Article

pubs.acs.org/IECR

Design and Control of an Extractive Distillation System for Benzene/

Acetonitrile Separation Using Dimethyl Sulfoxide as an Entrainer
Shengkai Yang,*, Yujie Wang,*, Guangyue Bai,*, and Yong Zhu

School of Chemistry and Chemical Engineering, Henan Institute of Science and Technology, Xinxiang, Henan, 453003, China
School of Chemistry and Chemical Engineering, Key Laboratory of Green Chemical Media and Reactions, Ministry of Education,
Henan Normal University, Xinxiang, Henan, 453003, China

ABSTRACT: A method for benzene/acetonitrile separation using extractive distillation is presented, and dimethyl sulfoxide
(DMSO) is selected as the entrainer. Steady state and dynamic simulations for this process are implemented by commercial
simulators (Aspen Plus and Aspen Dynamics). On the basis of global economic optimization, a design with optimized operation
conditions for this process is developed. Two single temperature control structures with xed reux ratio or xed reux-to-feed
ratio and a dual-end temperature control structure for entrainer recovery column are presented to evaluate the dynamic
performance with feed ow rate and feed composition disturbances, and the last structure is quite eective.
where si,j is the relative volatility of component i and component j in the presence of entrainer s, K
i,s is the innite dilution
K value for a trace of species i in the entrainer, and K
i,s is the
innite dilution K value for a trace of species j in the entrainer.
Of all candidate solvents used for the separation of the
benzene and acetonitrile azeotrope mixture, the following
three entrainers are studied in this paper: dimethyl sulfoxide
(DMSO), phenol (PhOH), and sulfolane (SFO). Their K
values at innite dilution and the relative volatility are listed in
Table 1. Because DMSO does not lead into further azeotrope
in the system and shows a higher relative volatility (2.139),
it is chosen as entrainer in the simulation. This large relative
volatility is helpful to gain an economical separation sequence.
Figure 1BC gives Txy diagrams for benzene/DMSO and
acetonitrile/DMSO mixtures, respectively. The former plays an
important role in the top of the extractive column, and the
latter applies in the solvent-recovery column.
2.2. Thermodynamic Model Used in the Simulation.
According to the refs 2 and 4, the best t was obtained by the
Wilson model for the binary isobaric VLE data composed of
the benzene/acetonitrile and acetonitrile/DMSO system. No
isobaric VLE experimental data were found for the benzene/
DMSO system. The predicted azeotropic temperature and
azeotropic composition for benzene/acetonitrile at 0.43 atm
using the Wilson model are 73.46 C and 68.64 wt %
(53.50 mol %), respectively, which were in very good agreement with experimental data.
In this simulation, the Wilson model was used to describe
the nonideality of the liquid phase while the vapor phase was
assumed to be ideal. The Wilson model parameters of the
three pairs were taken from Aspen Plus, and all other physical
property model parameters were taken from the built-in values
in Aspen Plus.

1. INTRODUCTION
2-Picoline is an important pharmaceutical intermediate and a
raw organic chemical material. Catalyzed by organic cobalt, ethyne
and acetonitrile are used to produce 2-picoline presented by
Qin et al.,1 and the synthesis process achieved wide-plant production scale in 2006. In the synthesis method, organic cobalt
is dissolved in pure benzene solution as catalytic agent, and
simultaneously, benzene is also one of the byproducts. After
2-picoline and some other byproducts are separated from reactant
mixture, there are many benzene/acetonitrile mixtures left, and it
is very necessary to separate them for recycle use.
According to the ref 2, benzene (normal bp 80.09 C) and
acetonitrile (normal bp 81.60 C) at 1 atm form a minimumboiling azeotrope with azeotropic temperature at 73 C and
azeotropic composition at 52.9 mol % benzene. Figure 1A give
the Txy curve for the benzene/acetonitrile system.
In this paper, we attempt to use an extractive distillation
process to separate benzene/acetonitrile. Among some suitable
candidate solvents, dimethyl sulfoxide (DMSO) is elected as
entrainer according to the values of relative volatility. The
thermodynamics model Wilson is used in the simulation calculation. Using DMSO as entrainer, an optimized design for the
extractive distillation process is developed using total annual
costs (TAC) as an objective function from many alternatives.
Finally, appropriate control structures were introduced, and
their dynamic performances were evaluated.
2. STEADY STATE DESIGN
2.1. Entrainer Selection. Since the entrainer is a key factor
in extractive distillation, more attention should be paid to
its election. A criterion for entrainer selection is through the
comparison of relative volatilities in the presence of dierent
entrainers.3 The higher the relative volatility, the easier the
separation. The relative volatility is dened as
is, j =

Received: March 15, 2013

Revised: July 20, 2013
Accepted: August 14, 2013

K i
,s
K
j,s

(1)
XXXX American Chemical Society

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Table 1. Results of the Entrainer Selection for an Extractive

Distillation System
benzene(1)/acetonitrile(2) using the Wilson model
solvent

Tb/K

K
1,s

K
2,s

1,2

DMSO
phenol
sulfolane

464.00
454.99
560.45

27.12
19.50
79.40

12.68
10.88
53.17

2.139
1.792
1.493

2.3. Residue Curve Map (RCM) for the System. The

RCM of ternary system can be used to design and distinguish
between feasible and infeasible sequences and can be mapped
by Aspen Plus. Using the Wilson model, the RCM of the
benzene/acetonitrile/DMSO ternary system is drawn and
shown in Figure 2. It can be seen that the benzene/acetonitrile
azeotrope is the unstable node, DMSO is the stable node, and
both benzene and acetonitrile are the saddles. No distillation
boundary exists to the system, which is an ideal situation for
selection of an extractive distillation process. Material balance
lines on behalf of the extractive distillation process were also
drawn in Figure 2. It is noticed that M, denoting the mixture of
the raw material and entainer, can be separated into D1 and B1
on extractive distillation column, and B1 can be separated into
D2 and B2 on entainer recovery column. This means that the
feed F may be separated into relatively pure two products with
the aid of the entrainer. To balance the tiny loss of entrainer in
both D1 and D2 streams, a small makeup stream of DMSO
should be added (not displayed in Figure 2).
2.4. Process Design and Economic Analysis. 2.4.1. Process Design. In this paper, the raw material used is from several
local plants and mainly composed of benzene and acetonitrile
with a little 2-picoline. After pretreatment, 2-picoline was removed from the raw material completely. The composition was
analyzed by gas chromatography. The extractive distillation
process was simulated with the following data: the feed was a
mixture made up of 65.5 wt % of benzene and 34.5 wt % of

Figure 1. Txy diagram for (A) benzene/acetonitrile or (B) benzene/

DMSO at 0.43 atm and (C) acetonitrile/DMSO at 0.33 atm.

Figure 2. Residue curve map at 0.43 atm for the benzene/acetonitrile/DMSO system.
B

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Figure 3. Eect of RR1 and entrainer ow rate S in extractive column (NT = 47) on (A) benzene and (B) acetonitrile.

Figure 4. Optimal process owsheet for extractive distillation.

Figure 5. Extractive distillation column C1: (A) temperature prole;

(B) composition prole.

Figure 6. Entrainer recovery column C2: (A) temperature prole;

(B) composition prole.
C

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Figure 7. Basic control structure (S1) with xed reux ratio for C1 and C2 columns.

Figure 8. Improved control structure (S2) with xed reux-to-feed ratios for C1 and C2 columns.

acetonitrile, with a ow rate of 3500 kg per hour with 7200

working hours annually. Aspen Plus and Aspen Dynamics
are used to do the steady state and dynamic simulations. The
Wilson activity model is chosen to predict the vapor liquid
equilibrium in the simulator. To ensure the products are
available for recycling, the two product specications are set to
be as follows: the acetonitrile impurity in the benzene product
is not more than 1 wt %, and the acetonitrile product has a
purity of 99.9 wt %. Here, Aspen notation of numbering stages
from the top, with stage 1 being the ux drum and the last stage
being the rebolier, is adopted.
For an extractive distillation column (denoted as C1), when
the total stages, operating pressure, and feed location are xed,
there are three design degrees of freedom: reux ratio (RR1),

Table 2. Temperature Controllers Tuning Parameters for

the Basic Control Structure
parameters

TC1

TC2

TCHX

controlled variable
manipulated variable
transmitter range (K)
controller output range (GJ/h)
ultimate gain
ultimate period (min)
gain, Kc
integral time, (min)

T1,40
QR1
273443
07.71
8.1037
6.0
2.5324
13.2

T2,10
QR2
273556
03.37
2.9728
4.8
0.9290
10.56

Trecycle
QHX
273370
4.040
0.5200
2.4
0.1625
5.28

entrainer ow rate (FE), and reboiler heat duty (QR1). Since

almost all the benzene that is present in the C1 bottom product
D

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Figure 9. Dynamic responses for basic control structure (S1) with xed reux ratio for columns C1 and C2: feed ow rate disturbances. (Solid lines
are denoted as +20% ow rate, and dashed lines are denoted as 20% ow rate.)

reboiler, and condenser, and a payback period of 3 years is

assumed. Small items such as reux drums, pumps, valves, and
pipes are usually not considered due to their much lower costs.
The operating costs include the steam and cooling water, and
only the former was reckoned in this simulation owing to its
much higher cost. The heat transfer area for the condensers and
reboilers is determined using the overall heat transfer coecient
and a dierential temperature driving force. Here, the overall
heat transfer coecients and the calculation formula for the
above equipment are all taken from Luybens book.5
The Tray Sizing function in Aspen Plus is employed to size
the column vessels, and a sieve plate is selected. The Design
Spec/Vary function was used to satisfy the product composition. The weir height of 0.025 m is adopted in order to maintain the pressure drop required, while other parameters use the
default values. The stages are counted from top to bottom with
the condenser as the rst stage and the reboiler as the last stage
for both columns.
The pressure selection is very important; lower pressure
leads to easier separation, but the pressure value is restricted by
the adopted cooling water temperature, simultaneously, due to

will go to the top of the entrainer recovery column (denoted

as C2), to achieve the desired acetonitrile product, the mass
ow rate of benzene in the bottom product of the C1 is held at
1.2 kg/h (calculated from the material balance) by manipulating the reboiler heat duty QR1.
2.4.2. Economical Optimization. It is known that, for
the extractive distillation process, an increase in the entrainer
ow rate will reduce the heat duty of the extractive distillation
column, but the heat duty of the entrainer recovery column will
increase, and a larger column diameter is expected. Thus, a
trade-o between the extractive column costs (include both the
xed capital costs and operating costs) and entrainer recovery
column costs needs to be made. Thus, when the theoretical
plates were xed, there exists an optimal entrainer ow rate
that minimizes TAC (total annual costs, dened in Luybens
book5). When the entrainer ow rate is larger than the optimal
value, the costs of the entrainer recovery column become more
dominant and TAC increase.
It is a convention to use the TAC as the objective function
to be minimized, which includes annualized capital costs and
operating costs. The capital costs include the column shell,
E

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Figure 10. Dynamic responses for basic control structure (S1) with xed reux ratio for columns C1 and C2: feed composition disturbances. (Solid
lines are denoted as +0.05 benzene mass composition, and dashed lines are denoted as 0.05 benzene mass composition.)

In the optimization process, the six design variables, namely,

the total stages of the extractive distillation column (N1), the
fresh feed location (NF1), the entrainer feed location (NFE), the
total stages of the solvent recycle column (N2), the feed
location of solvent recycle column (NF2), and the solvent feed
rate (FE) should be determined by minimizing the total TAC.
The procedure to search the optimal value of each design
variable is summarized below:
(1) Guess the six design variables, N1, NF1, NFE, N2, NF2, and FE.
(2) Run the simulation until a normal result without any
wrong was achieved.
(3) Calculate the total TAC. If the new calculated TAC was
smaller than the minimum obtained from previous
rounds, the new design value was adopted, and
otherwise, the search process should be stopped.
(4) Change the design variable based on the new calculated
TAC value and go back to step 2.
All the six design variables should be optimized according to
the procedure above. After a round search, namely, all the six

the lower material temperature along with its pressure

reduction. As the adopted temperature of the cooling water is
constant at 308.15 K and the temperature dierence is constant
at 13.9 K for the column top condenser and heat exchanger
according to Luybens book,5 the C2 column top temperature is
322.05 K (i.e., the sum of cooling water temperature and
the temperature dierence of heat transfer) and its pressure is
calculated from Antoine extended formulation, namely,
0.33 atm. Also, as the same cooling water and temperature
dierence was adopted, the material ow from C2 bottom is
also cooled to 322.05 K by the heat exchange (denoted as HX),
namely, the recycling entrainer ow temperature input to C1
column. According to the suggestion of Knight and Doherty,6
the temperature dierence of recycling entrainer ow temperature and C1 column top should be 515 K, and the temperature of C1 column top was xed at 327.37 K (here the abovementioned temperature dierence being at 5.32 K). Thus, the
C1 column top pressure is calculated from Antoine extended
formulation to be 0.43 atm.
F

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Figure 11. Dynamic responses for improved control structure (S2) with xed reux-to-feed ratio for columns C1 and C2: feed ow rate disturbances.
(Solid lines are denoted as +20% ow rate, and dashed lines are denoted as 20% ow rate.)

that the reux ratio of 1.138 is indeed the minimum of the two
possible reux ratios.
Figure 4 gives the nal optimal ow sheet for this system,
with detailed steam information, heat duties, equipment sizes,
and operating conditions at the steady state design conditions.
Figures 5 and 6 show the temperatures and composition proles of C1 and C2 columns for the ow sheet, respectively.
There is a rapid rise in the temperature for stage 4 and a rapid
fall for stage 31 in Figure 5A, at which the entrainer and fresh
feed are fed. It is obvious that stage 40 displays a fairly steep
slope for the temperature and benzene composition proles
with the extractive distillation column shown in Figure 5B.
In Figure 6, two steep slopes are found near the 4th and 10th
stages. The prole distinguishing features indicate the proper
temperature control point for the two columns.

design variables optimized once, the next round search should

be done until all the six design variables were not changed at a
certain round. In the search process, step size for the theoretical
plate number and feed position were xed at 1 stage and the
FE feed rate was xed at 100 kg/h. The search method is
intuitive and eective but rather time-consuming in a plantwide
optimization.
According to the optimal results, it is found that the optimal
mass ow rate of the entrainer (FE) is 9000 kg/h, and the
optimal total number of stages is 47 for the extractive distillation column and 12 for the entrainer recovery distillation
column, respectively. The best feed position NFE is at the 4th
stage, NF1 at the 31st stage for the extractive distillation column,
and NF2 at the 7th stage for the entainer recovery column. The
optimal reux ratios for C1 and C2 are 1.138 and 0.467, respectively. The nal minimum value of TAC is 451 150$/y.
Extractive distillation systems have the interesting feature of
two dierent values of reux ratio that yield the same separation. Figure 3A,B manifests a plot of benzene purity or acetonitrile impurity from C1 column top ow versus reux ratio at
xed solvent rate, respectively. From Figure 3A,B, we can conclude

3. CONTROL SYSTEM DESIGN

3.1. Basic and Improved Control Structure. Single
temperature control structure is the rst to be considered due
to its less expensive cost. For the extractive distillation process,
basic control structure, namely, xed reux ratio for C1 and C2
G

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Figure 12. Dynamic responses for improved control structure (S2) with xed reux-to-feed ratio for columns C1 and C2: feed composition
disturbances. (Solid lines are denoted as +0.05 benzene mass composition, and dashed lines are denoted as 0.05 benzene mass composition.)

column (denoted as S1), and its improved control structure,

namely, xed reux-to-feed ratio (denoted as S2), are often
adopted. Before starting the dynamic simulation, the plumbling
system and major equipment sizes must be specied.
The commonly used heuristic for reux drums and column bases
sizing is to provide 5 min of liquid holdup when half full. All the
control valves pressure drops are 3 bar with the valve half open at
the design ow rate. Then, the steady state owsheet is pressurechecked, and the Aspen Plus le is exported to Aspen Dynamics.
The temperature at the 40th stage is adopted as the temperature control point for the extractive column, and the temperature at the 10th stage is used as the temperature control point
for the extrainer recovery column. To the control schemes of S1
and S2, the following control structure is proposed for the
extractive distillation control system.
(1) Feed is ow-controlled (reverse acting).
(2) Reux drum levels in both columns are held by manipulating the ow of distillates (direct acting).
(3) Base level in extractive distillation column is held by
manipulating the ow of the bottoms (direct acting).

(4) Base level in entrainer recovery distillation column is

held by manipulating the makeup DMSO ow rate
(reverse acting).
(5) The total entrainer ow is in proportion to the feed ow.
(6) The pressure in the two columns is controlled by
manipulating the heat removal rate in the condenser of
the two columns (reverse acting).
(7) The reux ratios for C1 and C2 columns are xed for the
basic control structure (S1), and the reux-to-feed ratios
for C1 and C2 columns are xed for the improved control
structure (S2).
(8) Entrainer feed temperature is held by manipulating the
cooler HX heat duty (reverse acting).
(9) The temperature for the 40th stage in the extractive distillation column is controlled by manipulating the reboiler heat
input into the extractive distillation column (reverse acting).
(10) The temperatures in the 10th stage in the entrainer recovery column are controlled by manipulating the
reboiler heat input into the entrainer recovery column
(reverse acting).
H

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Figure 13. Dynamic responses for control structure (S3) with xed reux ratio for columns C1 and dual temperature control for column C2: feed
ow rate disturbances. (Solid lines are denoted as +20% ow rate, and dashed lines are denoted as 20% ow rate.)

A noteworthy feature revealed here is that the base level in

the entrainer recovery distillation column is held by manipulating the makeup DMSO ow rate suggested by Grassi and
Luyben.7,8 Figures 7 and 8 demonstrate the basic and improved
control structures for this extractive distillation system, respectively.
Proportional controllers are used for all liquid levels with
Kc = 2, and conventional PI controllers are used for all other

controllers. The proportional and integral (PI) settings of

the top pressure control loops for both columns are set
at Kc = 20 and I = 12 min. Three dead time elements
are inserted into the corresponding temperature control
loops with a dead-time of 1 min. Using the Tyreus-Luyben
tuning, relay-feedback tests are run on the temperature
controllers to determine ultimate gains and periods, and the
I

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Figure 14. Dynamic responses for control structure (S3) with xed reux ratio for columns C1 and dual temperature control for column C2: feed
composition disturbances. (Solid lines are denoted as +0.05 benzene mass composition, and dashed lines are denoted as 0.05 benzene mass composition.)

purity is held close its desired value, while acetonitrile product

purity is 0.9898 mass fraction at the new steady state in 8 h,
having large deviation to its desired value. It is found that the
two controlled tray temperatures were brought back to their set
points and the reboiler duties of two columns reached new
steady state values in 5 h. Figure 10 shows the dynamic
responses of the basic control structure for positive and

parameters are shown in Table 2 for S 1 or S 2 control

schemes.
Now, the dynamic performance of the control structure is
evaluated by feed ow rate and composition disturbances.
Figure 9 shows the dynamic responses of the basic control
structure to positive and negative 20% step changes in feed ow
rate at t = 0.2 h. As you can see from Figure 9, benzene product
J

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two products with the same disturbance variations than the

improved control structure in 5h. Economic accounting decides
the select of improved or dual temperature control scheme.

negative 0.05 benzene composition disturbances in the feed at

t = 0.2 h. From Figure 10, acetonitrile product purity is 0.9566,
having large deviation to its desired value. Other control
variables remaining, i.e., benzene product purity, the two
controlled tray temperatures, and two columns reboiler duties,
have almost similar responses as those in the feed ow rate
disturbance.
The dynamic responses of improved control structure were
shown in Figure 11 to the feed ow rate positive and negative
20% disturbance and in Figure 12 to the benzene composition
positive and negative 0.05 disturbances in the feed at t = 0.2 h.
The acetonitrile product purities are 0.9879 and 0.9902 to the
same feed ow rate and benzene composition disturbance in
the feed, respectively, and the benzene product purity has great
improvement simultaneously (from 0.9882 to 0.9927 mass
fraction) to the negative 0.05 benzene composition disturbance
in the feed than that in the basic control structure.
3.2. Dual Temperature Control Structure. To the single
temperature control structure, the scheme of S2 has a better test
result to rate and component disturbance than S1, but to the
disturbances of positive 20% feed ow rate and positive 0.05
feed benzene composition, deviations of the acetonitrile
product purity from C2 top at the new steady state are still
too large in strict product requirements. To improve the
control performance, a dual temperature control structure
(denoted as S3) was presented, in which xed reux ratio was
adopted for C1 column, and stage 4 and stage 10 were
controlled by reux rate and by reboiler duty in the C2 column,
respectively, along with the same other control strategy
mentioned above in single temperature control schemes. The
test results were shown in Figures 13 and 14, from which the
acetonitrile product purities have great improvement under the
same uctuation. The acetonitrile product purities are 0.9963 to
the feed ow disturbance and 0.9987 to the feed benzene
composition disturbance, respectively. In actual production,
which one to be adopted for S2 or S3, depends on the purity of
the product requirements, or the trade-o between the added
value from improved purity of the two products and the
increased costs if S3 was adopted.

AUTHOR INFORMATION

Corresponding Authors

*Tel: +86 13462354555. E-mail: skyang111@163.com.

*Tel: +86 15903023407. E-mail: yujiewang2001@yahoo.com.
*Tel: +86 13938729275. E-mail: baiguangyue@htu.cn.
Notes

The authors declare no competing nancial interest.

NOMENCLATURE
i,j = separation factor of component i and j
C1 = extractive distillation column
C2 = entrainer recovery column
IDn = internal diameter for column n (m)
Ki = K factor of component i
NFE = feeding location for the entrainer
NF = feeding location for the fresh feed
NF2 = feeding location for the feed to column C2
NTn = number of theoretical plates for column n
QCn = condenser heat removal for column n (KW)
QHX = heat duty of the heat exchanger HX
QRn = reboiler heat input for column n (KW)
Rn = reux ratio for column n
T = absolute temperature (K)
TAC = total annual costs
Tn,m = temperature for tray m in column n (K)
REFERENCES

(1) Qin, B. W.; Gao, J. J. Chinese Patent, CN 1869023A, 2006.

(2) Shri, K.; Raghunath, P. T.; Bachan, S. R. Isobaric Vapor-Liquid
Equilibria of Binary Systems of Acetonitrile with Benzene, Toluene,
and Methylcyclohexane. J. Chem. Eng. Data 1980, 25, 1113.
(3) Dyk, B. V.; Nieuwoudt, I. Design of Solvents for Extractive
Distillation. Ind. Eng. Chem. Res. 2000, 39, 14231429.
(4) Wang, Q. Y.; Zeng, H.; Song, H.; Liu, Q. S.; Yao, S. Vapor-Liquid
Equilibria for the Ternary System Acetonitrile + 1-Propanol +
Dimethyl Sulfoxide and the Corresponding Binary Systems at 101.3
kPa. J. Chem. Eng. Data 2010, 55, 52715275.
(5) Luyben, W. L. Distillation Design and Control Using Aspen
Simulation; John Wiley &Sons, Inc: New York, 2006.
(6) Knight, J. R.; Doherty, M. F. Optimal Design and Synthesis of
Homogeneous Azeotropic Distillation Sequences. Ind. Eng. Chem. Res.
1989, 28, 564572.
(7) Grassi, V. G. Practical Distillation Control; Van Nostand Reinhold
Press: New York, 1992.
(8) Luyben, W. L. Plantwide Control of an Isopropyl Alcohol
Dehydration Process. AIChE J. 2006, 52, 22902296.

4. CONCLUSIONS
Design and control of an extractive distillation process for
separation of benzene/acetonitrile are investigated in our work.
DMSO is chosen as a suitable entrainer by comparing the relative volatility. The Wilson model is used to calculate the
thermodynamics properties. Using the total annual cost as the
objective function, the optimal design of the extractive
distillation process is presented. According to the simulation
results, it is found that the optimal mass ow rate of the
entrainer (S) is 9000 kg/h, and the optimal total number of
stages is 47 for the extractive distillation column and 12 for
the entrainer recovery distillation column, respectively. The
optimal solvent and raw feed position for extractive distillation
column are the 4th stage plate and the 31st stage plate,
respectively, and the optimal feed position is the 7th stage plate
for entrainer recovery column.
Two single temperature control structures, i.e., basic and
improved control scheme, and a dual temperature control
scheme were presented and tested to the feed ow rate and
composition disturbance. The improved control scheme with
xed reux-to-feed ratio has slightly better tested results than
the basic control scheme with xed reux ratio, while the dual
temperature control structure can maintain higher purity of the
K

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