Lab Name: Separation process
Desired composition achievement through changing Reflux ratio
in Continuous Distillation Column
Grading
Obtained Marks:
Total Marks:
Lab Report Group 1
Submitted By
Name Registration No.
Ahmad Kamal Shaheryar 11-3-1-003-2021
Ali Ahmad 11-3-1-005-2021
Abdullah Afridi 11-3-1-001-2021
Bilal Janjua 11-3-1-024-2020
Ahmad Yar 11-3-1-004-2021
Department of Chemical Engineering
Pakistan Institute of Engineering and Applied Sciences
P. O. Nilore, Islamabad, Pakistan
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Contents
List of Figures........................................................................................................................................ iii
List of Equations ................................................................................................................................... iv
Abstract .................................................................................................................................................. 1
Introduction........................................................................................................................................... 2
Background ........................................................................................................................................ 2
Experimental Setup ............................................................................................................................... 2
Objectives .............................................................................................................................................. 3
Procedure .............................................................................................................................................. 3
Experimental Setup ........................................................................................................................... 3
Startup ............................................................................................................................................... 3
Shutdown Procedure ........................................................................................................................ 3
Procedure of Experiment ................................................................................................................. 3
No Distillate Collection ...................................................................................................................... 4
Constant Distillate Collection............................................................................................................ 4
Safety Precautions ............................................................................................................................ 4
Observation and Calculation ................................................................................................................ 5
For feed composition: ....................................................................................................................... 5
At Total reflux .................................................................................................................................... 5
At Partial Reflux ................................................................................................................................. 6
Results and Discussion........................................................................................................................... 7
Conclusion.............................................................................................................................................. 8
References ............................................................................................................................................. 9
ii
List of Figures
Figure 1 Continuous Distillation Column ............................................................................................. 2
Figure 2 PPE for Lab .............................................................................................................................. 4
iii
List of Equations
Equation i ............................................................................................................................................... 5
Equation ii .............................................................................................................................................. 5
Equation iii ............................................................................................................................................. 5
Equation iv ............................................................................................................................................. 6
Equation v .............................................................................................................................................. 6
Equation vi ............................................................................................................................................. 6
iv
Abstract
The objective of the experiment was to separate a binary mixture of ethanol and water into their
individual constituents using continuous distillation apparatus. Experiment was performed under
two cases of total reflux and partial reflux. In the case of total reflux, no distillate was collected
and all condensed vapor were returned to the distillation column. The second part is done by
taking the Constant Distillate Collection Phase, where reflux and distillate flow rates were
measured.
The experiment emphasized the significant role of reflux ratio in continuous distillation process
which can optimize the separation efficiency and throughput of process. We can compare the
results of both cases to analyze which one is better to use in industrial process and designing.
1
Introduction
Background
Continuous distillation stands out for its ability to maintain a steady-state operation, making it a
crucial unit operation in industrial processes. This process profoundly influences the equilibrium
between liquid and vapor phases within the distillation column, directly impacting the composition
and purity of the distillate product. The experiment unfolds in two distinct phases. First, a Total
Reflux Phase is conducted, during which no distillate is collected, and all condensed vapor is
directed back into the column. Subsequently, a Constant Distillate Collection Phase ensues,
wherein meticulous measurements of both reflux and distillate flow rates are recorded. Through
rigorous data analysis, we endeavor to quantify precisely how alterations in the reflux ratio affect
the quality and quantity of the distillate output. This investigation not only provides practical
insights into the determination of reflux ratio but also serves as a tangible demonstration of the
theoretical underpinnings governing distillation processes.
Experimental Setup
Figure 1 Continuous Distillation Column
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Objectives
To understand the working of continuous distillation column
To determine effect of different reflux ratios in product composition
To investigate the separation efficiency of the distillation process
Procedure
Experimental Setup
The experiment setup consists of the following components:
1. Boiler
2. Distillation column with packed bed
3. Condenser
4. Sample collection vessel
5. Ethanol water mixture
Startup
1. Verify that the distillation column and associated components are securely connected and
sealed to prevent any leaks.
2. Turn on the heating element under the feed and set it to the desired operating temperature
for the distillation process.
3. Allow the system to equilibrate until the desired temperature is reached and stabilized.
Shutdown Procedure
6. Gradually reduce the temperature to prevent abrupt cooling of column
7. Disconnect the heating source
8. Allow distillation column to cool down
Procedure of Experiment
The experimental procedure consisted of the following steps:
1. Follow the startup procedure and operate the distillation column
2. Adjust the vacuum carefully
3. Turn on the water inlet and adjust the water inlet flow rate
4. Record pressure and temperature data in regular intervals
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5. Collect sample at different time intervals
6. Perform the experiment at constant and total reflux ratio
No Distillate Collection
7. Close the distillate collection valve to prevent any distillate from being collected.
8. Gradually increase the reflux flow rate until a stable total reflux condition is achieved.
9. Record the flow rate of the reflux (L) once equilibrium is reached.
Constant Distillate Collection
10. Open the distillate collection valve to allow the distillate to be collected at a steady rate.
11. Adjust the reflux flow rate to maintain a constant value while collecting the distillate.
12. Record both the reflux flow rate (L) and the distillate flow rate (D) once stable conditions
are established
Safety Precautions
1. Always wear appropriate personal protective equipment (PPE) such as a lab coat, safety
goggles, and gloves when handling chemicals or operating the equipment.
2. Be cautious of hot surfaces and equipment. Use heat-resistant gloves or mitts when
handling hot glassware.
Figure 2 PPE for Lab
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Observation and Calculation
𝐿
𝑉̇ = 6
𝑚𝑖𝑛
𝑊𝑀𝑖𝑥𝑡𝑢𝑟𝑒 = 0.106 𝑘𝑔
𝑉𝑜𝑙𝑢𝑚𝑒(𝑉) = 1.4 × 10−4 𝑚3
𝑘𝑔
𝜌𝑀𝑖𝑥𝑡𝑢𝑟𝑒 = 815.4
𝑚3
𝜌𝐷𝑖𝑠𝑡𝑖𝑙𝑙𝑎𝑡𝑒 = 𝑋 × 𝜌𝐸𝑡ℎ𝑎𝑛𝑜𝑙 + (1 − 𝑋) × 𝜌𝑊𝑎𝑡𝑒𝑟
Equation i
Substituting values to equate X
𝑘𝑔
𝜌𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = 784
𝑚3
X = 0.85 (in final product)
For feed composition:
Feed density=927.27 𝑘𝑔𝑚−3
𝑘𝑔
𝜌𝐹𝑒𝑒𝑑 = 927.27
𝑚3
Using
X=0.33 (feed composition)
At Total reflux
𝑉 =𝐿+𝐷
Equation ii
𝑇1 = 61°𝐶
𝑇2 = 73℃
𝑘𝐽
𝐶𝑝 = 4200
𝑘𝑔 × 𝐾
𝑄 = 𝑚 × 𝐶𝑃 × (𝑇2 − 𝑇1 )
Equation iii
𝐿 𝑘𝑔
𝑚̇ = 6 = 0.1
𝑚𝑖𝑛 𝑠𝑒𝑐
Using Equation iii
5
𝑘𝐽
𝑄̇ = 4939.2
𝑠
𝑄̇
𝑚=
𝜆
Equation iv
𝑘𝐽
𝜆 = 846
𝑘𝑔
Using Equation iv
𝑘𝑔
𝑚̇ = 5.8
𝑠
At Partial Reflux
Using Equation ii
𝑉𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = 120𝑚𝑙
𝐷 = 0.09 𝑘𝑔
𝑇1 = 62°𝐶
𝑇2 = 70℃
Using Equation iii & Equation iv
𝑚 = 0.147 𝑘𝑔
𝑅𝑒𝑓𝑙𝑢𝑥(𝐿) = 𝑚
Equation v
𝐿 = 0.147𝑘𝑔
𝐿
𝑅=
𝐷
Equation vi
𝑹 = 𝟔𝟑. 𝟒
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Results and Discussion
The experimental results reveal the substantial impact of the reflux ratio on the continuous
distillation process. The Total Reflux Phase, characterized by the absence of distillate collection,
established a stable baseline condition. Subsequently, in the Constant Distillate Collection Phase,
with a defined distillate flow rate, a thorough analysis demonstrated the varying energy demands.
Specifically, the absence of distillate collection led to higher energy input, aligning with theoretical
expectations. As distillate collection commenced, the energy demand decreased, indicating
potential energy savings. The calculated reflux ratio of 63.4 serves as a crucial operational
benchmark for similar binary mixtures. Overall, this experiment underscores the significance of
reflux ratio control in achieving desired separation efficiencies 6 and provides valuable insights
for optimizing distillation processes in practical industrial applications.
The possible errors in the results could be from different sources:
Personal error in the data collection of compositions may cause error in result
Instrumental error was also involved as the pressure adjustment was difficult, the
temperature measurements may include uncertainty which can cause inaccurate results
We assumed the latent heat of vaporization to be constant, this assumption can also cause
deviation from real world conditions and affect the results
Neglecting various losses such as vapor leakage, heat losses can lead to result inaccuracy.
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Conclusion
This experiment focused on determining the reflux ratio's impact on a continuous distillation
process for a binary mixture of ethanol and water. The two-phase approach, encompassing a Total
Reflux Phase followed by a Constant Distillate Collection Phase, allowed for a comprehensive
examination of the process dynamics. The calculated reflux ratio of 63.4 in the Constant Distillate
Collection Phase proved to be a pivotal operational parameter, offering a benchmark for similar
binary mixtures. The experiment demonstrated that alterations in the reflux ratio significantly
influence the efficiency and energy consumption of the distillation process. The observed shift in
distillate composition towards higher methanol content underscored the process's effectiveness in
separating components based on volatility.
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References
1. https://en.wikipedia.org/wiki/Continuous_distillation
2. http://enggyd.blogspot.com/2012/02/distillation-operator-functions-and.html
3. file:///C:/Users/Yasar/Downloads/Continuous%20Distillation%20Procedure%20Edit%20
%231%20(1).pdf
