107

8.86x107

0.7

Separator X-100

Heat Flow (kJ/hr)

2.85x106

2.7x106

5.3

Condenser T-103

Heat Flow (kJ/hr)

5.79 x107

5.656x107

2.3

Reboiler T-103

Heat Flow (kJ/hr)

5.63 x107

5.657x107

0.5

Unit Operation

Parameters

Mixer MIX-100

% Deviation

5-8

KKEK 4281 Design Project

Chapter 5: Mass and Energy Balance

5.6

Group 6
Acrylic Acid Project

Comparison Energy Balance Result between Hand Calculation and

HYSIS

The discrepancies of results in energy balance were mainly due to those assumptions made in
order to simplify the calculations such as negligible heat of dilution, negligible heat of mixing,
negligible heat change due to pressure change, negligible heat loss to surrounding, negligible
kinetic and potential energy and etc. Most of the mixer have small deviation with the HYSIS
results compare with others unit operations maybe because mixing do not involve others heat
such as heat of reaction and heat of formation. Beside that, sometime the assumptions such as the
components in some stream are all change to vapor, or maybe the components all remain in
liquid state are made when we do the hand calculation. In the other hand, the constant value such
as heat capacity, heat of formation, heat of vaporization that we take from literature which the
reference state are different with in the HYSIS make the deviation.

5-9

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

CHAPTER 6: PACKED BED REACTOR 1

6.1 Chemical Design of Reactor 1
6.1.1 Introduction
In the first reactor, crude glycerol (C3H8O3) is dehydrated to acrolein(C3H4O) via heterogeneous
catalytic endothermic reaction:

C3 H 8O3
C3 H 4O + 2 H 2O

(Equation 1)

The raw material is crude glycerol obtained from biodiesel plant with purity of 88%. The catalyst
used is aluminasilicates supported silicotungstic acid. The pressure and temperature of the
reactor is maintained at 1 atm and 275oC. Under these conditions, the conversion of glycerol is
98.3% and the selectivity of the acrolein is 86.2%. The mass ratio of steam to glycerol is
controlled to 4 to 1 while the proportion of oxygen to the total mass is controlled to 0.07. Steam
is added as inert gas to control the rate of the reaction. Air which consists of oxygen and nitrogen
is added to increase the lifetime of the catalyst by reducing coke formation or any undesired
adsorption.
The condition and composition of the reactor feed (Stream 5) and product (Stream 6) are shown
below:

Conversion = 98.3%
Selectivity = 86.2%

F5 = 3932.41 kmol/h
Phase = Vapour
FGly_5 = 137.22 kmol/h
Fwater_5 = 2780.9 kmol/h
FO2_5 = 205.91 kmol/h
FN2_5 = 774.55 kmol/h
FAce_5 = 12.31 kmol/h
FAcro_5 = 21.52 kmol/h

65 = 4201.39 kmol/h
Phase = Vapour
FGly_6 = 2.33 kmol/h
Fwater_6 = 3049.90 kmol/h
FO2_6 = 205.91 kmol/h
FN2_6 = 774.55 kmol/h
FAce_6 = 13.10 kmol/h
FAcro 6 = 21.52 kmol/h

Figure 6.1: Schematic Diagram of Reactor 1

6- 1

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

6.1.2 Type of Catalyst

The catalyst used for the glycerol dehydration reaction is aluminosilicate supported silicotungstic
acid. Some properties of the catalyst are shown in Table 1[1].
Assumption:
(i) The catalyst is in spherical shape.
(ii) The bed porosity = 0.7
Table 6.1: Property of catalyst

Parameter
Catalyst used
Shape
BET surface area (m2/g)
Diameter (m)
Surface density (mol/m2)

Value
aluminosilicate supported silicotungstic acid
Porous spherical shape
309.2
315-500
0.197

Bed porosity,

0.7

Solid particle density, c (kg/m3)

885

6.1.3 Type of Reactor

The dehydration of glycerol to acrolein is endothermic heterogeneous catalytic reaction with the
feeds are in gaseous form and the catalyst used is in solid form. The reactors that can be used to
handle this 2 phase reaction are either packed bed reactor and fluidized bed reactor.
The dimension and performance of packed bed reactor and fluidized bed reactor are compared.
The type of reactor which can achieve 98.3% of conversion of glycerol with a most economic
design is chosen.

6.1.3.1 Packed Bed Reactor

Packed bed reactor is suitable to be used as reactor 1 as it provided higher conversion per unit
weight of catalyst, low operating cost and can be run continuously. A packed-bed reactor is
essentially a tubular reactor consists of one or more tubes packed with solid catalyst particles, in
which the reactants and products flow through.

6- 2

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

Since the reaction is endothermic, extra heat has to be supplied to maintain the optimum
temperature in the reactor. In the conceptual design, it is proposed that the feed itself served as
the heating fluid. However in packed bed reactor, such heating method is not applicable as the
temperature in reactor will become uneven. Hence a heating fluid is introduced into the reactor to
maintain the reactor temperature. Since the reaction temperature is at 275oC, the heating fluid
used is hot molten salt.

Figure 6.2: Shell-and-tube packed-bed reactor with co-current heating

6.1.3.1.1 Type of Heat Transfer Fluid

Hot molten salt is used as the heating medium to maintain the reactor 1 temperature at 275oC.
We have decided to use HITEC Heat Transfer Salt supplied by Coastal Chemical Co. as the hot
molten salt. HITEC is a white, granular solid; when melted, pale yellow. HITEC is an eutectic
mixture of water-soluble, inorganic salts of potassium nitrate, sodium nitrite and sodium nitrate.
We have decided to use HITEC Heat Transfer Salt supplied by Coastal Chemical Co. as the hot
molten salt. HITEC is a white, granular solid; when melted, pale yellow. HITEC is a eutectic
mixture of water-soluble, inorganic salts of potassium nitrate, sodium nitrite and sodium nitrate.
It is a heat transfer medium for heating and cooling between 300-1100F (149-538C) and is
suitable to be used as the heating fluid for reactor 1.
HITEC is chosen because it has a low melting point (288F, 142C), high heat transfer
coefficient, thermal stability, and low cost. It is nonfouling a commonly recognized defect of
6- 3

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

many organic heat transfer media. HITEC is non-flammable, non-explosive and evolves no toxic
vapours under recommended conditions of use. Besides, it has a low degree of corrosivity toward
common materials of construction. Plain carbon steel, for example, can be used for installations
that operate up to 850F (454C).
The properties of HITEC are listed in Table 2[2]. The property is evaluated at 275C and 1atm
since the inlet temperature of hot molten salt is set to be 275C.
Table 6.2: Property of hot molten salt (HITEC)

Parameter

Value

Heat capacity, Cp_salt (J/kgC)

3420

Viscosity, salt (Pas)

2.1 x 10-3

Density, salt (kg/m3)

1980

Thermal conductivity, ksalt (W/mK)

0.57024

6.1.3.1.2 Packed Bed Reactor Dimension

Since the inlet flow rate is very high, 2 reactors which operate in parallel are used instead of one.
Packed bed reactor with 1 shell pass and 1 tube pass is chosen because it easier to operate and
control. The reactant (glycerol) and product (acrolein) are not corrosive in nature. However some
of the by-product formed such as acrylic acid is corrosive. Hence tubes with BWF 40 are used to
prevent tube leaking due to corrosiveness of the reactant and product. Triangular pitch is chosen
to enhance the turbulence of molten salt (heating medium) in shell which resulting in higher heat
transfer. Besides that more tubes can be placed in triangular pitch.
Table 6.3: Dimension of Packed Bed Reactor [3]

Parameter
Type
No. of reactor operated in parallel
Nominal tube size

Value
1 shell pass and 1 tube pass
2
1.5in tube of BWG 14

Outer diameter of tube, ODtube

1.5in.

Inner diameter of tube, IDtube

1.33in.

Tube pitch, PT

1.875in. triangular pitch

6- 4

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

Tube clearance, C

0.375in.

Baffle spacing, B

0.1m

6.1.3.1.3 Equation Involved in Packed Bed Reactor Design

6.1.3.1.3.1 Rate law

Assumption:
1. The reaction is first order reaction.
2. The gas reactant and product obey ideal gas law.
3. Partial pressure of the reactant is calculated according to inlet pressure.
4. The reactor is assumed to be isothermal.
5. 80% of reactor is filled by catalyst.
Rate Law:
mol Gly
rGly 3
= k1 PGly
m catalyst s
mol Gly 1
Hence, rGly
k1 PGly
=
kg catalyst s c

m3gas
19
Where k1 3
= 1.00 10 e
m catalyst s

248000

RT [4]

For reaction with pressure drop:

CGly =

CGlyo (1 X ) P To

1 + X Po T

From ideal gas law

PGly = CGly RT
Since it is assumed that the reactor is isothermal, T=To
PGly =

PGlyo (1 X ) P To

1 + 0.0698 X Po T

6- 5

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

mol Gly 1
rGly
=
kg catalyst s c

19

1.00
10
e

248000

RT

PGlyo (1 X ) P

1 + 0.0698 X Po

To

T

(1)

6.1.3.1.3.2 Mole balance

The design equation for packed-bed reactor is given as:

FGlyo

dX
= rGly
dW

248000
PGlyo (1 X ) P To
dX 1
19 RT
1.00 10 e
=

dW c FGlyo
1 + 0.0698 X Po T

Let

Y=

P
Po

dX 1
=
dW c FGlyo

Z=

and

T
To

248000

CGlyo (1 X ) Y
19 RT
1.00
10
e

1 + 0.0698 X Z

(2)

6.1.3.1.3.3 Ergun equation for pressure drop

The gas-phase reaction is catalyzed by passing the reactant through a packed bed of catalyst

particles. The equation used most to calculate pressure drop in a packed bed is the Ergun
equation.
From Ergun equation, differential pressure drop across the tube is given as:

dP
G 1 150 (1 )
=
+ 1.75G
3
dz
dP
dP

(3)

Where z = length down the packed bed of tube

At the entrance to the reactor:
P To

Po T

= o

FTo

FT

(4)

Substitute (4) into (3):

dP
P T
= o o
dz
P To

FT

FTo

(5)

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Chapter 6: Packed Bed Reactor 1

o =

Where

Group 6
Acrylic Acid Project

G (1 ) 150 (1 )

+ 1.75G
3
o d P
dP

(6)

Weight of catalyst, W = Volume of solid catalyst x Density of catalyst

Weight of catalyst, W = Volume of reactor x (1 bed porosity) x Density of catalyst
W = (1 ) Ac z c = b Ac z

b = c (1 )

Where

dz =

dW
b Ac

(7)

Substitute (7) into (5):

P T F
dP
= o o T
dW
b Ac P To FTo
However,

FT
= 1+ X
FTo
T
(1 + X )
To

P
dP
= o o
dW
b Ac P

o Z
dY
=
(1 + 0.0698 X )
b Ac Po Y
dW

(9)

6.1.3.1.3.4 Simultaneous Ordinary Differential Equations

The conversion and pressure profiles for the packed-bed reactor are governed by 2 ODEs:
1)

248000
P 1 X ) Y
dX 1
19 RT Glyo (
e
=

1.00
10

dW c FGlyo
1 + 0.0698 X Z

2)

o Z
dY
=
(1 + 0.0698 X )
b Ac Po Y
dW

Since the reactor is assumed to be isothermal, Z=1.

The ODEs are solved simultaneously by substituting all the relevant values, with the aid of
MATLAB 7.0.

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Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

6.1.3.1.4 Packed Bed Reactor Optimization

The reactor size and performances are analyzed by using different parameters such as pressure,
temperature and the reactor shell diameter.
The analysis is done by computing the variables with different pressure, temperature and flow
area into the simultaneous equation. The result of weight of catalyst and the pressure ratio when
the conversion, X=0.983[1] are obtained by solving the simultaneous equations using MATLAB
software. The ratio of length and diameter of the reactor of different parameter are calculated.
The reactor size and performance are optimized based on the following criteria:
(i)

The ratio of length to diameter of the reactor (L/D) must be within the range of 510.[5]

(ii)

The pressure drop must be kept as low as possible or pressure ratio, Y as high as
possible to prevent loss in pressure energy.

(iii)

The amount of catalyst should not be extremely high due to the economic
consideration.

Example of the result of MATLAB by using P = 1 bar and T = 275oC.

The result is shown in the plot obtained from MATLAB:

Figure 6.3: Plot of Conversion and Pressure Ratio Obtained from Matlab

Legend: Blue = Conversion

Green = Pressure Ratio

The accurate result is obtained from the workplace of MATLAB:

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

Figure 6.4: Data of Conversion and Pressure Ratio Obtained from Matlab

6.1.3.1.4.1 Shell Diameter Analysis

Assume
Pressure, P = 1.5 bar

Temperature, T = 275oC

The number of tubes that can be placed in the reactor is depends on the size of the shell of the
reactor. Hence an analysis is done to study the performance of the reactor by using different size
of shell.
From the result of MATLAB, the weight of catalyst, W, pressure ratio, Y and the ratio of length
and diameter of reactor, L/D are obtained and plotted against number of tubes.

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Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

Table 6.4: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length to
Diameter, L/D at Different Number of Tube per Reactor [3]

Shell
Diameter,
IDs (m)

No. of
Tubes per
reactor, n

1.0
1.1
1.2
1.3
1.4
1.5

361
442
530
637
733
847

Flow
Area, Ac
(m2)

Weight of
Catalyst, W
(kg)

Pressure
Ratio, Y

Length of
Reactor,
L (m)*

Ratio of Length to
Diameter, L/D

4050
3820
3630
3510
3370
2980

0.872
0.898
0.917
0.932
0.9415
0.95

29.46
22.70
17.99
14.47
12.07
9.24

29.4609
20.6323
14.9882
11.1307
8.6238
6.1594

0.6472
0.7924
0.9502
1.1421
1.3142
1.5186
W
* Length of reactor, L =
b Ac 0.8
b = bed density (kg/m3)
Ac = Total tubes flow area (m2)
0.8 means reactor is 80% filled by catalyst

From Table 4, it shows that the dimensions of reactor with shell diameter = 1.4 m and number of
tube per reactor = 733 gives the result of length to diameter ratio = 8.6238 which is in the range
of design criteria (5-10). Hence it is the most suitable dimension of the reactor to optimize the
process.

6.1.3.1.4.2 Pressure Analysis

Set:
Shell inner diameter = 1.4 m

Number of tube per reactor, n = 733

Assume:
Temperature, T = 275oC

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Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

From reference [1], the optimum pressure lies between 1 bar to 2 bar.
From the result of MATLAB, the weight of catalyst, W, pressure ratio, Y and the ratio of length
and diameter of reactor, L/D are obtained and plotted against inlet pressure.

Table 6.5: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length to Diameter,
L/D at Different Inlet Pressure, Po

Inlet Pressure,
Po (bar)

Weight of
Catalyst, W (kg)

Pressure
Ratio, Y

Length of
Reactor, L (m)

Ratio of Length to
Diameter, L/D

1
1.1
1.2
1.3
1.4
1.5
1.6
1.7
1.8
1.9
2

2210
2440
2610
2850
3120
3370
3700
3800
3880
3970
4050

0.932
0.938
0.944
0.948
0.951
0.955
0.958
0.961
0.963
0.965
0.967

7.92
8.74
9.35
10.21
11.18
12.07
13.26
13.61
13.90
14.22
14.51

5.6552
6.2438
6.6788
7.2929
7.9838
8.6235
9.4680
9.7239
9.9286
10.1589
10.3636

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Chapter 6: Packed Bed Reactor 1

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From Table 5, the length to diameter ratio at pressure 1 to 1.8 bars is within the design range, 510. However, operating under low pressure might causes the pressure driving force not sufficient
to drive the reactant along the reactor. The situation become worse if there is clogging fouling
that causing the pressure drop across reactor higher than expected. The outlet pressure might
drop to less than 1 atm, which is vacuum condition under these situations. Hence it is better to
have a safety margin to operate at higher pressure. Pressure of 1.4 bar is selected as the catalyst
used is not too high and L/D ratio is still within 5-10.
6.1.3.1.4.3 Temperature Analysis

Set:
Shell inner diameter = 1.4 m

Number of tube per reactor, n = 733

Pressure, P = 1.4 bar

From reference [1], the optimum pressure lies between 260oC to 280oC.
From the result of MATLAB, the weight of catalyst, W, pressure ratio, Y and the ratio of length
and diameter of reactor, L/D are obtained and plotted against inlet temperature.

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

Table 6.6: Weight of Catalyst, W, Pressure Ratio, Y, Length of Reactor, L and Ratio of Length to Diameter,
L/D at Different Inlet Temperature, To

Inlet Temperature,
To (oC)

Weight of
Catalyst, W (kg)

Pressure
Ratio, Y

Length of
Reactor (m)

Ratio of Length to
Diameter, L/D

260
265
270
275
280

8020
6500
5020
3120
1990

0.712
0.853
0.917
0.951
0.971

28.73
23.29
17.98
11.18
7.13

20.5225
16.6330
12.8458
7.9838
5.0922

From the Table 6, it is clearly show that 275oC is the best temperature to be operated because at
275oC, the ratio of length to diameter of reactor is 7.9838 which is in the range of design
consideration, which is 5-10.

6.1.3.1.4.4 Result of Packed Bed Reactor Optimization Analysis

Table 6.7: Results of Packed Bed Reactor Optimization Analysis

Parameter

Value

Inlet Pressure, Po (bar)

1.4

Inlet Temperature, To (oC)

275

Number of Tubes per Reactor, n

733

Total Number of Tubes, N

1466

Shell Diameter, IDs (m)

1.4

Weight of Catalyst, W (kg)

3120

Pressure Ratio, Y

0.951

Outlet Pressure, P=YPo

1.3314

Length of Reactor, L (m)

11.18

Ratio of Length to Diameter, L/D

7.9838

6.1.3.2 Fluidized Bed Reactor

Fluidized bed reactor is operated by pumping in the inlet feed from the bottom of the reactor to

fluidize the catalyst particle in the reactor. The catalyst particle will fluidize if the inlet velocity
is greater than minimum fluidization velocity. If not the reactor will only serve as a packed bed

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

reactor. Fluidized bed reactor can produce uniform particle mixing and uniform temperature
gradient which can provide a more uniform conversion along the reactor.
Since the reaction is endothermic and additional heat has to be supplied to maintain the reactor
temperature. The inlet feed itself will serve as the heating medium by feed into the reactor at a
higher temperature to compensate the heat loss due to endothermic reaction. It is done by
preheated inlet feed to desired temperature before feed into reactor.

Figure 6.5: Schematic Diagram of Fluidized Bed Reactor

6.1.3.2.1 Equation Involved in Fluidized Bed Reactor Design

6.1.3.2.1.1 Conversion of Glycerol in Fluidized Bed Reactor

Assumption:
1. 20% of the reactor volume is occupied by gas bubbles and 80% by catalyst particle.
2. Mass transfer coefficient, kmav = 0.60 s-1.
3. The reaction is first order reaction.
From reference [6], conversion of glycerol in fluidized bed reactor is written as:

X = 1 exp[(

1
1 1 L
)
]
+
d k c km av ub

d = 0.80 (20% of reactor is filled by gas bubbles)

c = catalyst density = 885 kg/m3

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Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

kmav = mass transfer coefficient = 0.60 s-1

L = length of reactor
248000
19 RT

k = rate constant = 1.00 10 e

ub= feed velocity =
X = 1 exp[(

L=

m
( IDs ) 2 o

1
1 1 L
)
]
+
708k 0.6 ub

1
1
+
)
708k 0.6 ln(1 X )
ub

6.1.3.2.2 Fluidized Bed Reactor Optimization

The fluidized bed reactor size and performance are analyzed by using different operating
temperature and reactor diameter. The parameters to achieved conversion of glycerol = 0.983 [1]
are obtained and the reactor size and performance are optimized based on the following criteria:
(i)

The ratio of length to diameter of the reactor (L/D) must be within the range of 510.[5]

Since the inlet flow rate is very high, 5 reactors which operated in parallel are used in the process.

6.1.3.2.2.1 Temperature Analysis

Assume the reactor diameter = 1.5 m

ub =

m
= 2.515m / s
( IDs ) 2 o

From reference [1], the optimum pressure lies between 260oC to 280oC.

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

Table 1.8: Length of Reactor, L and Ratio of Length to Diameter, L/D at Different Inlet Temperature, To

Temperature

Rate Constant,
k (s-1)

Length of
Reactor, L (m)

Ratio of Length to
Diameter, L/D

260
265
270
275
280

3.012E-05
4.983E-05
8.166E-05
0.0001326
0.0002136

78.6707
48.6250
30.7206
19.9513
13.4146

52.4471
32.4166
20.4804
13.3009
8.9431

From the Table 8, it is clearly show that 280oC is the best temperature to be operated because at
280oC, the ratio of length to diameter of reactor is 8.9431 which is in the range of design
consideration, which is 5-10.

6.1.3.2.2.2 Reactor Diameter Analysis

Set temperature, T = 280oC

k = 0.0002136 s-1

Table 6.9: Length of Reactor, L and Ratio of Length to Diameter, L/D for Different Shell Diameter, IDs

Shell Diameter,
IDs (m)
1
1.1
1.2
1.3
1.4
1.5

Feed
velocity, ub
(ms-1)
5.6585
4.6764
3.9295
3.3482
2.8870
2.5149

Length of
Reactor, L (m)

5.9616
7.2136
8.5847
10.0751
11.6848
13.4136

Ratio of
Length to
Diameter, L/D
3.9744
4.8090
5.7232
6.7168
7.7899
8.9424

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Chapter 6: Packed Bed Reactor 1
1.6
1.7
1.8
1.9
2

Group 6
Acrylic Acid Project
2.2104
1.9580
1.7464
1.5675
1.4146

15.2617
17.2291
19.3156
21.5214
23.8465

10.1745
11.4861
12.8771
14.3476
15.8976

From Table 8, shell diameter of 1.4m is chosen because it gives a moderate value of length to
diameter ratio, which is 7.7899.

6.1.3.2.2.3 Result of Fluidized Bed Reactor Optimization Analysis

Table 6.10: Results of Fluidized Bed Reactor Optimization Analysis

Parameter

Value

Inlet Temperature, To (oC)

280

Shell Diameter, IDs (m)

1.4

Length of Reactor, L (m)

11.68 m

Ratio of Length to Diameter, L/D

7.7899

6.1.3.3 Comparison of Packed Bed and Fluidized Bed Reactor

From the optimization analysis, it shows that the reactor dimension and operating condition to
achieved glycerol conversion of 98.3% for both type of reactor are almost similar. However
fluidized bed reactor system required 5 reactors to operate in series while packed bed reactor
only requires 2. This is because fluidized bed reactor requires bigger vessel for fluidization of
catalyst. Hence less feed will pump into each reactor and more reactors are required. This
resulted in the higher initial capital cost for fluidized bed reactor compared to packed bed reactor.
Besides that higher pumping effect is required for fluidized bed reactor to ensure fluidization of
the catalyst. This result in higher operating cost compared to packed bed reactor. There is also a
possibility that the solid catalyst particle will entrained out along with the product and
contaminate the product. Furthermore severe agitation of catalyst will result in catalyst
destruction and dust formation.

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

6.1.4 Heat Duty of Heating Jacket

Q = m(H ) = msalt C p (Th,in Th ,out ) = U d A(TLMTD )
Table 6.11: Variables to Calculate Heat Duty

Symbol

Description

Value

Unit

Mass flow rate of reactant per reactor

12.936

kg/s

Heat of reaction

49000

J/kg

msalt

Mass flow rate of molten salt (heating medium)

15

kg/s

Cp

Specific heat capacity of molten salt

3420

J/kg.oC

Th,in

Inlet temperature of heating stream

330

Th ,out

Outlet temperature of heating medium

Overall heat capacity of the reaction

Heat transfer surface area, n(ID)L

TLMTD

W/m2. oC
869.72

m2

Log mean temperature difference of reactant and

heating stream

Q = (12.936)(49000) = 6.339 x 105 J/s

Q = msalt C p (Th ,in Th ,out )
Th ,out = Th ,in

Q
msalt C p

Th ,out = 305.3 oC

TLMTD =

(Th ,in T ) (Th ,out T )

T T
ln( h ,in
)
Th ,out T

TLMTD = 41.43
Q = U d A(TLMTD )
Ud = 182.92 W/m2. oC

6.1.5 Clean overall heat transfer coefficient

6.1.5.1 Tube-side film coefficient, hio
Table 6.12: Variables to Tube-side Film Coefficient

Symbol
Ac

Description

Tube side flow area

Value

Unit

1.3142

m2

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Chapter 6: Packed Bed Reactor 1
G
Ret
Prt

Group 6
Acrylic Acid Project

Tube side mass velocity, G =

9.843

m
Ac

Tube side Reynolds Number, Ret =

Tube-side Prandtl number, Prt =

n IDt Gt

kg/ m2

1.367x107

Cp

0.7526

kt

hi*

Convective heat transfer coefficient

6308.59

W/m2.oC

hio

ID
Tube-side film coefficient, hio = hi t
ODt

5593.61

W/m2.oC

*Since Ret >10000 and 0.7 <Prt <170, hence according to [5], Dittus-Boelters equation can be
used to evaluate the heat-transfer coefficient.
Tube-side Nusselt number,

Nut =

hi IDt
= 0.0243Ret 0.8 Prt 0.4
kt

k
hi = 0.0243Ret 0.8 Prt 0.4 t
IDt
hi = 202.87 W/m 2 C
6.1.5.2 Shell-side film coefficient, ho
Table 6.13: Variables to Shell-side Film Coefficient

Symbol

Description

Value

Unit

0.1

Baffle Spacing

Pt

Tube pitch (square pitch)

1.875

in

Tube clearance, C=Pt - ODt

0.375

in

0.02800

m2

535.77

kg/sm2

as

Gs

Shell-side flow area, as =

( IDshell ) ( C ' B )

Shell-side mass velocity, Gs =

Pt
msalt
as

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Chapter 6: Packed Bed Reactor 1

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De

ODt 2
4 PT 2

4
Equivalent diameter, De =
ODt

0.0377

ho*

Shell-side film coefficient

201.34

W/m2C

*The shell film coefficient is given as:

ho De
DG
= 0.36 e s
k

0.55

0.55

C p _ salt salt

ksalt

DG
Shell-side film coefficient, ho = 0.36 e s
salt

0.33

0.33

k salt

De

= 201.34 W/m2C

6.1.6 Fouling factor

Table 6.14: Variables to Calculate Fouling Factor

Symbol

Description

Value

Unit

Uc

h h
Clean overall heat transfer coefficient, U c = io o
hio + ho

194.34

W/m2C

Ud

Actual heat transfer coefficient

182.92

W/m2C

Rd

Fouling factor, Rd =

1
1

Ud Uc

0.00032

C/W

Fouling factor of 0.00032 m2C/W is sufficient to account for the flow across packed-bed of
catalyst. Hence, the designed reactor dimension is acceptable.

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

6.1.7 Summary of Specification of Reactor 1

Table 6.15: Summary of Specification of Reactor 1

Parameter

Description

Type of reactor

Shell-and-tube packed-bed reactor

Type of catalyst

aluminosilicate supported
silicotungstic acid

Heating Medium
Flow pattern
Conversion, X
No. of reactor operated in parallel

Molten Salt (HITEC)

Co- current
0.983
2

No. of tubes per bank

733

Total no. of tubes, n

1466

Nominal tube size

1.5in. BWF 14

Outer diameter of tube, ODtube

1.50in.

Inner diameter of tube, IDtube

1.33in.

Tube pitch, PT

1.875in. triangular pitch

Tube clearance, C = PT - ODtube

0.375in.

Internal diameter of shell, IDshell

1.4m

Weight of catalyst

3120 kg

Length of reactor

11.18 m

Actual overall heat transfer coefficient, Ud

182 W/m2C

Mass flow rate of hot molten salt, msalt

15 kg/s

Temperature of inlet reactant, To

275C

Temperature of outlet product, T

275C

Inlet temperature of molten salt

330C

Outlet temperature of molten salt

305.3C

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

Pressure at inlet of reactor

1.4bar

Pressure at outlet of reactor

1.3314bar

Heat transfer duty, Q

6.339 x 105 W

6.2 Mechanical Design of Reactor 1

6.2.1 Design Pressure
The reactor must be designed to withstand the maximum pressure to which is it likely to be subjected
in operation. For safety purpose, the design pressure normally is 5 to 10% above the operating
pressure to avoid spurious operation during minor process upsets. The operating pressure of the
packed bed reactor for dehydrogenation of glycerol is 1.4 bar. The reactor is designed to withstand
the pressure 10% higher than the operating pressure.
Design Pressure, PD = (1.4)(1.1) = 1.54 bar

6.2.2 Design Temperature

The strength of metals decreases with increasing temperature so the maximum allowable design
stress will depend on the material temperature. The design temperature at which the design stress
is evaluated should be taken as the maximum working temperature of the material, with due
allowance for any uncertainty involved in predicting vessel wall temperatures.
Design Temperature, TD = 275oC

6.2.3 Material of Construction

Since the reactant, glycerol and product, acrolein are not corrosive in nature, carbon steel should be
used as the construction material for reactor. However oxygen is supplied into the column to oxidize
the catalyst to elongate its lifetime. Carbon steel might be oxidized by the oxygen, resulting in the
rust formation. Furthermore the formation of certain by-product such as acrylic acid is corrosive in
nature. Hence Austenitic stainless steel type 304 is chosen for reactor fabrication due to its anti rust
and corrosive natures while the cost is reasonable.

6.2.4 Design Stress

According to reference [8],
Tensile strength of Austenitic stainless steel type 304 = 510 N/mm2

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Acrylic Acid Project

Design stress of Austenitic stainless steel type 304 at 275oC, f = 107.5 N/mm2 = 1.075 x 108 N/m2
Design stress is the maximum allowable stress that the Austenitic stainless steel type 304 could be
expected to withstand without failure under standard test condition.
It is noticed that the design pressure, PD = 1.54 x 105 N/m2 is much smaller than design stress,
therefore it is safe and suitable to use Austenitic stainless steel type 304 as the material of
construction.

6.2.5 Welded Joint Efficiency

The value of the joint factor used in design will depend on the type of joint and amount of
radiography required by the design code. Double-welded butt joint is chosen because it can
withstand more stress and due to its high efficiency. In this design, welded joint efficiency, J is
taken as 1.0 which implies that the join is equally as strong as the virgin plate. It is achieved by
radiographing the complete weld length, and cutting out and remaking any defects.
Welded Joint Efficiency, J =1.0

6.2.6 Corrosion Allowance

Corrosion allowance is the additional thickness of metal added to allow for material losses by
corrosion and erosion, or scaling. The allowance is generally based on the design experience.
Normally, the value is range from 2.0mm to 4.0 mm. Since the reactant and product of the reactor is
not corrosive, minimum corrosion allowance for alloy steels, which is 2mm is chosen.

Corrosion allowance, eallowance = 2.0mm

6.2.7 Minimum Practical Wall Thickness

Minimum wall thickness is required to ensure that the reactor is sufficiently rigid to withstand its
own weight and any identical loads. The packed bed reactor used is in cylindrical shape where the
minimum thickness required to resists internal pressure is given by:

emin =

Po IDs
2 J f Po

emin =

(1.4 x105 ) (1.4)

= 0.025m
2(1.0) (1.075 x108 ) 1.4 x105

where IDs = shell diameter

The wall thickness which includes corrosion allowance:

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ewall = emin + eallowance = 0.025 + 0.002 = 0.027 m

Outer diameter of shell:
ODS = IDS + 2ewall = 1.4 + 2(0.027) = 1.454m

6.2.8 Head and Closure

An ellipsoidal head is selected as operating pressure above 15 bars and it proved to be the most
economical closure. A commonly used ellipsoidal head has a ratio of base radius to depth of 2:1 (Fig.
a). The shape can be approximated by a spherical radius of 0.9D and a knuckle radius of 0.17D (Fig.
b). The thickness is obtained from the following equation:

ehead =
ehead

Po IDs
2 J f 0.2 Po

(1.4 x105 ) 1.4

=
= 0.025m
2(1.0) (1.075 x108 ) 0.2(1.4 x105 )

Thus, ehead _ new = ehead + eallowance = 0.025 + 0.002 = 0.027 m

Figure 6.6: Ellipsoidal Head [9]

6.2.9 Connection
Nozzles are used for the reactor connections. It consists of a pipe stub welded into the vessel and
terminating in a bolting flange.

6.2.10 Manhole
Two manholes with a cover plate were designed to permit for access to the internal of the reactor
during maintenance and inspection. One is located at the top and the other one is at the bottom.

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Both of the manholes are designed with the similar dimensions. According to BS 470, the
minimum manhole diameter, Dmanhole and the minimum length of manhole, Lmanhole that can
afford full rescue facilities with self-contained breathing apparatus shall be:

Dmanhole = 575 mm

Lmanhole = 500 mm.

6.2.11 Compensation for Openings

The presence of an opening weakens the shell, and gives rise to stress concentrations. Thus, to
compensate for the effect of an opening, sufficient reinforcement must be provided without
significantly altering the general dilation pattern of the vessel at the opening by increasing the
wall thickness in the region adjacent to the opening. The principal used to calculate the
reinforcement needed is based on A1=A2 method, equal in cross sectional area to the area
removed in forming the opening.

Figure 6.7: Schematic diagram of opening [8]

6.2.11.1 Compensate Opening for Feed

Diameter optimum, dt_optimum in mm for the feed opening is calculated by:

dt _ optimum = 226 m '0.5 o ( 0.35)

Table 6.16: Variables to Calculate Optimum Diameter in Feed Opening

Symbol

Description

Value

Unit

Mass flow rate of reactant

12.936

kg/s

Density of inlet feed

0.7276

kg/m3

dt _ optimum = 226 (12.936)0.5 (0.7276)( 0.35)

dt _ optimum = 251mm = 9.88in

Hence nominal pipe size chosen = 10 in
From reference [3], for stainless steel with schedule no 40 and nominal pipe size = 10 in,

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Outer diameter of inlet pipe = 10.75 in

Inter diameter of inlet pipe = 10.02 in
Thickness of compensate = 2.54 x (OD ID) = 2.54 x (10.75-10.02) = 1.8542 in = 0.047 m
Inlet flow rate and density of feed enter the reactor is the same as the product exit from reactor.
Hence, both openings for inlet and outlet of reactor have the same ID and compensate thickness.
6.2.11.2 Compensate Opening for Molten Salt (Heater)

Diameter optimum, dt_optimum in mm for the molten salt opening is calculated by:
dt _ optimum = 226 msalt 0.5 salt ( 0.35)
Table 6.17: Variables to Calculate Optimum Diameter in Molten Salt Opening

Symbol

msalt

Description

Mass flow rate of molten salt (heating medium)

Density of molten salt

Value

Unit

15

kg/s

1980

kg/m3

dt _ optimum = 226 (15)0.5 (1980)( 0.35)

dt _ optimum = 61.42mm = 2.42in

Hence nominal pipe size chosen = 2.5 in
From reference [3], for stainless steel with schedule no 40 and nominal pipe size = 2.5 in,
Outer diameter of inlet pipe = 2.88 in
Inter diameter of inlet pipe = 2.469 in
Thickness of compensate = 2.54 x (OD ID) = 2.54 x (2.88-2.469) = 1.0439 in = 0.041 m
It is assumed that the density of outlet molten salt does not change and the mass flow of outlet
molten is the same as inlet flow. Hence, both openings for inlet and outlet of molten salt have the
same ID and compensate thickness.

6.2.12 Dead Weight Load

6.2.12.1 Cylindrical Vessel

Total weight of shell, excluding internal fitting, is determined by:

Wv = 240Cv Dm ( L + 0.8 Dm )ewall

Table 6.18: Variables to Calculate Total Weight of Shell

Symbol

Description

Value

Unit

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Cv

A factor to account for internal supports

1.80

kN/m2

Dm

Mean diameter of vessel, Dm = (IDs +ewall)

1.427

IDs

Inner diameter of shell

1.4

Length of reactor

11.18

Wall thickness

0.027

L
ewall

Weight of shell, Wv = 205.09 kN

6.2.12.2 Tubes

Total weight of tubes is determined by:

Wt = n m& t L g
Table 6.19: Variables to Calculate Total Weight of Tube

Symbol

Description

Value

Unit

733

Total no. of tubes per reactor

Length of reactor

11.18

m& t

Specific mass per length of tube

5.45

kg/m

Gravitational acceleration

9.81

m/s2

Weight of tubes, Wt = 438.13 kN

6.2.12.3 Catalyst

Weight of catalyst, W = 3120 kg = 30.61 kN

6.2.12.4 Baffles

Total weight of baffles is determined by:

Wt = N B AB B 0.75
Table 6.20: Variables to Calculate Total Weight of Baffles

Symbol
NB

AB

Description

Value

Total no. of baffles per reactor

Flow area through shell, AB =
Density of baffle

Unit

11

IDS 2
4

n(

IDtube 2
4

1.538

m2

1120

N/m2

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0.75

Group 6
Acrylic Acid Project

25 % baffle cut

Weight of baffles, WB= 14.22 kN

6.2.12.5 Feed

Total weight of feed in reactor is determined by:

W f = Vt o g
Table 6.21: Variables to Calculate Total Weight of Feed

Symbol
Vt

Description

Total volume of tube, Vt = n(

Bed voidage

Density of inlet feed

IDtube 2
4

Value

Unit

0.2259

m3

0.7

m2

0.7276

kg/m3

Weight of feed in the reactor, Wf = 1.13 kN

6.2.12.6 Molten Salt

Total weight of molten salt in reactor is determined by:

Wsalt = AB L salt g
Table 6.22: Variables to Calculate Total Weight of Molten Salt

Symbol

AB
L

salt

Description

Value

Unit

1.538

m2

Length of reactor

11.18

Density of molten salt

1980

kg/m3

Flow area through shell, AB =

IDS 2
4

n(

IDtube 2
4

Weight of molten salt in the reactor, Wsalt = 333.99 kN

6.2.12.7 Insulation

The material used for the insulation of reactor is mineral wood.

Total weight of insulation of reactor is determined by:

Wi = Vi i g

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Table 6.23: Variables to Calculate Total Weight of Insulation

Symbol

Vi

Description

Volume of insulation, Vi = (

( IDS + ei )2
4

IDS 2
4

)L

Value

Unit

1.893

m3

ei

Thickness of insulation

0.075

Density of mineral wood

130

kg/m3

Weight of insulation of the reactor, Wi = 2.41 kN

6.2.12.8 Total Dead Weight

Total Dead weight of the reactor, Wreactor = Wv + Wt + WB = 657.44 kN

Total dead weight of load, Wload = Wv + Wt + W + WB + Wf + Wsalt + Wi = 1025.58 kN

6.2.13 Winds Load

Wind speed of 160 km/h is used as the preliminary design study, which equivalent to wind
pressure of 1280 N/m2.
Dynamic wind pressure, Pw = 1280 N/m2
Mean diameter of reactor, Dm = 1.427 m
Loading (per linear meter), Fw= Pw x Dm =1826.56 N/m
Bending moment at bottom tangent line, M x =

Fw L2
= 1.14 105 Nm
2

6.2.14 Analysis Stress

Reactor are subjected to various loads such as pressure, dead weight of vessel and contents, wind
and external loads imposed by piping and attached equipment. Thus, it must be designed to
withstand the worst combination of loading without failure. The primary stresses arising from
these loads are calculated as following:

6.2.14.1 Pressure Stress

At bottom tangent line, the longitudinal and circumference stresses due to pressure (internal and
external), given by:
Longitudinal stresses, L =

Po ( IDs )
= 1.96 107 N / m 2 = 19.6 N / mm 2
4ewall

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Chapter 6: Packed Bed Reactor 1
Circumference stresses, h =

Group 6
Acrylic Acid Project

Po ( IDs )
= 3.92 107 N / m 2 = 39.2 N / mm 2
2ewall

6.2.14.2 Dead Weight Stress

The direct stress w is due to the weight of the vessel, its contents, and any attachments. The
stress will be tensile (positive) for point below the plane of the vessel supports and compressive
(negative) for point above the supports.

w =

Wload
= 8.473 106 N / m 2 = 8.47 N / mm 2
( IDs + ewall )ewall

6.2.14.3 Bending Stress

The second moment of area of the vessel about the plane of bending, Iv:

Iv =

64

(ODs 4 IDs 4 ) = 0.0308m 4 = 3.08 1010 mm 4

The bending stress will be compressive or tensile (b), depending on location, and are given by:

b =

M x IDs
(
+ ewall ) = 2.69 106 N / m 2 = 2.69 N / mm 2
Iv 2

6.2.14.4 Resultant Longitudinal Stresses

z = L +w +b
z _ upwind = L + w + b = 30.76 N / mm 2
z _ downwind = L + w b = 25.38 N / mm 2
As there is no torsional shear stress, the principal stress will be z and h. The radial stress is
negligible.
The greatest difference between the principle stresses will be on down-wind.
= h + z _ downwind = 13.82 N / mm 2

which is smaller than design stress, f.

6.2.15 Vessel Support

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The method used to support a vessel will depend on the size, shape and weight of the vessel;
design temperature and pressure; the vessel location and arrangement; and the internal and
external fittings and attachments. Skirt supports are chosen as the supports for the reactor instead
of saddle supports or bracket supports. This is because saddle supports are mainly for horizontal
vessel while bracket supports are not recommended for tall, vertical vessel. Since the reactor is a
tall (11.18m) vertical vessel, skirt supports is more suitable. This supports consist of a cylindrical
shell.

6.2.15.1 Skirt Supports

A skirt support consists of a cylindrical or conical shell welded to the base of the vessel. A flange
at the bottom of the skirt transmits the load to the foundations. It is recommended for vertical
reactor as it does not impose concentrated loads on the reactor shell and they are particularly
suitable for use with tall columns subjected to wind loading. The skirt may be welded to the
bottom head of the vessel or welded flush with shell or welded to the outside of the vessel shell.
The skirt welded flush with shell is usually preferred.
Suggested skirt support height, Lsk = 0.1L=1.118 m (10% of total reactor height)
Skirt thickness, esk = 10mm (the minimum thickness should not be less than 6mm)
6.2.15.2 Total Weight

The maximum dead load on the skirt is when the vessel is full of water, during the hydrostatic
test. Therefore, approximately weight of vessel filled with water.
Wapp =

( IDs ) 2 L w g
4

= 168.83kN

Total dead weight, Wload = 1025.58kN

Total weight, WT = Wload + Wapp = 1194.41kN

6.2.15.3 Bending Stress

Bending moment at base of the skirt, M s =

Bending stress in skirt, bs =

Fw ( L + Lsk ) 2
= 138.13kN / m
2

4M s
= 2.23 106 N / m 2 = 2.23N / mm 2
( IDs + esk )esk ( IDs )

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6.2.15.4 Dead Weight Stress

Dead weight stress in the skirt,

ws _ test =

WT
= 2.70 107 N / m 2 = 27.0 N / mm 2
( IDs + esk )esk

ws _ operating =

Wload
= 2.32 107 N / m 2 = 23.2 N / mm 2
( IDs + esk )esk

6.2.15.5 Tensile Stress

ws _ tensile = bs ws _ operating = 20.97 N / mm 2

Tensile stress give a negative value because the bending moment obtained from wind loading
calculation is very small compare to dead weight and total weight vessel.

6.2.15.6 Compressive Stress

s _ compressive = bs + ws _ test = 29.23 N / mm 2

6.2.16 Criteria for Design

The skirt support is a straight cylindrical vessel (s =90o) of plain carbon steel, design stress, f
(107.5 N/mm2) and Modulus Young, E (200,000 N/mm2) at ambient temperature when Welded
Joint Efficiency, J is 1.
Table 6.24: Criteria For Design

Criteria 1
2

Criteria 2

s_tensile = -20.97 N/mm

f x J x sin (s) = 107.5 N/mm2

s_compressive =29.23 N/mm2

0.125E(esk / IDs)sin (s) = 178.57 N/mm2

s_tensile <f x J x sin (s)

s_compressive <0.125E(esk / IDs)sin (s)

Criteria 1 is satisfied

Criteria 2 is satisfied

Both design criteria are satisfied, adding the 2 mm corrosion allowance, the skirt thickness is
taken as 12 mm.

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6.2.17 Summary of Mechanical Design of Reactor 1

Table 6.25: Summary of Mechanical Design of Reactor 1

Parameter

Value

Design pressure, PD

1.54 bar

Design temperature, TD

275oC

Material of construction

Austenitic stainless steel type 304

Design stress, f

107.5 N/mm2

Welded joint efficiency, J

1.0

Corrosion allowance, eallowance

2.0 mm

Wall thickness, ewall

0.027 m

Type of closure

Ellipsoidal head

Head thickness, ehead_new

0.027 m

Manhole
Min diameter

575 mm

Max length

500 mm

Thickness of Compensation for Opening

Feed

0.047 m

Molten salt (heating medium)

0.041 m

Dead Weight Load

Shell, Wv

205.09 kN

Tube, Wt

438.13 kN

Catalyst, W

30.61 kN

Baffle, WB

14.22 kN

Feed, Wf

1.13 kN

Molten salt, Wsalt

333.99 kN

Insulation, Wi

2.41 kN

Total dead weight of reactor, Wreactor

657.44 kN

Total dead weight load, Wload

1025.58 kN

Wind loads

1.14 x 105 Nm

Skirt Supports
Type

Cylindrical

Thickness of skirt

12 mm

Skirt support height

1.118 m

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

Figure 6.9: Detail A of Mechanical Drawing

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Chapter 6: Packed Bed Reactor 1

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Acrylic Acid Project

6.3 Safety and Process Control of Reactor 1

6.3.1 Safety Consideration
Results from a kinetic and process optimization study may indicate operating conditions that are
unsafe from the view point of fire safety, equipment damage potential and operating sensitivity.
The design of the plant should be such that the gas mixtures handled are always outside the
explosive limit. The actual safe operating ranges are dependent on operating temperatures,
pressures, equipment configurations, gas compositions, ignition sources present, and the
dynamics of the catalyst, process and instrumentation system.

6.3.1.1 Safety Review

The principle causes incidents which may occur in industry are:
a. Scale-up Failure
Failure to scale-up properly and to take appropriate precautions may lead to the loss of
process control. Hence, runaway endothermic reaction and generation of toxic materials
in the reactor can occur. These failures may lead to multiple fatalities, severe damage to
property, environmental damage and business loss. Thus, the first and most critical step
in the scale-up procedure is to undertake a risk assessment of the proposed chemical
process at the concept stage which should include a study of thermo chemistry of the
proposed reaction.
b. Mechanical Impact (Stress Failure)
Stress failure normally occurs due to the metals are subjected to repeated stress exceeding
their limit. Excessive stresses can develop in vessels that are not free to expand and
contracted with temperature changes. If the stresses are allowed to recur too frequently,
eventually failure from fatigue can be expected. Hence, the maximum allowable stresses
must be identified for a reactor design and all possibility sources of stress must take into
account. Over-designing is not encouraged, but under design would lead to accident and
fatality.
c. Human Error
Incorrect operating procedures conducted by the operators may cause severe damage and
consequences to the plant properties. Reactor operated by non-technically qualified and
inappropriately trained competent personnel is actually placing the plant into high disk

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condition. Wrong specification will not only affect the reaction output and decrease the
overall yield but most importantly, it will cause fire and explosion if the equipment is not
properly handled. The extra unknown or unforeseen hazards associated with the pilot
plant should be compensated for by better instrumentation and technical control by the
operators.
d. Poor Maintenance of Safety Device
Protective devices such as safety valves and any electronic devices which cause
shutdown when the pressure, temperature, liquid or gas level exceed permissible limits
fail to protect the equipment if they are not properly installed to the vessels, or pipe work
according to the correct setting. Safety devices which are in poor condition are unable to
give clear warning or signal to the operator either by sight or sound during emergency.
Thus, prompt action cannot be taken by operator to overcome the situations. Improper
functioning can result in disaster both to life and equipment. All safety devices should be
tested regularly by an authorized person according to the schedule set.

6.3.1.2 Reactor Potential Hazards

Reactor should be operating under its design condition. It may function outside its normal design
limits and could cause certain potential hazards. Accident hazards for a reactor can be listed
under fires, explosion, leakage, toxic release, mechanical impact and exposure to extremely hot
corrosive materials. Reactor is a major source of hazard because it contains large amount of
flammable material. There also could be some hot spots in the reactor and it occurs when heat
exchanger does not functioning well due to dirt accumulation. This situation is likely to cause
fire or explosion. Sudden releases of certain material such as acrolein which is toxic to human
beings.

6.3.1.3 Reactor Safety Practices

Precautions must be taken to prevent accident that may lead to injuries or fatalities. Before the
operation is carried out, it is important to study the thermal effect of the reaction of the reactor,
the catalyst behavior and materials handling procedures for safety operating limit and control.
Safety devices can be installed on the vessel to reduce the temperature and pressure deviation

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from the reactor such as sensor, vent system, safety valve, bursting discs, alarm and indicator.
Most importantly is to ensure that all the safety devices in are properly maintained.

6.3.2 Hazard and Operability Studies (HAZOP) Analysis

HAZOP analysis is a set of formal hazard identification and elimination procedure designed to
identify hazards to people, process plants and environment in a chemical process facility. It uses
a systematic process to identify all possible deviations from normal operations and to ensure that
appropriate safeguards are in place to help for preventing accidents. It is essentially a qualitative
process.

6.3.2.1 Objectives of HAZOP

HAZOP is carried out to ensure the overall safety of the reactor and to prevent the errors or
problems that could occur as show at the previous part. HAZOP is done:
a. To examine the inadequacies of the reactor by considering it as a fully integrated
dynamic unit, rather than the ad hoc design approach.
b. To coordinate the various discipline involved in the design of the reactor and provide a
mean for systematic analysis of the reactor system.
c. To identify hazards or deficiency and operability problem that may occur in the reactor,
which may lead to hazard such as fire, explosion, toxic release or reduce productivity.
d. To prevent hazards in process plants that is growing in complexity with standards that are
no longer adequate.

6.3.2.2 HAZOP Procedures

The HAZOP is done by systematically examine the reactor design and asking questions using
guide words representing deviations from the intended parameters of the process. A Process and
Instrumentation Diagram (PID) is developed by referring to the HAZOP analysis which is shown
in Figure 3.1.

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Table 6.26: HAZOP Analysis on Packed Bed Reactor 1 Streamline 5

HAZARD AND OPERABILITY STUDY ACTION REPORT

Prepared by: Jackson Toh
Equipment: Acrolein Packed Bed Reactor
Line No: 5
Intention: Transfer of Glycerol feed at 275oC and 1.4 bar into the reactor
Type of
Guide
Possible Causes
Consequences
Deviation
Word
Flow
(A)
(B)
No
1.1 Major piping leakage and 2.1 No flow of feed into the reactor
poor pipe connection
2.2 No reaction occur in the reactor
1.2 Piping blockage due to
2.3 High pressure in pipeline
impurities
1.3 Feed (FIC 1) controller
failure
1.4 Blockage of valve (V102)

Temperature

Less

(D)
1.1 Partial piping blockage
1.2 Minor pipe leakage

More

(G)
1.1 Shutdown system failure
1.2 Operator error
- Incorrect specification
and amount of process
fluid charge

Less

(J)

(E)
2.1 Less flow of feed into the
reactor
2.2 Reactor under filling
2.3 Runaway reaction may occur
2.4 Product yield decrease
(H)
2.1 Reactor overfilling
2.2 Pipeline overpressure
2.3 High temperature in the reactor
2.4 As (E): 2.3 2.4
2.5 Rupture in the reactor
2.6 Potential fire and explosion
hazard
(K)

Actions
(C)
3.1 Regularly inspection and
maintenance for FIC1 and V-102
3.2 Check for piping connection
3.3 Install analyzers to detect
leakage
3.4 Install no flow alarm
3.5 Install pressure safety valve
(PRV)
(F)
3.1 As for (C): 3.1 3.3
3.2 Install low flow alarm

(I)
3.1 Install flow indicator and
controller (FIC1)
3.2 Install control valve (V-102)
3.4 Prepare a checklist for
operator

(L)

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KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

More

Pressure

Less

More

Contamination High

Group 6
Acrylic Acid Project

1.1 Heat loss

1.2 Temperature indicator
(TIC1) is failure
1.3 Changes in ambient
temperature
1.4 Input flow rate is too low
1.5 Heating system failure in
the reactor
(M)
1.1 High ambient temperature
1.2 Input flow rate is too high
1.3 External heat source
1.4 More heating medium
inflow
1.5 Increase in pressure
1.6 Higher heat transfer in the
reactor
(P)
1.1 Pressure indicator (PIC1)
failure
1.2 External cooling
1.3 Undetectable leakage

2.1 Decrease in reaction temperature

2.2 Incomplete reaction in the
reactor
2.3 Decrease product yield
2.4 Phase change of substances
2.5 Poor heating effect in the
reactor

3.1 Install low temperature alarm

(TAH & TAL)
3.2 Install temperature indicator
(TIC1)

(N)
2.1 Increase in reaction temperature
2.3 As for (H): 2.3 2.6

(S)
1.1 Under cooling in the
reactor
1.2 Imbalance of input and
output
1.3 Exposure to heat source
1.4 Thermal shock

(T)
2.1 Pipe surging
2.2 As for (H): 2.1 2.6

(V)
1.1 Feed source contaminated

(W)
2.1 Possible poisoning the catalyst

(O)
3.1 Isolation from external heat
and ignition source
3.2 Install temperature indicator
(TIC1)
3.3 Install high temperature alarm
(TAH)
3.4 Regularly maintenance of the
reactor
(R)
3.1 Install low pressure alarm
(PAL)
3.2 Install pressure indicator
(PIC1)
3.3 As for (C): 3.1 3.3
(U)
3.1 Install high pressure alarm
(PAH)
3.2 Install pressure gauge
3.3 Install fire alarm and explosion
relief (FER)
3.4 As for (O): 3.1
3.5 As for (I): 3.4
(X)
3.1 As for (O): 3.3 3.4

(Q)
2.1 Poor heat transfer in the reactor
2.2 As for (E): 2.1 2.4

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2.2 Unexpected reaction
2.3 As for (H): 2.3 2.6
Table 6.27: HAZOP Analysis on Packed Bed Reactor 1 Streamline 6

HAZARD AND OPERABILITY STUDY ACTION REPORT

Prepared by: Jackson Toh
Equipment: Acrolein Packed Bed Reactor
Line No: 6
Intention: Transfer of acrolein product out from the reactor
Type of
Guide
Possible Causes
Consequences
Deviation
Word
1.1 As for (A): 1.1 1.2
2.1 Pipeline under pressure
Flow
No
1.2 Equipment and flange
2.2 No feed to collecting column
failure
2.3 As for (H): 2.3 2.6
1.3 No flow to reactor
1.1 As for (D): 1.1 1.3
2.1 Collecting column under filling
Less
2.2 Pipeline under pressure
2.3 As for (H): 2.3 2.6
1.2 As for (G): 1.2 1.3
2.1 Collecting column may rupture
More
2.2 Pipeline overpressure
2.3 Vapor cloud explosion may occur
1.1 As for (J): 1.2 1.3
2.1 Change condition in collecting
Temperature
Less
1.2 Heating system failure in
column
the reactor
2.2 Phase change of substances
- poor heat transfer
2.3 Poor heating effect in the reactor
- heating medium failure
1.1 As for (M): 1.1 1.3
2.1 Over heating effect in the reactor
More
1.2 Heating system failure in
2.2 Fouling
the reactor
2.3 Injuries and fatalities
- overheating from the molten
2.4 As for (H): 2.3 2.6
salt
1.1 As for (P): 1.1 1.3
2.1 Under filling in collecting column
Pressure
Less
1.2 Generation of vacuum
2.2 Additional pump is needed to

Actions
3.1 Install flow indicator (FI1)
3.2 As for C: 3.1 3.5

3.1 As for (F): 3.1 3.3

3.1 As for (I): 3.1 3.4

3.1 As for (L): 3.1 3.2

3.2 Provide accurate temperature
monitoring in the reactor
3.3 Ensure the heating system
function well
3.1 As for (O): 3.1 3.3
3.2 Regularly maintenance of the
reactor heating system

3.1 As for (L): 3.1 3.2

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Acrylic Acid Project

condition

More

1.1 Uncontrolled reaction in

reactor
1.2 Pressure relief valve (PRV)
failure
1.3 overfilling in the reactor
1.4 As for (S): 1.2 1.4

increase the pressure of product to

collecting column
2.1 Pipe surging
2.2 Overfilling in collecting column
2.3 Overpressure in collecting system
2.2 As for (H): 2.3 2.6

3.1 As for (U): 3.1 3.4

3.2 Install pressure indicator (PI1)

Table 6.28: HAZOP Analysis on Packed Bed Reactor 1 Streamline H_1

HAZARD AND OPERABILITY STUDY ACTION REPORT

Prepared by: Jackson Toh
Equipment: Acrolein Packed Bed Reactor
Line No: H_1
Intention: Transfer of hot molten salt into the reactor
Type of
Guide
Possible Causes
Consequences
Deviation
Word
Flow
1.1 As for (A): 1.1 1.3
2.1 No hot molten salt flow into the
No
1.2 Equipment and flange
reactor
failure
2.2 No heat transfer takes place
2.3 As for (K): 2.1-2.5

More

1.1 As for (D): 1.1 1.3

1.2 Fouling in the reactor
1.1 As for (G): 1.1 1.2

Temperature

Less

1.1 As for (J): 1.1 1.4

Pressure

More
Less

1.1 As for (M): 1.1 1.3

1.1 Reverse heating flow
1.2 As for (P): 1.1 1.3

Less

Actions
3.1 As for (L): 3.1 3.2

2.1 As for (K): 2.1-2.5

3.1 As for (F): 3.1 3.3

2.1 Improper heating in the reactor

2.2 Pipeline overpressure
2.3 Possible runaway on heating
2.1 Poor heat transfer in the
reactor
2.1 As for (N): 2.1 2.3
2.1 Reverse flow in the reactor
2.2 Accumulation of hot molten salt

3.1 As for (I): 3.1 3.4

3.1 As for (L): 3.1 3.2

3.1 As for (O): 3.1 3.3
3.1 As for (R): 3.1 3.3

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KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

More

Group 6
Acrylic Acid Project

1.1 Overfilling of hot molten

salt
1.2 Pressure relief valve
failure

in the reactor
2.3 Fouling
2.4 Blockage
2.5 Poor heat transfer in the reactor
2.1 As for (T): 2.1 2.2

3.1 As for (U): 3.1 3.5

Table 6.29: HAZOP Analysis on Packed Bed Reactor 1 Streamline H_2

HAZARD AND OPERABILITY STUDY ACTION REPORT

Prepared by: Jackson Toh
Equipment: Acrolein Packed Bed Reactor
Line No: H_1
Intention: Transfer of hot molten salt out from the reactor
Type of
Guide
Possible Causes
Consequences
Deviation
Word
Flow
1.1 As for (A): 1.1 1.3
2.1 High pressure in the reactor
No
1.2 No flow into pump P-108 2.1 As for (H): 2.3-2.6
Less

More

Temperature

Less
More

1.1 As for (D): 1.1 1.3

1.2 Fouling in the reactor
1.3 Accumulation of hot
molten salt in the reactor
1.1 Incorrect specification of
hot molten salt charged

1.1 As for (J): 1.1 1.3

1.2 Poor heating effect
1.1 As for (M): 1.1 1.3
1.2 Fouling

Actions
3.1 As for (C): 3.1 3.5

2.1 As for (N): 2.1-2.3

3.1 As for (F): 3.1 3.3

2.1 Pipeline overpressure

2.3 Corrosion and erosion
2.3 Reverse flow due to incorrect
pressure different
2.1 As for (H): 2.3 2.6

3.1 As for (I): 3.1 3.4

2.1 Overpressure in the reactor

2.2 Loss control of reaction rate in

3.1 As for (O): 3.1 3.3

3.2 Regularly maintenance of the

3.1 As for (L): 3.1 3.3

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KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Pressure

Less

More

1.3 Low reaction rate in the

reactor
1.5 Low pressure in the
reactor
1.1 Generation of vacuum
condition
1.2 As for (P): 1.1 1.3
1.1 Overpressure in the
reactor
1.2 Uncontrolled reaction in
the reactor
1.3 Pressure relief valve
failure
1.4 As for (S): 1.3 1.4

Group 6
Acrylic Acid Project
the reactor
2.3 Effect the final productivity

reactor heating system

2.1 Poor heat transfer in the reactor

3.1 As for (R): 3.1 3.3

2.1 Overfilling of heating medium

2.2 As for (H): 2.2 2.6

3.1 As for (U): 3.1 3.5

6- 44

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

6.3.3 Process Control and Instrumentation

A control system is designed for glycerol dehydration reactor to minimize down time,
eliminating disturbance that tend to change operating conditions, compositions, and physical
properties of the streams and also prevent quality loss and hazard in the process. The automatic
control system is designed and all the data and signal are sent to control room for supervision.

6.3.3.1 Description of Instruments

Table 6.30: Description of Instrument

Symbol
FIC

Description
Flow Indicator Controller
Measure the flow rate of particular stream, send the data signal to control
room and control valve for regulating the flow rate

PIC/TIC

Pressure/ Temperature Indicator Controller

Measure the pressure/ temperature of particular stream or reactor, send the
data signal to control room and control valve for regulating the flow rate

FT/PT/TT

Flow/ Pressure/ Temperature Transmitter

Measure the flow rate/ pressure/ temperature of particular stream or reactor
and send the data signal to controller for control action

FI

Flow/ Pressure/ Temperature Indicator

Measure the flow rate/ pressure/ temperature of particular stream and send
the data signal to control room

CV

Control Valve
Control the flow rate of particular stream after receiving data signal from
controller

PRV

Pressure Relief Valve

Relief the pressure of reactor when the pressure of the reactor greater than
the set pressure

6.3.3.2 Description of Control System

6.3.3.2.1 Inlet Feed Temperature Control
Table 6.31: Description of Inlet Feed Temperature Control

Type of Control System

Feed back temperature control

Measured Variable

Inlet feed temperature

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KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

Manipulated Variable

Inlet heating molten salt flow for heat exchanger E-107

Control Action

Control the molten salt flow rate by regulating control valve, CV101

Set Point

275oC
If the temperature of the inlet feed appears to be +-10% of set point,
temperature high/low alarm will be activated.

6.3.3.2.2 Inlet Feed Flow and Pressure Control

Table 6.32: Description of Inlet Feed Flow and Temperature Control

Type of Control System

Measured Variable
Manipulated Variable
Control Action

Set Point

Cascade pressure control

Primary loop: Reactor pressure
Secondary loop: Inlet feed flow rate
Inlet feed flow rate
Secondary loop: Flow controller
Control the inlet feed flow rate by regulating control valve CV102
Primary loop: Pressure controller
Maintain the reactor pressure by regulating the inlet feed flow rate
1.4 bar
If the pressure of the reactor appears to be +-10% of set point,
pressure high/low alarm will be activated.

6.3.3.2.3 Molten Salt (Heating Stream) Temperature Control

Table 6.33: Description of Molten Salt Temperature Control

Type of Control System

Measured Variable
Manipulated Variable
Control Action

Set Point

Cascade temperature control

Primary loop: Reactor temperature
Secondary loop: Molten salt flow rate
Molten salt flow rate
Secondary loop: Flow controller
Control the molten salt flow rate by regulating control valve CV103
Primary loop: Temperature controller
Maintain the reactor temperature by regulating the inlet flow rate of
molten salt
275oC
If the temperature of the reactor appears to be +-10% of set point,
temperature high/low alarm will be activated.

6- 46

Acrylic Acid Production Plant

Reactor 1

FI 1

TI 1

PI 1

PRODUCT

FI 2

Symbol

Description

FT

Flow Transmitter

TT

Temperature Transmitter

PT

Pressure Transmitter

FIC

Flow Indicator Control

TIC

Temperature Indicator Control

PIC

Pressure Indicator Control

FI

Flow Indicator

TI

Temperature Indicator

PI

Pressure Indicator

TAH

Temperature Alarm High

TAL

Temperature Alarm Low

PAH

Pressure Alarm High

PAL

Pressure Alarm Low

TI 2

MOLTEN
SALT

TT 2

TAH
TIC 2

TAL

PT 1

FT 2

PAH
PIC 1

FIC2

TO STACK

TAH
PAL
TT 1

TIC 1

V-103
TAL

FIC 1

FT 1

SET
30 PSI

Reactor 1

P-101

HOT
MOLTEN
SALT

PRV

HOT
MOLTEN
SALT

MOLTEN
SALT

V-101

V-102
E-107

PRV

GLYCEROL
FEED

Pressure Relief Valve

Control Valve
ACRYLIC ACID PRODUCTION PLANT
GLYCEROL DEHYDRATION PLANT
(REACTOR 1)

Drawn By

Dwg No

Jackson
A138-112
Rev: 0

Figure 6.10: PID of Reactor 1

47
Chemical Engineering Department
UniversityofMalaya

KKEK 4281 Design Project

Chapter 6: Packed Bed Reactor 1

Group 6
Acrylic Acid Project

6.4 Reference
1. Hanan Atia, Udo Armbruster, Andreas Martin, Dehydration of glycerol in gas phase
using heteropolyacid catalysts as active compounds, 29 May 2008
2. http://www.coastalchem.com/PDFs/HITECSALT/HITEC%20Heat%20Transfer%20Salt.
pdf
3. Kern, D.Q. (1986). Process Heat Transfer. (International Student Edition). USA:
McGraw-Hill Ltd.
4. Masaru Watanabe, Toru Iida, Yuichi Aizawa, Taku M. Aida, Hiroshi Inomata, Acrolein
synthesis from glycerol in hot-compressed water, 4 May 2006
5. Smith, J.M. (1981). Chemical Engineering Kinetics. (3rd Edition). McGraw-Hill Book
Company.
6. Howard, J.R.(1989). Fluidized Bed Technology: Principle and Application. Adam Hilger.
7. Perry, R.H. & Green, D. (Ed.). (1997). Perrys Chemical Engineers Handbook. (7th ed.).
McGraw-Hill International edition.
8. Sinnott, R.K. (1999). Coulson & Richardsons Chemical Engineering Design Volume 6.
(3rd edition). Pergamon Press.
9. Farr, J.R. & Jawad, M.H. (1998). Guidebook For The Design of ASME Section VIII
Pressure Vessel. ASME Press, New York.
10. Crowl, D.A. & Louvar, J.F. (1990). Chemical Process Safety Fundamentals with
Application. Prentice Hall.
11. Coughanowr, D.R. (1991). Process System Analysis and Control. (2nd edition). McGraw-Hill Inc.

6- 48

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

CHAPTER 7: PACKED BED REACTOR 2

7.1. Chemical Design of Reactor 2
7.1.0 Introduction
7.1.0.1 Vapour Phase Oxidation of Propylene and Acrolein
From the earlier discoveries, during the late 1950s, of effective solid catalysts for the
vapour phase oxidation of acrolein to acrylic acid were probably incidental to study of
catalysts intended for the oxidation of propylene to acrolein (Hancock). That is to say that
acrylic acid was observed as a significant reaction product, and the natural assumption
readily confirmed by experiment. Widespread interest was aroused, that the acrylic acid
was derived from acrolein.
7.1.0.2 Objective
The objective is to design the reactor for production of acrylic acid from acrolein. The
plant produces 70,000 tonne of acrylic acid per year. It operates 24 hours for 330 days.
Oxidation of acrolein in reactor will produce acrylic acid as main product where acetic
acid as by product. The catalyst use is metallic salt components of the catalyst which
including molybdate, vanadate and tungstate. It is dissolved in the water and is in solid
phase.
7.1.0.3 Reactor Selection
The reaction scheme defines the way that the reactants are converted to products, and
additional rules can encode the related knowledge to produce synthetically feasible
molecules. Good reactor performance is important in determining the economic viability
of the overall design. Packed bed reactor is the first choice in economical production of
large amount of product. It is tubular and is filled with solid catalyst particles, most often
used to catalyzed gas reaction. It is preferred that the reactants flow upwards through the
reactor as this provides good mixing.

[1]

Packed bed reactor used primarily in

heterogeneous gas phase reactions with catalyst as it promotes advantages of high

conversion per unit mass of catalyst, lower operating cost, and continuous production.
Both packed bed reactor and fluidized bed reactor are designed and better one is chosen.
The oxidation reaction is an exothermic reaction. Thus, the packed bed reactor is
7-1

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

preferred constructed in shell and tubes, where the heat can easily be transferred to
maintain the conversion. The Mo10 W2 V3.5 Cu2 Sr0.8 catalyst was packed inside the tubes
side, where the cooling water is chosen as cooling fluid in shell side. (Refer to Chapter
1.6. for fluidized bed reactor design)

7.1.1 Process Description

In the packed bed reactor, acrolein is oxidized to form acrylic acid via heterogeneous
catalytic exothermic reaction. The catalyst used is Mo10 W2 V3.5 Cu2 Sr

0.8.

The

temperature of the reactor is maintained at 260oC by using cooling water. The pressure of
the reactor is set at 2 bars. The volume percentage of acrolein, oxygen, nitrogen and
water vapour fed to reactor is 10%, 16%, 64% and 10% respectively.[2] Steam is added as
inert gas to control the rate of the reaction. Air is supplied to provide the oxygen required
for the oxidation reaction. The nitrogen consists in air will act as an inert to control the
reaction. The gaseous product stream consists of air, water vapour, acrylic acid and acetic
acid which is a by product of the reaction, air and water vapour.
7.1.1.1 Feed Stream Condition
Table 7.1: Initial Condition of Feed Stream Reactant

Reactants

Mole Flow (kmol/hr)

Mass Flow (kg/hr)

Acrolein
Oxygen
Nitrogen
Water
Acetol

134.17
215.41
810.52
165.52
0.1308

7522.2
6893.1
22705
2981.8
9.6937

The total volumetric flow rate, of the feed stream is 46.1218 m3/ hr.
7.1.1.2 Properties of Feed Stream and Cooling Stream
Cooling water is chosen as the cooling stream because it is economical and available in
large amount. All properties of the cooling water at 25C and 1 atm is taken. Where,
properties of the feed stream are taken from the Hysys simulation. The physical and
chemical properties of both cooling and feed stream are important to determine the heat
transfer coefficient (h) and pressure drop (P).
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KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

Table 7.2: Properties of Feed Stream and Cooling Stream

Properties

Feed Stream

Cooling Water

Inlet Temperature (K)

533

298

Outlet Temperature (K)

533

323

Pressure (atm)

1.97

1.00

1.365

Density (kg/m )

2.55710

Viscosity (Pa.s)

997.050
-5

8.90910-4

Thermal conductivity
(W/m.K)

0.040

0.610

Heat capacity (kJ/kg.K)

1.253

4.201

7.1.1.3 Properties of Catalyst

The catalyst use is metallic salt components of the catalyst including molybdate, vanadate
and tungstate are dissolved in the water and it is in solid phase, Mo10 W2 V3.5 Cu2 Sr 0.8.
Table 7.3: Properties of Catalyst

Properties
Catalyst density, p (kg/m3)
Solid particle diameter, dp (m)
Catalyst porosity, p

5500
510-3
0.50

7.1.2 Process Principle

The purity of crude glycerol obtained from biodiesel plant is 88% purity. [3] Production of
acrylic acid from glycerol is by two process routes. First, crude glycerol (C3H8O3) is
dehydrated to acrolein (C3H4O) via acetol (C3H6O2) as intermediate (under heterogeneous
catalytic reaction. Acrolein is then oxidized to form acrylic acid in packed bed reactor
(Equation 1.1) via heterogeneous catalytic reaction. The reaction is exothermic. Acetic
acid will form as the major by product for the process (Equation 1.2).
7.1.2.1 Proposed Reaction Scheme for Oxidation of Acrylic Acid

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Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

Reaction 1: Formation of Acrylic Acid

1
O
2

C H O

C H O

Equation 7.1

Reaction 2: Formation of Acetic Acid

3
O
2

C H O

C H O

CO

Equation 7.2

Reaction rate:
kCA CB

rA

Equation 7.3

Reactants concentration:

CA

CA

CB

CA

0.5X
X

Equation 7.3.1

T
T

P
P

Equation 7.3.2

Where
CA

AO F
M .

AO

7.1.3 Chemical Design

7.1.3.1 Kinetic Parameter
The rate constant can determined by using Arrhenius Law and the rate constant are
expressed as
k

A e

E
RT

Equation 7.4

where the Ao is the pre exponential factor and E is the activation energy. [4]

Table 7.4: Kinetic Parameter for Oxidation of Acrolein

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KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project
Oxidation of Acrolein

Ao (mol/kg.hr.Pa3/2)
E (J/mol)
R (J/mol.K)

10.8
83678.51
8.314
6.80

k(
.

10

7.1.3.2 Assumptions
Assumptions are made for design of packed bed reactor.

Steady state condition.

No side reactions.

The reaction is an elementary reaction with the reaction-rate limiting step.

Conversion of the acrolein to acrylic acid is 98%.

The reactor contents are well mixed.

Isothermal operation since heat transfer limitations is negligible.

Physical and chemical properties are remaining constant.

Deactivation of the catalyst can be neglected under the reaction temperature.

7.1.3.3 Catalyst Weight and Pressure Drop

Based on the packed bed reactor design equation, the catalyst weight, W required can be
calculated:
dFA
dW
FA

X
W

rA

Equation 7.5

rA

Equation 7.5.1

By using MATLAB, both ordinary derivative of packed bed reactor design equation and
Ergun equation are solved simultaneously. (Appendix Figure A-1) The catalyst weight
and the pressure difference required for the reaction were obtained with X = 0.98.
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KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

Table 7.5: Determination of Catalyst Weight and Pressure Drop

dX
dW

rA

yA P
FA

Packed Bed
Reactor
Design
Equation:

dX
dW

Ergun
Equation:

dy
dx

G
g D

dP
dz

FA

dy
dW

1
2y

y
P

P T
P TO

A 1

Pressure
Drop:

PO

X
1

0.5X

150 1
D

1.75G

FT
FTO

Equation 7.5.2

Equation 7.6

Equation 7.6.1

P T
P TO

FT
FTO

Equation 7.6.2

Equation 7.6.3

0.98

0.98 200kPa

38000 kg

1.5

dP
dW

Weight of
catalyst:

196 kPa

4kPa

7.1.3.4 Reactor Sizes

Table 7.6: Determination of Reactor Sizes

7-6

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

Volume
Volume of Catalyst

Equation 7.7

6.91 m

13.80 m

27.60 m

Total Volume of Tubes

Volume of Reactor

Equation 7.7.1

Equation 7.7.2

7.1.3.5 Tube Size Selection

The stainless steel pipe with 2.5 in. normal pipe size (40S) 10 m length is selected.
Table 7.7: Properties of Pipe

Unit SI
40S
2.500 in
2.880 in
0.203 in
2.469 in
4.788 in2

Schedule number
Nominal pipe size
Outside diameter, do
Wall thickness, t
Inside diameter, di
Cross sectional area, Ac

0.0635 m
0.0732 m
0.0052 m
0.0627 m
0.0031 m2

7.1.3.6 Number of Tubes

Number of Tubes Required

V
A L

27.6
0.003089

10

895 tubes

7.1.3.7 Number of Tubes Passes

7-7

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

To provide good heat transfer of the tubes side, the flow condition of the tube should be
maintained at turbulent flow.
NR
N

Ud
1

2100

Vd
NA 1

N
895

2100

0.00309
1
1.365 4.147

0.5
2.557
0.0627

10

0.2092

Thus, minimum number of passes for turbulence flow is 1 pass.

7.1.3.8 Tube Pitch and Buddle Diameter

The triangular pattern for the tubes arrangement is chosen because it allow higher heat
transfer rate. It is essential in order to operate the reactor in isothermal condition. The
recommended tube pitch (distance between tube centres) is 1.25 times the tube outside
diameter. [5]
Tube Pitch
Bundle Diameter

1.25d
1.25 0.073152 0.091m
N /
895
.
d
0.073152
2.978 m
D
K
0.319
The dimensionless constant, K1 = 0.319 and n1 = 2.142 for a
triangular pitch with single shell pass and 1 tube passes.
(Appendix Figure A-3)

7.1.3.9 Shell Inside Diameter

For a fixed tube heat exchanger with 2.978 m bundle diameter, bundle diameter clearance
= 35.1745 mm. [5]
Shell Inside Diameter

Ds = 2.978+ 0.0351745= 3.013 m

7.1.3.10 Baffles
Baffles are used in the shell to direct the cooling fluid across the tubes, to increase the
fluid velocity and improve the rate of transfer. Single segmented baffle is selected
because it is the most commonly used type of baffle. The optimum baffle cut is 20% to
7-8

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

25%. The common baffle thickness, tb is 0.005 m. The optimum spacing, lB is usually
between 0.3 to 0.5 times the shell diameters. [5]
Table 7.8: Specifications of Baffles

Optimum Baffle Cut

20% to 25%

Baffle Thickness

0.005m

Spacing between Shell Diameter Optimum spacing usually between 0.3 to 0.5 times
the shell diameter [5].
Thus, value of 0.5 is chosen.
Baffle Spacing
Number of Baffles Required

Actual Baffle Spacing

0.3 DS

0.3 3.013

NB

L
B

10
0.904

lB

1
L

NB

10
11 1

0.904m
10.06

11

0.833m

7.1.4. Cooling stream requirement

The tube-side heat transfer coefficient, ht, shell-side heat transfer coefficient, hs, and
overall heat coefficient, Uo need to be determined to ensure effective the heat transfer
between the catalyst bed and the cooling water at the shell-side.
7.1.4.1 Log Mean Temperature Difference
Log Mean Temperature Difference LMTD

T
T
T

222.27K

7.1.4.2 Cooling Water Flow

From the energy balance for the isothermal reactor, the heat released from the reactor, Q
was found to be 3744 kJ/hr.

7-9

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project
m

Cooling Water Flow Rate

Q
C T

35.77kg/s

7.1.4.3 Tube Side Heat Transfer Coefficient

In the tube side of the reactor, the reactants flow through the voidage of catalyst bed.
Total flow area, Ac = 0.0031 m3.
Table 7.9: Determination of Tube Side Heat Transfer Coefficient

Mass Velocity

Reynolds
Number

Re

Prandtl Number

Heat Transfer
Factor
Heat Transfer
Coefficient

Pr

4.030kg
m .s

W
NA

G. d
1
C

19769 turbulent flow

0.0245

By taking account the ratio of L/D and Reynolds number of 19769,

jh=0.0025 [Appendix Figure A-4]
h

j . Re. Pr
d

.k

9.181W. m . K

7.1.4.4 Shell Side Heat Transfer Coefficient

Heat released from the reaction (exothermic reaction) is transferred by cooling water at
the shell side.
Table 7.10: Determination of Shell Side Heat Transfer Coefficient

Cross
Flow Area

Mass
Velocity

m
A

d D . lB
P

0.4923m

72.66kg. m . s

7-10

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2
Equivalent
D
Diameter
Reynolds
Number

Re

Prandtl
Number

Pr

1.10
P
d
D G

Group 6
Acrylic Acid Project

0.917d

0.0507m

4138 (Turbulent Flow)

C , .
k

6.115

By taking account the 25 percent of baffle cuts and Reynolds number of

4138,

Heat
Transfer
Factor

jh=0.023 [Appendix Figure A-5]

Heat
Transfer
Coefficient

j . Re. Pr
D

.k

2081.38W. m . K

7.1.4.5 Overall Heat Transfer Coefficient

Table 7.11: Determination of Overall Heat Transfer Coefficient

Thermal Conductivity of Stainless Steel

21W.m-2.K-1

Fouling Coefficient :
Rection mixture (heavy hydrocarbon) 2000W.m-2.K-1
6000W.m-2.K-1

Cooling water (tower)

Overall Heat Transfer Coefficient:
1
h

d
d
2k

d ln

1
U

1
h

513.61W. m . K

d 1
d h

d 1
d h

0.00195

7-11

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

7.1.4.6 Heat Transfer Area Required

Required

Heat Transfer Area

Available

Heat Transfer Area

N. .

d
2

.L

37.62m

Heat transfer surface area available is larger than the heat transfer surface area required.
Thus, cooling system is sufficient to meet the cooling requirement.

7.1.5. Pressure Drop

7.1.5.1 Tube Side Pressure Drop
Ergun equation used to calculate pressure drop in a packed porous bed.
dP
dz

G
g D

dP
NL
dz

150 1
D

17565 1 10

Percentage of pressure drop

1.75G

17.565Pa/m

1.7565kPa
1.7565
200

100%

0.88%

7.1.6.7 Shell Side Pressure Drop

By taking account the 25 percent of baffle cuts and Reynolds number of 4138, the friction
number, jf =0.023 [Sinnott, 1986].
Shell Side Pressure Drop P

8j

3.78kPa

7-12

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Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

7.1.6. fluidized bed reactor

Refer to Figure A-2 for design procedures of fluidized bed reactor.

Figure 7.1: Fluidized Bed Reactor

7.1.6.1 Minimum Fluidization Superficial Velocity, vsfm

Minimum
v
Fluidization
Superficial
v
Velocity

33.7
2.557 10
0.005 1.365

3.6

10

5500

1.365
1.365
2.557 10

0.005

9.81

2.719m/s

7.1.6.2 Minimum Bubbling Velocity, vmb

Applying Abrahamsen and Geldart correlation:
v

2.07exp 0.716F

4.885m/s

Minimum Bubbling Velocity

d
.

7-13

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

vmb > vsfm, thus bubbles are constantly splitting and coalescing, and a maximum stable
bubble size is achieved. This makes for good quality, smooth fluidization.
7.1.6.3 Terminal Velocity, ut
To avoid excessive particle carryover, the fluidization operation must be conducted in
such a way that: vsfm < vsf < ut. In practice, it has been observed that the ratio

ut
is
vsfm

between 10 (small particle) and 90 (large particle). Since the catalyst particle size is
500m, which is intermediate size, thus ratio of 50 is chosen.

50

2.719

135.95m/s

7.1.6.4 Superficial velocity, vsf

Operations are usually conducted with a superficial velocity, vsf 5 to 10 times higher than
vsfm:
5

v
v

10

7.1.6.5 Actual Velocity, v

v

0.5

7.1.6.6 Diameter of reactor, D

m

Av

ID v

4 11.1421

1.365

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Table 7.12: Inner Diameter of Reactor for Various

vsf
vsfm

vsfm

vsfm

Ratios

vsf (m/s)

v (m/s)

ID (m)

13.595
16.314
19.033
21.752
24.471
27.190

6.798
8.157
9.517
10.876
12.236
13.595

1.237
1.129
1.045
0.978
0.922
0.874

5
6
7
8
9
10
vsf

vsf

=10 is selected since the required inner diameter of reactor obtained is the smallest.

7.1.6.7 Minimum Reactor Wall Thickness, tm

2
2

Minimum Reactor Wall Thickness

64

0.2629

7.1.6.8 Outer Diameter, OD

Outer Diameter

OD = ID + 2tm = 34.4248 + 2(0.2629) = 34.95 in = 0.8877 m

7.1.6.9 Bubble Velocity, vB

For Group A particles, bubbles reach a maximum stable size which may be estimated
from Geldart (1992) equation.

Bubble Diameter

dB

2v
g

37.68m

Bubble velocity for Group A particles is given by Werther (1983) equation.

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Chapter 7: Packed Bed Reactor 2
vB

Bubble Velocity

7.1.6.10

Group 6
Acrylic Acid Project
.

A gdB

48.07m/s

Slugging Problem & Reactor Height at Minimum Fluidization, Hmf

The higher the value of Hmf, the higher conversion can be achieved. But too high Hmf can
cause slugging. Hence, optimum value of Hmf need to be determined.
According to Yagi and Muchi (1952), slugging will not occur if criterion below is
satisfied.
1.9
.

0.8744

Reactor Height at Minimum

Fluidization

0.6147

7.1.6.11 Reactor Height

By using Orcutt model, relation between conversions of fluidized reactor and height of
reactor.
1

Conversion

where
13.595 2.719
13.595

0.8

0.6147

0.98

0.804

0.45

1
1
0.0301

0.804
0.5

0.804

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Table 7.13: Determination of Height of Reactor

H mf (m)

H (m)

0.6

1.150

51.34

0.5

1.159

52.85

0.3

1.365

52.94

0.1

1.522

54.56

0.05

1.683

57.26

From table above, observed that the higher value of H mf , the lower value of reactor height,
H required to achieve 98% acrolein conversion. Thus, H mf = 0.6 m is selected which

give H = 51.34 m.
7.1.6.12. Pressure Drop
Pressure drop can be determined by applying Ergun Equation.

Ergun Equation

P
H

Pressure Drop

150

v
D

1.75

v
D

30725.22

30725.22

17.97

5.52

10 Pa

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7.1.6.13.Comparison Between FBR and PBR

Both PBR and FBR reactors can be used to achieve high conversion of acrolein. However,
by comparing the size of reactor required:
Table 7.14: Comparison between FBR and PBR

Volume of reactor, V (m3)

Packed bed reactor

Fluidized bed reactor

27.6

173.5

As expected, volume required for FBR to achieve the same conversion (98%) as PBR is
very large due to bed expansion. The volume required for FBR is about 6 times than that
of PBR. Pressure drop across fluidized bed reactor also much higher in comparison to
packed bed reactor. By considering economic aspect, PBR reactor is selected.

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7.1.7 Summary of Chemical engineering Design

Table 7.15: Summary of Chemical Engineering Design of Reactor

Catalyst Weight and Reactor Volume

Catalyst weight

38000

kg

Reactor volume

27.6

m3

Tube Dimension
Number of tube

Nominal pipe size

895
0.0635

Outside diameter

do

0.073152

Wall thickness

0.005162

Inside diameter

di

0.062713

Tube length

10

Triangular Tube Arrangement

Number of passes

Npass

Tube pitch

Pt

0.09100

Bundle diameter

Db

2.97800

3.01300

Shell Dimemsion
Shell inside diameter

Ds
Baffle Dimension

Baffle thickness

0.005

Baffle spacing

lB

0.833

Number of baffles

NB

11

Baffle cut

25

Cooling Requirement
Water flow rate

mw

35.77

kg/s

Tube side heat transfer coefficient

ht

9.18

W/m2.K

Tube side fouling coefficient

hid

2000

W/m2.K

Shell side heat transfer coefficient

hs

2081.38

W/m2.K

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Chapter 7: Packed Bed Reactor 2

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Shell side fouling coefficient

hod

6000

W/m2.K

Overall heat transfer coefficient

Uo

513.61

W/m2.K

Heat transfer area

37.62

m2

Pressure Drop
Tube side pressure drop

Pt

1.76

kPa

Shell side pressure drop

Ps

3.78

kPa

7.1.8 Cost Analysis [12]

Cost of Packed Bed Reactor = $10,000/m2 of heat transfer surface
Heat transfer area, A = 37.62 m2
Thus, cost of packed bed reactor = $376,200
Year

1999

2009

Cost Index, I

3.954

4.675

Cost

of

Packed

Bed $376,200
= RM1,429,560

Reactor

$444,798
=RM1,690,236

Thus, cost of packed bed reactor is estimated to be RM1, 690,236.

7.1.9 Comparison of the conversion

Table 7.16: Comparison of the Conversion Value with the HYSYS Simulation

Reaction

Assumed

HYSYS

Conversion (%)

Simulation

% difference

Conversion (%)
Acrolein to acrylic acid

98

98

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Chapter 7: Packed Bed Reactor 2

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7.1.10 Comparison of the molar flow of the components in reactor

product stream
Table 7.17: Comparison of the Component Molar Flow with the HYSYS Simulation

Components

Hand Calculation

HYSYS Simulation

Mole flow (kmole/h)

Mole flow (kmole/h)

0.0000

Water

165.65

165.52

0.0811

Nitrogen

810.52

810.52

0.0000

Oxygen

145.17

144.43

0.5137

Acrolein

2.55

2.68

5.0000

Acetol

0.13

0.13

0.0000

Acetic Acid

4.03

5.23

23.0780

Acrylic Acid

127.46

126.26

0.9516

4.43

5.23

15.3857

Glycerol

Carbon Dioxide

% difference

From Table 2.2.1., the result of the percentage difference between hand calculation and
HYSYS simulation for components such as acrolein and acrylic acid, are relatively small.
This is because the HYSYS simulation is achieved the conversion of acrolein, which
approximate to the conversion that used in hand calculation. The molar flow of glycerol,
nitrogen and oxygen also show the small deviation because the oxidation reaction of
acrolein is following the consecutive reaction mechanism. The percentage of deviation of
acetic acid and carbon dioxide are slightly higher than other component because the
conversion of the side reaction is slightly different with the conversion that used in hand
calculation. Low conversions of side reaction are preferable in order to minimize side
product or unwanted product. The amount of acrolein required is important in achieving a
certain conversion.

7.1.11 Case Study

The used of the case study tool is to monitor the steady state response of key process
variables to changes in the process.
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7.1.11.1

Group 6
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Optimization of Temperature

The reactor temperature was chosen as independent variable where the ratio of length and
diameter of reactor, L/D are chosen as dependent variable in this case study. With varies
the reactor temperature once at a time, and with each change, the ratio of length and
diameter of reactor, L/D are calculated. (Refer Table A-1 in Appendix)
Figure 7.2: Ratio of Length and Diameter, L/D vs. Inlet Temperature, To

RatioofLengthandDiameter,L/Dvs.Inlet
Temperature,To
RatioofLength
andDiameter, 18
L/D
16
14
12
10
8
6
4
2
0
230

240

250

260

270

280

290

InletTemperature,To

The reactor temperature is set with the lower bound of 230C to upper bound of 290C.
From the Figure 2.3.1.1., it is proved that 260oC is optimum temperature to be operated
because the ratio of length to diameter of reactor is around 7.877 which is in the range of
design consideration, which is 5 to 10 at that point.
7.1.11.2

Optimization of Pressure

The reactor operating pressure was chosen as independent variable where the ratio of
length and diameter of reactor, L/D are chosen as dependent variable in this case study.
With varies the reactor pressure once at a time, and with each change, the ratio of length
and diameter of reactor, L/D are calculated. (Table A-2 in Appendix)

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Figure 7.3: Ratio of Length and Diameter, L/D vs. Inlet Pressure, Po

RatioofLengthandDiameter,L/Dvs.Inlet
Pressure,Po

RatioofLength
andDiameter, 11
L/D
10
9
8
7
6
5

1.5

1.7

1.9

2.1

2.3

2.5

InletPressure,Po

The reactor operating pressure is set with the lower bound of 1.5 bars to upper bound of
2.5 bars. From the Figure 2.3.2.1., pressures 1.6 to 2.4 are fulfilling the criteria of the
length to diameter ratio to be 5 to 10. Optimum operating pressure is chosen among this
value. Operating reactor under too low pressure might cause the pressure driving force
not sufficient to drive the reactant along the reactor. Operating reactor under too high
pressure might cause clogging fouling effect of reactor. Thus, pressure of 2 bars is
selected as the catalyst used is not too high and L/D ratio is still within 5-10.
7.1.11.3 Summary Optimization Analysis
Parameter

Value

Inlet Pressure, Po (bar)

2.00

Inlet Temperature, To (oC)

260

Pressure Ratio, Y

0.980

Outlet Pressure, P (bar)

1.96

Weight of Catalyst, W (kg)

38000

Ratio of Length to Diameter, L/D

7.985

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7.2.0 Mechanical Engineering of Reactor 2

7.2.0.1 Codes and Standards
The most of the conventional pressure vessels for use in the chemical and allied
industries will invariably be designed and fabricated in accordance with the British
Standard specification for fusion-welded pressure vessels, PD 5500; or the American
Society of Mechanical Engineers code, Section VIII (the ASME code). In this
mechanical design, British Standard specification for fusion-welded pressure vessel, PD
5500 will be followed. In addition, the TEMA standards will be used as reference
because the packed bed reactor was constructed as tubular heat exchanger.

7.2.1 General Design Consideration

7.2.1.1 Design Pressure
A vessel must be designed to withstand the maximum pressure to which it is likely to be
subjected in operation. For vessel under internal pressure, the design pressure is normally
taken as the pressure at which the pressure relief device is set. This will normally be 5 to
10% above the normal working pressure. [5]
Table 7.18: Design Pressure for Tube Side and Shell Side

Design Pressure (kPa)

Tube side

Pt = 200 kPa x 1.1 = 220 kPa

Shell side

Ps = 101.325 kPa x 1.1 = 111.46 kPa

7.2.1.2 Design Temperature

The strength of the metals decreases with increasing temperature so the maximum
allowable design stress will depend on the materials temperature. The design temperature
at which the design stress is evaluated should be taken as the maximum working
temperature. The 10% allowance is given to cope with any uncertainty involved in
predicting vessel wall temperature. [5]

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Table 7.19: Design Temperature for Tube Side and Shell Side

Design Temperature (C)

Tube side

Tt = 260C x 1.1 = 286C

Shell side

Ts = 25C x 1.1 = 27.5C

7.2.1.3 Material of Construction

Selection of a suitable material must take into account the suitability of the material for
fabrication (particularly welding) as well as the compatibility of the material with the
process environment.

[5]

The reactant mixture contained most of acrolein is fed into the

tube side of the rector. Therefore the tube side was easily tend to exhibit corrosive
behavior compared to the shell side, which only containing cooling water. Thus, tubes are
selected to be made of Stainless steel 18Cr/8Ni Mo 2.5% (316). In order to easier the
material construction of the rector, normally the shell is also selected to be made of same
material of the tubes.
7.2.1.4 Design Stress (Nominal Design Strength)
It is necessary to decide a value of the maximum allowable stress that can be accepted in
the material of construction. This is determined by applying a suitable design stress
factor (safety factor) to the maximum stress that the material could be expected to
withstand without failure under standard test condition. (Refer FigureA-6 in Appendix)
For materials not subject to high temperature the design stress is based on the yield stress
(or proof stress), or the tensile strength (ultimate tensile stress) of the materials at the
design temperature. [9]
Table 7.20: Design Stress for Tube Side and Shell Side

Yield Stress

Tensile Strength
2

(N/mm )

Tube side

1.5

120

Shell side

1.5

175

Design Stress (N/mm2)

f
f

80.0MPa
116.7MPa

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7.2.1.5 Welded Joint Efficiency and Construction Categories

The possible lower strength of welded joint compared with the virgin plate is usually
allowed for in design by multiplying the allowable design stress for the material by a
welded joint factor J. The value of the joint factor used in the design will depend on the
type of joint and amount of radiography required by the design code. The joint factor of
1.0 with 100% degree of radiography is chosen which implies that the joint is equally
(double-welded butt) as strong as the virgin plate. This is achieved by radiographing the
complete weld length, and cutting out and remaking any defects. Moreover, this
construction category allows the use of all materials covered by the standard, with no
restricted on the plate thickness. [5]
7.2.1.6 Corrosion Allowance
The corrosion allowance is the additional thickness of metal for material lost by corrosion
and erosion. The allowance should be based on experience with the material of
construction under similar service conditions to those for the proposed design. However,
most of the design and standards specify a minimum allowance of 1.0mm. [5]

7.2.2 Shell and Tube Wall Thickness Design

7.2.2.1 Shell Wall Thickness and Outer Diameter
Cylindrical shell subjected to internal pressure, the minimum thickness, es,min can be
calculated from the equation below: [5]
Shell wall thickness

PD
2Jf P

1.4395mm

However, typical value for wall thickness for vessel diameter between 2.5 to 3.0 m
should not be less than 10 mm, includes a corrosion allowance of 2 mm.[5] Thus, the shell
thickness is taken to be 10 mm.
Outer shell diameter

Do = Ds + 2e = 3033.00 mm

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7.2.2.2 Tube Wall Thickness

The minimum tube thickness can be calculated using the same equation as for shell.
Tube Wall Thickness

PD
2Jf P

4.1496mm

The tube wall thickness selected according to schedule number of 40S is 5.16 mm, which
is larger than es,min. Thus the tube wall thickness is acceptable.
7.2.2.3 Head and Closure
Standard torispherical heads (ASME head) is chosen because it is most economical
closure and most commonly used end closure. The domed head is shown (Refer Figure
A-7 in Appendix). Besides, it is also ease of fabrication and required less space. The
design configuration and the limitation for the torispherical head is shown as below:
0.002Do e 0.12Do

Head thickness

6.066 mm e 363.96 mm
Thus, the head thickness, e can be taken to be same as shell wall
thickness. e =10mm
Knuckle radius,Rk

Rk 0.06Do
Rk 181.98 mm = 182 mm
Rk should be larger than two time of the shell wall thickness.
Thus, the knuckle radius is acceptable.
Rc Do

Crown radius

Using the standard configuration, Rc = Ds = 3033.00 mm

Outside
height

head

D
2

D
2

2R

513.61mm

7.2.2.4 Tube Sheet Thickness

The function of tube plate (tube-sheets) in tubular (shell and tube) packed bed reactor is
to support the tubes, and separate the shell and tube side fluids. The plates must be
designed to support the maximum differential pressure that is likely to occur in the shell
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side and tube side. Tube plate is essentially a perforated plate with an unperforated rim,
supported at its periphery.

[5]

The ligament efficiency of a perforated plate is calculated

with the hole pitch, Ph of 0.09144 m is shown as below:

d
P

0.3142

The plates must be thick enough to resist the bending and shear stresses caused by the
pressure load and any differential expansion of the shell and tube. Plate diameter must be
bigger than shell outside diameter including the flange dimension.
The minimum plate thickness to resist shear,
t

0.155D P

4.060 mm

The typical value for plate thickness for tube outer diameter of 85 mm should not be less
than 60 mm. So, the plate thickness is taken to be 60 mm. [5]

7.2.3

Design Loads

The reactor must be designed to resist gross plastic deformation and collapse under all the
conditions of the loading, such as major and subsidiary loading. The main sources of
loads which need to be considered are dead weight load and wind load.
7.2.3.1 Dead Weight Load
The major sources of dead weight loads are the vessel shell, tubes, insulation, and
catalyst in tubes, cooling water in shell side and reaction mixture in tube side.
7.2.3.2 Weight of Vessel
Vessel

Total weight of a steel vessel, Wv with domed end and uniform wall
thickness can be calculated as:
W

240C D

0.8D

103.6127kN

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where,
Cv = a factor to account for the weight of nozzles, manways, internal
supports, which can be taken as 1.15 (for vessel with support rings)
Dm = Mean vessel diameter = Ds + e = 3.023 m
Hv = Length of cylindrical section = 10+2(0.5136) = 11.0272 m
t = wall thickness =0.01 m
Tubes

Total weight of the tubes can be calculated as:

W

1
N gL d
4

765.9865kN

Where,
t = density of tube (stainless steel) = 7832 kg/m3
Insulation

Insulation thickness, ti for high pressure with operating temperature

between 150C to 300C of the vessel diameter larger than 8 inches
should be 3.5 inches (8.89cm)

[6]

Fiberglass is the most common type of

the insulation, made from molten glass spun into microfibers with density
of 100kg/m3. The weight of insulation can be calculated as:
W

gD H t

7.8805kN

The weight of insulation is doubled up to allow for fittings. Thus,

W
Catalyst

15.761kN

The weight of catalyst can be calculated as:

W

198.65kN

Fluid in tube Feed mixture occupied in the tubes side with the volume below,
Vt = (1-p)V = (1-0.5)(27.6) = 13.800 m3
Thus, the weight of feed mixture can be calculated as:
Wr = fVtg = 1.365(13.800)(9.81) = 0.1848 kN
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Fluid in shell Assuming that the shell side is fully occupied with cooling water. The
volume of cooling water, Vw = L(Ds2 do2N)/4 = 33.6844 m3
Thus, the weight of cooling water can be calculated as:
Wcw = wVwg = 330.444 kN

7.2.3.3 Total Dead Weight

Total dead
weight

WD=Wvessel + Wtubes + Winsulation + Wcatalyst + Wfeed mixture + Wcooling water

= 1414.64 kN

7.2.3.4 Wind Load

Wind loading will only be important on tall columns installed in the open. The load
imposed on any structure by the action of the wind will depend on the shape of the
structure and the wind velocity.

[5]

The local wind velocity in Gebeng area was found to

have an average value of 4.828 kph.

Dynamic Wind Pressure

Mean Diameter

Wind Loading

Bending Moment at Bottom

Tangential Line

0.05
D

2 t
P

F
D

1.165Pa
t

3.4087 m
3.9711 m

159.2095 Nm

7.2.4 Stress Analysis

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Pressure vessels are subjected to other loads in addition to pressure and must be designed
to withstand the worst combination of loading without failure. Resultant stress from all
load determined to ensure that the maximum allowable stress intensity is not exceeded at
any point. The main sources of load to considered are pressure, wind, dead weight of
vessel and content. [5]
Longitudinal Stresses
(referred to Figure A-9 in

PD
4t

16.5715 N/mm

PD
2t

33.1430 N/mm

Appendix)
Circumferential Stresses
(referred to Figure A-8 in
Appendix)
Direct Stresses
(stresses due to dead weight

14.8956 N/mm

t t

loads)
Bending Stresses

M
l

D
2

1.8302

10 N/mm

Where,
Mx = total bending moment at the considered plane
Iv

= the second moment of the area of the vessel

about

Resultant Longitudinal Stress

the plane of bending.

D
D
1.0849
64
L

upward
downward
Principal Stresses

31.4671

10 mm

1.8302

10

31.4689 N/mm
31.4653 N/mm

downward

1.678 MPa
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7.2.5 Vessel Support

The methods used to support the vessel will depend on the size, shape, and weight of the
vessel; the design temperature and pressure; the vessel location and arrangement; internal
and external fittings and attachments. The support must be designed to carry the weight,
content and wind loads of the vessel. Supports will impose localized loads on the vessel
wall, and the design must be checked to ensure that the resulting stress concentrations are
below the maximum allowable design stress. Support should be designed to allow easy
access to the vessel and fittings for inspection and maintenance. [5]
7.2.5.1 Design of Skirt Support
Skirt supports are used for all tall and vertical columns. A skirt support consists of a
cylindrical or conical shell welded to the base of the vessel. A flange at the bottom of the
skirt transmits the load. The openings are normally reinforced and must be provided in
the skirt for access and for any connecting pipes. The skirt welded flush with the shell to
the bottom head of the vessel is usually preferred.

[9, 15]

(Refer to Figure A-11 & Figure

A-12 in Appendix)
Maximum Dead Weight
Loads
(Occur when the vessel is
full with liquid)

Weight of Column Full

of Liquid
Bending Moment at
Base of Skirt

WD

D H
4

771.2984 kN

where, w = water density,1000 kg/m3

WD
F

W
H

2185.9384 kN
H

336.9636 Nm

where, Hs = skirt height = 2m

Bending Stress in the

Skirt

4M
D
t t D

4.7103

10

N/mm

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Where,
Skirt inside diameter, Ds = Di = 3013.00 mm
Skirt thickness, ts = t = 10 mm
Dead Weight Stress in
the Skirt

Maximum Dead Weight

Stress in the Skirt

WD
D
t t
WD
D
t t

14.8956 N/mm

23.0171 N/mm
23.0218 N/mm

Maximum Stresses in
the Skirt

Design Criteria
(2 criteria have to fulfil)

fs =135 N/mm2 (design stress for skirt)

14.8909 N/mm

E = Modulus Young of skirt, 200000 N/mm2

s = base angle of a conical skirt = 90
1st criteria:

2nd criteria:

f Jsin

135 N/mm

,
,

0.125E

t
sin
D

82.9738 N/mm

Both of the criteria have been fulfilled, so ts = 10mm is

satisfactory with 2mm is added in skirt thickness for corrosion.

7.2.5.2 Pipe Sizing for Nozzles and Flanges

In this design, there are four nozzles attached to the column as shown in the Appendix in
which stainless steel pipe are used for nozzles attachment. For stainless steel pipe, the
optimum diameter, dopt can be determined using the following expression: [5]
d

260G

Where, dopt = optimum diameter (mm), G= fluid flow rate(kg/s), = fluid density (kg/m3)
Table 7.21: Optimum Diameter for Inlet Streams and Outlet Streams

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Streams

G (kg/s)

(kg/m3)

dopt (mm)

dopt (inch)

Inlet Feed

11.1422

1.365

760.9078

29.957

Outlet Feed

11.1422

1.365

760.9078

29.957

Cooling fluid

35.77

997.05

28.0819

1.1056

Cooling fluid

35.77

997.05

28.0819

1.1056

Table 7.2.5.2.2. Selected Pipe Sizes for Nozzles [7], [8]

Streams

dopt
(in)

Schedul
e No.

Nominal
Pipe Size
(in)

Wall
thickness,
(mm.)

30.0

Outer
Diameter,
(mm)
30.00

0.312

Internal
Diameter,
(mm)
29.38

Inlet Feed

29.957

10S

Outlet Feed

29.957

10S

30.0

30.00

0.312

29.38

Cooling

1.1056

40S

1.25

42.16

3.556

35.05

1.1056

40S

1.25

42.16

3.556

35.05

fluid
Cooling
fluid

7.2.5.3 Manholes
Refer to BS 470: 1984 for the vessel with inside diameter more than 1.5 m, at least one
manhole is required.[9] Hence, 3 manholes are provided which are located at the top,
middle and bottom of column. The maximum length of a manhole is dependent on the
diameter. (Refer to Figure A-13 and A-14 in Appendix). From BS470: 1984, the standard
size of diameter and length is chosen as below:

Manhole

Diameter

Length

575mm

500mm

7-34

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

7.2.5.4 Base Ring and Anchor Bolt

The loads carried by the skirt are transmitted to the foundation slab by the skirt base ring
(bearing plate). The moment produced by wind and other lateral loads will tend to
overturn the vessel; this will be opposed by the couple set up by the weight of the vessel
and the tensile load in the anchor bolts.[5],[9],[10] By refer to the Figure A-15, A-16 & A-17
in the Appendix, the result of base ring and anchor bolt based on British Standard BS
470: 1984,BSI, 1984 are shown below:
Bolt Size and Bolt Pitch

Bolt Diameter

Dbolt = 1.8m

Number of Bolt

Nb = 8 (minimum 8 bolts)

Bolt Size

M24

Root Area of Bolt

353mm2

Bolt Pitch

lB
lB

D
N

707 mm

600

Thus, the anchor bolts with diameter 1.8 is satisfactory.

Total Compressive Load

4M

WD
D

149.4976 kN/m

Base Ring Width

Minimum Width

21.3568 mm

Where fc = maximum allowable bearing pressure= 7N/mm2

Actual Width

50

136 mm

Where
Lr = distance from the edge of the skirt to the outer edge of
the ring
= 76 mm

7-35

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Actual Bearing
Pressure

Group 6
Acrylic Acid Project
F
l

1.0992 N/mm

Minimum Base Ring

Thickness

3f
f

11.6640 mm

7.2.6 SUMMARY OF MECHANICAL ENGINEERING DESIGN

Shell
Design pressure

Ps

111.45

kPa

Design temperature

Ts

27.5

Design stress

fs

116.667

N/mm2

Ds,o

2657.64

mm

es

10

mm

Corrosion allowance

mm

Construction material

Stainless steel (316)

Type of joint

Double-welded butt

Shell outer diameter

Wall thickness

Tube
Design pressure

Pt

220

kPa

Design temperature

Tt

286

Design stress

ft

80

N/mm2

Wall thickness

et

4.1496

mm

Corrosion allowance

1.0

mm

Construction material

Stainless steel (316)

Head and Closure

Head thickness

eh

Corrosion allowance

10

mm

1.0

mm

Knuckle radius

Rk

182

mm

Crown radius

Rc

3033.00

mm

Head height

513.61

mm
7-36

KKEK 4281 Design Project

Chapter 7: Packed Bed Reactor 2

Group 6
Acrylic Acid Project

Construction material

Stainless steel (316)

Type of head

Torispherical
Tube Sheet

Tube sheet thickness

tp

60

mm

Diameter

Dp

3043.00

mm

Skirt Support
Skirt thickness

ts

10

mm

Skirt inner diameter

Ds

3033.00

mm

Design stress

fs

135

N/mm2

Modulus Young

200000

N/mm2

Base angle

90

Dbolt

1.8

mm

Nb

Base Ring and Anchor Bolt

Bolt diameter
Number of bolt
Bolt size

M24

Root area of bolt

353

mm2

Bolt pitch

lB

707

mm

Total compressive load

FB

149.4976

kN/m

Minimum base ring width

lb

21.3568

Mm

Actual base ring width

la

136

Mm

Actual bearing pressure

f c'

1.0992

kN/mm2

tbase

11.6640

mm

Minimum base ring thickness

Manholes
Diameter

Dm

575

Mm

Length

lm

500

mm

Pipe Sizing for Nozzles and Flanges

Streams

Schedule
No.

Nominal
Pipe Size
(in)

Wall
thickness
(mm.)

30.0

Outer
Diameter
(mm)
30.00

0.312

Internal
Diameter
(mm)
29.38

Feed stream

10S

Cooling fluid

40S

1.25

42.3164

3.556

35.052
7-37

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

7.3 Safety, Control and Instrumentation

7.3.1 The importance of safety
Process safety has become important due to a number of serious accidents occurred in processing
plant. Since the reactor is operating in high pressure and high temperature, safety should be put
in the first place during equipment design. All engineers have a duty to use their best endeavors
to ensure the plant is designed and operated under control. Not only treat safety as a legal duty, it
should also be considered as a moral obligation. This duty is wide reaching and can be divided
into a number of topics as follow:

Prevention of death or injury to workers

Prevention of death or injury to the general public

Prevention of damage to plant

Prevention of damage to third party property

Prevention of damage to the environment

7.3.1.1

Safety Considerations

One of the problems in reactor is generation of high-temperature portions referred to as hot spots
in catalyst layer. The reactor involves with exothermic reaction, therefore some methods that can
be used to avoid hot spots are:

Run heat transfer medium concurrently: The heat transfer medium which is cooling
water enters at its lowest temperature. By matching this low temperature with the
highest temperature zone in the packed bed reactor, the temperature gradient is the
largest at the reactor entrance, providing more heat removal.

Use inert solid: by randomly packing the tubes with inert solid (no catalytic activity), the
heat released per unit volume of packed bed reactor is reduced, thereby minimizing hot
spots.

Use catalyst gradients in packed bed reactor: this is similar to above. Here, a larger
fraction of inert solid is used where hot spots are anticipated. This minimizes hot spots.

738

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

7.3.1.1.1 Pressure Relief Systems

The installation of the pressure relief system is important to avoid an uncontrolled, azeotropic
release of the contents or the destruction of the vessel. The relief valves are also known as safety
valves are designed to operate under unsteady conditions. Usually, the safety valves on vessels or
process lines that open automatically at a certain pressure. The designs of the safety valves are
apparently important, as the worst case scenario must be considered.
7.3.1.1.2 Effects of Fouling
The calculation of the overall heat transfer coefficient contains the terms to account for the
thermal resistances of the fouling layers on the inside and outside heat transfer surfaces. These
fouling layers are known to increase the thickness with the time as the reactor is operated.
Fouling layers normally have s lower thermal conductivity than the fluids or the tube material,
thereby increasing the overall thermal resistance. In order that the reactor shall have sufficient
surface to maintain satisfactory performance in normal operation, with reasonable service time
between cleanings, it is important in design to provide a fouling allowance appropriate to the
expected operating and maintenance condition.
7.3.1.1.3 Corrosion Failure
Most pressure vessel is subjected to deterioration by corrosion or erosion, or both especially
when the substances are corrosive such as acrolein and acrylic acid. The effect of corrosion may
be pitting or grooving over either localized or large areas that may cause a general reduction of
the wall thickness. This will lead to cracking of vessel as well as contamination of the product.
To overcome this problem the wall is designed for corrosion allowance to reduce the corrosion
effect. For modern plant, weep holes are planted on the vessel for early stage detection of
corrosion.
7.3.1.1.4 Stress Failure
Excessive stresses can developing vessels that are not free to expand and contracted with
temperature changes. If the stresses are allowed to often, eventually failure can be occurred.
Hence, maximum allowable stresses must be identified for a reactor design and the possibility

739

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

sources of stress must be considered. Over designing is not encouraged, but under design would
lead to accident and fatality.

7.3.2 Process safety design

Safety is a very precise and a very vague term. It is vague because, to some extent, safety is a
value of judgment, but precise because in many cases, we can readily distinguish a safe design
from an unsafe one. There are four criteria that must be fulfilling to aid ensure a safe design.
First, a design must comply with the applicable law. Second, an acceptable design must meet the
standard of accepted engineering practice. Third, an alternative designs that are potentially safer
must be explored. Fourth, finished design must be rigorously tested. Moreover, the safety
performance should improve through a practical and economical way. The design of an
assessment of the safety programs such as safety and loss prevention activities, process safety
management (OSHA related), risk management planning, process hazard analysis and risk
awareness training are needed.

7.3.3 Process hazard analysis (HAZOP analysis)

HAZOP is a systematic, highly structured assessment relying on HAZOP guide words. It is a
modified brainstorming technique for identifying and resolving process hazards in order to
generate a comprehensive review and ensure that appropriate safeguards against accidents are in
place. It is considered is an important and common used method in identifying safety hazards
and operability problems of continuous process system and in reviewing procedures and
sequential operations. The Occupational Safety and Health Administration (OSHA) Process
Safety Management regulation required that the actions assigned be taken in a timely manner.
All process hazard analysis is updated at least every five years. For the oxidation reaction unit
operation, HAZOP analysis is done on the inlet and outlet streams of the reactor and water
cooling system. (Procedure refer to Figure A-18 in Appendix).

740

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO
Table 7.22: HAZOP Analysis on Feed Stream of the Reactor

Guide word
NO/ NONE

Deviation
No flow

Causes
Compressor failure
Blockage in pipeline
Large leakage in
pipeline

Consequences
No reaction
occur in reactor
Rate of reaction
drop

Control valve fails

Action
Install back up pump
Install flow indicator
Install low flow alarm
Install back-up control
valves
Install manual bypass

and closed
Controller fails and

valve
Install back-up controller

valve closes

Check compressor/
pump
MORE

More flow

Over pumping
capacity
Control valve fails
and open
Controller fails and
valve opens

Reaction altered

Install high flow alarm

Resident time

Install back-up control

decrease
Build up of
reactant
Runaway

valves
Install manual bypass
valve
Install back-up controller

reaction
LESS

Less flow

Defective pump

Reaction altered

Install flow indicator

Partial blockage in

Product yield

Install back-up control

pipeline
Small leakage in
pipeline

decrease
Loss of
productivity

Abnormal opening

valves
Install manual bypass
valve
Install back-up controller

of valve
REVERSE

Reverse

Pump reversed

Reaction altered

Install check valve

flow

Pump failure

Blockage of pipe

Install flow indicator

Reversed differential

Pipeline crack

Instruct operators on

pressure
Incorrect operation

under high

procedure

pressure

Flooding of reactor

741

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

MORE

More

Defective control

pressure

Compressor failure

Possible reactor
fractured
Over pressure of
reactor or vessel

Perform scheduled
maintenance
Install high pressure
alarm
Install back-up controller
Install high pressure
emergency shutdown
Install pressure relief
valve

LESS

Less

Compressor failure

pressure

Partial blockage in

Reaction altered

Install back-up pump

Install back-up controller
Install pressure indicator

tube
Leakage in tube

Instruct operators on

Abnormal opening

procedure

of valve
Defective control
MORE

More

More heating

temperature

Failed cooling
system
Defective control

High reactor
temperature
Runaway
reaction
Possible reactor
fractured
Production of
side product

Install high temperature

alarm to alert operator
Perform scheduled
maintenance
Install back-up controller
Install high temperature
emergency shutdown
Install flow rate
controller for coolant

LESS

Less

Less heating

temperature

Failed cooling
system
Defective control

Rate of reaction
drop

Perform scheduled
maintenance
Instruct operators on
procedure
Install flow rate
controller for cooling
system

742

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO
Table 7.23: HAZOP Analysis on Outlet Stream of Reactor

Guide word
NO

Deviation
No flow

Possible causes

Consequences

Action

Pump failure

Product loss

Install back up pump

Blockage in pipeline

Downtime to

Install flow indicator

Large leakage in
pipeline
Control valve fails
and closed

overall process
Reaction altered
Explosion
hazard

Controller fails and

Install back-up control

valves
Install manual bypass
valve
Install back-up controller

valve closes
MORE

More flow

Control valve fails

and open
Controller fails and
valve opens

Reaction altered

Install high flow alarm

Resident time

Install back-up control

decrease
Off-spec product

valves
Install manual bypass
valve
Install back-up controller

LESS

Less flow

Partial blockage in
pipeline
Small leakage in
pipeline
Abnormal opening

Reaction altered

Install flow indicator

Loss of

Install back-up control

productivity
Resident time
increase

valve

Reverse

Pump reversed

Reaction altered

Install check valve

flow

Reversed differential

Product

Install flow indicator

pressure

reduction

Incorrect operation
MORE

Install manual bypass

Install back-up controller

of valve
REVERSE

valves

More

Defective control

pressure

Pipe blockage

Instruct operators on
procedure

Possible reactor
fractured

Perform scheduled
maintenance
Install high pressure
alarm to alert operator
Install back-up controller
Install high pressure
emergency shutdown

743

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

LESS

Less

Pump failure

pressure

Partial blockage in

Reaction altered

Install back-up pump

Install back-up controller
Instruct operators on

tube
Leakage in tube

procedure

Abnormal opening
of valve
Defective control
MORE

More

More heating

Runaway

Install high temperature

temperature

Failed cooling

reaction

alarm to alert operator

system
Defective control

Possible reactor

Perform scheduled

fractured

maintenance

Production of

Install back-up controller

side product

Install high temperature

emergency shutdown

LESS

Less

Less heating

temperature

Failed cooling

Reduce reaction

Perform scheduled

rate

maintenance
Instruct operators on

system
Defective control

procedure

Table 7.24: HAZOP Analysis on Cooling Water Supply of Reactor

Guide word
NO

Deviation
No flow

Possible causes
Pump failure

Consequences

Blockage in pipeline

High temperature
in reactor

Large leakage in
pipeline

Possible thermal
runaway

Action

Install low flow alarm

Install emergency
shutdown

Control valve fails and

closed

Install backup control

valves

Controller fails and

valve closes

Install manual by pass

valve

Install backup cooling

water source

Install high temperature

alarm

744

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO
MORE

More flow

Control valve fails and

open
Controller fails and
valve opens

LESS

Less flow

Reaction altered

Install high flow alarm

Reactor cools

Install back-up control

valves

Install back-up controller

Low conversion
Low reaction rate

Partial blockage in
pipeline
Small leakage in
pipeline

Referred under

Referred under NO

NO

Partial water source

supply
REVERSE

AS WELL
AS

PART OF

Water source failure

Temperature rises

Reverse pressure
differential

Possible runaway
by improper
cooling

Install high temperature

alarm and check valve

Instruct operators on
procedure

Reactor
product in
shell

leakage in tubes

Loss of
productivity

Perform scheduled
maintenance

Contamination of
water

Continuous monitoring

Partial
cooling

failure of the control

valve

Reverse
flow

reverse pressure
differential

Partially plugged
cooling water supply

Referred under

Referred under NO

NO

Partial water source

supply
REVERSE

Reverse
cooling
water flow

Pump reversed

Improper cooling

Install check valve

Loss of cooling water

pressure

Possible thermal
runaway

Perform scheduled
maintenance

Possible loss of
cooling
performance

Monitoring of cooling
water source quality

Install filters to prevent

contaminant from
entering

Install check valve and

high temperature alarm

Backward flow due to

backpressure
OTHER
THAN

Other
material

Water source
contaminated
Backflow from sewer
Leakage from tube

possible reaction
runaway

745

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

7.3.4 The importance of control system

A control system is critically important to maintain equipment performance within the bounds of
safe operation. It is also used as protection to process equipment and environment. In addition,
the control systems are becoming more critical to the profitable operation of process plant
because of rising energy costs, limited availability of raw material, and tighter safety and
environmental regulations. Objectives of control systems and instrumentation are:
(a) Safety of plant operation
Maintain the operating temperature at 260oC to avoid overheating or overcooling while
the operating pressure at 200 kPa to avoid pressure build up and cause explosion hazard.
(b) Production rate
Achieve the desired product output which is 98% conversion of acrolein in reactor.
(c) Product quality
Produce acrylic acid with standard requirement and ensure the better product quality
control

Since the reaction was carried out in the packed bed reactor at pressure of 200 kPa and
temperature of 260C, it is required of installation the temperature indicator as well as pressure
indicator to measured the reactor condition for convenient the process monitoring. Beside, the
high level alarm and low level alarm of temperature, pressure and flow is installed to alert
operators in case of runaway in process condition. The gate valves are utilized as isolation valve
and check valve to prevent the back flow.
7.3.4.1 Types of Controller
7.3.4.1.1 Temperature Control
The primary control variable in most oxidation reaction is temperature. For a closer control, a
cascade system is preferred for temperature control where cooling water is used to remove the
exothermic heat of reaction. The control variable, reactor temperature which responds slowly to
the change in heat transfer medium flow (cooling water as manipulated variable) is allowed to
adjust the set point of temperature secondary loop which respond rapidly to the flow changes.
746

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

The purpose of secondary loop is to correct the outside disturbances (i.e. temperature changes in
heat transfer medium) without allowing them to affect the reaction temperature. If temperature
exists more or less than 10% of set point, high or low temperature alarm will be activated. PID is
chosen as it gives faster response, avoid lag time to system and eliminate the offset of the set
point. [11]
7.3.4.1.2 Pressure Control
When the pressure rises, that is the indication of excess gaseous reactant accumulation in the
reactor. Thus, the pressure controller will reduce the gas flow. As the result, the gas consumption
balance will re-establish. If the pressure exists more or less than 10% of the set point, high or low
pressure alarm will be activated. PID controller is used to achieve effective control systems. [11]
7.3.4.1.3 Level Control
Level is important in reactor and it should be maintained to achieve the desired conversion. If the
inflow to the reactor varies, the easiest way to maintain the level is by manipulating reactor
outflow. The ratio of volume to outflow is controlled by manipulating on the flow rate of the
outlet stream from the reactor. Cascade control is used and PI controller is chosen because of its
efficiency in controlling the level of reactor.
7.3.4.1.4 Feed Flow Control
The objective of flow control is to maintain a constant production rate and make sure the amount
of catalyst is sufficient enough for the occurrence of reaction. Flow transmitter (FT) is installed
to detect the flow of the inlet stream to the reactor. Signal is then send to Flow Controller (FC)
that will be controlling the limitation of feed flow rate at set point value by adjusting the final
control element (control valve). For flow control system, feed forward control configuration is
applied. If flow rate exist more or less than 10% of the set point, high or low flow alarm will be
activated. PI controller is used since it is sufficient for controlling the feed flow. [11]
7.3.4.1.5 Feed Composition Control
The molar ratio of reactant affects the conversion of the reaction and the composition of the
product. Hence, to maintain these two output variable at desired set point, chemical composition
747

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

analyzer is installed such as infrared analyzer, conductometric analysis ultraviolet or visible

radiation analyzer to detect the concentration of the components. PI controller is selected because
the integral action can eliminate the offset thereby establish precise ratio of streams. [11]

7.3.4.2 Control System Loop

7.3.4.2.1 Feed Flow Control (Control System Loop 1)
This control system is used to control the reactor feed stream in a constant flow rate. The flow
transmitter is utilized to detect the changes of the feed flow. A signal will be generated by the
flow transmitter and send to the flow controller. The flow controller will convert the received
signal and send to the flow control valve, which adjust the flow of the feed stream to the desired
flow rate.
7.3.4.2.2 Reactor Pressure Control (Control System Loop 2)
This control system is used to control the reactor pressure in a constant value. The pressure
transmitter is utilized to measure the pressure of the reactor. When the reactor pressure is high
than the set point value, the pressure transmitter send a signal to the pressure controller and the
high pressure alarm will sounded to instruct the operators. The pressure controller and then will
adjust the flow to maintain set point value.
7.3.4.2.3 Cooling Stream and Reactor Temperature Control (Control System Loop 3)
This control system is used to control the cooling system to maintain reactor temperature. Heat
transfer is necessary in the exothermic reaction to maintain the reactor in isothermal condition.
Normally, heat transfer in the reactor is a slow process. Therefore, the reactor temperature can
easily undergo a large deviation from the set point before control is again established. In order to
have a better response to the temperature fluctuation, Cascade control is utilized rather than other
control because can provide faster response of reactor temperature control to a disturbance in
cooling water temperature. In this system, the output of primary controller becomes the set point
of secondary controller which is used to control the flow rate of cooling water into the reactor.
Under these conditions, the primary controller adjusts indirectly the flow rate of cooling water.
748

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO

The control and instrumentations of packed bed reactor is show as below:

Figure 7.4: Control System for Packed Bed Reactor

FC

Flowcontroller

TC

Temperaturecontroller

PC

Pressurecontroller

FI

Flowindicator

TI

Temperatureindicator

PI

Pressureindicator

FT

Flowtransmitter

TT

Temperaturetransmitter

PT

Pressuretransmitter

FAH

Highflowalarm

TAH

HighTemperaturealarm

PAH

HighPressurealarm

FAL

Lowflowalarm

TAL

LowTemperaturealarm

PAL

LowPressurealarm

749

ACRYLIC ACID PRODUCTION BY USING GLYCEROL

7.0: PACKED BED REACTOR TWO
Table 7.25: Control Variables for Packed Bed Reactor

Control
Variables

Manipulated Disturbances
Variables

Type of

Control

Control

Action

Set Point

Loop/
Controller
Reactor

Cooling

temperature

water flow
rate

Change in
inlet

Cascade/

Control

PID

water

temperature.

cooling

Feed flow

flow rate

260oC 10%

rate.
Change in
reactor
pressure.
Reactor
pressure

Gaseous inlet Acrolein flow

flow rate

rate

Cascade/

Control

PID

gaseous

2 bar 10%

inlet flow
rate
Reactor

Flow rate of

Flow rate of

level

product

reactant

Cascade/ PI

Control

80% of reactor

product

height

stream
flow rate
Molar ratio
of reactants

Acrolein feed

Control

Acrolein:O2:N2:H2O

rate from

feed flow

is 1:1.6:6.4:1

oxidation

rate

Feed flow

Cascade/ PI

reactor

750

KKEK 4281 Design Project

Chapter 8: Quenching Tower

Group 6
Acrylic Acid Project

CHAPTER 8: QUENCHING TOWER

8.1 Chemical Design of Quenching Tower (Absorber)
8.1.1 Objective
The objectives of this project is the design a quenching tower, which is also called as an
absorber, to separate the acrylic acid and acetic acid from the gas stream from reactor by
using water as solvent.

8.1.2 Introduction
The removal of one or more selected components from a mixture of gases by absorption
into a suitable liquid is the second major operation of chemical engineering that is based
on interphase mass transfer controlled largely by rate of diffusion. The product stream
from Reactor 2 at 170oC and flow rate of 1260kmol/hr is fed into quenching tower
counter-current to separate out the air and form aqueous solution. Water is fed from the
top of the tower and the product stream from the bottom of the tower. Water will wash
the product stream in counter current flow. Air, water vapour and other minor component
exited the tower at the top. Acrylic acid and acetic acid will dissolve in water and form
aqueous solution.
8.1.2.1 The Mechanism of Absorption
According to two film theory, material is transfer in the bulk of phases by convection
currents, and concentration differences are regarded as negligible accepts in the vicinity if
the interface between the phases [1]. On either sides of this interface it is supposed that
the current die out and that there exists a thin film of fluid through which the transferred
is affected solely by molecular diffusion. This film will be slightly thicker than the
laminar sub layer because it offers the residence equivalent to that or the whole of the
boundary layer. According to Ficks Law, the rate of transfer by diffusion is proportional
to the concentration gradient and to the area of interface over which the diffusion is
occurring. Ficks Law is limited to cases where the concentration of the absorbed
component is low [3].

8-1

KKEK 4281 Design Project

Chapter 8: Quenching Tower

Group 6
Acrylic Acid Project

The direction of transfer of the material across the interface is not dependent solely on the
concentration difference, but also in the equilibrium relationship. There is, therefore, a
very big concentration gradient across the interface, but this is not the controlling factor
in the mass transfer, as it generally assumed that there is no resistance at the interface
itself, where equilibrium conditions will exist, the controlling factor will be the rate of
diffusion through the two films where all the resistance is considered to lie.

8.1.3 General Design Decisions

Before designing the quenching tower, some information below needs to be considered
and determine:
i.

Entering gas and liquid flow rate, composition, temperature, and pressure

ii.

Desired degree of recovery of one or more solutes

iii.

Choice of solvent

iv.

Operating pressure and temperature

8-2

KKEK 4281 Design Project

Chapter 8: Quenching Tower
v.

Group 6
Acrylic Acid Project

Minimum solvent flow rate and actual solvent flow rate as a multiple of the
minimum rate needed to make the separation.

vi.

Number of equilibrium stages

vii.

Type of quenching tower

viii.

Height and diameter of quenching tower

8.1.3.1 Choices of solvent

An important decision in the design process was which solvent to be used. The ideal
solvent should:

Have high solubility for solutes

Have low volatility to reduce loss of solvent

Be non-corrosive

Have low viscosity to provide a low-pressure drop

Be non-toxic

Be available and not expensive

For our case, we chose water as our solvent to dissolve the acrylic acid and acetic acid
since it fulfills all the requirements above.
8.1.3.2 Determination of operating pressure and temperature
In general, operating pressure should be high and temperature low for quenching tower,
to minimize stage requirement and/or solvent flow rate to lower the equipment volume
required accommodating the gas flow.
8.1.3.3 Selection of the type of quenching tower
The equipment used for contacting liquid and gas streams continuously may be a packed
tower with regular or irregular solid packing material, a plate-type unit containing a
number of bubble-cap or sieve plates, an empty tower wetted- wall column or a stirred or
sparked vessel. Ordinarily, the gas and liquid stream are made to flow counter-currently
pass each other through the equipment so that the greatest rate of absorption maybe
obtained. A plate column is chosen in this design problem. This is based on some reason
listed below:
i. Plate column can handle a wider range of liquid and gas flow rates.
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ii. The efficiency of plate can be predicted with more certainty than the equipment
term for packing.
iii. Plate column can be designed with more assurance than packed column.
iv. It is easier to make provision for the withdraw of side stream form plate column
rather than packed column where the dimension in the packed are calculated
based on height and diameter only.
v. Packing should always be considered for a small diameter column.
vi. The total weight of a plate tower is usually less than that of the packed tower for
the same duty. The limited cracking strength of many packing materials may
make use of multiple packing support plates mandatory, to bear the weight of
tall packed column.
8.1.3.4 Simulation of design problem
Quenching tower is used to separate the acrylic acid and acetic acid from the gas stream.
The schematic diagram of the quenching tower is given in the Figure 8.1 as an illustration
of this design problem. The chemical engineering design of the quenching tower is based
on the material and energy balance that is stimulated by HYSIS software. In order to
dissolve as much as possible the acrylic acid and acetic acid in water, the pressure and
temperature of the quenching tower is important to be controlled for not being too high.

Stream 27
Phase: Liquid
Temperature: 42.17 oC
Pressure: 101.3 kPa
Mass Flow: 7206.0 kg/hr
Mw = 18.02 kg/mole
Density = 994.3 kg/m3
.........................................................
Water: 7206.0 kg/hr

Stream 25
Phase: Gas
Temperature: 170oC
Pressure: 180 kPa
Mass Flow: 40111.85kg/hr
Mw= 31.83 kg/mol
Density= 1.556 kg/m3
.........................................................
Water: 2981.9kg/hr
Oxygen: 4621.4kg/hr

Stream 28
Phase: Gas
Temperature: 69.7oC
Pressure: 101.3kPa
Mass Flow: 35048.78kg/hr
Mw = 25.64 kg/mol
Density = 0.9128 kg/m3
.........................................................
Water: 7259.40kg/hr
Oxygen: 4631.40kg/hr
Nitrogen: 22705.00kg/hr
Acrolein: 142.71kg/hr
Acrylic Acid: 41.83kg/hr
Carbon Dioxide: 230.13kg/hr
Acetic Acid: 48.32kg/hr

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Stream 29
Phase: Liquid
Temperature: 72.88oC
Pressure: 101.3kPa
Mass Flow: 12269.11kg/hr
Mw = 41.88 kg/mol
Density = 967.2 kg/m3
...................................................
Water: 2928.5kg/hr
Oxygen: 0.044kg/hr
Nitrogen: 0.103kg/hr
Acetol: 10.371kg/hr
Acrolein: 8.106kg/hr
Acrylic Acid: 9056.2kg/hr
Acetic Acid: 265.52kg/hr

Figure 8.1 Schematic diagram of quenching tower

8.1.3.5 Physical properties data
There are several sets of physical properties that need to be calculated before the
subsequent design can be calculated for each stream. Determination of these properties
through the correlation involves a very complex step. Therefore, HYSIS software is used
in generating most of property data. The values of the physical properties vary from top
of top bottom of the absorber column.
The physical properties need to be obtained in each stream for quenching tower design
calculations include:
i.

Density

ii.

Viscosity

iii.

Average molecular weight

iv.

Surface tension

8.1.3.6 Prediction of overall column efficiency

For the overall efficiency of quenching tower, it is the same as the overall column
efficiency of absorber. In OConnells paper, the plate efficiency is correlated with a
function involving Henrys constant, the total pressure and the solvent viscosity at the

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operating temperature. After convert the equation to SI unit, it is convenient to express

this function in the following form [3]:

s
x = 0.062

KM s s
Where:
Ms= molecular weight of solvent= 18.02
s = solvent viscosity, mNs/m2 = 0.6254
s = solvent density, kg/m3 = 994.3
K = equilibrium constant for the solute = 0.3762
Substitute the value given in equation above,
s
x = 0.062

KM s s
994.3

= 0.062
0.3762 18.02 0.6254
= 14.54

With this value, use the graph from Figure 8.2 (from Figure 11.14 reference [2]) below to
determine the quenching tower overall column efficiency.
From the graph, the overall efficiency, Eo is around 63%

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Figure 8.2: Absorber column efficiency [2]

8.1.2.7 Number of stage

In order to get the require mass flow rate for the liquid outlet flowrate and vapour outlet
flowrate with desired mole fraction, we set up a model of quenching tower in HYSIS, by
trial and error, the required number of stage to reach the target is 13. So, a quenching
tower with 13 number of stage will be designed with all the specification as below.

8.1.4 Plate Specifications and Configurations

8.1.4.1 Plate contactors

Cross flow plates are the most common type of plate contactor and used in this quenching
tower design. In a cross flow plate, the liquid flows across the plate and the vapour up
through the plate. The following liquid is transferred from plate to plate through the
vertical channels called downcomers. A pool of liquid is retained on the plate by an outlet
weir.

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Figure8.3: Typical cross flow plate (sieve) [2]

Figure 8.4: Column operation regimes

Base on figure above, following information can be obtained:
Column flooding:
Occurs at a maximum vapour flow above which liquid back-up in the downcomer
reaches the plate above, complete flooding leads to liquid leaving with the vapour steam.

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Downcomer flooding:
Liquid backup caused by too small downcomer areas, or too high liquid flows. As long as
downcomer area is 10% or greater and tray spacing is 60cm or greater, this rarely occurs.
Entrainment flooding:
Excessive carry-over of one liquid by the gas to the tray above. The entrained liquid
causes the liquid flowing down to increase exceeding the capacity of the downcomers
and causing total flooding. Entrainment flooding normally limits operation and is the
basis for column diameter estimation.
Weeping:
Liquid weeps through the perforations when the gas flow is too low. Excessive
weeping reduces efficiency as the contact with the liquid phase is reduces.
Turn-down ratio: The vapour rate at flooding to the minimum vapour rate.
8.1.4.2 Choice of plate type

There are three types of cross flow tray, which are bubble cap plate, sieve plate and valve
plate. The principle factor to consider when comparing the performance of these three
plates, cost, capacity, operating range, efficiency, and pressure drop. The comparisons are
summarized in the table below:
Table 8.1: Comparison between different trays
Type of plate

Sieve

Bubble cap

Valve

Cost

Less expensive

Most expensive

Expensive

Capacity

Highest

Low

Moderate

Operating
range

Satisfactory range 50% 120% of design capacity

At very low vapour

rates

Efficiency

Same

Same

Same

Lowest
Highest
High
Pressure drop
From the table above, the sieve is chosen due to some considerations of many aspects.
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8.1.4.3 Plate design algorithm

A trial and error approach is necessary in plate design starting with a rough plate layout,
checking key performance factor and revising the design as necessary until a satisfactory
design is achieved. The algorithm of the design is simplifies Figure 8.5 below.

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Calculate maximum and minimum vapour

and liquid flow rate from physical properties

Select trial spacing

Estimate column diameter based on

flooding consideration

Describe flow arrangement

Make a trial layout

Check weeping rate

Check plate pressure drop

Check downcomer backup

Decide plate layout

Recalculate percentage flooding based on

chosen diameter

Check entrainment

Recalculate percentage flooding based on

chosen diameter

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Figure 8.5: Plate design algorithm

8.1.4.4 Physical properties

From the HYSIS results, some physical properties need to be obtained which are
important before the subsequent design is calculated.
Mass flow rate gas inlet, FGin

= 11.14kg/s
= 1.56 kg/m3

Density of gas inlet, Gin

Mass flow rate of gas outlet, FGout

= 9.74 kg/s

Density of gas outlet, Gout

= 0.92 kg/m3

Mass flow rate liquid inlet, FLin

= 2.00 kg/s
= 994.30 kg/m3

Density of liquid inlet, Lin

Mass flow rate of liquid outlet, FLout

= 3.41 kg/s
= 967.20 kg/m3

Density of liquid outlet, Lout

The liquid-vapour flow factor for bottom is given by:
FLVbottom =

FLout
FGin

Gin
Lout

3.41 1.56
11.14 967.2
= 0.0123
=

8.1.4.5 Plate spacing

The overall height of the column will depend on the plate spacing. Plate spacing from
0.15m and 1.0m are normally used. The spacing will depend on the column diameter and
operating conditions.
Take plate spacing as 0.5m.
Then from Figure 8.6 (from Figure 11.27 reference [2]) below, a value of K1 can be
determined.
Bottom, K1

= 0.09

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Figure 8.6: Flooding velocity, sieve plate [2]

8.1.4.6 Column diameter

From the correlation given by Fair (1961),

1

- 2
U f_bottom =K 2 Lout Gin
Gin
1

967.20 1.56 2
= 0.09

1.56

= 2.239m/s

Design 85% flooding at maximum rate,

U v_bottom = 0.85 U f_bottom

= 0.85 2.239
= 1.9m/s
The maximum volumetric flow rate,

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bottom =
=

FGin
Gin
1.9
=1.22m3 /s
1.56

Thus, the net area required,

A n_bottom =

bottom
U v_bottom

1.22
1.9
=0.642m 2
=

For trial, the downcomer area as 12% of total column cross section area was chosen,

A c_bottom =

A n_bottom

100%-12%
0.642
=
100%-12%
=0.73m 2

Therefore, the column diameter is calculated from the equation below,

1

Dc _ bottom

42
A
= c _ bottom

0.73 4 2
=

= 0.964m

Thus column diameter taken is 0.964m.

Uf (bottom)

Where
K1

= flooding velocity, m/s

= constant obtained from Figure 8.5 [11.27]

Uv (bottom) = superficial vapour velocity

(bottom) = volumetric flowrate
An (bottom) = net area required
Ac (bottom) = column area
Dc (bottom) = column diameter

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8.1.4.7 Flow arrangements

Cross flow trays are also classified according to number of liquid passes on the plate. The
choice of liquid flow pattern is depends on the liquid flow rate and column diameter.
liq =

FLout
Lout
3.41
967.20
=3.536 103 m3 /s
=

Base on Figure 8.7 (from Figure 11.28 reference [2]) below, when the column diameter is
0.964m, and liquid flow rate is 0.003536m3/s, the plate diameter outside range of the
figure, but it is clear that a single pass plate can be used.

Figure 8.7: Selection of liquid flow arrangement [2]

8.1.4.8 Provisional Plate Design

Column diameter,

Dc = 0.964m

Column area,

A c = 0.73m 2

Downcomer area,
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A d = 0.12 A c
= 0.12 0.73
= 0.088m 2
Net area,

A n = A c -A d
= 0.73 0.088m 2
= 0.642m 2
Active area,

A a = A c 2A d
= 0.73 2(0.088)
= 0.554m 2
Hole area,

A h = 0.10 A a
= 0.10 0.554
= 0.0554m 2
The relationship between the weir length and downcomer area is given in Figure 8.8
(from Figure 11.31 reference [2]).
Ad
0.088
100% =
100%
Ac
0.73
= 12%
From the Figure 8.8[2] below,

Lw
= 0.76
Dc

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Figure 8.8: Relationship between the weir length and downcomer area [2]
Thus the weir length,

L w = 0.76 Dc
= 0.76 0.964
= 0.733m
The height of weir determined the volume of liquid on the plate and is important f
actor in determining the plate efficiency. A high weir will increase the plate pressure drop.
For columns operating above atmospheric pressure, the weir height will normally
between 40mm to 90mm.
Take weir height,

h w = 50mm

Hole diameter,

d h = 5mm

Plate thickness,

t = 5mm

8.1.4.9 Weep point

The lower limit of the operating range occurs when it is known leakage through the plate
excessive. This is known as the weep point. The vapour velocity at the weep point is the
minimum value for stable operating. The hole area must be close so that at the lowest

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operating rate the vapour flow velocity is still well above weep point. The one that is
simplest to use and reliable is given by Chase (1967):
= K 2 -0.9(25.4-d h )
U
h
Gin 0.5

Where
h = minimum vapour velocity through the hole, m/s
dh = hole diameter, mm
K2 = constant, dependent on the depth of clear liquid on plate (from Figure 8.9[2])
It is important, to determine the maximum liquid rate that flows through the plates.
Maxliq = FLout

Minimum liquid rate (at 70% turn-down),

Min liq = 0.7 Max liq
= 0.7 3.41
= 2.387kg/s

The height of the liquid crest over the weir can be estimated using Francis weir formula.
For a segmental downcomer this can be written as,
2

Maxh ow

Max liq 3
= 750

Lout L w
2

3.41

3
= 750
967.2 0.733
= 21.37mm

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2

Minh ow

Min liq 3
= 750

Lout L w
2

2.387

3
= 750
967.2 0.733
= 16.85mm
Where
how

= weir crest, mm liq

Lw

=weir length, m

At minimum rate,

h w +Minh ow = 50 + 16.859.63
= 66.85mm

Base on Figure 8.9 (from Figure 11.30 reference [2]), K2 = 30.6

Therefore, the minimum vapour velocity can be obtained.
= K 2 -0.9(25.4-d h )
U
h
0.5
( Gin )
30.6-0.9(25.4-5)
1.560.5
= 9.08m/s
=

Actual minimum vapour velocity through holes,

70%(bottom )

U
h_actual =
Ah
0.7 1.22
0.066
= 12.94m/s
=

So the minimum operating rate velocity will be above weep point.

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Figure 8.9: Weep point correlation [2]

8.1.4.10

Pressure Drop

The pressure drop over the plates is an important design configuration. There are two
main sources of pressure loss, that due to the vapour through the holes and due to the
static head liquid on the plate. A simple additive model is normally used to predict the
total pressure drop; the total is taken as the sum of the pressure calculated from the flow
of vapour through the dry plate, the head of clear liquid on the plate, and terms account
for other, minor, sources of pressure loss, the so-called residual loss. The residual loss is
the different between the experimental pressure drop and the simple sum of the dry plate
and the clear liquid height. It accounts for two effects, the energy to form the vapour
bubbles, and the fact that an operating plate the liquid head will not be clear liquid but a
head of aerated liquid froth and the froth density and height will be different from that of
clear liquid. It is convenient to express the pressure drop in terms of mm of liquid. It is
important to estimate the bottom pressure drop before calculate the dry plate pressure
drop.
8.1.4.10.1

Column pressure drop estimation

Assume 100mm water, pressure drop per plate,

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P = 100 103 m 1000

kg
m
9.81 2 13
3
m
s

= 12753kg/ms 2 ( Pa )

Top pressure,

Ptop = 101334.6kg/ms2

So, estimated bottom pressure for the column,

Pbottom = Ptop + P
= 101334.6 + 12753
= 114087.6kg/ms 2 = 1.14bar

8.1.4.10.2

Dry plate drop

Maximum vapour velocity through hole,

U h max =

bottom
Ah

1.22
0.0554
= 22.02m/s
=

From Fig 8.10(from Figure 11.34 reference [2]) below, for thickness/hole diameter =1,
Ah Ah

= 0.1
Ap Aa
Co = 0.84

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Figure 8.10: Discharge coefficient, sieve plates (Liebson et al., 1957) [2]
The pressure drop through the dry plate can be estimated using expression derived for
flow through orifices.
2

U

h d = 51 h max Gin
Co Lout
2

18.48 1.56
= 51
0.84 967.2
= 39.81mm

Where the orifices coefficients, Co is a function of the plate thickness, hole diameter, and
the hole to perforated area ratio. Co can be obtained from Figure 8.11, which has been
adapted from a similar figure by Liebson et.al (1957), Uh max is the maximum vapour
velocity through the holes.

8.1.4.10.3

Residual head,

By using the equation Hunt (1955)

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12.5 103
hr =
Lout
12500
967.20
= 12.92mm liquid
=

8.1.4.10.4

Total plate pressure drop,

h total = h d +h r +(h w +Maxh ow )
= 39.81 + 12.92 + 50 + 21.37
= 124.1mm liquid

Since 100 mm liquid was assumed to calculate the bottom pressure. Therefore, 124.1 mm
liquid per plate is acceptable.
8.1.4.11

Downcomer Liquid Back-up

The downcomer area and plate spacing must be such that the level of the liquid and forth
in the downcomer is well below the top of outlet weir on the plate above. If the level rises
above the outlet weir the column will flood. The back-up of the liquid in the downcomer
is caused by the pressure drop over the plate and the resistance to flow in the downcomer
itself. In terms of liquid, the downcomer back-up is given by:

h b = h w +h ow +h total +h dc
The main resistance to flow will be caused by the constriction at the downcomer outlet,
and the head loss in the downcomer can be estimated using this equation;

Maxh ow
h dc = 166

Lout A m

h w = 50mm
h ap = h w 10
= 50 10
= 40mm

Where
hb

= downcomer backup, measured from plate surface, mm

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hdc

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= head loss in the downcomer, mm

Maxhow = Liquid flowrate in downcomer, kg/s

Am

=either the downcomer area, Ad or the clearance area under the downcomer, Aap,
whichever is smaller, m2

The clearance under the downcomer area is given by,

Aap = hap x Lw
Where
Downcomer pressure drop, hap = 40mm
Thus, area under apron

,
Aap = (40 103 ) 0.733
= 0.02932m 2

Ap is less than Ad (0.088), by using equation for hd,

Max liq
h dc = 166

Lout A m

3.41

= 166
967.2 0.02932
say 3mm
= 2.4mm

Applying equation for hb,

h b = h w +h ow +h total +h dc
= 3 + 50 + 21.37 + 124.1
= 198.47mm = 0.198m
1
1
( plate spacing + L w ) = ( 0.05 + 0.733)
2
2
= 0.3915m

Standard design for hb design;

hb < [0.5(plate spacing + weir height)]
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0.198 <

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1
( plate spacing + L w ) = 0.3915
2

This tray spacing is acceptable.

8.1.4.12

Residence time

Sufficient residence time must be allowed in the downcomer for the entrained vapour to
disengage from the liquid stream; to prevent heavily aerated liquid being carried under
downcomer. A time of at least 3seconds is recommended.
tr =

A d h b Lout
Max liq

0.088 0.198 967.2

3.41
= 16.85s > 3s

Where
tr

= residence time, s

hb

= clear liquid backup, m

The residence time is more than 3s, considered satisfied.

8.1.4.13

Entrainment

Entrainment can be estimated from the correlation given by Fair (1961), Figure 8.12
(from Figure 11.29 reference [2]) which gives the fractional entrainment, as the
function of liquid vapour factor, FLV with the percentage approach to flooding as a
parameter.
Uv =

bottom
An

1.22
0.642
= 1.9m/s

The flooding percentage,

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% Flooding =

Uv
U f_bottom

100

1.9
100
2.239
= 84.86%
=

Base on Figure 8.11 (from Figure 11.29 reference [2]) below, with FLVbottom = 0.0123,
= 0.15, which is below 0.1, so it is satisfactory.

Figure 8.11: Entrainment correlation for sieve plates [2]

Actual % flooding is less than 85% of estimated, thus the design is acceptable.
8.1.4.14

Trial Layout

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Use cartridge-type construction.

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Allow 50mm unperforated strip round plate edge

50mm wide calming zones.

Dc = 0.964m

Lw = 0.733

0.05m

0.964

0.733
m

0.05m
Figure 8.12: Trial layout of the plate design
8.1.4.14.1

Perforated area
From Figure 8.13 (from Figure 11.32
c = 98o

reference [2]), at

L w 0.733
=
= 0.76
D c 0.964

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Figure 8.13: Relation between downcomer area and weir length

Angle subtended at plated by unperforated strip,
s = [180 c ]o = 180 98

= 82o
Mean length of unperforated edge strips

lmean = (Dc -0.05) s
180

82
= (0.964-0.05)

180
= 1.31m
Area of unperforated edge strips

Au = 0.05 lmean = 0.05 1.31

= 0.066m 2
Mean length of calming zone (approximate),

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lcz = (Dc -h w ) sin c
2

98
= (0.964-0.05) sin
2
= 0.69m
Area of calming zones

A cz = 2(lcz h w )
= 2(0.69 0.05)
= 0.069m 2
Total area available for perforation
A p = A a -(A u + A cz )
= 0.554-(0.066 + 0.069)
= 0.419m 2

8.1.4.15

Hole Pitch

The hole pitch (distance between the hole centre), lp should not be less than 2.0 hole
diameters, and the normal range will be 2.5 to 4.0 diameters. Within this range, the pitch
can be selected to gives the number of active hole required for the total area specified.
The total hole area as a fraction of the perforated area, Ap is given by the following
expression,

d
Ah
= 0.9 h
Ap
lp

This equation is plotted in Figure 8.14 (from Figure 11.33 from reference [2]).
From Figure 8.14, when

l
A h 0.054
=
= 0.129 p = 2.65
A p 0.419
, dh

It is satisfactory within 2.5 to 4.0.

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Figure 8.14: Relation between hole area and pitch 2]

Area of one hole,

d
A hole = h
2

0.005
=
2
= 1.963 105 m 2
Number of hole

n hole =

Ah
A hole

0.054
1.963 105
= 2750.9

2751
Where
Ahole

= area of one hole, m2

dh

= hole diameter, mm

nhole

= number of hole
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Ad

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= downcomer area, m2

8.1.4.16 Height of column

Once the tray plate or tray value is optimized, the height of column can be calculated
using the following equation,
H = (N x plate spacing) + Ho
Where
Nact

= number of stage

Ho

= skirt height, estimated = 1.5m

Therefore,
H

= (0.5 x 13) + 1.5

= 8m

8.1.5 Summary of Chemical Design parameter

Table 1.2: Summary of chemical design parameter for the quenching tower
Column area

0.73m2

Column diameter

0.964m

Downcomer area

0.088m2

Active area

0.554m2

Hole area

0.0554m2

Weir height

0.733m

Hole diameter

0.005m

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Plate thickness

0.05m

Plate pressure drop

124.1mm liquid

Residence time

16.58s

% Flooding

84.86%

Hole area

1.963 x 10-5

Number of hole

2751 hole

Column efficiency

62%

Column height

8m

Mechanical Engineering Design of Quenching Tower

8.2.1 Introduction
The design of most structures states above is mainly based on factor of safety approach.
The unknown items, such as extent of yielding and material behaviour, are consider to be
provided for the use of working stresses that are admittedly below thise the member will
fail. The design parameters, which required evaluation at this stage, are material of
construction, insulation, vessel dimensions, wall thickness, ends (type, thickness) and
support

8.2.2 Vessel Function

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The vessel will be designed in accordance with the British Standard specifications for
fusion welded pressure vessel. Pressure vessel component generally consists of a few
basic parts, such as cylinder, opening and various shaped closure heads. The cylindrical
part is selected at the vessel diameter is in the size range of procurable tabular products.

8.2.3 Operating Design Pressure and Temperature

8.2.3.1 Design pressure

A vessel must be designed to withstand the maximum pressure to which it is likely to be

subjected in the operation. For vessels under internal pressure, the design pressure is
recommended to take 10% above the working pressure.
Design pressure

= (101325N/m2) x 1.1
=

0.1115N/mm2
8.2.3.2 Design Temperature

The strength of material decreases with temperature so that the maximum allowable
design stress will depend on the material temperature. The design temperature at which
the design stress is evaluated should be taken as the maximum working temperature of
the material, with due allowance for any uncertainty involved in predicting vessel wall
temperatures. Thus, the design temperature is taken as 10% above the highest
temperature of the inlet. Therefore,
T = (170 x 1.1) oC
= 187 oC

8.2.4 Material of Construction

Material of construction have an important bearing on the safe handling of chemical,
Since acrylic acid and acetic acid are highly corrosive, so we had to chose stainless steel
grade 316 as the material of construction. This is because stainless steel 316 is excellent
in a range of atmospheric environments and many corrosive media, it generally more
resistant than 304.

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8.2.5 Maximum Allowable Stress Value

In mechanical designing, it is necessary to decide the maximum allowable stress
(nominal design strength) that can be accepted as in the material of construction (stainless
steel grade 316). This is determined by applying suitable design stress factor (factor of
safety) to maximum stress that the material could be expected to withstand without
failure under standard test conditions. The design stress factor allows for any uncertainty
in the design methods, the loading, the quality of materials and the workmanship.
The approximate material standard should be consulted for particular grades and plate
thickness. From reference [6]
Design stress factor for SS316 = 1.5
Based on design temperature and material SS316,
Typical design stress

= 125.19N/mm2

Practical design stress, f = 125.19/1.5

= 83.46N/mm2

8.2.6 Welded Joint Efficiency

The strength of a welded joint will depend on the type of joint and the quality of the
welding. The value of the joint factor used in design will depend on the type of joint and
amount of radiography required by the design code. In this design, the welding joint
factor is taken as 1 implies that the joint is equally as strong as the virgin plate. Thus,
The NDT Examination = 100% Radiography
So

Joint efficiency, J = 1.00

8.2.7 Corrosion Allowance

The corrosion allowance is an additional thickness of metal to allow for material lost by
of corrosion and erosion or scaling. The allowance used should be agreed between the
customer and manufacturer. Corrosion is the complex phenomenon, and it is not possible
to give specific rules for the estimation of the corrosion allowance required for all
circumstances. The allowance should base on experience with the material of
construction under similar service conditions to those for the proposed design.
Nevertheless, 1-4 mm of allowance is used based on the different working conditions. In
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this design, the recommended corrosion allowance for absorber is taken as 3mm for
severe corrosion effect.
Corrosion Allowance, C.A = 3mm

8.2.8 Design of Thin Walled Vessel

8.2.8.1.1

Minimum practical wall thickness

The minimum wall thickness must be calculated in order to ensure that the vessel can
withstand its own weight.

PDi
2Jf- 0.2P
(0.1115N/mm 2 )(964mm)
e=
2 (1 83.46N/mm 2 ) - 0.2(0.1115N/mm 2 )
e=

= 0.64mm
Where
Di

= inside diameter of cylindrical (mm)

= design pressure, N/mm2

= joint factor

= design stress, N/mm2

Adding corrosion allowance 3mm, the minimum practical wall thickness, e= 3.64mm
But minimum thickness required for construction is 6 mm. So the minimum required
thickness of the cover is taken as 6 mm.

8.2.9 Torispherical Head Design

Torispherical head is chosen since it is most commonly used for vessel under internal
pressure less than 15bar.

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Figure 8.15: Torispherical head

Most standard torispherical head are manufactures with a major and minor axis ratie of
2:1. For this ratio, following equation can be used to calculated the minimum thickness
required.
PDi
2Jf- 0.2P
(0.1115N/mm 2 )(964mm)
e=
2 (1 83.46N/mm 2 ) - 0.2(0.1115N/mm 2 )
e=

= 0.64mm
Adding corrosion allowance 3mm, the minimum practical wall thickness, e= 3.64mm
But minimum thickness required for construction is 6 mm. So the minimum required
thickness of the cover is taken as 6 mm.

8.2.10 Design of Vessel Subject to Combined Loading

8.2.10.1

8.2.10.1.1

Dead Weight of Vessel

Shell

The approximate weight of a cylindrical vessel with domed end and uniform wall
thickness can be estimated from the following equation.

w v =Cv m Dm g (H v + 0.8D)t 103

Where wv

= total weight of shell excluding internal fittings, N

Cv

= account factor =1.08

Hv

= height between tangent lines = 2.5m

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= gravitation acceleration = 9.81m/s2

= wall thickness, 0.005m

= density of vessel material, 8000 kg/m3

Dm

= Di + e = 0.964+0.006= 0.97m

Therefore,

w v =Cv m Dm g (H v + 0.8D)t 103

= 2450N
8.2.10.1.2

Plates

Weight for a single plate,

w p = m g

Di 2
t
4

= 78N
Total weight of plates,
= 78N x 13 = 1014N
8.2.10.1.3

Insulation

Weight of insulation,
Mineral wool density

=130kg/m3

Approximate volume of insulation,

= D m height insulator thickness
= 0.39m3

Weight of insulation

=130 x 0.39 x9.81

= 500N

Total stress due to dead weight,

w

= shell + plate + insulation

= 2450 + 1014+ 500
= 3964N

8.2.10.2

Wind Loading

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Assuming maximum wind velocity 160km/hr

Vw = 160km/hr
Wind Pressure
= 0.05 x Vw2

Pw

= 1280N/m2
Mean diameter including insulation
=0.97 + 2(5 + 25) 103
= 1.03m

Loading
Fw = Pw x Mean diameter including insulation
= 860N/m
Bending moment at bottom tangent line,
860
2.52
2
= 2700Nm

M=

8.2.10.3

Analysis of Stress

8.2.10.3.1

Pressure stresses

8.2.10.3.2

= 65psi

Di

= 0.964m

= 0.05m

Longitudinal and circumferential stresses due to pressure

PDi
4t
= 13.4N/mm 2

L =

PDi
2t
= 26.8N/mm 2

h =

8.2.10.3.3

Dead weight stress

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w =

W
(Di + t)t

= 0.4N/mm 2

8.2.10.3.4

Bending stress
Do = 0.87m
Iv =

(D o 4 -Di 4 )

64
= 4.6 108 mm 4

b =

M Di

+ t

Iv 2

= 1.8N/mm 2

The resultant longitudinal stress is

x = L + w b
x is compressive and therefore negative

x (upwind) = L + w + b
= 14.8N/mm 2

x (downwind) = L + w b
= 11.2N/mm 2
As there is no torsional shear stress, the principle stresses will be x and h .
18.9

7.1

26.8

28.8

Upwind

Downwind

Figure 8.16: Analysis of stresses

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The greatest different between the principle stress will be on the downwind side
26.8-7.1 = 19.7 N/mm4
Maximum allowable design stress

= 12700psi

=86.4N/mm2

So, well below the maximum allowable design stress

8.2.10.3.5

Check Elastic Stability (Bucking)

Critical buckling stress

t

Do
161.3N/mm 2

c = 2 104

The maximum compressive stress will occur when the vessel is not under pressure =
0.4+1.8= 2.2N/mm2, so the design is satisfactory.

8.2.11 Design of Skirt Support

Skirt is the most frequently used as support for vertical vessel. It is attached by
continuous welding to the head and usually the required size of this welding determines
the thickness of the skirt. Code UW-12 may be used. The minimum thickness for a skirt
is 1/4 in (6.25mm).
In the design, the butt weld joint is chosen.
Outside diameter of skirt, Ds = 1.03m
Butt weld joint factor, R
8.2.11.1

8.2.11.1.1

=0.6

Operating weight

Weight of Full Liquid

Column dimensions
Di

= 0.964m
Hv

=8m
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Density of liquid

= 967.2kg/m3

Volume of shell,

( Di )

4
= 5.83m3

Hv

From reference [5], the volume of 2 torispherical heads are:

Vh

= 2 x 0.65 ft3
= 0.37m3

Volume of full liquid,

5.83 + 0.37
= 6.2m3
Weight of full liquid,

= 6.2 L g
= 5996.64N

8.2.11.1.2

Weight of skirt

Material of skirt = Carbon steel SA-283 Grade C

Density of material

= 8000kg/m3

ts

= 6.25 mm

= 9.81mm

Minimum thickness of skirt

Gravitational constant

Height of skirt

hs

= 1.5m

Dm

= 0.97m

Mean of diameter

Weight of skirt

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w s = D m m gt s h s
= 2242.1N

Vessel weight,

wo

= shell + plate + insulation + skirt + full liquid

= 12202.74N
8.2.11.2

Thickness of Skirt

Wind pressure, Pw
Wind load, Fw

= 1280N
= 860N/m

Height from bottom, hb

= 8m

Bending moment at bottom tangent line

860 2
8
2
= 27520Nm

MT =

With

Do
E

= 620mm
= 0.62
Mt

= 27520Nm

Ro

= 310mm

Sr

= 86.4N/mm2

wo

= Operating weight

C.A

= 3mm

Required thickness of skirt, ts

ts =

wo
MT 1000
+
+ C.A
2
R o SrE Do SrE

= 6mm
So the minimum thickness of skirt 6.25mm is acceptable.

8.2.12 Opening
There are 4 nozzles attached to the column, 2 nozzles on the shell of column for gas
stream and 2 nozzles for the liquid streams. An approximate of the economic pipe
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diameter for normal pipe runs can be developed from an expression for stainless steel.
d opt = 226G 0.5 0.35

Where
dopt

= optimum pipe diameter

= mass flow rate, kg/s

= density, kg/m3

The equation above is carried to determine the piping size for the 4 streams. The
calculation is summarized in the Table 8.6 below.
Table 8.3: Piping system
Gas In

Gas Out

Liquid In

Liquid Out

No of nozzles

Flow rates, G(kg/s)

9.74

11.14

2.00

3.41

Density, (kg/m3)

994.3

1.55

0.92

967.2

Optimum diameter, dopt (mm)

62.89

647.05

329.08

37.63

Nominal pipe size(in)

2.5

30

14

1.5

Outer diameter, do (mm)

73.02

762

355.6

48.26

Inner diameter, di (mm)

65

750

350

40

Thickness, hi(mm)

5.156

9.53

9.53

3.683

Note that the nominal pipe size, OD and ID for each nozzle is obtained from Perry
Chemical Engineering Handbook, Chapter 10[1].

8.2.13 Design of Manhole

The requirements for provisions and dimensions of sight hole, handle, head hole and
manhole opening into static and mobile pressure vessels are specified in BS470 Series.
One manhole accordance with Table 8.7 BS470:1984 for vessel inner diameter over 1.5m,
located on vessel shell and bottom of the column. The dimensions of manholes are
selected based on BS 470 1984 the minimum size to afford full rescue facilities with selfcontained breathing apparatus shall inner diameter, Dim = 575mm and length =500mm.

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Minimum thickness of manhole,

PDim
2Jf- P

e=

(0.1115N/mm 2 )(575mm)
2 (1 83.46N/mm 2 ) - 0.2(0.1115N/mm 2 )

= 0.38mm

Adding corrosion allowance 3mm, the minimum practical wall thickness, e= 3.38mm
But minimum thickness required for construction is 6 mm. So the minimum required
thickness of the cover is taken as 6 mm.

8.2.14 Design of Anchor Bolt

8.2.14.1 Design anchor bolt

A simplified method for the design anchor bolts is to assume the bolts being replaced by
a continuous ring which diameter is equal to the bolt circle. The required area of bolts
shall be calculated for empty condition of column.
Empty weight of column
Wm

= Operating weight full liquid weight\

= 6206.1N

Maximum allowable stress

Sm

= 15000psi
= 102N/mm2

MT

= 27520Nm

Assume bolt circle = 625mm

Area within the bolt circle,
6252
4
= 306800mm 2

As =

Circumference of circle,
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Cb

= x 625
= 1963mm

Number of anchor bolts

N = 4 (for both circle 25 inch)
Maximum Tension
T=

1000MT Ws

AB
CB

= 14.93N/mm
Required area of one bolt
BA =

T Cs
SB N

= 71.8mm 2 (0.115in 2 )

From Table A in page 63 of reference [5]

The root area of 0.5 in bolt size is 0.126 in2. Adding 0.125in for corrosion, use 4(5/8 in)
size both.
8.2.14.2 Checking stress in anchor bolt

CB = 0.126 in2 (28.75mm2)

SB =

T Cs
BA N

= 93.04N/mm 2

Since the maximum allowable stress is 100 N/mm2, the selected number and size of bolts
are satisfactory.

8.2.15 Design of Base Ring

8.2.15.1

Design base ring

Area of base ring

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( d o 2 d12 )

AR =

4
= 0.072m 2

Area within the skirt

As =

Do 2

4
= 0.302m 2

Circumference on O.D of skirt

Cs = Do
= 1948mm
Safe bearing load on concrete

fb = 500psi(for design)
= 3.45N/mm 2
Moment at the base due to wind
MT = 27520N
Operating weight
wo =6206.06N
Maximum compression
Pc =

1000 MT Wo
+
As
Cs

= 24N/mm
Approximate width of base ring
l1 =

Pc
fb

= 6.75mm
But the minimum dimension for l1 = 38.55mm
So take the greater
l1 = 38.55mm
Approximate thickness of base ring

t b = 0.31 l1
= 12.34mm
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Use 0.5 in (12.5mm) thick base ring

8.2.15.2

Checking Stress

Bearing stress
S1 =

Pc C s
AR

= 0.63N/mm 2

Bending stress
S2 =

3 S1 l1
t B2

= 18.45N/mm 2

Use carbon steel SA-283 Grade C for base ring, allowable stress of 86.4N/mm2 can be
taken for structural purposes. Thus the width and thickness of the base ring are
satisfactory.

8.2.16 Design Parameters

Table 8.4: Mechanical design parameter for quenching tower
Designed Column Dimensions

Inside diameter

0.964m

Column height

8m

Shell thickness

0.005m

Corrosion allowance

0.003m

Dead Weight Load

Weight of shell

2450N

Weight of plates

1014N

Weight of insulation

500N

Weight of skirt

2242.1N

Skirt Support Design

Material of construction

Carbon steel SA-283 Grade C

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Maximum allowable stress

86.4N/mm2

Skirt height

1.5m

Outer diameter

1.03m

Joint factor

0.6

Type of joint

Butt weld joint

Skirt thickness

0.00625m

Anchor Bolt Design

Material of anchor bolt

Carbon steel SA-283 Grade C

Maximum allowable stress

102N/mm2

Number of bolts

Bolts diameter

0.625in

Base Ring Design

Material of bolt ring

Carbon steel SA-283 Grade C

Maximum allowable stress

86.4N.m2

Base ring thickness

0.5in

Outer diameter

1.15m

Inner diameter

0.96m

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Safety, Control & Instrumentation of Quenching Tower

8.3.1 Safety Analysis

8.3.1.1 Introduction

Hazard is always connected with accident. Hazard always present in a chemical plant. It
is an advantage if we could identify in advance and take extra precaution step before
hand. Unfortunately, it is difficult to identify hazard before accident occur, and this is
very risky and costly. So it is essential to develop a mechanism in order to identify
hazards that could threat the plant operation. There are several methods available for
performing hazard identification and risk assessment. Four commonly practiced hazard
identification methods are:
1. Process hazard checklist
2. Hazard surveys
3. Hazard and operability study (HAZOP)
4. Safety review
8.3.1.2 Hazardous and operability study

In assessing hazard in a unit operation, HAZOP is the most reliable method because:
9 It is very specific and objective but in the same time promotes the freedom flor of

thought.
9 It is considers various event and situation for the unit operation with prediction of

failure and action required.

HAZOP study requires a committee with several experts in their field. The HAZOP
procedures use the following steps to complete an analysis.
i.

Break flow sheet into unit operation. In this case, a quenching tower.

ii.

Choose a study mode.

iii.

Pick a process parameter: flow, temperature, pressure, concentration.

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iv.

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Apply guide word to the parameter to suggest possible deviation (I.e. no, less,
high, etc.) The usage of guide word varies with different parameter.

v.

Determine possible causes and note any protectable systems.

vi.

Evaluate the consequences (if any) and recommended action.

The full HAZOP study have been done and compiled at the appendix 8. With all the
study node and parameter applied with the appropriate guide word.
8.3.1.3 Conclusion

Process specification resulting for the HAZOP studies are as the following:
1. Installation of controller valve in each stream
2. Installation of a backup controller valve to all steam in case of the controller valve
failure.
3. Installation of High Pressure Alarm (PAH), Low Pressure Alarm (LAL), and High
Level Alarm (LAH) to alert the operator in case of emergency or deviation in the
process.
4. Installation of gas detector and alarm in case of any leakage or spill in order to let the
operator aware.
5. Installation of check valve in every line to prevent reverse flow.
6. Installation of pressure indicator to line gas feed.
7. Ensure maintenance on equipment and pipeline are kept done often.
8. Installation of temperature indicator.

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8.3.2 Control and Instrumentation

8.3.2.1 Introduction

Control system is the essential part of chemical engineering operation. In all processes, it
is a must to keep all the parameters such as temperature and flow to be in a certain
boundary in order to ensure a safe and compatible process. Automatic control is most
desired because manual control (human operated) will definitely have a lot of down fall.
Basically, process control is done by measuring the variable that we desired to control
(variable), comparing the value with the desired set point, and adjusting a control variable
which has a direct effect on the control variable.
The objective of process control is to ensure safety in process, environmental protection,
to meet the product specification, economics factor, and the final one, to overcome
process limitation.
8.3.2.2 Control of quenching tower

Objectives:
To ensure the liquid level (h) in the column base at desired value.
To ensued the pressure (P) at desired balue.
To keep the desired value of bottom product (B)
8.3.2.3 Control variable and parameter

Table 8.5: Control variable and parameter

Control

Measured

Manipulated

Description

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variable
Flow rate of

variable
Liquid inlet flow

variable
Gas inlet flow

gas out

rate

rate

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Liquid flow rate can be measured directly

using sensor.
Effect of this flow rate on gas out flow and

concentration is directly and fast

Liquid level

Liquid level

Flow rate of

Fast level control can be achieved by

existing liquid

measuring h and manipulating flow rate od

stream

existing liquid stream

High level alarm (LAH) and low level alarm

(LAL) are installed as safety precautions.

LAL and LAH enable immediate action taken
by operator to control the level if the valve at
the existing liquid stream is out of function.
Temperature

Temperature

Flow rate of
water

Deviation in temperature will alter the

process

In this design procedure, two type of controller is used. Ration controller between two
feed steam is used since the ratio of those twp parameter is known and can be set within
the operation. Other streams are controlled by feedback controller.
The ratio control and feedback control loop can be summarized as Figure 8.19 and Figure
8.20. Both controllers will ensure the operation condition operates as normal.
Ratio controller was chosen because it is the simplest way to maintain the required ratio
of inlet liquid and vapour. Since the required ratio between liquid and vapour is known.

Ratio controller operates by maintaining two flows by taking flow reading of one stream
(wild stream) and controlling the other. Feedback control is use on other stream in order
to retain the three parameters define above. The full control of quenching tower is shown
is Figure 8.20.

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+
GC

GF

GP

+
GM

Figure 8.18: Feedback control loop in quenching tower

GP
+
Gm1

Kr

GC

GV

+
Gm2

Figure 8.19: Ratio control loop in absorbed

8.4

NOMENCLATURES
Dimension
MLT

Aa

Active area

L2
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Ac

Column area

L2

Ad

Downcomer area

L2

Ah

Hole area

L2

An

Net area

L2

Ap

Total area available for perforation

L2

As

Area of unperforated edge strip

L2

Av

Cross sectional area

L2

Az

Calming zone area

L2

Co

Constant

Dc

Actual column diameter

Column diameter

dh

Hole diameter

hb

Backup in downcomer

hd

Dry plate drop, head of liquid

ho

Weir height

ht

Total plate pressure drop, head of liquid

hap

Area under apron

L2

hdc

Head loss in downcomer

how1

Maximum height of liquid crest over the weir

how2

Minimum height of liquid crest over the weir

K1, K2

Constant

Lm

Minimum liquid rate

Ls

Molar flow rate of solute free liquid per unit cross section
area

MT
ML-2T-1

hw

Weir length

Number of holes

Operating pressure

Operating temperature

Plate thickness

tr

Residence time

Ur

Velocity of feed

LT

L
ML-1T-2

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Uh

Maximum vapour velocity

LT

Uw

Gaseous flow rate

LT

Uac

Velocity at actual percentage of flooding

LT-1

Vs

Volume of gas in S.T.P

Mol of solute _ per mol of solvent in liquid phase

Mol fraction _ in liquid phase

Mol solute _per mol inert gas without _ in gas phase

Mol fraction _ in gaseous phase

Constant

Fractional entrainment

Density of liquid

ML-3

Density of vapour

ML-3

A1

Area of excess vessel

L2

A2

Area of excess nozzle

L2

A3

Area of inside extension of nozzle

L2

A4

Area of weld

L2

A5

Area of reinforcement pad

L2

AB

Area within the bolt circle

L2

AR

Area of base ring

L2

AS

Area within the skirt

L2

BA

Area of one bolt

L2

Cv

Account factor

C.A

Corrosion allowance

Cb

Bolt circle circumference

Cs

Outer skirt circumference

Di

Inner diameter of quenching tower

Inner diameter of pad

Dm

Mean diameter of quenching tower

Do

Outer diameter of quenching tower

Outer diameter of pad

Inner diameter of opening

Dipad

Dopad
d

L3

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Chapter 8: Quenching Tower

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Acrylic Acid Project

di

Inner diameter of base ring

do

Outer diameter of base ring

Joint factor

Fw

Wind loading

MT2

Thinning factor

fb

Safe bearing load on concrete

Gravitational acceleration

Ht

Column height

Hv

Height between tangent lines

hb

Height from bottom

hs

Height of skirt

Inside radius of dish

Total bending moment

ML2T-2

Bending moment at base due to wind

ML2T-2

MT

LT-2

Number of anchor bolts

Design pressure

ML-1T-2

Pc

Maximum compression

ML-1T-2

Pw

Wind pressure

ML-1T-2

Ri

Inner radius of quenching tower

Inner radius of knuckle

r
S1, S2

Bearing stress

ML-1T-2

Sa

Maximum allowable stress (base ring)

ML-1T-2

Sr

Maximum allowable stress (shell and head)

ML-1T-2

Thickness of wall less C.A

tb

Required thickness of base ring

ta

Thickness of pad less C.A

tn

Nominal thickness of shell and head

tr

Required thickness of shell and head less C.A

ta

Required thickness of skirt

trn

Required thickness of nozzle

Pad thickness

tpad

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Chapter 8: Quenching Tower

8.5

Group 6
Acrylic Acid Project

tmin

Minimum thickness

Design temperature

Tt

Maximum tension

MT-2

Vh

Volume of torispherical head

Vw

Maximum wind speed

Total dead weight

MLT-2

Wa

Empty column weight

MLT-2

Wa

Operating weight

MLT-2

Wo

Weight of plates

MLT-2

Wv

Total weight of shell

MLT-2

Liquid density

ML-3

Vessel material density

ML-3

Bending stress

ML-1T-2

Critical buckling stress

ML-1T-2

Circumferential stress due to pressure

ML-1T-2

Longitudinal stress due to pressure

ML-1T-2

Dead weight stress

ML-1T-2

Resultant longitudinal stress

ML-1T-2

L3
LT-2

REFERENCES

1. R.E. Treybal, Mass Transfer Operation, 3rd Edition, McGraw Hill.

2. Coulson, J.M and Richardson, J.F, An Introduction to Chemical Engineering
Design, Chemical Engineering Series, Vil 6 by Sinott R.K, Pergamon Press.
3. Perry, J.H and Chilton, C.H., Chemical Engineers Handbook, 5th Edition, McGraw
Hill, 1973.
4. Stanley M. W., Chemical Process Equipment: Selection and Design, ButterworthHeinemann.
5. Eugene F. Megyesy, Pressure Vessel Handbook, Pressure Vessel Handbook
Publishing Inc.
6. American Society of Mechanical Engineers (A.S.M.E. Codes)

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Chapter 9: Extractive Distillation Column

Group 6
Acrylic Acid Project

CHAPTER 9: EXTRACTIVE DISTILLATION COLUMN

9.1: CHEMICAL ENGINEERING DESIGN
9.1.1 Introduction
Distillation is the most widely used separation technique in the chemical process industries. Not
all liquid mixtures can be separated by ordinary fractional distillation, however when the
components to be separated of system have relative volatilities of close to 1.00 (i.e. close boiling
mixture), separation becomes difficult and expensive because a large number of trays and a high
reflux ratio are necessary.

In this case, extractive distillation is used. The extractive distillation column works because an
heavy solvent is specially chosen to interact differently with the components of the original
mixture, thereby altering their relative volatilities.

In our Acrylic Acid production plant, in order to produce acrylic acid which is our product purity
up to 99.7%, we have decided to use extractive distillation column with the recovery of solvent
system in our separation section.

9.1.2 Objective
The objective of this design project is to design a extractive distillation column which can
remove the impurities mainly are acetic acid and water from the acrylic acid with the highest
purity of acrylic acid and lowest energy consumption.

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Chapter 9: Extractive Distillation Column

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Acrylic Acid Project

9.1.3 Process Description

Figure 9.1: Flow Diagram for Extractive Distillation Column

The liquid stream consists of acrylic acid, acetic acid and water is fed into extractive distillation
column. The solvent used is a mixture of cyclohexane and isopropyl acetate. The solvent and
polymer inhibitor with higher density is fed from top while the liquid stream is fed from bottom.
Under solvent extraction acetic acid will be extracted by the solvent and leave at the top along
with water. Acrylic acid discharged at the bottom of the column as raffinate is pure acrylic acid
with 99.7% purity. The solvent along with the extracted acetic acid and water is a two phases
liquid with water phase and solvent phase. The mixture is fed into decanter with water is
separated and recycle. The solvent and acetic acid is then fed into solvent recovery distillation
column. The solvent with 99.8% is recovered and recycle back to extraction distillation column.

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Chapter 9: Extractive Distillation Column

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9.1.4 Selection of Column

9.1.4.1 Selection of Internal Column
Table 9.1: Comparison between Plate Column and Packed Column

Plate Column

Packed Column

Wider range of liquid and gas flow rates

Lower liquid flow rates.

For higher column diameter

For small column diameter

Higher pressure drop

Lower pressure drop

Higher liquid hold up

Lower liquid hold up

Non-corrosive liquid

Corrosive liquid

Packed column is chosen because:

The feed liquid is flammable liquid which required low liquid hold-up for safety reason.

More economical when the diameter of the column is low.

The pressure drop in packed column is lower which more suitable for low pressure
system.

9.1.4.2 Packing Selection

Table 9.2: Comparison between Random Packing and Structured Packing

Random Packing

Structured Packing

Easy separation which significant different Close boiling point separation

between boiling point of the components.
Low cost

High cost

Random packing is chosen because:

More economically

Boiling point between the water, acrylic acid and acetic acid is significant.

9.1.4.3 Random Packing selection

Basically random packing grouped into 2 groups, rings and saddles. Intalox saddle is chosen due
to following reasons:

It gives a better liquid distribution and larger free area.

Lower manufacture cost.

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Chapter 9: Extractive Distillation Column

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9.1.5 Packed Column Design

9.1.5.1 Selection of Solvent
The solvent used is a mixture of cyclohexane (45%) and isopropyl acetate (55%) which is
preferentially extracts the water and acetic acid from acrylic acid stream. Besides that it is noncorrosive and it has relatively low cost.

9.1.5.2 Composition and condition of feed stream, distillate and bottom

Table 9. 3: Molar Flow Rate of the Inlet Streams and Outlet Streams of Extractive Distillation Column

Component

Make up solvent

From Quenching Tower

Top

Bottom

(kmol/hr)

(kmol/hr)

(kmol/hr)

(kmol/hr)

Acrylic acid

0.00

125.67

1.32

124.36

H2O

0.19

162.58

162.62

0.15

Acetol

0.00

0.13

0.00

0.13

Acetic Acid

0.32

4.43

4.69

0.06

Acrolein

0.00

0.14

0.14

0.00

Cyclohexane

191.25

0.00

191.25

0.00

i-p-Acetate

233.75

0.00

233.75

0.00

Table 9.4: Operating Condition of the Inlet Streams and Outlet Streams of Extractive Distillation Column

Parameter

Make up solvent

From Quenching Tower

Top

Bottom

32

72.88

35.68

87.87

101.3

101.3

15

15

Temperature
(C)
Pressure
(kPa)

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Chapter 9: Extractive Distillation Column

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9.1.5.3 Number of theoretical stages, N

Table 9.5: Equilibrium Data for Raffinate Phase

Extracted

Solvent

(water + acetic acid) %

(cyclohexane and isopropyl acetate) %

67.1

17.6

41.8

9.9

10.8

2.3

2.7

0.34

Table 9.6: Equilibrium Data for Extracted Phase

Extracted

Solvent

(water + acetic acid) %

(cyclohexane and isopropyl acetate)%

11.23

78.5

51.6

46.9

46.7

9.1

18.8

2.1

We can find the equilibrium data of the solvent and extract and plot equilibrium curve for the
system. By using flow rate and composition of feed, solvent, extracted phase and raffinate phase,
we can get number of stages from the equilibrium curve. The number of theoretical plate obtain
is 10 stages.

9.1.5.4 Optimum Feed Location

The stream from quenching tower is fed at the bottom stage of the extractive distillation column
and the solvent is fed at the top stage of the extractive distillation column to achieve highest
purity of acrylic acid.
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Chapter 9: Extractive Distillation Column

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9.1.5.5 Optimum reflux ratio

Table 9.7: Purify of Product with vary Reflux Ratio

Reflux Ratio

Purify of Acrylic Acid

2.5

99.697%

3.0

99.725%

3.5

99.745%

With increasing of reflux ratio, the purify of Acrylic Acid can be increased. However the power
required is increase which cost a lot. Therefore reflux ratio 3.0 is chosen since our product target
is higher than 99.7% and it is more practicable by using reflux ratio as 3.0.

9.1.5.6 Column Diameter

Flow parameter,

0.2

For distillation column, the pressure drop is between 40 to 80mm water/m of packed height.
Thus, a pressure drop of 80mm H2O/m packed height was chosen in this design.

Figure 9.2: Flooding and Pressure Drop in Packed Column

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Chapter 9: Extractive Distillation Column

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K4 at pressure drop 80mm water/m = 1.5

K4 at flooding = 2.3
Percentage flooding =

1.5
100% = 80.7%(< 90%) -Acceptable
2.3

Packing diameter = 51mm

Packing Factor = 130
K 4 v ( L v )
Flow rate per unit column cross-sectional area, Vw =
13.1 Fp ( L / L )0.1

Required Area, A =

0.5

= 14.24kg / m 2 s

V
= 0.844m 2
Vw

Column Diameter, D =

4A

= 1.03m

The calculated column diameter is acceptable to avoid poor liquid distribution as the value is
higher than 0.9m for packing size of 51mm. Hence, the new column area = 0.85m2. Ratio of
column diameter/packing diameter (Dc/dp ) = 20.6 > 15 (acceptable). For saddles, the ratio
should be greater than 15 to ensure good liquid and gas distribution in the packing column.

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Chapter 9: Extractive Distillation Column

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9.1.5.7 Height of Packed Zone

Norton correlation is used to predict the height of theoretical plate (HEPT) packed zone.

HEPT = n 0.187 ln 0.213ln

Figure 9. 3: Table Constant for TETP Correlation

n = constant for HEPT correlation = 1.72330

Height of a Theoretical plate = 1.53
Column height = 15.3m
9.1.5.8 Wetting rate
The minimum wetting rate for random packing should be larger than 2x10-5m2/s to have good
contact between liquid.
Minimum wetting rate=

B
= 0.0147 m 2 s 1 (>2x10-5m2/s)
L AC

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Chapter 9: Extractive Distillation Column

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9.1.5.9 Liquid Hold-up

The void space in a packed bed is occupied by vapor and liquid during operation. A sufficient
amount of holdup can represent an incipient flooding condition. There are two different types of
liquid holdup in a packed bed which is static and operating.
Static hold up represents that volume of liquid per volume of packing that remains in the bed
after the gas and liquid flows stop and the bed has drained.
hs = 2.79

C1 C2 C3

l 0.37

where C1 =0.0055, C2 =0.04 and C3 =0.55 for saddles

Operating holdup is that volume of liquid per volume of packing that drains out of the bed after
the gas and liquid flows to the column stop.

1/3

u
2
ho = 22 L L 2 + 1.8 L
g d
gd
L p
p

1/2

Where L = liquid superficial velocity

g = gravitational constant = 9.81m/s2
dp = nominal packing size = 0.051 m
hs = 0.009
ho = 0.08
Total liquid hold up is the sum of the static holdup and the operating hold up.
ht = hs + h0 =0.089
9.1.5.10 Operating Void Space

The operating void space is the actual space that available for the gas to pass through the packed
bed during the operation. Hence, the effective void space o = ht = 0.69

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Chapter 9: Extractive Distillation Column

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Acrylic Acid Project

Table 9.8: Extractive Distillation Column Design Summary

Column Diameter, Dc

1.03 m

Packed bed height, Z

15.3m

Flooding percentage

80.7 %

Wetting Rate

0.0147 m2/s

Total liquid hold-up

0.089 m3

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Chapter 9: Extractive Distillation Column

Group 6
Acrylic Acid Project

9-1: MECHANICAL ENGINEERING DESIGN

9.2.1 Introduction
Basically mechanical design of the column includes three main stages below:

Material of construction including design pressure and temperature, construction

materials, design stress, welded joint factor and corrosion allowance.

Fittings which including internal column fitting, manhole, pipe sizing, safe pressure and
compensation for opening.

Column design which include cover thickness of cylindrical shell, vessel head, vessel
height, dead load of vessel, wind load and analysis of stresses.

9.2.2 Material of construction

9.2.1.1 Design Pressure

The vessel must be designed withstand the maximum operating pressure, which is generally 1015% more than the maximum operating pressure.
Design pressure = 101325Pa x 110% = 111457.5Pa

9.2.2.2 Design temperature

The strength of metals decreases with increasing temperature.

Design temperature = 87.57 x 110% = 96.33C

9.2.2.3 Material of construction

Stainless steel is the most suitable construction material for the extractive distillation column to
provide better corrosion resistance. For the vessel support and piping, carbon steel is used
because it easy to fabricate, ductility, cheap, high yield and tensile strength.

9.2.2.4 Design stress

The design stress is a value for the maximum allowable stress that can be accepted in the
material of construction, so that the material could be withstand without failure under standard
test conditions. A design stress factor of 1.5 is applied to the maximum stress. The design stress
for the design temperature is 150N/mm2.
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Chapter 9: Extractive Distillation Column
The design stress f =

Group 6
Acrylic Acid Project

150
= 100 N / mm 2
1.5

9.2.2.5 Welded joint factor

The column requires 100% non-destructive testing of weld. The welded joint factor is taken as
1.0 by assuming the joint is quality and strong.

9.2.2.6 Corrosion Allowance

The corrosion allowance is the additional thickness of metal added to allow for material lost by
corrosion and erosion, or scaling. According to Corrosion Data Survey by NACE, the tendency
of pitting corrosion is 0.005in deep per year. Assuming the system is run for 10 years, the
minimum corrosion allowance is 1.270mm. We take it as 2mm for the corrosion allowance.

9.2.3 Internal Fitting

9.2.3.1 Packing support

The primary function of the packing support plate is to serve as a physical support for the tower
packing

9.2.3.2 Vapor distributor

In this packed columns need no vapor distribution devices.

9.2.3.3 Hold down plate

It also called bed limiter. It used to provide space to permit gas disengagement from the packed
bed.

9.2.3.4 Liquid distributors

Liquid distributors is required at the location where liquid stream is introduced. It provide
uniform liquid distribution pattern to the packed bed.

9.2.3.5 Liquid redistributors

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Chapter 9: Extractive Distillation Column

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Redistributors are used to collect liquid that has migrated to the column walls and redistribute it
evenly over the packing. It should be installed for every 3m of packing to prevent channeling of
liquid.

9.2.3.6 Mist eliminator (Demister)

It can be designed for up to 99% removal of liquid droplets and it is located at above of the liquid
feed pipe. The pad height of the mesh droplet separators in most application lies between 100
and 150mm. it consists of coils or layers of knitted wire mesh. They are usually held together by
top and bottom support grids.

9.2.3.7 Support ledges

The plates in the tower internal are designed to rest on a ledge. This ledge should be level and
perpendicular to the towers vertical axis and flat to provide a uniform load-bearing surface.

9.2.3.8 Manhole

Three manholes are provided for cleaning, maintenance and inspection. The manholes with
diameter 500mm are located at top, middle and bottom of the extractive distillation column.

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Chapter 9: Extractive Distillation Column

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9.2.4 Column Design

9.2.4.1 Cylindrical Shell Thickness

The minimum cylindrical shell wall thickness that sufficiently rigid to withstand its own weight.
Temperature (C)
20
150
87.97

Young Modulus E (N/mm2)

202000
192000
196800

Inner Diameter, Di = 1.03m

Outer Diameter, Do = Di + 2t
L = effective length between the ends = 0.4m
Kc = collapse coefficient

Assume t = 4 mm
Do/t = 155
L/Do = 0.26
Kc = 25

Pc = K c E (

t 3
) = 1.37N/mm2 (> design pressure)
Do

By taking wall thickness of the column with corrosion allowance 2mm, the wall thickness will be
6mm.

9.2.4.2 Vessel Head

A hemispherical head is the strongest shape, it capable of resisting about twice the pressure of a
torispherical head of the same thickness but the cost is higher. A torispherical head of Korbbogen is

chosen as vessel head due to its economical factor since in this design is not high pressure
system. The optimum thickness ratio is basically taken as 0.6. Thus, the head thickness is 0.6 x (shell
thickness + corrosion allowance) = 5mm.

9.2.4.3 Vessel Height

The height of the column is determined by summing up height of packed zones as well as the
internal fittings and vessel head.

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Chapter 9: Extractive Distillation Column

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9.2.4.4 Flange

Flange is a short cylindrical section between the cylinder body and the formed domed head. This
ensures that the weld line is away from the point of discontinuity between the head and the
cylindrical section of the vessel.

9.2.4.5 Load Analysis

9.2.4.5.1 Dead Weight loads

For loads Analysis, dead weight loads and wind loads is considered. The major sources of dead
weight loads are vessel shell, internal and external fittings and insulation. In the design, the dead
weight loads is 20.5 x 103N.

9.2.4.5.2 Wind load

The wind load imposed on any structure by the action will depend on the shape of the structure
and the wind velocity. By using wind speed of 160 km/h (equivalent to wind pressure of 1280 N/m2)
for preliminary study, the wind load per unit length of column estimated, Fw, is 371.456N/m.

9.2.4.6 Stress analysis

A number of stress conditions can occur simultaneously during the normal operation of the
vessel. The standard procedure is to sum up all the stresses to determine the total stress on the
pressure vessel. The total stress with the largest magnitude will be the expected stress applied to
the vessel and this stress must not more than the maximum allowable stress. The type of stress
including pressure stress, longitudinal stress, circumferential stress, dead weight stress and
bending stress. The maximum compressive stress must be lower than critical bucking stress. In
this design, the maximum compressive stress is 49.8N which is lower than the critical bucking
stress, 349.18N.

9.2.4.7 Support
The method used to support a vessel will depend on:

Size, shape, and weight of the vessel

The design temperature and pressure

The vessel location and arrangement

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Chapter 9: Extractive Distillation Column

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The internal and external fittings and attachments

Skirt support is used for the tall, vertical columns, as they do not impose concentrated loads on
the vessel shell. Brackets support is chosen as vessel support since it is normally used to support
short vertical vessel that is less than 20m height. It is more economical to use compare to the
skirt support.

9.2.4.8 Pipe Sizing for Nozzles

For stainless steel pipe, the optimum diameter is given by equation:

dopt = 226G 0.5 0.35

Where dopt = optimum diameter in mm, G=fluid flow rate and =density of the fluid.
Streams

dopt
(inch)

Feed
Extracted
Raffinate
Solvent

0.1095
0.0703
0.0994
0.0923

Nominal
pipe size
(in)
0.125
0.125
0.125
0.125

do (in)

0.405
0.405
0.405
0.405

Wall
Schedule
thickness
no.
(in)
40ST,40S 0.068
40ST,40S 0.068
40ST,40S 0.068
40ST,40S 0.068

di (in)

0.269
0.269
0.269
0.269

do
(mm)

di
(mm)

10.287
10.287
10.287
10.287

6.8326
6.8326
6.8326
6.8326

9.2.4.9 Reinforcement of Openings

All the openings such as nozzle connections for piping and the openings for inspection above 2
in diameter are reinforced to compensate for the weakening effect of the openings.

Streams

do (mm)

di(mm)

hi(mm)

l(mm)

ho(mm)

t(mm)

All

10.2870

1.7272

6.8326

1.6891

2.8258

7.2232

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Chapter 9: Extractive Distillation Column

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9-3: SAFETY, CONTROL AND INSTRUMENTATION

9.3.1 Introduction
Control system for the extractive distillation column is important to provide a safe and
health environment to the operator. It also help to protect the environment from pollution since it
can avoid spillage of toxic chemical.

9.3.2 Control
Process control of the extractive distillation column is important to maintain the product quality
and ensure stable operation. Proper control system also important to avoid overflow of chemical
and flooding in the extractive distillation column.

Figure 9.4: Flow Diagram with Controller

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Chapter 9: Extractive Distillation Column

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Table 9.9: Control System for Extractive Distillation Column

Loop

Controlled

Manipulated

Objective

Controller

variables

variables

Liquid level

Feed flow

avoid overflow

Solenoid valve

in column

rate, Solvent

Avoid dry hole problem.

Flow transmitter

feed flow rate

Ensure column work in

Flow Controller

Pressure

flow rate required and

maintain the composition
of the bottom product
(quality product).
2

Column

Feed flow

Pressure

rate, solvent

the column which may

flow rate

break the column.

Avoid excess pressure in

transmitter
-

Ensure the purity of

product since the

Pressure
Controller

Safety valve

Temperature

composition of the outlet

stream will vary with
different pressure
3

Bottom

Steam flow

temperature

rate

To ensure efficient
separation.

To maintain product

transmitter.
-

quality

Temperature
Controller

Flow transmitter

Flow controller

Solenoid valve

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Chapter 9: Extractive Distillation Column

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9.3.3 Safety

Safety analysis is important to ensure all people who operate the column are in safe condition
and minimize the accident occur.

9.3.3.1 HAZOP analysis

A Hazop and Operability Study (HAZOP) is a set of formal hazard identification and elimination
procedures designed to identify hazards to people, process plants, and the environment. It can
predict all the potential accident.

Table 9.10: HAZOP Analysis

Guide

Deviation

word

No

Possible

Consequences

Actions

Causes

No Flow

Pipe

blockage

Pipe burst due to -

Install flow indicator and

overpressure in

alarm.

the pipeline.
-

No product

Install pressure indicator and

alarm

Perform regular checking on

the pipe line

Failure

of -

solenoid

overpressure in

valve

the pipeline.
-

More

More flow

Pipe burst due to -

Failure

of -

flow
transmitter

Install manual bypass valve.

No product
Purify

of -

Regular checking on the flow

product affected.

alarms.

Low efficiency -

Install high level alarm.

separation.
More

Failure

Pressure

solenoid
valve

of -

Purify

of -

Regular

checking

on the

product affected.

pressure alarms.

Low efficiency -

Install high pressure alarm.

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Chapter 9: Extractive Distillation Column

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separation.

More

Pipe

temperature blockage
-

Less

Less flow

Pipe leakage

Purify

of -

Regular

checking

product affected.

temperature alarms.

Low efficiency -

Install

separation.

alarm.

Product

spills -

Perform

high

on the

temperature

corrosion

out and bring

regularly.

dangerous

Install a flow indicator.

to -

test

operator.
-

Product quality
affected.

Less

Pipe leakage

pressure

Malfunction

Product quality -

Install low pressure alarm

affected.

of valve
Reverse Reverse
flow

Valve
malfunction

Pressure

Install check valve

decrease in the
column

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Chapter 9: Extractive Distillation Column

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References
1. Perry, R.H. and Green, D.W. (1997). Perrys Chemical Engineers Handbook (7th Ed.).
McGraw-Hill Co.
2. Janet K. Standard handbook of environmental science, health, and technology
3. Saint-Gobain NorPro (2007). Packed tower internals guide, retrieved 20th February
2009 from http://www.soint-gobain.com
4. Khoury.F.M (2005), Multistage Separation Processes.
5. Henry Z. Kister. Distillation Design
6. Lloyd, E.B. and Edwin, H.Y, (1959). Process Equipment Design. John Wiley & Sons.
Inc, New York.
7. Thomas, E.M. (1995). Process Control: Designing Processes and Control Systems for
Dynamic Performance. McGraw-Hill, United States of America.

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Chapter 10: Distillation Column

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Acrylic Acid Project

CHAPTER 10: DISTILLATION COLUMN

10.1. CHEMICAL ENGINEERING DESIGN
10.1.1. Introduction
Distillation is probably the most widely used separation process. It is a method used to separate
the components of a liquid solution, which depends on the distribution of these various
components between a vapor and liquid phase. All components are present in both phases. The
vapor phase is created from the liquid phase by vaporization at the boiling point.
The general principles of design of multi-component distillation column are the same in some
aspects as those described for binary systems. But the calculations for multi-component
distillation are much more complex than for binary systems. When the feed contains more than
two components, it is not possible to specify the complete composition of the top and bottom
products independently. One component may be more volatile than the average in one part of the
column and less volatile than the average in another part, which leads to complex concentration
profiles. The separation between the top and bottom products is specified by having two key
components, between which it is desired to make the separation.
Trial and error calculations will be needed to solve this problem. For a completely rigorous
solution the compositions must be adjusted and the calculations repeated until a satisfactory
solution is obtained. Clearly, the greater the number of components, the more complicated.
In this chapter, chemical engineering design will be carried out based on the material and energy
balance completed during the previous semester. The solvent and acetic acid is then fed into
solvent recovery distillation column, T-102.The bottom product will become residual of the
process and sent to waste treatment plant.The solvent with 99.8% is recovered and recycle back
to extraction distillation column, T-101.

10.1.2. Distillation Column Design

The algorithms for the design of distillation column are as follows:
a) Establish preliminary compositions for the top and bottom products.
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b) Determine column-operating conditions (temperature and pressure) at the top and

c) Bottom of the column.
d) Select type of contacting device plates or packing
e) Estimate the theoretical number of equilibrium stages
f) Estimate the minimum reflux ratio
g) Estimate reflux ratio and number of equilibrium stages and number of stages
h) Estimate the feed-point location
i) Determine the column diameter
j) Specify column internals plates, distributors, packing support
k) Check for pressure drop, weeping and entrainment
10.1.2.1. Schematic Diagram of T-102

Figure 10.1: Schematic Diagram of Distillation Column T-102

Table 10.1: Stream Description for Distillation Column T-102

Stream

Feed

Top

Bottom

Phase

Pressure (kPa)

15

15

15

Temperature (C)

31.87

31.26

45.66

Mole Flow

439.30

410

29.28

8.13

0.14

Component (kmol/h)
Water

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Acrylic Acid

1.32

1.32

Acetic Acid

4.69

0.3

4.38

0.14

0.14

Cyclohexane

191.25

191.08

0.17

I-P-Acetate

233.75

218.33

15.42

Molten Salt

Acetol
Acrolein

10.1.2.2. Type of Column of T-102

For large scale distillation, continuous distillation is the preferable choice. Comparing between
plate or packed columns, plate column is chosen due to these factors :
a) Plate columns can handle a wider range of liquid and gas flow-rates.
b) A column with large diameter is not suitable for packing, as it would increases cost
c) The process materials are not foaming, non-toxic, and inflammable. Thus the use of
packed column is not considered.

10.1.3. Key Components

Key components are components whose volatility that is its boiling point or vapor pressure
characteristics relative to each other makes them adjacent in the listing of the component in the
feed.
Light key component, LK the component that is desired to keep out of the bottom product.
Heavy key component, HK the component that is desired to keep out of the top product.
In further calculation and discussion, the light key is the product.

10.1.4. Number of Stages

10.1.4.1. Relative Volatility
The key to the separation is the relative volatility between the compounds to be separated. The
higher the volatility, the easier the separation is and vice versa. If two components have very
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similar vapor pressure characteristic, their relative volatility will be close to unity. This means
that they have similar boiling points and therefore, it will be difficult to separate via distillation.
For multi-component distillation, the relative volatility is calculated with respect to the heavy
key.

10.1.4.2. Number of Stages and Operating Reflux Ratio

10.1.4.2.1. Minimum Number of Stages
The Fenske equation (Fenske, 1932) can be used to estimate the minimum stages required at total
reflux. Normally the separation required will be specified in terms of the key components, and
given as:

Minimum number of stages,Nm = 36.63 stages

10.1.4.2.2. Minimum Operating Reflux Ratio

Reflux ratio is the amount of flow from the top product that is returned into the column. The
limiting conditions occur at minimum reflux ratio where the separation can only be achieved
with an infinite umber of stages.
Colburn (1941) and Underwood (1948) have derived equations for estimating the minimum
reflux ratio for multi-component distillations. The equation can be stated in the form:

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In the derivation of the equations above, the relative volatilities are taken to be constant. The
geometric average of values estimated at the distillate and bottom temperatures should be used,
in the same manner as described earlier.
The value of is found by trial and error, and must lie between the values of the relative
volatility of the light and heavy keys. By trial and error (using EXCEL),thus minimum operating
reflux ratio,Rm = 4.343

10.1.4.3. Number of Theoretical Stages

One of the most frequently used empirical method for estimating the stage requirements for
multi-component distillations is the correlation published by Erbar and Maddox (1961). This
correlation gives the ratio of number of stages required to the number at total reflux ratio, with
the minimum reflux ratio as a parameter.
From the correlation, it is observed that the stage requirement is reduced as reflux ratio is
increased beyond the minimum reflux. This thus leads to reduction in the cost of column.
However, a marked reduction is only achievable at values near Rm where further increment has a
little effect on the number of stages, as shown in the table below.
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Table 10.2: Stage Requirement at Different Reflux Ratio

R / Rm

1.1

1.2

1.3

1.4

1.5

1.6

1.7

4.776925

5.211191

5.645457

6.079723

6.513989

6.948255

7.382521

R /(R + 1)

0.826898

0.839

0.848752

0.849521

0.866915

0.874186

0.880704

Nm / N

0.375

0.483

0.56

0.625

0.67

0.67

0.7

97.66655

75.82067

65.40171

58.59993

54.66411

54.66411

52.32137

Practical values of reflux ratio are usually 1.1 -1.5 times the minimum, with much higher value
being employed. Thus,
R = 1.5Rm = 6.5
With theoretical number of stages, N = 54.66 stages
10.1.4.4. Overall Column Efficiency
The concept of the stage efficiency is used to link the performance of practical contacting stages
to the theoretical equilibrium stage. It is defined as:

The correlation by OConnell (1946) to estimate the ove

rall column efficiency is expressed

by
Eduljee (1958) in the form of an equation:

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10.1.4.5. Actual Number of Stages

10.1.5. Feed Point Location

A limitation of the Erbar-Maddox, and similar other empirical methods, is that they do not give
the feed-point location. An estimate can be made by using the Fenske equation to calculate the
number of stages in the rectifying and stripping sections separately, but this requires an estimate
of the feed-point temperature. An alternative approach is to use the empirical equation given by
Kirkbride (1944):

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From the Kirkbride (1944) equation,Nr = 67.5 = 68.Thus the feed location is at 68th stage.

10.1.6. Plate Specification

10.1.6.1. Plate Spacing
The overall height of the column depends on the plate spacing. For columns above 1 m in
diameter, plate spacing of 0.3 to 0.6 m will normally be used. This plate spacing is selected to
minimize entrainment. A larger spacing will be needed between certain plates to accommodate
feed and side stream arrangement, and for manways.

10.1.6.2. Type of Plate

In selecting the type of plates, several principal factors are to be considered:
- Cost
- Efficiency
- Capacity
- Operating pressure
- Pressure drop
Based on the above criteria, the sieve (perforated) tray is chosen; over the high-cost and high
pressure drop bubble cap tray; and the valve trays.

10.1.6.3. Liquid and Vapor Flows in a Plate Column

Each plate has 2 conduits, one on each side, called downcomer. Liquid falls through the
downcomers by gravity from one plate to the one below it. The flow across each plate is shown
in Figure 1.3. A weir on the plate ensures that there is always some liquid (backup) on the plate
and is designed such that the holdup is at a suitable height.
Being lighter, vapor flows up the column and is forced to pass through the liquid, via the
openings on each plate. The area allowed for the passage of vapor on each tray is called the
active plate area.
At the hotter vapor passes through the liquid on the plate above, it transfers heat to the liquid. In
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doing so, some of the vapor condenses adding to the liquid on the plate. The condensate,
however, is richer in the less volatile components than it is in the vapor.
Additionally, because of the heat input from the vapor, the liquid on the plate boils, generating
more vapors. This vapor, which moves up to the next plate in the column, is richer in the more
volatile components. This continuous contact between vapor and liquid occurs on each plate in
the column and brings about the separation between low boiling point components and those
with higher boiling points.

Figure 10.2: Flow of Vapor and Liquid Across Each Plate

10.1.7. Plate Design Procedure

A trial-and-error approach is necessary in plate design: starting with a rough plate layout,
checking key performance factors and revising the design, as necessary, until a satisfactory
design is achieved. A typical design procedure is set out as below:
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a) Calculate the maximum and minimum vapour and liquid flow rate for the turn down
b) ratio required.
c) Collect or estimate the system physical properties.
d) Select trial plate spacing.
e) Estimate the column diameter, based on flooding consideration.
f) Decide the liquid flow arrangement.
g) Make a trial plate layout: downcomer area, active area, hole area, hole size, weir
h) height.
i) Check the weeping rate.
j) Check the plate pressure drop.
k) Decide plate layout details (calming zones, unperforated areas). Check hole pitch.
l) Recalculate the percentage flooding based on chosen column diameter.
m) Check entrainment.
n) Optimize design.
o) Finalize design.
10.1.7.1. Vapor and Liquid Flow Rates
Since the liquid and vapor flow rates and composition vary throughout the column, tray design
should be made above and below the feed-point. Calculations for the molar flow rate are
tabulated.
Table 10.3: Vapor and Liquid Flow Rates

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10.1.7.2. Physical Properties

The physical properties at the bottom and top of the column are obtained for further calculation
of the plate design.

Table 10.4: Physical Properties

10.1.7.3. Column Diameter

10.1.7.3.1. Liquid-Vapor Flow Factor
The liquid-vapor flow factor to be used Figure 1A-2 is given by the equation

Therefore Top FLv = 0.01 and Bottom FLV = 0.07

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10.1.7.3.2. Flooding Velocity

The flooding condition fixes the upper limit of vapor velocity. The velocity will normally be
between 70 to 90 percent of that which would cause flooding. For design, a value of 80 to 85
percent should be used. Flooding velocity is estimated from the correlation by Fair (1961):

With surface tension correction which is

Take tray spacing as 0.4 m. From Figure 1A-2,

Top : K = 0.068 K ' = 0.093
Bottom : K = 0.069 K ' = 0.080
Flooding velocity
Top : u f = 1.907 m / s
Bottom : u f = 1.194 m / s
Design for 85% flooding velocity at maximum flow rate, uv =0.85 u f
Top : uv = 1.621 m / s
Bottom : uv = 1.015 m / s

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10.1.7.3.3 Maximum Volumetric Flow Rate

V

88.082 m3 / s

X
V

78.710 m3 / s

10.1.0.7.3.4. Column Diameter

To estimate the column diameter, an estimate of the net area is required,
Thus using this equation :
Q

Top : An = 54.351 m2
Bottom : An = 77.581
The column cross-sectional area (taking the downcomer as 10 percent of total area),
Therefore using this equation:
A
.

Therefore, the column diameter can be calculated as:

Top :
Bottom :

= 8.768 m
= 10.476

The diameter of the column is taken as

= 10.5 m , for the whole column, reducing the

perforated
area for plates above the feed-point stage.

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10.1.7.4. Liquid Flow Pattern

The maximum volumetric liquid flow rate is calculated as

Although the value is out of range (refer to Figure 1A-3), it is clear that a double pass pattern
flow plate should be used. Double pass plates are used for high liquid flow-rates and large
diameter columns.

10.1.7.5 Provisional Plate Design

Table 10.5: Provisional Design

10.1.7.6. Check Weeping

Weeping is a phenomenon caused by low vapor flow. The pressure exerted by the vapor is
insufficient to hold up the liquid on the plate. This causes the liquid to leak through the
perforations. The vapor velocity at the weep point is the minimum value for stable operation.
Thus the holes area must be chosen so that at the lowest operating rate the vapor velocity is still
well above the weep point.
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10.1.7.6.1. Weir Liquid Crest

The height of the liquid crest over the weir can be estimated using the Francis weir formula. This
can be written as:

Maximum liquid flow rate,

274.313

/s

Minimum liquid flow rate, at 65% turn down = 0.6 x 274.313 = 178.304 kg / s
Therefore
Maximum weir liquid crest, how = 97.242 mm liquid
Minimum weir liquid crest, how = 72.968 mm liquid
At minimum rate = 112.968 mm liquid , and from Figure 1A-5, K2 = 31.17
The minimum design vapor velocity, given by Eduljee (1959):

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Actual minimum vapor velocity,

From the calculation,we know that the minimum operating rate is above weep point.
10.1.7.7. Plate Pressure Drop
There are two main sources of pressure loss: that due to vapor flow through holes and that due to
the static head of liquid on the plate. The total is taken as the sum of the pressure drop:
a) The flow of vapor through the dry plate
b) The head of clear liquid on the plate
c) Residual loss which accounts for others; minor sources of pressure loss

10.1.7.7.1. Dry Plate Drop

The pressure drop through the dry plate can be estimated using expressions derived for flow
through orifices.

Maximum velocity through the holes,

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Dry plate drop,

51

37.2

10.1.7.7.2. Residual Head

The residual head can be estimated by equation proposed by Hunt et al. (1955).
12.5

10

16.083

10.1.7.7.3 Total Pressure Drop

The total pressure drop,

The pressure drop is conveniently expressed in Pa with the following equation,

10.1.7.8. Check Entrainment

Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by high
vapor flow rates. Entrainment can be estimated from the correlation given by Fair (1961), which
gives the fractional entrainment (kg/kg gross liquid flow) as a function of the liquid-vapor
factor FLV, with the percentage approach to flooding as a parameter.

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Percent flooding defined as,

Actual velocity,

Therefore, percentage flooding = 84.6%

10.1.8. Trial Layout

Figure 10.3: Trial Plate Layout

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10.1.9. Perforated Area

The area available for perforation will be reduced by the obstruction caused by structural
members (the support rings and beams), and by the use of calming zones. Calming zones are
unperforated strips of plate at the inlet and outlet sides of the plate. A strip of unperforated plate
plate will be left around the edge of catridge-type trays to stiffen plate.
Allow 50 mm of unperforated strip around plate edge.
1

8,

0.72

93

The angle subtended at plate edge by unperforated strip = 180 93 = 87

Mean length, unperforated edge strips,

Area of unperforated edge strips,

Area of calming zone,

(Dc 0.05) = 15.14 m

0.05

= 2(0.05)[

- 2(0.05)] = 0.746

Thus, total area available for perforation,

Therefore,

= 0.757

= 0.102,and from figure 1A-9.

-(

) = 67.78

- 2.883

This is accordingly to the normal range of 2.5 to 4.0 hole diameter, and of satisfactory value
The hole pitch,

= 2.883 X

= 14.42 mm

10.1.0.1. Number of Holes

Area of one hole,

= 1.964 x 10

Number of holes,

= 352841 holes

10.1.10. Column Height

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Height of 90 plates at 0.4 m spacing, and 6 mm thickness,
Tower skirt height,
Ratio of

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= 36.54 m

=7m

4.147 , thus the column is stable, having a ratio of 3 to 5.

10.1.11. Simulation by HYSYS

To further prove the design that has been made is practical and achievable, simulation of the
distillation column with the specification obtained is carried out. The simulation software used is
HYSIS.
10.1.11.1 .Approach of Manual Calculation
The manual calculation for this plant was calculated by making several assumptions for the
purpose to simplify the equation. Since there is lack of literature values of date such as
equilibrium constant, some of the thermodynamics data were obtained from HYSIS whenever it
was necessary. In order to simplify the whole manual calculation, the input values of every unit
operations are taken from the HYSIS results which the recycle streams were already considered.
Assumption such as ideal mixing, and constant heat capacity with a wide range of pressure were
made for the energy calculation.
10.1.11.2. Approach of HYSIS Simulation
Simulation was carried out using HYSIS 3.2 software. The package was used: NRTL for the
acrylic acid production. Below are the tables that presented the mass and energy balance of each
stream and its deviations with the HYSIS.

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Table 10.6: Molar Flow Rate of Feed Stream and its Comparison with Hysys

Table 10.7: Molar flow rate of Top stream and its comparison with Hysys

Table 10.8: Molar flow rate of Bottom Stream and its Comparison with Hysys

The discrepancies obtained mainly revolve around the fact that during simulation, calculation
done on the composition of each and every tray is rigorous. Manual calculation for every single
tray is possible but for 90 stages of distillation proves to be quite a burden. HYSIS is able to do a
more rigorous computational calculation.

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10.2 MECHANICAL DESIGN

10.2.1. Introduction
The mechanical design of this chapter is to develop and specify the basic design information for
the distillation column T-102. Basic data needed by the specialist designer to further design the
column in detail will be:
a) Vessel function
b) Process material and services
c) Operating and design temperature and pressure
d) Materials of construction
e) Vessel dimensions and orientation
f) Type of vessel heads to be used
g) Openings and connections required
h) Specification of heating and cooling jacket or coils
i) Type of agitator
j) Specification of internal fittings

10.2.2. General Design Consideration of Pressure Vessel

10.2.2.1. Design Pressure, P
A vessel must be designed to withstand the maximum pressure to which it is likely to be
subjected in operation. For vessels under internal pressure, the design pressure is normally taken
as the pressure at which the relief device is set, normally 5 to 10 percent above the normal
working pressure. This is to avoid spurious operation during minor process upsets.
Working pressure,15 kPa or 0.15 bar
For a safety factor of 10 percent, design pressure,110% x 0.15bar = 0.17 bar

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10.2.2.2 . Design Temperature, T

The design temperature at which the design stress is evaluated should be taken as the maximum
working temperature of the material, with 20 percent allowance for any uncertainty involved in
predicting vessel wall temperatures.
Maximum operating temperature = 45.66 C
Design temperature, T = 120% X 45.66C = 54.79 C
10.2.2.3. Materials of Construction
Selection of material must take into account the suitability of the material for fabrication
(particularly welding) as well as compatibility of the material with the process environment.
With the nature of the processed material not corrosive neither fouling, use of low-alloy steel is
sufficient. Carbon steel being the most versatile metal used in the industry, with excellent
ductility, and great ease of fabrication, is further improved with the existence of alloying agents.
Such is carbon-manganese (AISI 4340) which contains 0.40 percent C, 0.70 percent Mn, 1.85
percent Ni, 0.80 percent Cr, and 0.25 percent Mo.
10.2.2.4. Design Stress
It is necessary to decide a value for the maximum allowable stress that can be acceptable in the
material construction. Maximum allowable stress a material can withstand without failure under
operating conditions should be determined. This is done by applying a suitable design stress
factor to the maximum stress. The design stress factor allows for any uncertainty in the design
methods, the loading, the quality of the materials and workmanship.
From Table 2A-1,
Design stress factor = 1.5
At design temperature of 54.79C, from Table 2A-2,
Design stress = 120.3
Practical design stress,

.
.

= 80.2

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10.2.2.5 .Welded Joint Efficiency

The strength of weld joint will depend on the type of joint and the quality of the welding. The
soundness of welds is checked by visual inspection and by non-destructive testing (radiography).
The value of the joint factor used in the design will depend on the type of joint and the amount of
radiography required by the design code. Taking 100 percent degree of radiography implies that
the joint is equally as strong as the virgin plate while the use of lower joint factors in design,
though saving costs on radiography, will result in a thicker, heavier, vessel. There must be a
balance in any cost savings on inspection and fabrication against the increased cost of material.
From Table 2A-3,
Maximum allowable joint efficiency for double-welded butt, J = 0.85
10.2.2.6. Corrosion Allowance
The corrosion allowance is the additional thickness of metal added to allow for material lost by
corrosion and erosion, or scaling. The allowance should be based on experience with the material
of construction under similar service conditions to those for the purpose design. From Materials
of Construction pg 28-29, Ref [2] carbon-manganese steel is frequently used in services with
corrosion rates of 0.13 to 0.5 mm/y.
For 20 years of operation,
Minimum corrosion allowance = 0.13 x 20
= 2.66mm = 3mm

10.2.3. Design of Column

10.2.3.1. Wall Thickness
certain wall thickness is required to ensure that any vessel in sufficiently rigid to withstand its
own weight and any incidental loads, together with the internal pressure.

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Including the welded joint factor, minimum thickness required with,

= 8.65mm

10.5

Therefore, wall thickness with corrosion allowance = 12 mm

10.2.3.2. Design of Vessel Heads
10.2.3.2.1. Choice of Closure
The ends of a cylindrical vessel are closed by heads of various shapes. The principal types used
are:
a) Flat plates and formed flat heads
b) Hemispherical heads
c) Ellipsoidal heads
d) Torispherical heads

Formed flat heads or flange-only ends are the cheapest but their use is limited to low-pressure
and small-diameter vessels. As operation is carried out at 1.1 bar, the standard torispherical head
is used due to its higher range of operating pressure and column size. Use of hemispherical head
however, will lead to excessive cost at the same thickness, although it is the strongest shape.
10.2.3.2.2 .Design of Torispherical Head
There are two junctions in a torispherical end closure: that between the cylindrical section and
the head, and that at the junction of the crown and the knuckle radii. One approach taken is to
use the basic equation for a hemisphere and to introduce a stress concentration, or shape factor to
allow for the increased stress due to the discontinuity. The stress concentration factor is a
function of the knuckle and crown radii.

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To avoid buckling;
0.06

a) Ratio of the knuckle radii to crown radii:

b) Crown radius:
Stress concentration factor, with
=

10.5

) = 1.7706

Minimum wall thickness, e =

12.7

13

Thus, thickness of the torispherical head with corrosion allowance

16 mm. For practical

purposes, the thickness of the whole column is taken as 16 mm.

10.2.4. Design of Vessel Loads

Pressure vessels are subjected to other loads in addition to pressure and are designed to withstand
the worst combination of loading without failure. The main sources of load to consider are:
a) Pressure.
b) Dead weight of vessel and contents.
c) Wind.
d) Earthquake (seismic).
e) External loads imposed by piping and attached equipment.

10.2.4.1 .Weight Loads

The major sources of dead weight loads are:
a) The vessel shell
b) The vessel fitting: man ways, nozzles
c) Internal fittings: plates plus the fluid on the plates; heating and cooling coil
d) External fitting: ladders, platforms, piping
e) Auxiliary equipment which is not self supported: condenser, agitators
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f) Insulation
g) The weight of liquid to fill the vessel. The vessel will be filled with water for the
h) hydraulic pressure test, and may fill with process liquid due to misoperation.
10.2.4.2. Vessel Weight, Wv
240

0.8

2087.55

Where Cv = a factor to account for the weight of nozzles, manways, internal support = 1.15 (for
DC)
= height of cylindrical section = 36.54 m
t = wall thickness = 16 mm
2

Dm = mean diameter of vessel =

10.532

10.2.4.3. Plates Weight, Wp

Plate area,

= 86.59
9351.7

Weight of a plate,
Where

= contacting plates, steel, including typical liquid = 1.2 kN/m2 plate area
N = number of plates = 90

10.2.4.4. Cage Ladder Weight, Wl

0.360

13.154

10.2.4.5. Platform Steels Weight, Wf

1.7

Weight of one platform steel,

Using two platform steels,

147.2
294.4

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10.2.4.6. Total Load Weight, Wt

= 11.75 x 103 kN

10.2.5. Wind Loads

For tall columns, the force that produces bending is a function of wind velocity and the shape of
the column. Since the column is to be installed in the open, wind loading will be an important
factor. Initially, the load imposed on the column structure by the action of wind (or named as
wind pressure) is needed to be determined first. The maximum wind pressure should be used in
the calculation of bending stress. The maximum wind pressure is considered as wind velocity of
160 km/hr, which is equivalent to wind pressure of 1280 N/m2.
10.2.5.1. Load per Unit Length, Fw
13.99

Where

= effective column diameter

= mean diameter + allowance for attachment
=

0.4

10.932

10.2.5.2. Bending Moment, Mx at Column Base

9341.5 10

= 9341.5 x 103 Kn/m

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10.2.6. Analysis of Stresses

10.2.6.1 Pressure Stresses
.

Longitudinal stress,

19.85
.

Circumferential stress,

39.7

10.2.6.2. Dead Weight Stress

The dead weight stress due to the weight of the column, its contents and attachment is given by:
.

Dead weight stress,

2.22

10.2.6.3 .Bending Stress

Bending stress resulting form the bending moments to which the vessel is subjected. The
bending stresses will be compressive of tensile, depending on location, and are given by:
(

6.73

Where Iv is the second moment of area of vessel about the plane of bending and is given by:
(

) = 7.31 x 10

10.2.6.4. Principal Stress

The resultant longitudinal stress is:

Where w is compressive and therefore is a negative value.

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As there is torsional stress, the principal stresses will be z and h.

The radial stress is negligible

= 0.0605 N/mm2

The greatest difference between the principle stresses will be on the down wind side,
48.81

Well below the maximum allowable design stress which is 120.3 N/mm2.
10.2.6.5. Critical Buckling Stress (Elastic Stability)
A column design must be checked to ensure that the maximum value of the axial stress does not
exceed the critical value at which buckling occurred.
2 104

Critical buckling stress,

The maximum compressive stress (

2.22

6.73

11.43 N/mm2

must be below the critical buckling stress.

8.95 N/mm2

thus the design of the column is satisfactory.

10.2.7. Vessel Support

The method used to support a vessel will depend on the size, shape, and weight of the vessel, the
design temperature and pressure; the vessel location and arrangement; and the internal and
external fittings and attachment. The support must be designed to carry the weight of the vessel
and contents, and any superimposed loads, such as wind loads. Support will imposed localized
loads on the vessel wall, and the design must be checked to ensure that the resulting stress
concentrations are below the maximum allowable design stress. Supports should be designed to
allow easy access to the vessel and fittings for inspection and maintenance.
In this design, skirt support is used for tall, vertical columns. A skirt support consists of a
cylindrical or conical shell welded to the base of the vessel. A flange at the bottom of the skirt
transmits the loads of the foundations.
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10.2.7.1 .Skirt Thickness

The skirt must be able to withstand the dead weight loads and bending moments imposed on it
by the columns. The maximum dead weight load on the skirt will occur when the vessel is full of
water.
31038.88

Approximate weight,
Where

= density of water = 1000 kg/m3

W=

42.79

10 Kn

10.2.7.2. Bending Moment at Base of Skirt, Ms

13260

Where Hs = skirt height = 7 m

As a first trial, take the skirt thickness, ts as the same as the bottom section of the column, 16
mm.
10.2.0.7.2.1. Bending Stress in the Skirt
=

9.556 N/mm2

10.2.7.2.2. Dead Weight Stress in the Skirt, ws

Dead weight stress in the skirt for hydraulic test condition,

5.06 N/mm2

Dead weight stress under operating conditions,

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3.949 N/mm2

10.2.7.3. Design Criteria

The skirt thickness should be such that under the worst combination of wind and dead weight
loading the following design criteria are not exceeded.

Both criteria are satisfied. Therefore, the skirt support of 7 m height, with an inside diameter of
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10.5 m, and thickness of 16 mm is acceptable.

10.2.8. Manhole
Manhole is an opening that permits a person entry and exit the vessel for inspection and vessel
examination of the interior. BS 470 (1984) is used for manholes design. According to BS 470,
the minimum number of manhole for column over 1500mm internal diameter is 1. Therefore, in
this design, 5 manholes are provided, to cater for the 36 m high column. One of the manholes is
located at the centre of the column, with the other 4 located at every 9 m of the column.
The minimum size to afford rescue facilities with self-contained breathing apparatus is 575 mm
diameter with length not restricted. Therefore, in this design, a size of 575 mm diameter is used
with length 500 mm.

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10.2.9. Summary
Table 10.9: Summary of Chemical Engineering Design

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10.3. Safety, Control and instrumentation

10.3.1. Introduction
Control is one form or another is an essential part of any chemical engineering operation.
In all process there arises the necessity of keeping flows, pressures, temperatures,
composition, etc, within certain limits for reasons of safety or specification. Such control
is most often accomplish simply by measuring the variable it is required to control (the
controlled variable), comparing this measurement with the value at which it is desired to
maintained the controlled variable (the desired value or set point) and adjusting some
other variable (the manipulated variable) which has a direct effect on the controlled
variable until the desired value is obtained.
It can be seen that automatic operation is highly desirable, as manual control would
accessitate continuous monitoring of the controlled variable by a human operator. The
efficiency of observation of the operator would inevitably fall off with time. Furthermore,
fluctuations in the controlled variable may be too rapid and frequent for manual
adjustment to suffice.
A chemical plant is an arrangement of processing units integrated with one another in a
systematic and rational manner. The primary objectives when specifying instrumentation
and control schemes are discussed in later sections.
10.3.1.1. Safety
The safety of people in the plant and in the surrounding community is of paramount
importance. Where no human activity is without risk, the typical goal is that working at
an industrial plant should involve mush less risk than any other activity in a persons life.
Plants are designed safely at expected temperatures and pressures; however, improper
operation can lead to equipment failure and release of potentially hazardous materials.
Therefore, the process control strategies contribute to the overall plant safety by
maintaining key variables, near their desired values.
10.3.1.2. Environment Protection
Protection of the environment is critically important. The objective is mostly a process
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design issue; that is, the process must have the capacity to convert potentially toxic
components to design material. Again, control can contribute to the proper operation of
these units, resulting in consistently low effluent concentrations.
10.3.1.3. Equipment Protection
Much of the equipment in a plant is expensive and difficult to replace without costly
delays. Therefore, operating conditions must be maintained within bounds to prevent
damage. The types of control strategies for equipment protection are similar to those for
personnel protection; that is, controls to maintain conditions near desired values and
emergency controls to stop operation safely when the process reaches boundary.
10.3.1.4. Smooth Plant Operation
A chemical plant includes a complex network of interacting processes; thus, the smooth
operation of a process is desirable, because it results in few disturbances to all integrated
unit. Naturally, key variables in streams leaving the process should be maintained.
10.3.1.5. Product Quality
The final products from the plant must meet demanding quality specifications set by
purchaser. Process control can maintain the optimum operation condition required for
excellent product quality.
10.3.1.6. Profit
To have a higher profit, the plant has designed to produce product at lowest cost.
However, before achieving the profit-oriented goal, selected independent variables are
adjusted to satisfy the first five higher priority control objectives. The control strategy
must increase profit while satisfying all other objectives.
10.3.1.7. Monitoring and Diagnosis
Complex chemical plants require monitoring and diagnosis by people as well as excellent
automation. Since people cannot monitor all variables simultaneously, the control system
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includes an alarm feature, which draws the operators attention to variables that are near
limiting values selected to indicate serious maloperation.
Good control design addresses a hierarchy of control objectives, ranging from safety to
product quality and profit, which depend on the operating objectives for the plant.
The control is an important factor in plant design. The plant design must included
measurement element of plant output variables (or disturbance input) and final control
element. The measurement element must respond rapidly so that the control action can be
taken in real time. The final element in chemical process (in this process also) usually are
the control valves that affect fluid flows.

10.3.2. Distillation Control Objective

The philosophy of process control has a few objectives:
a) Product quality control
-Maintain either the overhead or bottoms composition at specified value.
-Maintain the composition at the other end of the column as close as possible to a
desired composition.
b) Material balance control
-Cause the average sum of distillate and tails streams to be exactly equal to
average feed rate
-The resulting adjustment in process flows must be smooth and gradual to avoid
psetting either the column or downstream process equipment fed by the column
-Column hold-up, and overhead and bottom inventories, should be maintained
between maximum and minimum limits.
c) Constraints
-For safe, satisfactory operation of the column, certain constraints must be
observed. For example:The column should not flood
-Column pressure drop should be high enough to maintain effective column
Operation.
-The temperature difference in the reboiler should not exceed the critical
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temperature difference
d) Disturbances
-The preceding objectives must be satisfied in the face of possible disturbances in
-Feed flow rate
-Feed composition
-Feed thermal condition
-Steam supply pressure
-Cooling water supply temperature
-Ambient temperature, such as that caused by rainstorms
e) Special consideration
If a column, its auxiliaries, and its controls are designed to accomplish the
preceding objective, it may be shown that the consumption of utilities such as
steam and cooling water is minimums, except in one instance. For any given feed
composition and feed thermal condition, there will be an optimum feed tray
location-optimum in the sense of requiring less reflux or boil-up and thereby less
utilities, and n permitting the column to operate changes sufficiently, the column,
control system, whether manual or automatic, should recognize this and select a
new feed tray.

10.3.3. Column Control

10.3.3.1. Feed Stream Control
A typical method to flow in the distillation column is using a feed forward system.
Instead of temperature, flow is considering a critical parameter, since the temperature of
the flow is controlled in the bottom line of previous column. At the same time, pressure is
also maintained at indicated column pressure. Therefore it is assumed that accurate vapor
liquid flow rate will be produced at accurate temperature and pressure of the expansion
valve.

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10.3.3.2. Product Quality Control

The basic approach to composition control is to use feed forward from feed flow rate.
This control maintains the reflux to feed ratio. The reflux ratio is reset by the overhead
composition controller. In this configuration, wild stream is feed line. It is measured and
manipulated by reflux line to desired reflux to feed ratio. Any disturbance to
composition, composition control will send signal to ratio and indirectly adjust the reflux
flow rate.

10.3.3.3. Top Stream Control

Generally, top stream control system is more complicated than either feed stream of
bottom stream control system. The control system must provide adequate coolant to
condenser, the correct flow rate back to column and the distillate with the require
composition. It also needs to satisfy all the operation condition.
Pressure is the critical parameter to control compared to temperature or flow in the
distillate. Any disturbance of pressure at the top column will disrupt the equilibrium of
the components separation. The chief function of pressure control is to ensure that the
rate of condensation is exactly equal, on the average, to the rate of vapor flow to the
condenser. In this approach, the cooling water stream is manipulated to maintain the
desired column pressure. Therefore, the pressure is controlled using a feedback loop by
throttling the flow of the coolant entering the condenser. Any changes of top column
pressure, a signal will be sent to the pressure controller to adjust the amount of coolant to
the condenser in order to control the changes of pressure.
The flow of product has adjusted by a level controller. A feedback level controller is
fixed to the reflux drum. The main purpose of the level controller is to prevent the
overflow of the receiver. The increase of level in the reflux will detect by the controller.
The control valve will be adjusted to allow more distillate get out.

10.3.3.4. Bottom Stream Control

The stream which enters reboiler must be controlled to provide desired flow to reboiler
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without overload the reboiler. Feed forward flow controller controls this stream
independently. The appropriate flow rate should be controlled so that the reboiler does
not overflow and the circulation rate to reboiler can be maintained.
In bottom section, temperature is the most critical parameter. High temperature will
change the composition of the product. Thus, a feedback temperature controller is fixed.
The bottom liquid hold-up is used by the controller as a basic to manipulate steam flow
rate. The variation in temperature on bottom liquid hold-up will actuate the controller
value in steam stream.
Level controller is fixed to control the flow rate at line 3 (bottom product stream). This is
because the level of liquid hold-up in the column will affect the flow. The disturbance in
feed flow rate will change the product distribution of material balance in the column.

10.3.4. Instruments Notation

Flow
FC

Flow controller

FT

Flow transmitter

Level
LT

Level transmitter

LC

Level controller

Pressure
PC

Pressure controller

PT

Pressure transmitter

Temperature
TC

Temperature controller

TT

Temperature transmitter

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10.3.5. Instrumentation
Instruments are provided to monitor the key process variables during plant operation.
They may be used for the manual monitoring of the process unit operation or
incorporated in automatic control loops. They may also be part of an automatic computer
data logging system. Instruments while monitoring critical process variables will be fitted
with automatic alarms to alert the operation is near or at hazards situations.
10.3.5.1. Pressure Measurement
For the measurement of pressure, a Strain-Gauge Pressure Transducer is selected. It
consists of elastic elements to which one or more strain-gauges have been attached to
measure the deformation. The strain-gauges are bonded directly to the surface of the
elastic elements whose strain is to be measured.
The advantage of this type of pressure measurement gadget is that it has an extremely fast
response time.

10.3.5.2. Flow Measurement

Turbine meter is selected as the flow rate sensor. A turbine wheel is placed in a flowing
fluid pipe and its rotary speed depends on the flow rate of the fluid. A turbine is designed
whose speed varies linearly with flow rate. The speed can be measured accurately by
counting the rate at which turbine blades pass a given point, suing magnetic pickup to
produce voltage pulses. The flow rate can be measured by feeding these pulses to an
electronic pulse-rate meter.
The advantages are turbine meter are available at a wide scale of flow rate, has a low
pressure drop and very accurate as its fluid/mechanical time constant is of the order of 210 msec.

10.3.5.3. Level Measurement

Magnetic Coupled Devices is selected for the level measurement. Typical devices are
magnetically operated level switched and magnetic-bond float gauges. A magnetic-bond
float gauge consists of a hollow magnet-carrying float that rides along a vertical
nonmagnetic guide tube. The follower magnet is connected and drives an indicating dial
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similar to that on a conventional tape float gauge. The float and guide tube are in contact
with the measured fluid tape gauge. The float and guide tube are in contact with the
measured fluid and come in a variety of materials for resistance to corrosion and to
withstand vacuum pressure.

10.3.5.4 .Temperature Measurement

Thermocouple is selected as the temperature sensor for measuring the temperature of the
distillation column and the streams. Temperature measurements using thermocouple is
based on the discovery by Seedbeck that an electric flows in a continuous circuits of two
different metallic wires if two junctions are at different temperatures. The advantages of
this devices are the suitability for high and wide temperature range, great sensibility and
economically cheap.

Figure 10.4: Complete Process Control and Instrumentation Diagram of Distillation Column

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10.3.6. Hazards and Operability Study (HAZOP)

Essentially the HAZOP procedure involves taking a full description of a process and
systematically questioning every part of it to establish how deviations from the design intent can
arise. Once identified, an assessment is made as to whether such deviations and their
consequences can have a negative effect upon the safe and efficient operation of the plant. If
considered necessary, action is then taken to remedy the situation. This critical analysis is
applied in a structured way by the HAZOP team, and it relies upon them releasing
theirimagination in an effort to discover credible causes of deviations. The great advantage of the
technique is that it encourages the team to consider other less obvious ways inwhich a deviation
may occur, however unlikely they may seem at first consideration. In this way the study becomes
much more than a mechanistic check-list type of review. The result is that there is a good chance
that potential failures and problems will be identified which had not previously been experienced
in the type of plant being studied.An essential feature in this process of questioning and
systematic analysis is the use of keywords to focus the attention of the team upon deviations and
their possible causes. These keywords are divided into primary keywords and secondary
keywords. Primary keywords which focus attention upon a particular aspect of the design intent
or an associated process condition or parameter. The primary keywords using in this HAZOP
analysis include temperature, pressure, flow and composition. Secondary Keywords which, when
combined with a primary keyword, suggest possible deviations. The secondary keywords applied
here included no, more, other, less, reverse and part of.

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