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Content

1.0 Introduction ... 4

2.0 Process description . 5

3.0 Material balance ..... 6

4.0 Control strategy . 8

5.0 Money balance . 9

6.0 Conclusion . 10

7.0 Reference . 11

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Abstract: - Solvent recovery is becoming a major issue in specialy chemical industries. Solvent
recovery by conventional batch distillation is limited by the frequent presence of azeotropes in the
used solvent mixtures. Most distillation processes for the separation of azeotropic or difficult
zeotropic mixtures involve the addition of an entrainer (homogeneous and heterogeneous
azeotropic distillation or extractive distillation).

In this study, an isopropyl alcohol (IPA) dehydration process via extractive distillation have been
investigated. The heavy-boiling entrainer used to aid the separation is dimethyl sulfoxide (DMSO).
The design flowsheet includes an extractive distillation column and an entrainer recovery column
with the top product of the extractive distillation column to be IPA (99.97-99.99% pure) and the
top product of the entrainer recovery column to be water. The bottom product of the entrainer
recovery column is the recovered DMSO which is recycled back to the extractive distillation
column. The optimal design flowsheet of this complete process has been established showing that
the total annual cost and the needed steam cost of this design flowsheet is significantly less than a
competing design flowsheet via heterogeneous azeotropic distillation.

This process is continues process and the cost of this process is 30% less than the cyclohexane
Entrainer process. Also this process contains only two distillation column one is extractive
distillation and another entrainer recovery meanwhile in cyclohexane process three distillation
column needed only for extractive column and additionally entrainer recovery is too much costly
but in this process entrainer recovery is easy

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1.0 Introduction

The solvent stream contains mainly isopropyl alcohol and water which contains a minimum-
boiling azeotrope and, thus, is difficult to separate. The usual practice in industry for the separation
of a mixture with these two components is to add cyclohexane (CyH) as an entrainer via
heterogeneous azeotropic distillation. However, it is well known that heterogeneous azeotropic
distillation can exhibit high parametric sensitivity, multiple steady-states, long transients, and
nonlinear dynamics, which can limit the operating range of this IPA dehydration system under
feed disturbances. An alternative way for the separation of this mixture is to use extractive
distillation by adding a heavy-boiling entrainer into this system. The entrainer acts to increase the
relative volatility of the IPA and water mixture far away from unity without inducing liquid-liquid
phase separation and also does not form additional azeotropes with any of the other components.

Entrainer screening is an important step in extractive distillation before designing a distillation

sequence. Several rules should be followed to get a good entrainer candidate for azeotropic
mixtures. The presence of the entrainer is the key difference between extractive distillation and
simple distillation; however, it presents more degrees of freedom in the overall system to be
designed. The proper amount of the entrainer feed should be designed for economical purposes
which complicates the design and optimization of extractive distillation. Quite a few papers in the
open literature have studied the feasibility of the design and synthesis of this type of processes. A
residue curve map (RCM) can be used as a simple method for designing and distinguishing
between feasible and infeasible sequences in extractive distillation. Thermal integration in
extractive distillation has also been studied in the literature

In extractive distillation, infinite reflux does not always imply maximum separation. Separations
which are infeasible at infinite reflux may be feasible at finite reflux. This is an important property
of extractive distillation and plays an important role in the entrainer selection procedure.
Bifurcation/multiple steady states are well-known in extractive distillation. It has great effect upon
the flexibility, operability, and controllability of the column. Steady state design also effects the
complexity of the dynamic and control problem of an extractive column. Several authors have
studied the dynamic and control of extractive distillation. In a recent paper by Luyben, the plant
wide control strategy of an isopropyl alcohol process using ethylene glycol as the entrainer has
been studied.

In this report, instead of using ethylene glycol as the entrainer, dimethyl sulfoxide (DMSO) will
be used for isopropyl alcohol dehydration. Studied five entrainers for the IPA-water system and

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found dimethyl sulfoxide (DMSO) to be the best candidate which has the largest separation factor
and introduces no further azeotrope in the system.

2.0 Process description

The proposed flow sheet for the IPA-water separation with DMSO as the entrainer can be seen in
Figure. The IPA-water mixture and the entrainer are fed into the extractive distillation column with
the stages above the entrainer feed as the rectifying section, the stages between the feed stages of
the entrainer and the IPA water mixture as the extractive section, and the stages below the feed
stage of the IPA-water mixture as the stripping section. The presence of DMSO alters the relative
volatility between IPA and water causing IPA to move toward the top part and water to move
toward the bottom part of the column. In the rectifying section, there is essentially no water, thus
the simple separation between IPA and DMSO is performed with pure IPA going to the distillate
and DMSO returning to the extractive section for entrainer usage. In the stripping section, IPA as
the lightest component is stripping toward the extractive section of the column resulting in only
negligible IPA in the column bottoms stream. This column bottoms stream is fed into the entrainer
recovery column to produce almost pure water in the distillate and almost pure DMSO in the
column bottoms. DMSO as a heavy entrainer will be recycled back to the extractive distillation
column. To balance tiny entrainer losses in both D1 and D2 streams, small makeup stream of
entrainer should be added.

The product specifications are set to be exactly the same they are the following: 99.9999 mol %
of IPA in D1 and 99.9 mol % of water in D2. The reason for the ultrahigh purity in IPA is for
semiconductor industry usage. The feed composition as in a typical waste IPA stream in the
semiconductor industry contains equal moles of IPA and water. With this feed composition not far
from the azeotropic composition, the flowsheet arrangement with a preconcentrator column was
not considered for the sake of having a simpler process as well as simpler instrumental and control
equipment. The feed flow rate is assumed to be 100 kmol/h (1666.67 mol/min), For easy operation
purposes, reflux drums of both columns are operated at atmospheric pressure with the column
pressure drop automatically calculated in the Aspen simulation.

The design variables to be determined in the flowsheet include the following: the feed ratio
(FE/FF), total stages of the extractive distillation column (N1), entrainer and fresh feed tray
locations (NFE and NFF), total stages of the entrainer recovery Column (N2), and feed tray
location of the entrainer recovery column (NF2). entrainer feed temperature can also be considered
as another design variable, thus a cooler is included in Figure.

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 Fig. owsheet of IPA dehydration process via extractive distillation
column.

3.0control strategy
The steady-state economics of the overall process via extractive distillation is much better than
the overall process via heterogeneous azeotropic distillation. In the following, we will investigate
the control strategy of this complete process in Figure. We would like to restrict ourselves to use
tray temperature control loop(s) to indirectly hold the product purity for wider industrial
application purpose. Large feed disturbances ((20% changes in the feed composition and also
(20% changes in the fresh feed flow) will be used to test the proposed overall control strategy.

Pressure-driven simulation in Aspen Dynamics is used in the control strategy development.

Before converting the Aspen Plus result to Aspen Dynamics, sizing of all equipment is needed.
The tray sizing tool in Aspen Plus is used to calculate the column diameters of both columns to
be 0.78 and 0.82 m for the first and the second column, respectively. Tray spacing and weir
height of both columns are assumed to be 0.6096 and 0.0508 m, respectively. A 10-min holdup

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time with a 50% liquid level is used to calculate volume of each column base and reflux drum of
each column. The top pressures of the first and the second column are set at atmospheric
pressure. The tray rating tool in Aspen Plus is used to automatically calculate the pressure drop
along both columns.

Some simple regulatory control loops are determined first: the levels of the reflux drums for
both columns are controlled by manipulating the distillate; top pressures of both columns are
controlled by the condenser duty; the bottom level of the extractive distillation column is
controlled by manipulating the bottom flow; and the entrainer feed temperature is controlled at
72 C by manipulating the cooler duty. For the two reflux flows, an immediate thinking is to
keep the two reflux ratios at their nominal values during disturbances. This was also used in the
overall control structure.

An important inventory control loop in this overall process is the bottom level of the entrainer
recovery column. The control of the entrainer makeup flow. However, because this flow is very
small, the bottom level essentially floats as changes in the

Fig. Overall control strategy with reux ratio

xed.

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4.0Material balance
In material balance assume that the composition of IPA-Water is 50% because in industry we can
not get every time 75% solution And the feed rate is assumed 100Kmol/hour(1666.66mol/min)
and the other parameter is fixed by aspen plus simulation The optimal material balance is shown
in fig.

Fig. optimal material balance of extractive distillation column

5.0 Money balance

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The total cost is calculated by per annual total annual cost(TAC).TAC is given below for this
process at optimal production of IPA

Second column Cost in $

First column Cost in $

Reboiler cost 44470

FE/FF feed ratio 1.025

Condenser cost 25070

Reboiler cost 55670

Column cost 101770

Condenser cost 32510

Tray cost 8790

Column cost 153530

Steam cost 164730

Tray cost 14520

Cooling water 2740

Steam cost 158260
cost in condenser
Cooling water cost 2870 Entrainer cost 290

Cooler cost 33670

Cooling water 2010

cost in cooler

Total cost Cost in $

TCA 8009000

If consider the optimal production then the cost of production 1 liter of pure IPA is
1.57 Rs (< 2Rs) this method cheapest method for dehydration of IPA

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6.0 Conclusion

Design and control of an IPA dehydration process using extractive distillation is thoroughly
investigated. Using TAC as the objection function, the optimal design owsheet of the process of
a two-column system is developed. This optimal design owsheet can be compared directly
heterogeneous azeotropic distillation. The extractive distillation process is much more
economical than the heterogeneous azeotropic distillation process. The TAC is reduced by as
much as 32.7%, and the steam cost is cut by 30.3%. The two drawbacks for the extractive
distillation process are a taller extractive distillation column and the higher base temperatures,
which require higher pressure steam in the two reboilers.

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7.0 Reference

1. Arin S. and I. L. Chien, Design and control of an isopropyl alcohol dehydration process
via extractive distillation using dimethyl sulfoxide as an entrainer, Ind. Engng Chem.
Res., 47, 790803 (2008).
2. Laroche L., N. Bekiaris, H. W. Andersen, and M. Morari, Homogeneous azeotropic
distillation. Comparing entrainers, Can. J. Chem. Eng., 69, 13021319 (1991).
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llmann,Synthesisofdistillationprocessusingthermodynamicmodelsand the Dortmund
Data Bank, Ind. Engng Chem. Res., 37, 31123123 (1998).
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azeotropic distillation column system, Ind. Engng. Chem. Res., 43, 21602174 (2004).
5. Arin S. and I. L. Chien, Combined preconcentrator/recovery column design for
isopropyl alcohol dehydration process, Ind. Engng Chem. Res., 46, 25352543 (2007).
6. Knight J. R. and M. F. Doherty, Optimal design and synthesis of homogeneous
azeotropic distillation sequences, Ind. Engng Chem. Res., 28, 564572 (1989).
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Hill, New York, NY, 2001.
8. Douglas J. M., Conceptual Design of Chemical Processes, McGraw-Hill, New York, NY,
1988.324 ISOPROPANOLWATER (DIMETHYL SULFOXIDE AS THE
ENTRAINER)
9. Luyben W. L., Plantwide control of an isopropyl alcohol dehydration process, AIChE J.,
52, 22902296 (2006).
10. GrassiV.G.,Processdesignandcontrolofextractivedistillation.InPracticalDistillationControl
, Van Nostrand Reinhold Press, New York, 1992, pp. 370404.
11. Luyben W. L., Plantwide Dynamic Simulators in Chemical Processing and Control,
Marcel Dekker, New York, 2002. 12. Chien I. L. and P. S. Fruehauf, Consider IMC
tuning to improve controller performance, Chem. Eng. Prog., 86, 3341 (Oct., 1990).

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