INDIAN INSTITUTE OF TECHNOLOGY, KANPUR

SURGE-2019

A Project Report

Design and control of extractive distillation column for separation of

homogeneous binary azeotrope using heavy entrainer

Submitted by:

Nishant Gupta
Roll no. S190094
Department of Chemical Engineering

National Institute of Technology, Hamirpur

Project supervised by:

Dr. Nitin Kaistha

Professor, Department of Chemical Engineering

Indian Institute of Technology, Kanpur

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 CERTIFICATE

This is to certify that the project entitled ‘Design and control of extractive distillation column
for separation of homogeneous binary azeotrope using heavy entrainer’ submitted by Nishant
Gupta (S190094) as a part of Students-Undergraduate Research and Graduate Excellence 2019
offered by the Indian Institute of Technology, Kanpur, is a bonafide record of the work done by
his/her under my guidance and supervision at the Indian Institute of Technology, Kanpur from
13thMay, 2019 to 10th July, 2019.
Dr. Nitin Kaistha
Professor, CHE, IIT-K

Department of Chemical Engineering

Indian Institute of Technology, Kanpur

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 Table of Contents
Abstract
Acknowledgements

1. Introduction
1.1. Prelude
1.2. Methods
1.3. Applications
1.4. Research objectives

2. Literature Review
2.1. Extractive Distillation
2.2. Description of process
2.3. Study of azeotropic system
2.3.1. Selection of Entrainer
2.4. Control structure of Extractive distillation process

3. Simulation – setup & results

3.1. Steady state simulation
3.1.1. Design Variables
3.1.2. Simulation results
3.1.3. Analysis of results
3.2. Dynamic simulation
3.2.1. Dynamic run results
3.2.2. Analysis of results

4. Conclusions
5. References

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Abstract

Keywords: extractive distillation, homogeneous binary azeotrope, design and control, Aspen Plus
simulation

Of few methods of separating binary azeotropes, extractive distillation has been chosen. Design
and control strategy of an extractive distillation column for separating homogeneous azeotropic
binary mixture has been tested in this work. Ethanol-water azeotropic system has been chosen for
the purpose. A simulation has been developed on Aspen Plus V8.8 using RadFrac model for
distillation column.

A third component added, called an entrainer, takes up one of the component of the mixture and
carries it along with it thus altering the relative volatility of the components. Extractive distillation
uses a heavy entrainer for separation of homogeneous azeotropes and mixtures with low relative
volatility. Selection of entrainer is based on use of Residue curve maps and iso-volatility curves.
Ethylene glycol has been used for the purpose.

Important design parameters of an extractive column are solvent to feed flow ratio, number of
stages in extractive column, feed and entrainer tray location. Minimizing reboiler duty is intended.

Luyben control strategy with modifications has been tested for a 10% disturbance in feed flow and
feed composition. This slight modification has resulted in a more robust control. Makeup entrainer
has been used to control sump level of recovery column.

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 Acknowledgements

Firstly, I would like to thanks SURGE team and IIT Kanpur for such a wonderful experience. I am
indebted to Dr. Nitin Kaistha for believing in me and for all the guidance.
I am equally indebted to Mr. Kalp Mishra, my co-mentor, without whom it would not be possible
to complete the project. I am thankful to him for all his efforts, discussions and days he spent
working along with me. I am grateful to Mr. Vivek Kumar for all his guidance and support. I also
appreciate the efforts from all my colleagues in Dr. Nitin’s lab.
I would like to thanks faculty members at NIT Hamirpur. I am grateful to Dr. Tapas Palai and Dr.
Leela Manohar for believing in me and recommending me for joining the program.
I am thankful to my friends for the wonderful time. I appreciate the efforts from my friend Mr.
Adil Wazeer for the helping me out in writing reports and technical papers.
I am always grateful to my nana and mummie for always backing me up.

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1. Introduction

In this project we have discussed about the fundamental design and control strategy of an extractive
distillation column for separation of azeotropic mixtures. Study has been carried out on ethanol-
water system. Ethylene glycol has been chosen as entrainer.

1.1. Prelude:
Distillation is a method of separating the components of a solution which depends upon the
distribution of the substances between a liquid and a gas phase, applied to cases where all
components are present in both phases (Treybal, 1980). It is the relative volatility of the
components of the mixture that determines the ease of separation.
Distillation is most frequently carried out in multi-tray columns, generally having a rectifying
section and a stripping section. The lighter component is drawn-off the top as distillate while the
heavier component is withdrawn from bottoms. A part of the distillate is returned to the column as
reflux. Being a very energy-intensive technique a distillation column is provided with a reboiler.
Many mixtures have vapor and liquid phases that have identical compositions. Such mixtures are
called azeotropes. This means using simple distillation separation beyond azeotropic composition
cannot be achieved, no matter how large the reflux ratio may be or how many plates we put in.
Azeotropes occur because of non-ideal phase equilibrium resulting from the molecular interaction
of dissimilar chemical components.
Azeotropes are much common in industries. The most important example is ethanol, which forms
a minimum-boiling homogeneous binary azeotrope with water. Butanol is another biofuel example
that forms an azeotrope with water. The non-ideality in this system is so large that the azeotrope
is heterogeneous, forming two liquid phases.

1.2. Methods:
Homogeneous binary azeotropes can be separated using several methods.
1. Pressure-swing distillation
2. Azeotropic distillation (uses a light entrainer)
3. Extractive distillation (uses a heavy entrainer)
4. Batch Extractive distillation
Heterogeneous binary azeotropes can be separated by taking advantage of the liquid–liquid phase
separation in a decanter.
Membranes can also be used to purify a mixture and attain composition beyond the azeotropic
composition. The pervaporation process features a liquid feed, a liquid retentate, and a vapor
permeate. Divided wall columns are recent advancements in this sector.

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Throughput, quality and economics are key parameters for any production unit. As such design
and control of process is essential. With advancements in numerical methods and computational
techniques rigorous steady-state and dynamic simulation tools (Aspen Plus and Aspen Dynamics)
are used for design calculations and rigorous dynamic simulations. Aspen plus software.
The design and control of azeotropic systems is a challenging area, requiring application of many
chemical engineering principles: thermodynamics of phase equilibrium, mass and energy balances,
and dynamics and control.

1.3. Applications:
The petroleum industry seldom encounters azeotropes because the hydrocarbon components have
similar molecular structures. The chemical industry, on the other hand, frequently deals with
components of different types, which often produce azeotropes. Common examples are the
production of methyl acetate, tetrahydrofuran, tert-amyl methyl ether, isopropanol, vinyl acetate,
and many others. The emerging biofuel processes typically have fermentation products that form
azeotropes with water, which is present in large excess in the fermenter. Ethanol is the most
common example.

1.4. Research objectives:

 Selection of suitable entrainer and creating distillation sequence.
 To study functioning of an extractive distillation column in steady state.
 To develop control strategy for the column.
 Future prospects.

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2. Literature review

2.1. Extractive Distillation:

In most chemical systems, the predominant non-ideality occurs because of molecular interactions.
Homogeneous azeotropic and low-relative-volatility mixtures are common industry, and their
separation cannot be realized by conventional distillation. Extractive distillation is a suitable
widely used technique for separating such mixtures.
The essence of the process lies in the fact that a third component E added to a mixture A-B (with
A having a lower boiling temperature than B), preferentially soaks up one of the components,
alters the relative volatility and carries it along the bottom. The third component added is called
an entrainer and it is the heaviest component the system.
According to the definition from Doherty and Malone, “extractive distillation” is a method of
separating minimum-boiling binary azeotropes by use of an entrainer that is the heaviest species
in the mixture, does not form any azeotropes with the original components, and is completely
miscible with them in all proportions. Adding this heavy entrainer into the system causes the
relative volatility of the original two components to be enhanced so that one original component
can go overhead and the other component will go with the heavy entrainer to the column bottoms.

2.2. Description of process:

The extractive distillation system consists of two distillation columns, first being an extractive
column and the second being a recovery column. Feed is introduced to the extractive column
somewhere in middle. The entrainer is added somewhere near the top, but not at the top, of the
extractive column. The lightest key A is drawn off as distillate while the heavier key and the
entrainer move to bottoms. Distillate contains nearly pure A with some entrainer E as the key
impurity. The bottom contains heavier component B and nearly all entrainer E, with less than
negligible A.
The upper section of the column (above the entrainer feed location) is called the rectifying section,
and its purpose is to separate the lightest key A and the entrainer. The middle section of the column
(between the entrainer feed stage and the fresh feed stage) is called the extractive section. The
purpose of this section is to suppress B from going up the column. The bottom section of the
column (below the fresh feed location) is called the stripping section, and its purpose is to keep A
from going down the column.
The bottom product from the extractor is fed to the recovery column where nearly all of B escapes
as distillate and entrainer E is recovered into bottom stream. The recovered entrainer along with
some make-up is recycled through the system.

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The schematic diagram of the process is shown below:

MIXR

DISTL-A DISTL-B
MKUP RECVR

ENTR

EXTR

FEED BTMS-B+E

HETR
REC-ENTR BTMS-E

Fig.1: Flowsheet of extractive distillation process designed on Aspen Plus V8.8

2.3. Study of azeotropic system:

Ethanol-water forms a minimum boiling azeotrope at 90 mol% ethanol at atmospheric pressure.
Therefore, no matter how large the reflux ratio may be or how long the tower is we cannot achieve
purity any better than 90% ethanol by conventional distillation. T-xy and x-y curve for ethanol-
water at 1 atm pressure have plotted using NRTL base method.

T-xy diagram for ETHANOL/WATER y-x diagram for ETHANOL/WATER

101 1.00

100 x 1.0133 bar 1.0133 bar

0.95
y 1.0133 bar
99
0.90
98
0.85
97
0.80
96

95 0.75

94 0.70

93 0.65
92
Vapor mole fraction, ETHANOL

0.60
91
Temperatu re, C

0.55
90
0.50
89

88 0.45

87 0.40

86 0.35

85
0.30
84
0.25
83
0.20
82
0.15
81

80 0.10

79 0.05

78 0.00
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00
Liquid/vapor mole fraction, ETHANOL Liquid/vapor mole fraction, ETHANOL

Fig. 2: a) T-xy curve for ethanol-water system b): x-y curve for ethanol-water system using NRTL base method

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2.3.1. Selection of entrainer:
For a solvent to be used as an entrained it should have following characteristics:
 Enhance the relative volatility of the key component.
 Entrainer to feed ratio should be small.
 It must be soluble with feed in all proportions and must not form two phase with it.
 It should be easily separated from the bottoms.
 Inexpensive and readily available.
 Stable at operating temperatures.
 Non-reactive with other components and equipment.
 Low latent heat.
 Non-corrosive, non-toxic, non-flammable.
For selection of most suitable entrainer residue curves and iso-volatility curve may be generated.

Residue curves graphically depict azeotropes, heterogeneous phase location, separation feasibility,
and distillation paths for the extractive distillation tower. These curves are very useful in
determining the process design of extractive distillation systems. A residue curve map is liquid
phase composition profile one would get in a distillation column operated at total reflux condition.
Possible distillation products and phase equilibria are evident by residue curves.

A iso-volatility curve traces the unity relative volatility of a binary mixture by adding another
component into the system.

Residue curves and iso-volatility curve for ethanol-water system with two candidate entrainers,
Glycol and DMSO are plotted below.

WA TER(1 00.0 2 C)
T e r na r y M a p ( M o le B a s is )
WA TER(1 00.0 2 C)
T e r na r y M a p ( M o le B a s is )
0.95
0.95
0.90
0.90
0.85
0.85
0.80
0.80
0.75
0.75
0.70
0.70
0.65
0.65
0.60
0.60
0.55
0.55
0.50
0.50
0.45
0.45
0.40 0.40
0.35 0.35
0.30 0.30
0.25 0.25
0.20 0.20
0.15 0.15
78.15 C 78.15 C
0.10 0.10
0.05 0.05
GLYCOL ETHA NOL DMSO ETHA NOL
(197 .08 C ) 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 (78.3 1 C) (190 .74 C ) 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 (78.3 1 C)

Fig. 3: residue curves and iso-volatility curves for a): ethanol-water-glycol b): ethanol-water-DMSO system

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The cyan line are the residue curves for different initial compositions. They originate from the
azeotropic composition for minimum boiling systems i.e. the lowest temperature of the system,
here 78ºC, moves through intermediate temperatures and terminate at highest temperature, which
corresponds to entrainer boiling point, here 197.08 ºC for glycol. Both glycol and DMSO
corresponds to stable nodes and can be used as entrainers. Water being at saddle point can never
be product of extractive column.
The dashed red lines are the iso-volatility lines. The nearer the intersect to A on A-E edge, lesser
the entrainer required. With glycol as entrainer, iso-volatility curve intersects nearer to ethanol
corner than in case of DMSO, hence is a better entrainer.
Use of equi-volatility curves for screening of entrainers have been there in many literatures.

2.4 Control structure for extractive distillation process:

The following control strategy developed by Luyben has been tested, with some modifications.
1. The levels of the reflux drums for both columns are controlled by manipulating the distillate.
2. Top pressures of both columns are controlled by the condenser duty.
3. The bottom level of the extractive distillation column is controlled by manipulating the bottoms
flow.
4. The recycle entrainer feed temperature is controlled by manipulating the cooler duty.
5. Reflux rates in the two columns are controlled by manipulating the fresh feed rate.
6. Bottom level of the entrainer in recovery column is controlled by the entrainer makeup flow.
The entrainer is recirculating in the system, its level in the recovery column sump never changes
except for some small losses.
7. The entrainer flow to the column to the fresh feed flow has been ratioed.
8. Two reboiler duties that can be used in a tray temperature control loop in each column. The
temperature control point is selected at a particular stage with high sensitivity and also with near
linear behavior.

Fig. 4: The schematic diagram of the modified Luyben control structure

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3. Simulation- setup & results:
Steady state and dynamic model of an extractive column was simulated on Aspen Plus V8.8
software.

3.1. Steady-state simulation:

Design of extractive distillation column is our objective. The two distillation columns were
simulated using Radfrac model. Radfrac model uses rigorous plate-by-plate calculation based on
MESH analysis. There are two input streams to the first column: one for feed and other for
entrainer, fed somewhere above the feed tray. Bottoms are fed to the second column. A makeup
stream accounts for the lost entrainer in the recycle stream. The simulated flowsheet of the process
is shown in figure.
There are four design variables to be determined for extractive column: entrainer to feed flow rate
ratio, no. of plates in column, entrainer and feed tray location. The TAC is used as the objective
function to be minimized, which includes annualized capital costs and operating costs. The capital
costs include column shell, trays, reboiler, and condenser.
However, only reboiler duty is considered as objective function. We have tried to optimize the
flowsheet manually by iteratively varying each of the parameters. Alternatively, sensitivity block
may be used to optimize the flowsheet by varying different process parameters and selecting those
for which objective function is minimized.
The property method chosen for the ethanol-water-glycol mixture was NRTL (non-random two
liquid). NRTL base method is recommended for highly non-ideal systems such as ethanol-water-
glycol.

3.1.1. Design variables:

Feed: ethanol-water mixture Entrainer: ethylene glycol (recycle + makeup)
Flow rate: 100 kmol/hr. Flow rate: 100 kmol/hr.
Composition: equimolar Temperature: 72ºC; Pressure: 1 atm
Temperature: 25ºC; Pressure: 1 atm Solvent to feed ratio is: 1
The extractive column had 44 trays including a total condenser and kettle type reboiler. For
homogeneous systems vapor-liquid phase are valid. Convergence method was opted for strongly
non-ideal liquid. The Fresh feed is fed to 27th stage while the entrainer is fed to 4th stage of the
column. Stage pressure drop was taken to be 0.0068 atm with condenser operating at 1 atm.
The two design specifications are setting top composition at 99.99 mol% ethanol and the purity of
ethanol in the bottom stream to be 0.0001. The two design specifications are met by varying the
remaining two degrees of freedom in this column: reboiler duty and distillate rate.
The recovery column had 40 stages including total condenser and kettle type reboiler. For
homogeneous systems vapor-liquid phase are valid. Convergence method for strongly non-ideal

12
liquid may be opted. The feed is fed to 20th stage. Stage pressure drop was taken to be 0.0068 atm
with condenser operating at 1 atm. Recovered glycol is fed to a cooler to lower its temperature to
72ºC.
A makeup stream accounts for the lost entrainer. A calculator block used adds to the recycle stream
pure entrainer just enough to make up for the losses.

3.1.2. Simulation results:

Following are the result tables for various streams and blocks:
stream FEED MKUP ENTR DISTL-A BTMS-B+EDISTIL-B BTMS-E
Phase: Units: Liquid Liquid Liquid Liquid Liquid Liquid Liquid
ETHANOL KMOL/HR 50 0 2.09E-25 49.985 0.015001 0.015001 2.09E-25
WATER KMOL/HR 5.00E+01 0 1.00E-04 4.00E-05 50.00006 5.00E+01 1.00E-04
GLYCOL KMOL/HR 0.00E+00 0.004959 1.00E+02 0.004959 99.99504 1.11E-26 99.99504
Mole Flow KMOL/HR 100 4.96E-03 1.00E+02 49.99 1.50E+02 50.01496 99.99514
Mass Flow KG/HR 3204.216 3.08E-01 6206.846 2303.069 7107.992 901.4544 6206.538
Volume Flow L/MIN 63.15097 0.00476861 96.16075 52.33195 119.2118 16.3631 110.1201
Temperature C 27 7.20E+01 72 78.31275 140.8545 99.92042 205.1264
Pressure BAR 4.356975 4.25565 1.2159 1.01325 1.309524 1.01325 1.281964
Vapor Fraction 0 0 0 0 0 0 0
Liquid Fraction 1 1 1 1 1 1 1
Solid Fraction 0 0 0 0 0 0 0
Molar Enthalpy CAL/MOL -67268.2 -107830 -107830 -64596 -92169.8 -66872.4 -102320
Mass Enthalpy CAL/GM ######## -1.74E+03 -1737.344 -1402.11 -1945.19 ######## -1648.47
Enthalpy Flow CAL/SEC -1868600 -148.5416 -2995400 -896990 -3840700 -929060 -2842000
Molar Entropy CAL/MOL-K ######## -102.3162 -1.02E+02 ######## ######## ######## ########
Mass Entropy CAL/GM-K -1.87496 -1.648442 -1.648442 -1.68566 -1.54685 -1.9341 -1.43335
Molar Density MOL/CC 0.026392 0.017332 0.017332 0.015921 0.020972 0.050943 0.015134
Mass Density GM/CC 0.84565 1.075776 1.075776 0.733481 0.993748 0.918178 0.939359
Avg. Mol. Wt. 32.04216 62.06844 62.0684 46.0706 47.38342 18.02369 62.0684
Tab 1: Streams results

EXTR. COND. EXTR. REBOILER RECVR. COND. RECVR. REBOILER

Units Name Value Name Value Name Value Name
C Temperature 78.3127518 Temperature 140.854456 Temperature 99.92042 Temperature 205.1264
kW Heat duty -882.5926 Heat duty 1409.955862 Heat duty -1300.75 Heat duty 1896.568
kmol/hr Distillate rate 49.989998 Bottoms rate 150.010102 Distillate rate 50.01496 Bottoms rate 99.99514
kmol/hr Reflux rate 31.050985 Boilup rate 111.661037 Reflux rate 65.01945 Boilup rate 68.36547
Reflux ratio 0.62114395 Boilup ratio 0.744356786 Reflux ratio 1.3 Boilup ratio 0.683687

Tab 1: Block results

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Following are the temperature and concentration profiles for the extractive and recovery column:
Block EXTR: Temperature Profile
145

140 Temperature C

135

130

125

120

115
Temperature C

110

105

100

95

90

85

80

75
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44
Stage

plots 1: 1) extr. col. Temp. profile; 2) extr. col. composition profile; 3) revcr. col. Temp. profile; 4) recvr. col. composition profile

14
3.1.3. Analysis of results:
Mole purity of Ethanol: 0.99989 Entrainer recovered:99.99505%
% recovery of Ethanol: 99.97% Entrainer loss: 0.004959 kmol/hr.
Entrainer recycled:99.99505 kmol/hr. Total Reboiler Duty: 3306.53 kW
Extractive column: Recovery column:
Reflux Ratio: 0.6211 Reflux Ratio: 1.3
Reboiler Duty: 1409.96 kW Reboiler Duty: 1896.57 kW
Most sensitive stage: 41 Most sensitive stage: 34
A sharp change in temperatures have been observed on stages where feed is introduced. Ethylene
glycol remained almost completely in liquid phase. Water composition almost died in stages
above 23 due to ethylene glycol. So in effect glycol could have been introduced in stages lower
than 4 to prevent any minor losses. In recovery column temperature remained above 100 ºC and
almost all of water remained in vapor phase. Some of the glycol vaporized as well. So, we could
have reduced the reboiler duty to bring out the same separation.

3.2 Dynamic simulation:

For dynamic simulation the flowsheet has to be pressure driven. A pressure drop of 3atm. has been
generated using compressors and valves. Sizing of equipment is necessary before running the
dynamics. The tray sizing tool in Aspen Plus is used to calculate the column diameters of both
columns to be 0.677m and 0.812m for the first and the second column, respectively. Tray spacing
and weir height of both columns are assumed to be 0.6096 m and 0.0508 m respectively. A 10 min
holdup time with 50% liquid level is used to calculate the volume of each column base and reflux
drum. For extractor reflux drum height was 1.62751m and diameter was 0.81375m, while the
height and diameter of sump was taken to be 3.3087m and 0.667308m. For recovery column height
and diameter of reflux drum was set to 1.35723m and 0.678613 m respectively. Dimensions of its
sump were 3.99895m and 0.908146m in height and diameter. Top pressures of both columns are
set at atmospheric pressure. Pressure drops are automatically calculated. The steady state flow
sheet is now imported to Aspen dynamics.
In Aspen dynamics, PID controllers were installed according to the strategy. In ratioing the
entrainer flow rate proportional controller has been used. Default controller tuning were used
(derivative action is inactive). Controller action was chosen accordingly. Temperature controller
was set at 41st stage of the extractive column while it was set at 34th plate of the recovery column.
The flowsheet with controllers installed is shown on the next page.
A 10% disturbance was introduced in feed flow rate and the feed composition at time t=5 min and
response were recorded.

15
 Fig. 5: Flowsheet of extractive distillation with control structure in Aspen Dynamics

3.2.1 Dynamic run results:

For a 10% disturbance in feed flow rate the response of various variables is shown:

Plots 2: a) distillate rate from extractive column, b) ethanol

purity mole frac. In distillate, c) water mol frac. In distillate
from recovery column, d) temp. of 41st stage in extractive
column, e) temp. of 34th stage in recovery column.

16
For a 10% disturbance in composition rate the response of various variables is shown:

Plots 3: a) distillate rate from extractive column, b) ethanol purity

mole frac. In distillate, c) water mol frac. In distillate from
recovery column, d) temp. of 41st stage in extractive column, e)
temp. of 34th stage in recovery column.

3.2.2. Analysis of results:

When a disturbance of +10% was introduced in feed flow rate, the temperature in the column
dropped so that the reboiler duty increased to regain the same temperature. Similar was the
temperature response of the recovery column. Distillate rate increased as obvious. Purity of top
stream dropped a slightly. Purity of water leaving the second column dropped suddenly but was
restored to a value slightly less than the original one. Reverse of this response was observed, except
for ethanol purity which dropped initially, for -10% disturbance in response. However, the purities
did not change much. In either cases the system settled within 1.5 hrs.
When a disturbance of +10% was introduced in composition, both the temperature controllers
performed well to regain the same temperature. Distillate flow rate from the first column increased
as obvious. Purity of ethanol dropped a little, while that of water increased. Reverse of this was
seen with -10% composition change. In either cases the system settled within 1.1 hrs.

17
In this control strategy we ratioed the reflux rate with fresh feed rate as against original Luyben
scheme, where reflux was manipulated by distillate (fixed RR). This has resulted in a more robust
control structure. Bottoms level of recovery column need not necessarily be controlled (ideally).
Entrainer accumulated in bottoms is circulates in a closed loop, thus bottom level do not vary
whatever be the rate of circulation, except for small leaks. Makeup stream is used to keep the
entrainer level controlled.

18
4. Conclusions

From the simulation results of an extractive distillation column the following conclusions can be
drawn:
1. Residue curve maps are effective in depicting azeotropes, heterogeneous phase location,
separation feasibility, and distillation paths for the extractive distillation tower. Selection
of most suitable entrainer is based on iso-volatility and equi-volatility curves. Among
ethylene glycol and DMSO, glycol is a suitable entrainer.
2. Fresh feed and entrainer must be fed at different stages, with entrainer stage above the feed
stage. This is to maintain sufficient entrainer on each stage for altering VLE.
3. For controlling composition temperature of stage with maximum sensitivity and linearity
should be controlled by manipulating reboiler duty.
4. Control of recovery column sump level need not necessarily be controlled. Minor changes
in level due to entrainer loss can be controlled makeup entrainer.
5. Controlling reflux rate with fresh feed flow rate resulted in more robust control than
response we get by fixing the reflux ratio.

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5. References

[1] Luyben, W. L., Distillation Design and Control Using Aspen Simulation (2006), 2nd ed.
AIChE John Wiley & Sons, Inc.
[2] Luyben, W. L. and Chien, I. Lung, Design and control of distillation systems for separating
azeotropes (2010), 1st ed. AIChE John Wiley & Sons, Inc.
[3] Luyben W. L., Plantwide control of an isopropyl alcohol dehydration process, AIChE J.,
52, 2290–2296 (2006).
[4] Wang, Y., Cui, P., Ma, Y., Zhang, Z., Extractive Distillation and Pressure-swing
Distillation for THF/Ethanol Separation (2014), Journal of Chemical Technology &
Biotechnology 90(8).
[5] Grassi V.G. (1992), Process Design and Control of Extractive Distillation, Springer, New
York, NY.
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