Distillation Basics

Mihir P.Shah,
Chemical Engineering Dept.
DDU, Nadiad
Dharmsinh Desai University
College Road, Nadiad- 387 001
1
 Separation Process

• Separation
– Reverse procedure of mixing (unmixing)
– Those operations which transform a
mixture of substances into two or more
products which differ from one another in
composition

2
 Separation Process

• Second Law of Thermodynamics

– All natural processes take place so as
to increase the entropy, or randomness,
of the universe
• Mixing
– Causes an increase in entropy

3
 Separation Process

• Separation, therefore, into products of

different compositions requires a process
where equivalent to thermodynamic work
must be supplied to cause a separation to
occur

4
 Separation Process
• Separation operations are interphase mass
transfer processes because they involve the
creation of second phase, by the addition of
heat as in distillation or contacting with the
foreign component as in absorption or
extraction.

5
 Separation

mixed separated

6
 Choice of separation
• If all the components are relatively volatile and required to be
separated in pure form then distillation is first choice.
• If relative volatility is very high then go for evaporation.
• If relative volatility is very low, (close to or equal to 1) then go
for special type of distillation like azeotropic or extractive
distillation.
– 10-30% by mass acetic acid in water is separated by butyl acetate
– Azeotropic mixture of 95.6% ethanol in water by benzene.
• For last case liquid-liquid extraction or crystallization followed
by distillation will be more economical.
• For recovery of only component from mixture, it is preferable to
go for absorption/stripping/extraction rather then directly doing
7
distillation.
8
 Criteria for selection
• For separation of penicilin from complex mixture, liquid-liquid
extraction is used.
• For removal of hydrogen and methane from aromatics, stripping is
used.
• For removal of propane from mixture called asphalt, stripping is used.
• For the removal of hydrogen sulfide from the natural gas mixture,
absorption using MEA as solvent is used.
• For removal of ammonia from lean aqueous solution, steam stripping
is preferred.
• If all components of air are to be separated in pure form cryogenic
distillation is preferred. But if only nitrogen in pure form is to be
separated from air then pressure swing adsorption is preferred.
History &Growth of Distillation
• The art of distillation dates back to at least 1st century A.D.
• By 11th century, it was being used in Italy to produce
alcoholic beverages (Batch operation).
– Early applications used vaporization and condensation
separately in two different chambers.
• The word Distillation : Latin word “ Destillare” means dripping
or trickling down
• By 16th century, it was improved by providing multiple vapor –
liquid stages in a so called rectificatorium which gave born to
the word “ Rectification”
• Rectification : Latin word “recte facere” means to improve.
• By 18th century, it was most widely used industrial method
with progressive modifications in process.

10
History &Growth of Distillation
• 1813 Cellier – Blumenthal in France
• 1820 Clement Germany – Packed tower
• 1822 Perrier in England – bubble cap tray
• 1830 Coffey seive tray column
• 1893 Ernest Soral – La Rectification de l’alcohol

11
 Dr.Frits J.Zuiderweg, 1988
Distillation is the most important and most visible separation
technology. The skyline of many refineries and chemical plants
is dominated by tall distillation towers, and it cannot be denied
that their spatial arrangements often amounts to architectural
beauty. Less spectacular, but also visible are the smoke stakes of
these industrial complexes; they represent the energy used in the
processing, the major part of which is consumed by distillation
processes.
16-Nov-17 12
 Dr.James R.Fair, 1990
Distillation, King in separation will remain as the
workhorse separations device of the process industries. Even
though it is old in the art, with a relatively mature technology
support base, it attracts research and professional interest.
Without question, distillation will sail into the future with clear
skies and a strong wind. It will remain the key separation
method against which alternate methods must be judged.
16-Nov-17 13
 DISTILLATION
• A process in which a liquid or vapor
mixture of 2 or more substances is
separated into its component fractions of
desired purity based on boiling points
difference, by application or removal of
heat.
• Application – Useful products such as in
petroleum refining, beverages, chemical
processing, petrochemicals, and natural
14
gas processing.
 Principle of separation
• Difference in boiling points of individual components and
vapor pressure characteristics of liquid mixtures.
• Separation of mixture into two or more products that have
difference in boiling points, preferentially boiling the more
volatile compound (MVC) out of the mixture.
• Distillation is based on the fact that the vapor of a boiling
mixture will be richer in the components that have lower
boiling points.
• If vapors are cooled less volatile compound (LVC) will have
greater tendency to condense than MVC.

15
 Why distillation?
• The preeminence of distillation is due to
strong fundamental base : Kinetics and
Thermodynamics
• Inherently lower thermodynamic
efficiency (10%)
• No other processes are more efficient than
Distillation
• Inter-condensers or inter-reboilers can
enhance the separation.
16
 Used except
1. The difference in the volatility between
the components are small.
2. A small quantity of LVC is to be
recovered.
3. A compound is thermally unstable even
under vacuum conditions.
4. The mixture is extremely corrosive or
highly fouling.
17
VLE IN DISTILLATION

18
 DISTILLATION
• Distillation is carried out by either of 2
principal methods;
– Based on production of vapor by boiling
liquid mixture to be separated and
condensing the vapors without allowing any
liquid to return to the still (Reflux);
– Based on the return part of the condensate
to the still (Reflux) under such conditions that
the returning liquid is brought into intimate
contact with the vapors on their way to the
condenser
19
 TYPE OF DISTILLATION

• BASED ON MODE OF OPERATION:

– FLASH
– BATCH
– CONTINUOUS

• BASED ON NUMBER OF COMPONENTS

TO BE SEPARATED:
– BINARY
– MULTICOMPONENT

20
 DISTILLATION
• BATCH
– The feed to the column is introduced batch-wise. That
is the column is charged with a batch and then the
distillation process is carried out. When the desired task
is achieved, a next batch of feed is introduced.
– Quality is poor but quantity can be maintained.
• CONTINUOUS
– The feed to the column is continuous. No interruption
occur unless there is a problem with the column or the
surrounding process units. They are capable of
handling high throughputs and are the most common of
the 2 types.
– Quality is appreciable. 21
 DISTILLATION
• BINARY DISTILLATION
– Separation of 2 chemicals.
– E.g. separation of ethyl alcohol (ethanol) from water
• MULTICOMPONENT DISTILLATION
– Separation of a mixture of chemicals
– E.g. petroleum refining. Crude oil is a very complex
mixture of hydrocarbons with literally thousands of
different molecules. Nearly all commercial distillation is
multicomponent distillation

22
 How Distillation Occurs?
P0b(T) > P0t(T)
yb > zb Vapor
Vapor
(Benzene Rich) yb

Feed liquid
Benzene +
Toluene
Q
Feed zb
Liquid
Liquid
(Toluene Rich) xb

23
Two Stage Process
y’b

yb

x’b

xb
24
 Production for Pure Benzene
VN

VN-1
VN-2 LN

LN-1
V1

V0

L1
Feed

25 25
L0
 VN

VN-1
VN-2 LN

V1
LN-1

V0
L1
Feed
V’1
L’0

V’M-1
L’1 V’M-2
V’M
L’M-1

LM
26 26
 VN

VN-1

LN
V2
LN-1
V1
L2
V0
L1 Separation Process
Feed V’1
L’0
V’2
L’1
V’M-1
L’2
V’M
L’M-1
27 27
LM
 A Distillation Column

Dr Ranjan K Malik 28 28
29
Towers

30
Old vs New Distillation Operation

31
32
 Complex Columns
(Refineries & Petrochemicals)
1. Crude Distillation Column
(Atmospheric Column)
2. Vacuum Distillation Column
(Dry and Wet Operations)
3. FCC Fractionator
4. Visbreaker Fractionator
5. Demethanizer
6. Azeotropic/Extractive/Reactive
33 33
34
35
36
Company with
multiple
Distillation
units

37
Crude Petroleum Unit at Night

38
A Complex Column

39 39
40
Crude Distillation Column

41
 BASIC COMPONENTS OF
DISTILLATION
• and operations;
– A vertical shell where the separation of liquid
components is carried out
– Column internals such as trays/plates and/or packings
which are used to enhance component separations
– A reboiler to provide the necessary vaporization for the
distillation process
– A condenser to cool and condense the vapor leaving the
top of the column
– A reflux drum to hold the condensed vapor from the top
of the column so that liquid (reflux) can be recycled
back to the column
42
Basic operation and terminology
DISTILLATION
• FEED is the liquid/Vapor mixture that is to be
processed
• Introduced usually somewhere near the
middle(???) of the column to a tray known as
the feed tray.
• The feed tray divides the column into a top
(enriching or rectification) section and a bottom
(stripping) section. The feed flows down the
column where it is collected at the bottom in the43
reboiler.
 Heat Supply in DISTILLATION
• Heat is supplied to the reboiler to
generate vapor. The source of heat
input can be any suitable fluid,
although in most chemical plants this
is normally steam.
• In refineries, the heating source may
be the output streams of other
columns. (Heat integration based on
pinch analysis)
• The vapor raised in the reboiler is re-
introduced into the unit at the bottom
of the column.
• The liquid removed from the reboiler
is known as the bottoms product or 44

simply, bottoms.
 Heat Removed from DISTILLATION

• The vapor moves up the column, and as it exits the top of the
unit, it is cooled by a condenser.
• The condensed liquid is stored in a holding vessel known as the
reflux drum.
• Some of this liquid is recycled back to the top of the column and
this is called the reflux.
• The condensed liquid that is removed from the system is known 45
as the distillate or top product.
 Over Head Product

Reflux
Liquid Distributor

Packing

Liquid Collector
Feed

Trays

Down-comer

Steam

46
Bottom Product
 Reboilers
Top Tray
Top Tray

Heating
Heating Medium
Medium

Bottoms Product
Bottoms Product

Circulating Pump

Forced Circulation Vertical Thermosiphon

47
 Reboilers
Top Tray
Top Tray

Heating
Heating Medium
Medium

Bottoms Product

Bottoms Product

Kettle Horizontal Thermosiphon

48
49
50
Kettle Type Reboiler

51
 Key Components
• For system of binary this concept is not existing, means
this has a significance for multi-component system.
• For a binary system, one can always carry out product
distribution independently.
• For multi-component system containing N components,
not possible to obtain pure component in single
column. If all components are need to be in pure form
then N-1 distillation columns are needed.
• In multi-component distillation, one cannot specify the
complete composition of top and bottom products
independently. But one can fix only distribution of any
two components of feed mixture.
16-Nov-17 52
 Key Components
• Two key components are selected.
• Key components are two components of
feed mixture between which one likes to
make sharp separation.
• Heavy Key Component and Light Key
Component.
• Species other than key components are
called Non-Key Components.
• Eg. Ethane, Propane, Butane.
• Decide HK and LK…….
16-Nov-17 53
 Operating Pressure
• Based on available cheapest cooling medium able to condense
top vapor.
• Bubble point of distillate should be sufficiently greater than
cooling water temperature.
• In case of partial condenser, bubble point of reflux should be
sufficiently greater than temperature of cooling water.
• If by this criterion, operating pressure is very high then go for
chilled water or brine solution.
• Operating pressure is always less than the critical temperature of
top product or temperature of cooling medium of overhead
condenser cannot be greater than critical temperature of top
product.
16-Nov-17 54
 Examples of deciding Operating
Pressure
• Acetaldehyde – ethanol – water system.
• Top product pure acetaldehyde (B.P. 20C)
• In country like India cooling water is available at 32C.
• Acetaldehyde is stored in bullet type storage tank. To avoid
storage cost like refrigeration, insulation etc it is necessary to
increase the B.P. of acetaldehyde.
• It was required to have B.P. > 50C (To use water as cooling
media).
• It was decided to keep B.P. = 60C.
• This requires to have top product at 3.6atm g pressure (V.P. of
acetaldehyde at 60C).
16-Nov-17 55
 Examples contd……
• Mixture of chloromethanes  methyl
chloride (B.P. -24C)
• V.P. of MC at 47.5C is 10atm to avail
cooling water facility.

16-Nov-17 56
 Examples contd……
• Separation of ethane from ethane-propane and butane
cooling water can not be used as cooling medium. Why?
• Because tc = 32.3C. (not much greater than cooling water
temperature of 32C).
• Minimum driving force required in STHE is 3-5C.
• At 10C V.P. of ethane 30atm. So one can use chilled water
as cooling medium but has to work with 30atm pressure.
• At 20atm, B.P. -6.4C, one can use proper brine solution,
but it will require higher cost of refrigeration and insulation.
• If this column is followed by demethanizer, then top
product stream of demethanizer can be used as cooling
medium.
16-Nov-17 57
 Vacuum system
• Heat sensitive materials
• To facilitate the use of cheaper heating
medium in reboiler
• Alter vapor-liquid equilibrium data.

16-Nov-17 58
 Advantages of using Vacuum
• Prevents thermal decomposition of heat sensitive
materials.
– Separation of MCAA – AA. (B.P. of MCAA =
120C)
• Allows use of more economical heating medium
such as steam against hot oil in high capacity
plants.
– EG – Water (B.P. EG = 197C (bottom),
superheated steam = 180C)
• Requires fewer stages or lower reflux ratio or both
in many cases where relative volatility increases
16-Nov-17 59
with decrease in the operating pressure.
 Advantages contd….
• In some cases vacuum breaks azeotrope and make the
separation easier.
– Ethanol – water P < 70torr no azeotrope
• Reduces undesirable side reactions in reactive
distillation.
– Ethyl benzene – styrene under vacuum does not polymerize
• Provides safety in distillation of toxic and hazardous
material.
– Separation of HNO3 from azeotrope of HNO3 - water
• Increases product recovery when dealing with
maximum temperature constraints.
16-Nov-17 60
– Refinery Vacuum towers
 Disadvantages
• Required larger column diameter and larger
vapor line diameter
• Costlier cooling source is required for
condensation.
• Presence of air as non-condensables
reduces the efficiency of main condenser.
• Increases the possibility of contamination of
products by air or other components.
16-Nov-17 61
 Conditions of Operations: usually fixed
• Feed composition and quantity.
• Reflux ratio (known or unknown)
• Thermal condition of feed (q line or value)
• Degree, type or amount of fractionation or condensation of
overhead, including composition of overhead or bottoms.
• Column operating pressure or temperature of
condensation of overhead including type of condensation,
i.e. total or partial condenser
• Constant molal overflow from stage to stage for simple
ideal systems following Raoult‟s law.

16-Nov-17 62
 Total condenser
• Overhead vapor is condensed to liquid state
• Total vapor pressure of condensate =
pressure inside condenser + pressure
inside accumulator
• When heat load on condenser is exactly
equal to the latent heat of saturated vapor,
condensed liquid will be bubble point liquid.
• Condensate is divided to two streams one
going to top of the column being reflux and
second will be distillate.
16-Nov-17 63
 Partial Condenser
• Product will be vapor in equilibrium with
liquid.
• Will be designed as top external tray of
distillation column.
• All condensed liquid is returned to column
as reflux, while all vapor is withdrawn from
the accumulator as product. In this case yc
= xD
• Both liquid and vapor products are
withdrawn, with liquid reflux composition
16-Nov-17 64
being equal to liquid product composition.
 Partial and total condenser

Liquid
Product

16-Nov-17 65
16-Nov-17 66
 Total Reflux : Minimum Plates
• When all overhead vapor from top tray is condensed and
returned to the top tray.
• Usually column is brought to equilibrium at total reflux for
test.
• Minimum number of plates are required under this
condition.
• Called as no feed, no product condition.
• Infinite heat requirements, L/V =1.
• One of the extreme condition of distillation used for
measure of complexity or difficulty of separation.
• In McCabe-Thiele Method, Operating line will coincide with
45o line.
16-Nov-17 67
 Minimum Number of Stages for McCabe-Thiele
Equilibrium
curve

y
2

yN
3

yB

xB x=zF xD

By returning all the exiting vapor as Although this is the minimum number
reflux and all the exiting liquid as of stages, no product is produced
boilup the operating lines have slope (note the feed must then go to zero).
of one.
16-Nov-17 68
 Minimum Reflux : Infinite plates
• As reflux ratio is decreased from infinity for total reflux
condition, more theoretical steps or trays are required to
complete a given separation.
• Another limiting condition for column operation.
• Below this ratio the specified separation cannot be made even
with infinite number of plates.
• Actual reflux ratio is generally considered as 1.2 to 1.5 times
minimum reflux ratio.
• Graphically it is evaluated as the line with smallest slope from
xD intersecting with equilibrium curve at the same point as the
“q” line for the mixture following Raoult’s Law.
16-Nov-17 69
 Minimum Reflux Ratio
• External Reflux Ratio = L/D
• Internal Reflux Ratio = L/V

L L D x  yC
 
 
L D  1 x
min D

 V  min D  xC
min

 D
L
min

x D  yC
yC  xC

16-Nov-17 70
 Minimum Reflux for McCabe-Thiele
Equilibrium
curve

yN

yB

xB x=zF xD

By returning no exiting vapor as reflux Although this is the minimum amount

and no exiting liquid as boilup the of reflux, it takes infinite stages (note
operating line intersection is as far to the pinch point between the operating
the left as equilibrium allows. lines and equilibrium).

16-Nov-17 71
 Minimum Reflux for Non-ideal McCabe-Thiele
Equilibrium
curve

yN

yB

xB xD F
x=z

Although this is the minimum amount

of reflux, it takes infinite stages (note
the pinch point between the operating
16-Nov-17 lines and equilibrium). 72
 Optimum Reflux Ratio
• Should be optimum and the most economical.
• Optimum reflux is the value of reflux ratio for
which the total cost of distillation is minimum.
• Depends upon : Type of system/ feed, specified
separation and operating condition.
• Change in the desired purity of products will also
change the optimum value.
• At the minimum reflux : column requires infinite
number of trays or packing height so infinite fixed
cost, but minimum operating cost (heating, cooling
mediums, reflux).
16-Nov-17 73
 Optimum Reflux Ratio
• As reflux increases: no of trays and packing decreases, but
Dc, size of condenser and reboiler will increases, reflux
pump cost will increases so fixed cost decreases and but
operating cost increases.
• This is not continued as the reflux increases, at certain
value, no of trays required will become constant but size of
heat exchanger, pump of reflux is still increases.
• That means, fixed value will pass through a minimum value
at some reflux ratio after that it will again increase.
• Operating cost always increases.
• Total annual cost = fixed cost + operating cost
• So optimum reflux ratio will minimize above cost.
16-Nov-17 74
 Optimum Reflux Ratio
• Many hydrocarbon distillations, R = 1.2 to
1.5Rm
• Difficult distillations R > 1.5Rm.
• Azeotropic mixture R is very high.

16-Nov-17 75
 Feed Stage Considerations
In determining the operating lines for the rectifying and stripping sections we needed the bottoms and
distillate compositions and reflux and reboil ratios. The compositions can be independently specified, but R
and VB are related to the vapor to liquid ratio in the feed.

Subcooled Liquid Bubble Point Liquid Partially Vaporized

VV V  VF  V
L V V L
L

F F
F

L  FL V L  F L V L  L  LF V

Dew Point Vapor V  F V Superheated Vapor V  F V

L L

F F

76
LL V LL V
77
 Selection of equipment for
Distillation
• Plate columns can be designed to handle a wider range of liquid and gas flow-
rates than packed columns.
• Packed columns are not suitable for very low liquid rates.
• The efficiency of a plate can be predicted with more certainty than the
equivalent term for packing (HETP or HTU).
• Plate columns can be designed with more assurance than packed columns.
There is always some doubt that good liquid distribution can be maintained
throughout a packed column under all operating conditions, particularly in
large columns.
• It is easier to make provision for cooling in a plate column; coils can be
installed on the plates.
• It is easier to make provision for the withdrawal of side-streams from plate
columns.

78
 Selection of equipment for
Distillation
• If the liquid causes fouling, or contains solids, it is easier to make provision
for cleaning in a plate column; man ways can be installed on the plates. With
small diameter columns it may be cheaper to use packing and replace the
packing when it becomes fouled.
• For corrosive liquids a packed column will usually be cheaper than the
equivalent plate column.
• The liquid hold-up is appreciably lower in a packed column than a plate
column. This can be important when the inventory of toxic or flammable
liquids needs to be kept as small as possible for safety reasons.
• Packed columns are more suitable for handling foaming systems.
• The pressure drop per equilibrium stage (HETP) can be lower for packing
than plates; and packing should be considered for vacuum columns.
• Packing should always be considered for small diameter columns, say less
than 0.6 m, where plates would be difficult to install, and expensive.
79
 Packed column are called
continuous contact column

Tray columns are called

staged contact column

80
 Packed Vs Plate column
Sr.No System Favoring Tray System favoring Packed
Column Column
1 Solid Handling Vacuum system
2 High Liquid rate Low pressure drop application
3 Variable feed composition and Pressure drop reduction can be
temperature translated into capacity gainn,
energy gain or separation
improvement
4 Large Diameter column Small diameter column
5 Performance prediction is easy Corrosive system
6 Less Weight so saving in coset Foaming system
of foundation and support
7 Interboilers, Intercondensers, Low liquid hold up
cooling coils and side draw
8 High turn down requiirement Polymerization and degradation
9 Chemical reactions Batch Distillation 81
 Selection of Equipments for Vacuum Distillation
• For high vacuum distillation, a packed tower is selected.
– Packed tower generally provides lower pressure drop and
lower residence time for liquid as compared to tray towers.
– For very high vacuum distillation, short path distillation is
used.
– For separation of MCAA and AA, the absolute pressure
inside Reboiler should be less than 50torr.
– The rate of thermal cracking increase exponentially with the
temperature.
– Separation of Vitamin E from the crude mixture is carried out
in short path distillation columns.
• For very small tower diameter packed tower is preferred. With
large diameters, tray tower is preferred. With very small
diameter (<150mm), fabrication of trays is difficult while large
diameter, liquid distribution is difficult in the packed tower.
 Tray Tower
• This is a high, round pillar.
• Within, a sequence of containers are placed, one above the other.
• The containers are used to carry the increasing fumes and
dropping liquid into romantic get in touch with.
• Much more effective in the separating procedure than loaded
systems and, they are also more expensive.
• There are various kinds of tray in use and the kind of chosen
relies on the level of item cleanliness needed, the kind of liquids,
liquid speed and other procedure factors of the program

83
Tray Tower

84
Tray towers

85
TRAY TOWERS

86
Detailed view of Distillation Column

87
 TRAY TOWER INTERNALS
• Trays : Provide a platform for sufficient contact between
liquid and vapor
• Downcomer: lead the liquid from one tray to the ext
• Weirs: maintains the depth of the liquid on the tray
• Distribution baffles
• Tray drainage : Permit drainage to liquid hold up of column
in case of shut down
• Feed system
• Draw offs
• Manholes and hand-holes

88
89
 TRAY TOWERS
• Tray towers are vertical cylinders.
• Liquid and vapor are contacted in stepwise
fashion on trays.
• Liquid enters at top and flows downward by
gravity.
• It flows across each tray and through a downspout to
tray below.
• Vapor flow upward through openings into
liquids in the form of bubbles.
• Overall effect is a multiple countercurrent
contact of vapor and liquid. 90
 TRAY TOWERS
• Each tray of the tower serves as a stage.
• No of equilibrium stages depends only upon the
difficulty of the separation.
• No of equilibrium stages are determined by,
• Material balance calculations
• Equilibrium considerations
• Stage efficiency (Real trays) is determined by,
• Mechanical design
• The condition of operation

91
 TRAY TOWERS
• Higher stage efficiencies depend upon:
• Sufficient contact time
• Large interfacial surface
• Higher intensity of turbulence
• The diameter of the tower depends upon
the quantities of the liquid and gas flowing
through tower per unit time.

92
 Functional Zones
• Active area of mixing of vapor and liquid
– Mass transfer area
• Vapor space above the active area
– Liquid is separated from vapor
• Downcomer between trays
– Transfers liquid from upper tray to lower tray
– Disengaging vapor from liquid

93
Classification of tray area

94
Tray Operative

95
 TYPES OF TRAYS
• Sieve trays
• Valve trays
• Bubble cap trays

96
Sieve type tray with down comers

97
 BDH type Rounded type

Snap in type
Gauge type
Valve type tray/ perforated tray

98
Flow pattern in various types of tray

99
100
 Valves
• Valve trays are perforated sheet metal decks on which
round, liftable valves are mounted.
• The vapour flows through valves which are installed
parallel to the outlet weir.
• Valve trays combine high capacity and excellent efficiency
with a wide operating range.
• Advantages:
– Excellent liquid/ vapour contacting.
– Higher capacity.
– Higher flexibility than sieve trays.
– Can handle higher loadings.
– Low-pressure drop than bubble cap.
101
 Sieve plates
• Sieve trays are flat perforated plate in which vapour rises
through small holes in tray floor, & bubbles through liquid
in fairly uniform manner.
• They have comparable capacity as valve trays.
• Has no separation contacting device.
• Advantages:
– Simple construction Low entrainment,
– Low cost Low maintenance cost
– Low fouling tendency
• Disadvantages:
– Less-flexible to varying loads than other two types

102
 Bubble caps
• Large number of holes over which cylindrical risers or chimneys are placed
• Inverted cups are located over the risers
• The vapor rises up through the holes and the risers and subsequently through
the number of rectangular, triangular or trapezoidal slots provided at the rim of
the caps.
• The riser diameter is normally 60 – 70% of the cap diameter
• Skirt clearance is 13 – 38mm is recommended to prevent plugging of the slots
due to residue building up
• Advantages:
– Moderate capacity
– Most flexible (high & low vap. & liquid rates)
– Can provide excellent turndown.
• Disadvantages:
– High entrainment, High fouling tendency
– High cost,
103
– High pressure drop
104
105
Sr. Factor Sieve Tray Valve Tray Bubble Cap Tray
No Comparison between various
1 Capacity High High Moderately High
2 Efficiency type ofHighPackingModerately High
High
3 Turn Down ~50% ~25-30% 10%
4 Entrainment Moderate Moderate High
5 Pressure Moderate Moderate High
Drop
6 Cost Low ~1.2 times sieve ~2-3 times sieve tray
tray
7 Maintenance Low Mow to moderate Relatively High
8 Fouling Low Low to moderate Relatively high : tends
to collect solids
9 Corrosion Low Low to moderate Relatively high
10 Design Well known Proprietary but Well known
Information readily available
11 Main Often used Where high Extremely low lliquid
Application when turndown is flow & when leakage
turndown is requried must be minimized 106
not critical
 Proprietary types of trays
• MD Trays – Linde / UOP,
• Ripple Trays – Stone & Webster Engg. Corp.
• Rectangular Valve (BDH),
• Valve Grid (MVG/SVG),
• SHELL HIFI, Con Sep Trays – Sulzer Ballast
Tray,
• Flexi tray, Bi-FRAC, SUPERFRAC and
ULTRAFRAC Trays – Koch-Glitsch Engg.Co.,
Tunnel Trays - Montz,
• Nye trays - Nye Engg Co, 107
 Down comers
Plates without down comers
• Plates are slightly smaller in diameter than the internal diameter
of the shell.
• They are having large number of holes or slots for the liquid and
vapor to pass through.
Plates with down comers
• Down comer Area is 12% of the total cross sectional area of the
plate.
• The function of down comer is to provide a passage for the
downward flow of the liquid from a top tray to the lower tray.
• An inlet weir helps to distribute the liquid as it enters the tray
from the down comer, and prevents direct impingement of the
liquid on the contacting device.
• The length of the weir is generally 60 to 75% of the diameter for
a cross flow tray and 50 to 60% of the diameter for the
multipass. 108
 Distribution baffles
• With uniform cap spacing it is not possible to
locate all caps at the end of the rows close to the
column wall.
• Due to excessive end clearance the liquid will
tend to short circuit such rows.
• If the end space exceeds the spacing by 2.5cm,
the gaps are closed by redistribution baffles.
• The clearance between these baffles and the
caps should be equal to the cap spacing.

109
 Tray drainage
• Tray drain holes are required to permit
drainage of the liquid hold up of the column
in case of shut down.
• These holes must be sufficiently large, so
that they may not plugged by sediments or
polymers.
• The current practice is to make holes of 1 to
1.5cm diameter along the weir.

110
 Feed system
• Feed nozzles are sized for a flow velocity of 1m
per second.
• The jet of entering liquid should break up
immediately on entering the column.
• Liquid feed to the column is above the top tray
and at intermediate positions.
• A pipe line located above the top tray, and just
opposite the inlet weir, feed the top tray.
• A baffle if provided opposite the feed pipe to
create uniform distribution.
• Various methods of intermediate feed
arrangement are shown in the figure below.
111
Feed Distributors
 Draw offs
• The drawing of the liquid from the bottom of the
column is either by use of a chimney tray or by a
draw pan as indicated in the figure.
• The chimney tray has no downcomer and is in
flush with a draw nozzle.
• Chimneys are normally of the size approximately
15% of column area.
• These should be so located as to prevent
directing vapor against the adjoining downcomer.

113
114
 Manholes and hand-holes
• Trays should be inspected for corrosion,
fouling and damage, a few weeks after star-up
and at six monthly intervals thereafter.
• Manholes are necessary at intervals in the
column so that each manhole serves 15-20
trays.
• The manhole size is usually 1000mm internal
diameter or 500x500mm opening in
rectangular size.
• In packed columns, the manholes are
necessary at each distributor and support plate
to be dismantled and removed.
115
 TRAY TOWER PERFORMANCE
• Flooding :
– It is excessive accumulation of liquid inside the column due to
high pressure drop.
– High pressure drop condition would occur when liquid leaves
one tray at low pressure and enters other tray at high
pressure.
– At low liquid flow rates, most of the liquid on the tray is in the
form of liquid drops. As the vapor velocity is raised, a
condition is reached where the bulk of these drops are
entrained into the tray above. Entire space between two trays
is filled with liquid. The liquid accumulates on the tray above
instead of flowing to the tray below. The tower is then flooded.
– Due to flooding, tray efficiency falls to a lower value.

116
 TRAY TOWER PERFORMANCE
• Weeping :
– A condition occurring where vapor rate in not
large enough to hold all the liquid on the tray so
that part of liquid flows over the weir and
remaining may rain down through the
openings.
• Dumping :
– A condition when none of the liquid reaches the
downcomer, all draining down through the tray
holes ( at very low gas rates).
117
 Flooding and Weeping

Weeping Flooding

Flow weeps through Liquid cannot get

the holes at low vapor down the column
velocity at high vapor velocity
Tray Hydraulics

119
 Multiple Pass Trays

Single Pass Two Pass Four Pass

120
121
122
Parts of Bubble Cap

123
124
125
Packed type column
• Packed towers are used for
gas-liq and liq-liq operation.
• Used for distillation,
absorption, liq-liq extraction.
• As its name indicates, the
packed structure is a straight,
metal pillar which contains
„Beds‟ of packaging content
which are used to carry the
increasing vapours into
romantic get in touch with
dropping fluid within the
structure..
• It is desire that pressure drop
be kept as maximum as
possible.
126
Packed Column Overview

127
 Packed bed column
The basic unit consists of:
• Shell
• Packing
• Packing support
• Liquid distributor
• Intermediate support and redistributors
• Gas and liquid entrances and nozzles.

128
 Packing
• Provides large surface area: a Packing General service application
high interfacial area between material
gas and liquid Glazed and Natural and acid conditions
• contain adequate passages unglazed, except hydrofluoric, solvent, not
(void volume) for both streams porcelain or good in caustic condition
without excessive liquid hold-up chemical
or pressure drop Stoneware
• Have an open structure: less Carbon Hot alkali, all acids except
resistance to gas flow nitric, no oxidizing atmospheres
• Perform uniform liquid
distribution on the packing
Plastic Alkali, salts, aqueous and acids,
surface depending on resin
• Promote uniform vapor gas flow
across the column cross
section. Steel and other Hot alkalis for steel, other
• strong but without excessive light gauge service to suit metals
weight metals

129
Random Packings

130
 Random Packing
• Random packings are simply dumped into
the tower during installation.
• Rasching ring:
– Hollow cylinder
– Diameter: 6 – 100 mm
– MOC: Porecelain (except alkalis and HF acid)
– MOC: Carbon( except highly oxidizing atm)
– MOC: Plastics (except organic solvents)

131
 Random Packing
• Lessing rings and other packings with
internal partition are less frequently used.
• The saddle shaped packings like berl
saddle and Intalox are available in the sizes
from 6 to 75 mm.

132
133
134
135
136
137
 Regular (Structured) packing
• The counter flow trays are a form of regular
packing.
• They offer the great advantage of low pressure
drop for the gas and greater possible fluid flow
rates.
• Stacked rasching rings are economically possible
only in very large sizes.
• Wood grids or hurdles are generally inexpensive
and frequently used where large void volumes are
used.

138
Structured Packing

Fair, J.R., Seibert, A.F., Behrens, M., Saraber, P.P., and Olujic, Z. “Structured
Packing Performance-Experimental Evaluation of Two Predictive Models ”,
Ind. Eng. Chem. Res. 39 (6), 1788-1796 (2000).

139
Structured Packing Wetted Area

140
141
Comparison between various
packing

142
 Packing support
• The function of support
plate is to carry weight of
the wet packing, which
allowing free passage of
the gas and liquid.
• Poorly designed support
will give high pressure
drop and cause local
flooding.
• Simple grid or perforated
plates are used as
support.
• Made from plastic,
ceramic or metals 143
144
145
 Liquid distributors
• Performance of packed bed
depends on proper distribution of
liquid in column.
• Central feed pipe, spray nozzle,
weir type, orifice type, feed pipe
with nozzles on it.
• Liquid redistributors
• They are used to recollect the liquid
that has migrated to the column
walls and redistribute it evenly over
the packing.
• Does dual work packing support
and liquid distribution.
• Wall wiper type
146
147
Packing Size Bulk Surface Packing
density area factor
in Mm Kg/m3 m2/m3 Fp
Rasching ring

Ceramic 0.5 13 881 368 640

1.0 25 673 190 160
1.5 38 689 128 95
2.0 51 651 95 65
3.0 76 561 69 36
Metal 0.5 13 1201 417 300
1.0 25 625 207 115
1.5 38 781 141 83
2.0 51 593 102 57
3.0 76 400 72 32

148
Pall ring Size Bulk Surface Packing
density area factor
Ceramic 0.62 16 593 341 70
5
1.0 25 481 210 48
1.5 38 385 128 28
2.0 51 353 102 20
3.0 76 273 66 16
Metal 0.62 16 112 341 97
5
1.0 25 88 207 52
1.5 38 76 128 40
2.0 51 68 102 25
3.0 76 64 85 16
Intalox saddle

Ceramic 0.5 13 737 480 200

1.0 25 673 253 92
1.5 38 625 194 52
2.0 51 609 108 40
149
3.0 76 577 22
 Hold down plates
• At higher gas rates, if surging occurs, the top layer
of packing will fluidized.
• This may lead to break up of packing or some
time blow out.
• Also called as bed limiters by avoiding bed
expansion.
• Hole size on the hold down plates should be less
than the diameter of the packing but higher
enough to give proper flow of gas and liquid
through it.

150
 Installing packing
• Ceramic and metal packing are normally dumped
to the column “WET”.
• The column is partially filled with water and the
packing dumped into the water.
• The height of the water is always kept higher than
the packing length.
• In case of dry packing, packing are send into
column through the bucket and spread over to the
column by maintaining randomness.

151
 Characteristics of Packed
Columns
• Low pressure drop / smaller diameter
• Random packing scale-up for HETP is difficult;
structured packing scale-up is predictable
• HETP prediction less well developed than for trays
• Low to moderate cost for random packing; high
cost for structured packing
• Not suitable for fouling service
• Feed point flexibility is difficult
152
 SELECTION OF EQUIPMENT
FOR DISTILLATION
• For high vacuum distillation, a packed column is
selected due to small pressure drop requirement.
• For very small tower diameter packed tower is
preferred.
• For handling very high ratio of liquid flow rate, tray
towers are preferred.
• For corrosive system, packed tower with plastic
packings (PP) , glass fiber etc. is more
economical than tray made of metals.
• If side products are to be drawn from the
153
distillation column, tray tower are preferred.
 CONDITIONS OF OPERATION
REQUIRED
• Feed composition and quantity
• Minimum reflux ratio and actual reflux ratio
• Thermal condition of feed (q line)
• Degree of separation including composition of
distillate and bottom
• Column operating pressure and temperature
• Constant molal overflow from stage to stage for
simple ideal system

154
 TRAY DESIGN
Three type of trays
• Bubble cap tray (BC)
• Sieve type tray/ perforated tray (ST)
• Valve type tray (VT)

155
 Factors to be consider for
selection
• cost : depends on MOC; for MS
BC:ST:VT = 3.0:1.5:1.0
• capacity : ST>VT>BC
• operating range : vapor and liquid rates;
ST<BT<VT; should be flexible for startup
and shut down loads
• efficiency : not much change in all trays
• pressure drop on each tray :
ST< VT<BT
156
 The “Real” World

Fouled Structured Packing Damaged Valve Tray

157
 The “Real” World

Plugged Distributor Tray “Blanking” Strips

158
Major Tray Damage

159
Fouling Resistant Design

160
Fouled Bubble Cap Tray

161
 Column
Internals from
SULZER
 Distillation Design

•Process Design of Distillation Column

•Mechanical Design of Distillation Column

Thank you….

164