International Journal of Advanced Technology and Engineering Exploration, Vol 3(24)

ISSN (Print): 2394-5443 ISSN (Online): 2394-7454

Research Article
http://dx.doi.org/10.19101/IJATEE.2016.324004

A case study on separation of IPA-water mixture by extractive distillation

using aspen plus
Sarita Kalla, Sushant Upadhyaya*, Kailash Singh, Rajeev Kumar Dohare and Madhu Agarwal
Department of Chemical Engineering, Malaviya National Institute of Technology, Jaipur, India

©2016 ACCENTS

Abstract
Extractive distillation is one of the popular methods being leveraged to separate isopropyl alcohol (IPA) from water
present in waste stream in semi-conductor industries. In this context, the paper aims to carry out simulation study for
separation of isopropyl alcohol-water azeotrope mixture using ethylene glycol as entrainer. In particular, temperature,
pressure and concentration profile has been studied. Aspen plus® (version 8.8) has been used as simulation tool and
optimum number of stages for the simulation turns out to be 42. The results show that top of the column contains IPA of
99.974 mol % purity and bottom product contains water-ethylene glycol mixture. Moreover, sensitivity analysis for
different parameters and analysis of residue curve for ternary system have been also performed.

Keywords
IPA-water, Extractive distillation, Simulation, Entrainer.

1. Introduction 2. Process simulation

Isopropyl alcohol is generally used as the cleaning
agent and solvent in chemical industries. Because of
its cleaning property it is also known as rubbing
alcohol. IPA is soluble in water and it forms
azeotrope with water at temperature 80.3-80.4 0C.
IPA and water forms a homogeneous minimum
boiling azeotrope, at 68.1-67.5 mole% (87.4-87.7
mass %) under atmospheric conditions [1]. This close
boiling point azeotrope does not separate by
conventional distillation but may be competently
separated by extractive distillation.
Extractive distillation is an important separation
method for azeotrope mixture. In extractive
distillation, an entrainer (separating agent) is used to
revamp the relative volatility of component to be
separated [2].
In IPA-Water mixture, ethylene glycol used as
entrainer is combines with water and separated as
bottom product and pure IPA is collected from the
top of the column. Due to high boiling point of the
solvent the ethylene glycol-water mixture may be
easily separated in second distillation column. The
separated ethylene glycol can be reuse as entrainer in
first distillation column.
*Author for correspondence
187
2.1 Thermodynamic model
Thermodynamic model is used to describe phase
equilibria properties of the system. For the design of
chemical separation operations the phase equilibrium
properties like temperature, pressure and
compositions are required. In phase equilibria
calculations the activity coefficients are used to
calculate the component non-ideal liquid behaviour
[3]. In this simulation study Non-Random Two
Liquid (NRTL) model is used [4]. In this context,
Figure 1 shows the xy plot and Txy plot for
Isopropyl Alcohol-Water mixture.
2.2 Residue curve analysis
Residue Curve Analysis is useful in studying the
ternary system. Residue cure enumerate the change
of column composition with time in the column.
Figure 2 shows the residue curve for IPA-Water-
Ethylene glycol, ternary system [5].
2.3 Configuration
The simulation of IPA-Water mixture is carried out
using RADFRAC distillation model from the Aspen
Plus simulator. Simulation operating conditions are
specified in Table 1. Figure 3 shows the flow sheet
for simulation of extractive column. Input Stream F1
and FE1 shows the feed stream of IPA-Water mixture
and entrainer, respectively and output stream D1 and
B1 shows the pure IPA and ethylene glycol-water
mixture, respectively [6] [7].
Sarita Kalla et al.

(a)
T-xy diagram for ISOPR-01/WATER
101
100 x 1.0 atm
99 y 1.0 atm

98
97
96

95
94
93
92
Temperature, C

91

90
89
88
87
86

85

84
83
82
81
80
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, ISOPR-01

(b)
Figure 1: (a) Vapour-liquid equilibrium plot for isopropyl alcohol-water (b) txy plot for isopropyl alcohol-water

Residue curve for ISOPR- 01/WATER/ETHYL-01

0.05 Curve 1.0 (PRES = 1.01325 bar)

0.90 Curve 2.0 (PRES = 1.01325 bar)

1

Curve 3.0 (PRES = 1.01325 bar)

0.15
-0

Curve 4.0 (PRES = 1.01325 bar)

Mo
YL

0.80 Curve 5.0 (PRES = 1.01325 bar)

H

l ef

0.25 Curve 6.0 (PRES = 1.01325 bar)

ET

rac

0.70 Curve 7.0 (PRES = 1.01325 bar)

rac

Curve 8.0 (PRES = 1.01325 bar)

0.35
W
l ef

AT

0.60
Mo

ER

0.45
0.50
0.55
0.40
0.65
0.30
0.75
0.20
0.85
0.10
0.95

0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90

Molefrac ISOPR-01

Figure 2 Residue curve for ternary system

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 International Journal of Advanced Technology and Engineering Exploration, Vol 3(24)

Figure 3 Flow sheet for extractive distillation

Table 1 Simulation operating conditions 3.1 Temperature profile

Operating variable Extractive column From steady state temperature profile shown in
Feed Flow Rate (kmol/hr) 100 Figure 4, there is no significantly change in the
Entrainer flow Rate 100 temperature of the column from moving down the
(kmol/hr) condenser segment until it goes up to reaction
Feed Temperature (0C) 25 temperature i.e. 385 0C. From there sharply decrease
Feed Pressure (atm) 1.3
Entrainer Temperature (0C) 72
in temperature up to 370 0C and finally increase in
Entrainer Pressure (atm) 1.1 the temperature in the direction of the reboiler
Distillate Rate(kmol/hr) 50 section.
Molar Reflux Ratio 1
Number of theoretical 42 3.2 Composition profile
Stages Liquid mole fraction and Vapour mole fraction
composition profile of IPA, Water and ethylene
The binary mixture of IPA-Water has the following glycol is shown in the Figure 5 and Figure 6.
mole fraction composition- IPA-0.5 (mole/mole),
Water- 0.5 (mole/mole). Pure ethylene glycol adds as 3.3 Pressure profile
entrainer or separating agent. From Pressure profile shown in the Figure 7, the
pressure is increase with the number of stages in the
3. Results distillation column.

Block C1: Temperature Profile

415
410 Temperature K

405
400
395
Temperatu re K

390
385
380
375
370
365
360
355
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
Stage

Figure 4 Temperature profile for steady state simulation (Stage wise)

189
Sarita Kalla et al.

Block C1: Composition Profiles

1.0
Liquid mole fraction IPA
0.9
Liquid mole fraction WATER
0.8 Liquid mole fraction ETHYL-01
0.7
Mo le f ractio n

0.6

0.5

0.4

0.3

0.2

0.1

0.0
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
Stage
Figure 5 Liquid fraction composition profile for steady state simulation (Stage wise)

Block C1: Composition Profiles

1.0
Vapor mole fraction IPA
0.9
Vapor mole fraction WATER
0.8 Vapor mole fraction ETHYL-01
0.7
Mo le f ractio n

0.6

0.5

0.4

0.3

0.2

0.1

0.0
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
Stage
Figure 6 Vapour fraction composition profile for steady state simulation (Stage wise)
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 International Journal of Advanced Technology and Engineering Exploration, Vol 3(24)

Block C1: Pressure Profile

130000
Pressure N/sqm
125000

120000
P ress ure N/s qm

115000

110000

105000

100000
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
Stage

Figure 7 Pressure profile for steady state simulation (Stage wise)

4. Sensitivity analysis 4.1 Effect of molar reflux ratio on distillate (IPA

Sensitivity analysis is a method of determining mole fraction)
strength of relation between a given input and output As shown in Figure 8, the distillate mole fraction is
[8]. In aspen plus process simulator, inputs are increases with reflux ratio and it becomes maximum
allowed to vary and their effects on a set of results at reflux ratio value of 1. After this the distillate mole
can be calculated. Sensitivity analysis has a handful fraction becomes constant.
of benefits, like, studying the effect on process
outputs in changing input variables, graphically 4.2 Effect of feed flow rate (IPA-Water) on
shows the effects of input variables, validate that a distillate
solution to a design specification is possible or not As shown in Figure 9, as the feed flow rate increases,
etc. [9] [10]. the distillate mole fraction increases and it becomes
constant at 0.028 kmol/sec.

Sensitivity Results Curve

1.000
0.995 D1
0.990
0.985
0.980
0.975
0.970
0.965
D1

0.960
0.955
0.950
0.945
0.940
0.935
0.930
0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 1.80 1.85 1.90 1.95 2.00
VARY 1 C1 COL-SPEC MOLE-RR

Figure 8 Result of effect of reflux ratio on IPA mole fraction by sensitivity analysis
191
Sarita Kalla et al.

Sensitivity Results Curve

1.00
D1
0.95

0.90

0.85

0.80

0.75
D1

0.70

0.65

0.60

0.55

0.50
0.012 0.014 0.016 0.018 0.020 0.022 0.024 0.026 0.028 0.030 0.032 0.034 0.036 0.038 0.040 0.042
VARY 1 F1 MIXED TOTAL MOLEFLOW KMOL/SEC

Figure 9 Result of effect of feed flow rate on IPA mole fraction by sensitivity analysis

Sensitivity Results Curve

0.994725
D1
0.994700

0.994675

0.994650
D1

0.994625

0.994600

0.994575
298 300 302 304 306 308 310 312 314 316 318 320 322 324
VARY 1 F1 MIXED TEMPERATURE K

Figure 10 Result of effect of feed temperature on IPA mole fraction by sensitivity analysis

4.3 Effect of feed temperature on distillate Acknowledgment

As shown in Figure 10, as the feed temperature None.
increases, the distillate mole fraction is decreases due
to exothermic nature of the reaction. Conflicts of interest
The authors have no conflicts of interest to declare.
5. Conclusion
This work laid the foundation of operating conditions References
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the simulation results exhibits 99.974 mol % purity of 979-86.
IPA at the top of the column. The results of the [2] Lei Z, Chen B, Ding Z. Special distillation processes.
sensitivity analysis, therefore, reveal the effect of Elsevier; 2005.
molar reflux ratio, feed temperature and feed flow [3] Gebreyohannes S, Neely BJ, Gasem KA. One-
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this way could be used as solvent in different activity coefficient model. Fluid Phase Equilibria.
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[5] Luyben WL. Distillation design and control using
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Sarita Kalla obtained her B.E. from to
University of Rajasthan, Jaipur and
M.Tech. from Aligarh Muslim
University, Aligarh. She is presently
pursuing Ph.D from Chemical
Engineering Department, MNIT on Air
Gap Membrane Distillation.
Email:sarita87mishra@gmail.com
Dr. Sushant Upadhyaya obtained his
Ph.D. (Chemical Engineering) from
MNIT, M.Tech. and B.Tech. in
Chemical Engineering from UPTU,
Lucknow. He is presently Assistant
Professor in Department of Chemical
Engineering at MNIT. His research
areas are Transport Phenomena,
Modelling and Simulation, Wastewater Treatment,
Computational method for linear/non-linear problems,
Polymer Process Modelling, Mass Transfer, Membrane
Separation Piping Engineering, Numerical Modelling,
Computational Fluid Dynamics (CFD). He has published
several papers of International and National repute in his
research field.
193
Dr. Kailash Singh received his Ph.D.
from Curtin University of Technology,
Australia, M.Tech. from IIT Kanpur
B.E. from University of Roorkee. He is
currently Associate Professor and Head
in the Department of Chemical
Engineering, MNIT. His research areas
are Modelling and Simulation,
Advanced Process Control. He has published numerous
papers of International and National repute in his research
field.
Dr. Madhu Agarwal obtained her Ph.D.
from MNIT, Jaipur, M.Tech and B.Tech
from Calcutta University. She is currently
Assistant Professor at Department of
Chemical Engineering, MNIT. Her
research areas are Modelling and
Simulation, Bioprocess Engineering,
Biofuels, Biotechnology, Fluid Particle Mechanics,
Adsorption, Wastewater Treatment. She is actively working
in the area of bio fuels and water treatment. Published more
than twenty papers in Journals and forty papers in
conferences. She is working on two sponsored research
projects on Fluoride removal and fluoride detection.
Guiding B.Tech. & M.Tech. Students for their final year
projects and Dissertation work and her four Ph.D. Students
are working on alternative energy and water treatment.
Rajeev Kumar Dohare received his
Ph.D from MNIT, Jaipur, B.E from NIT,
Surat in 2002 and M.Tech from Aligarh
Muslim University, Aligarh, India in 2006
with first class. Now he is working as
Assistant Professor in the Department of
Chemical Engineering at Malaviya
National Institute of Technology Jaipur.
His Research areas are process modelling, simulation and
control, solid waste management, fluid mechanics, and
processes optimization. He has published several papers of
International and National repute in his research field.