PROCESS SYSTEMS ENGINEERING

Chinese Journal of Chemical Engineering, 19(1) 8996 (2011)

Dynamic Simulation and Analysis of Industrial Purified Terephthalic

Acid Solvent Dehydration Process*
LI Chengfei ()**
Wuyi University, Jiangmen 529020, China
Abstract Dynamic model for dehydration process of industrial purified terephthalic acid solvent is investigated to
understand and characterize the process. A temperature differential expression is presented, which ensures the equation to convergence and short computation time. The model is used to study the dynamic behavior of an azeotropic
distillation column separating acetic acid and water using n-butyl acetate as the entrainer. Responses of the column
to feed flow and aqueous reflux flow are simulated. The movement of temperature front is also simulated. The
comparison between simulation and industrial values shows that the model and algorithm are effective. On the basis
of simulation and analysis, control strategy, online optimization and so on can be implemented effectively in dehydration process of purified terephthalic acid solvent.
Keywords dynamic simulation, purified terephthalic acid, solvent dehydration, azeotropy

INTRODUCTION

Purified terephthalic acid (PTA) is an important

raw material for polyester production widely used in
textile and packaging industries. It is produced by
catalytic oxidization of PX (paraxylene) fo1lowed by
subsequent purification of the crude terephthalic acid
by selective hydrogenation
Acetic acid is the solvent in the PTA production
process and its concentration is an important quality
criterion. The content of acetic acid at the bottom of
solvent dehydration column directly influences the
product quality of upstream oxidation unit. Less acetic
acid lost at the top of solvent dehydration column results in more energy consumption. Thus it is necessary
to investigate the separation of acetic acid and water
in the recovery unit for saving energy and ensuring the
purity of PTA in the oxidation unit.
PTA production process is a typical heterogeneous azeotropic distillation system. The simulation for
steady state PTA production process has been carried
out [1, 2]. However, heterogeneous azeotropic distillation is very unstable and it is difficult to be controlled
[3-8]. Because the azeotropic distillation shows extremely complex dynamic behavior and is sensitive to
slight disturbances, it is difficult to operate it and to
design its controller, and a dynamic simulation is
needed to understand the nonlinear characteristics of
the system. Acetic acid dehydration is an important
operation in the azeotropic distillation, so its dynamic
simulation and analysis is important to control and
optimization of industrial PTA process. Design for
acetic acid dehydration system using an entrainer,
which is used to reduce the organic reflux and heat
duty in the dehydrating column, were reported in several publications [9]. Pham and Doherty took ethyl
acetate as entrainer [10], and Tanaka and Yamada used

n-butyl acetate [11]. Siirola used acetic ethyl acetate as

entrainer to design a complete acetic acid dehydration
process with multiple effect azeotropic distillation [12].
Wasylkiewicz et al. used geometric method for optimum process design of an acetic acid dehydration
column with n-butyl acetate as entrainer [13]. Luyben
and Tyreus used vinyl acetate monomer as an example
for simulation, design, and control studies [14]. Kurooka et al. proposed a nonlinear control system for
the acetic acid dehydration column with n-butyl acetate as entrainer [15, 16]. Gaubert et al. studied the industrial dehydration operation of an unnamed organic
acid using an immiscible entrainer [17], in which multiple steady states were confirmed for the heterogeneous column by simulation and experimental data.
Chien et al. designed an acetic acid dehydration system via heterogeneous azeotropic distillation [18], with
iso-butyl acetate as the entrainer. The optimum process design and operating condition were determined
for high acetic acid concentration at the bottom and
small loss of acetic acid through the top aqueous flow.
Chien and Kuo added a pre-concentrator column in
the upstream of the heterogeneous azeotropic distillation column [19] and investigated the necessity of the
pre-concentrator column from aspect of design and
control. For a typical waste isopropyl alcohol stream
with equal moles of isopropyl alcohol and water, the
design and control of the overall isopropyl alcohol
dehydration process were investigated [20] and a novel
side-stream operating strategy was proposed to maintain the impurity concentration inside the column for
an energy-efficient operation [21]. The optimum process design and operating condition were determined
by intelligence method [22].
The flowsheet of this study is similar to the column system in literature, with components of acetic
acid and water. The dynamic simulation and analysis

Received 2009-12-11, accepted 2010-07-12.

* Supported by the National Natural Science Foundation of China (61072127) and the Outstanding Young Innovative Personnel
Project of Guangdong Colleges (LYM08098).
** To whom correspondence should be addressed. E-mail: chengfeili@sina.com.cn

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Figure 1

Industrial purified terephthalic acid solvent dehydration system

on industrial PTA solvent dehydration with n-butyl

acetate as entrainer are investigated in this work to
understand and characterize the process, which have
been little discussed in literature.

TT511 with interface level controller of the phase

separating zone. Purified acetic acid as bottom product
of TT501 flows into the bottom acetic acid drum with
level control.

2 INDUSTRIAL PURIFIED TEREPHTHALIC

ACID SOLVENT DEHYDRATION SYSTEM

3
FORMATION OF AN IMPROVED DYNAMIC MODEL

Figure 1 shows the industrial purified terephthalic

acid solvent dehydration system. The solvent recovery
section recovers and purifies the acetic acid solvent
with an azeotropic distillation system, before it is recycled to other section. The condensate from the reflux drum containing water and small amount of organics formed in the reaction step and that from oxidation unit are collected in drum acetic acid. This dilute acetic acid solution is fed to 15th tray of distillation column TT501 through pumps with flow control.
This azeotropic distillation system utilizes another
solvent, n-butyl acetate (NBA) called the entrainer,
which is relatively immiscible with water. The entrainer forms azeotrope with water and increases the
relative volatility of water to acetic acid, which leads
to less reflux ratio and fewer distillation stages. The
water containing 0.1% (by mass) acetic acid is removed as distillate. The tower is operated at an external reflux ratio of approximate 0.6. The overhead
azeotropic vapor at 90 C is condensed, cooled to 40 C
in the condenser and flows into the reflux drum.
TD501 is internally divided by weir into the phase
separating zone, in which the condensate is separated
into entrainer phase and aqueous phase by decantation,
and the entrainer overflows the weir into the entrainer
collecting zone. The entrainer is refluxed to the top of
TT501 with flow control. A portion of aqueous phase
containing some dissolved entrainer is refluxed from
the bottom of the phase separating zone to the top of
TT501 with flow control through water reflux pumps.
The remainder is fed to the NBA recovery tower

Figure 2 shows the three phase equilibrium model

used in this study. Because the industrial PTA solvent
dehydration system shows extremely complex dynamic
and nonlinear characteristics, the model is developed
with following assumptions: perfect mixing in vapor
and liquid phases, equilibrium vapor-liquid-liquid phases,
ideal stage, negligible vapor holdup, and steam condensation at saturated temperature in reboiler.

Figure 2

Sketch of three phase equilibrium model

Vapor-liquid-liquid equilibrium (VLLE) is represented with the non-random two liquids (NSTL) equation. The model equations are described as follows:
d( M ij )
dt

= F jl zil, j + V j +1 yi , j +1 V j yi , j +
Llj 1 xil, j 1 Llj xil, j + Lllj 1 xill, j 1 Lllj xill, j

(1)

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Chin. J. Chem. Eng., Vol. 19, No. 1, February 2011

d( M i1 )
= V1 yi ,1 ( L1l + D l ) xil,1 ( L1ll + D ll ) xill,1
dt

(2)

d( M in )
= V1 yi ,1 + Lln xil, n B l xbl + Lllj xill, j B ll bbll (3)
dt

Variables L , xij , j , and H are introduced into the

formulation [23]. Here, is phase separation parameter(0j1).
L = Llj + Lllj

(4)

i =1

i =1

xil, j

=1

(5)

xill, j = 1

(6)

i =1

d( E j )
dt

(23)

xij = j xijl + (1 j ) xijll

(24)

On the basis of the above assumptions, the equilibrium constants are obtained as follows:
HAC equilibrium constant:
K HAC =

(7)

d( E1 )
= V2 H 2v V1 H1v L1l H1l L1ll H1ll Q1
dt
d( En )
= Vn H nv Lln H nl + Lln 1 H nl 1 + Qn
dt

(8)

(22)

H j = j H lj + (1 j ) H llj

= F j H fj V j H vj + V j +1 H vj +1 Llj H lj +
Llj 1 H lj 1 Lllj H llj + Lllj 1 H llj 1 + Q j

(21)

yi, j = 1

H l = H il xi

liquid mixture:

e16.808

3405.57
T 56.34
p

(25)

H2O equilibrium constant:

K H2O =

(9)

e18.3036

3816.44
T 46.13
p

(26)

E j uij h j = 0

(10)

NBA equilibrium constant:

i =1

Phase equilibrium equations are

yiv, j K ivl, j xil, j = 0

(11)

ll
yiv, j K ivll
, j xi , j = 0

(12)

xil, j K ill, j xill, j = 0

(13)

K NBA =

dt

0.1223(T 273.15) + 0.000321(T 273.15)

water vapor:
H iv

(14)

V j ( yi , j xi , j ) + L j 1 ( xi , j 1 xi , j ) M j (28)

0.09250(T 273.15)2 + 0.0009454(T 273.15)3 (15)

NBA vapor:
H iv

= 8600 + 9.34(T 273.15)

0.2799(T 273.15)2 + 0.002839(T 273.15)3 (16)

HAC vapor:
H il = H iv 4.18 (36.7063.43T0.3709)
water:

(17)

H il = H iv 4.18(22.34523.0138T0.3095) (18)

NBA liquid:
H il = H iv 4.18(56.38834.5935T0.3942)
vapor mixture:

H v = H iv yi
i

dH lj
dt

= 9719 + 4.1347(T 273.15)

(19)
(20)

(27)

= F j ( zi , j xi , j ) + V j +1 ( yi , j +1 xi , j )

H iv = 5660 + 2.993(T 273.15)

2

3151.09
T 69.15
p

where p is the system pressure, and T is the temperature.

When j = 1 , there is one liquid phase in the
tower. The equations are as follow:
d( xi , j )

The values of enthalpy are as follows:

HAC vapor:

e16.1836

{ (

= F j H fj H lj V j H vj H lj +

}M

V j +1 H vj +1 H lj + L j 1 H lj 1 H lj + Q j

(29)

This differential equation of liquid composition

and flux represents well the dynamic characteristic of
distillation column. Vapor flow changes sharply, so it
has little effect on the equation, while temperature is an
important process variable that represents the characteristic of distillation process. In steady state simulations, temperature is obtained using bubble-point
method based on phase equilibrium. In dynamic simulations, the bubble-point equation is nonlinear with
complicated iterative process and it is difficulty to
convergence and even leads to calculation failure. In
order to improve the convergence and reduce computation time, the differential equation for temperature is
obtained.
Equations (21)-(24), and (29) are changed to

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M j ( a1 + 2a2T j )

dT j
dt

= L j 1 a1T j 1 + a2T j21

( L j 1 + V j +1 V j + Fj ) ( a1T j + a2T j2 )

V j a1T j + a2 T j2 + V j +1 a1T j +1 + a2 T j2+1 +

F j ( a1Tf + a2 Tf

) + (V j +1 V j + Fj ) ( a0 a0 ) + Q j

(30)

where ai and ai (i = 0, 1, 2) are coefficients and are

determined by regression, Tf is the feed temperature,
and Q is the heat duty.
The algorithm for solving the problem is as follows.
Step 1 Calculate initial value.
Step 2 Calculate liquid composition xij according
to Eqs. (4), (5), (7), (11)-(13) and (24), and obtain xijl ,
xijll and j .

Step 3 Calculate the liquid composition by using

ll
Eq. (30), and update K ivl,j , K ivll
, j , and K i , j with the liquidliquid flash and bubble point temperature calculation.
Step 4 Calculate V and L .
Step 5 Repeat Step 2 to Step 4 until the convergence within a tolerance level is achieved.
The differential equation is solved with the ODE
(ordinary differential equation) algorithm in Matlab,
which is for solving nonlinear problem so convergence is ensured. The calculation results are shown in
Table 1 and Fig. 3. The simulation is satisfactory, indicating that the model is appropriate.
Table 1
Tray
number
top
5# tray
12# tray
20# tray
26# tray
29# tray
30# tray
bottom

Comparison of the simulation and industrial

values (feed flow rate 19565 kgh1)
Tray temperature/K
Industrial
Simulation
361.57
363.75
365.47
364.88
369.63
366.23
370.07
370.35
381.35
381.78
387.21
387.89
393.08
391.25

HAC composition/%
Industrial
Simulation

0.9321

DYNAMIC SIMULATION AND ANALYSIS

The optimum operating condition is determined

for high concentration of bottom acetic acid and small
acetic acid loss through the top aqueous stream. The
nonrandom two-liquids (NRTL) activity coefficient
model is used for vapour-liquid-liquid equilibrium for
the ternary system.
Since the relative volatility between water and
acetic acid is very small, n-butyl acetate is used as the
entrainer for efficient separation. In the heterogeneous
azeotropic distillation column, water is obtained from
the heavy phase in the decanter and acetic acid is
withdrawn from the bottom of the column. With this
three-component mixture, the liquid phase is heterogeneous not only in the decanter but also in the upper
part of the column. The column has two reflux flows,
i.e., the entrainer reflux and water reflux. The top vapor
stream forms two liquid phases. The organic phase is
refluxed to the column to provide enough entrainer, and
the aqueous phase containing mostly water is drawn
out from the system for further treatment. Some of the
aqueous phase is refluxed to the column if the organic
reflux is too small to fulfill the column specifications.
Therefore, there are three manipulated variables, i.e.,
entrainer reflux flow, water reflux flow, and vapor flow.
Figure 4 shows three parts of the temperature
profile. The temperature in the trays above the feed
tray, 15#, changes slowly, where vapor and two liquids
are in equilibrium. The main compositions are water
and NBA and the concentration of acetic acid is very
low. At stage 20#, three phases become two phases, so
that the temperature and composition change sharply.
The sharp decrease in concentration of NBA is accompanied by a steep increase of acetic acid, as shown
in Fig. 5. In those trays beneath the feed tray, NBA is
very little and does not function in the distillation.
Thus no azeotropic phenomenon happens in these
stages and it is a binary acetic-water distillation.

0.9368

Figure 4 Temperature vs. the number of tower stage

Figure 3 Comparison of simulation with industrial data

industrial value;
simulation value

The NBA concentration at trays toward tower

bottom lower than tray 15# decreases rapidly. The temperature at the tray at which the temperature changes
sharply (sensitive point) must be controlled to ensure
the HAC concentrations at the bottom and the top. The
temperature of sensitive point is manipulated by

Chin. J. Chem. Eng., Vol. 19, No. 1, February 2011

93

The dynamic analysis is as follows.

(1) Response of temperature to the change of reflux flow
Figures 8 and 9 indicate that the tray temperature
decreases as reflux flow increases, and increases as
reflux flow decreases.

Figure 5 Liquid composition vs. the number of tower stage

HAC;
H2O;
NBA

Figure 8 Response of temperature at the top to increase in

the reflux flow
reflux flow +1%;
reflux flow +2%

Figure 6 Temperature profile at different reflux flow

1reflux flow in crease 2%; 2reflux flow constant;
3reflux flow decrease 2%; 4reflux flow decrease 4%

controlling the reflux flow. Fig. 6 shows that temperature profile changes with reflux flow. If the temperature is increased (temperature front shifting toward
the tower top), the HAC concentration in the vapor increases, losing more HAC. The strategy is implemented
by increasing the reflux flow. However, the NBA reflux flow can not be excessive. It is seen from Figs. 5
and 6 that as the NBA reflux flow increases, the NBA
concentration in the liquid near the bottom of tower
increases. The NBA at the bottom is sent to the oxidation
unit of PTA to be dissolved, so the cost increases. Moreover, HAC concentration at the bottom will decrease.
Figure 7 shows that the heat flow of reboiler affects the tray temperature obviously. The temperature
increases with the heat flow.

Figure 7 Temperature profile at different reboil duties

reboil duty/kW: 013061.2; 113067.2; 213074.5;
313087.3; 413113.4; 513057.3; 613035.1

Figure 9 Response of temperature at the top to decrease in

the reflux flow
reflux flow 1%;
reflux flow 2%

(2) Response of concentration to the change of

feed flow
Figures 10 and 11 show that the change of feed
flow does not affect the concentration of top product.
Figs. 12 and 13 indicate that HAC concentration at the
bottom increases with feed flow increasing and decreases as the feed flow decreases.

Figure 10 Response of top HAC concentration to increase

in the feed flow
feed flow increase 5%

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Chin. J. Chem. Eng., Vol. 19, No. 1, February 2011

Figure 11 Response of top HAC concentration to decrease

in the feed flow
feed flow 5%

Figure 14 Response of top HAC concentration to increase

in the reflux flow rate
reflux flow +1%;
reflux flow +2%

Figure 12 Response of bottom HAC concentration to increase in the feed flow

feed flow +5%;
feed flow +10%

Figure 15 Response of bottom HAC concentration to increase in the reflux flow

reflux flow +1%;
reflux flow +2%

Figure 13 Response of bottom HAC concentration to decrease in the feed flow

feed flow 5%;
feed flow 10%

(3) Response of concentration to the change in

reflux flow
Figures 14 and 15 show that top and bottom
HAC concentrations increase as reflux flow decreases.
The increase of top HAC concentration should be
prevented, but the increase in bottom HAC concentration is desired, so it must be careful to decrease the
reflux flow. In PTA industry, the decision-maker usually ensures that the top HAC concentration is in the
range of preset values. Figs. 16 and 17 show that top
and bottom HAC concentrations decrease as reflux
flow increases. The decrease in top HAC concentration is desired, so it must be careful to manipulate the
reflux flow.

Figure 16 Response of top HAC concentration to decrease

in the reflux flow
reflux flow 1%;
reflux flow 2%

Figure 17 Response of bottom HAC concentration to decrease in the reflux flow

reflux flow 1%;
reflux flow 10%

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Chin. J. Chem. Eng., Vol. 19, No. 1, February 2011

Table 2
Number of stage

30

Feed flow/kgh1

Feed tray

15

Specification for the azeotropic distillation column

HAC

H2O

NBA

8647

10918

When the feed flow increases, tray temperature

front will move to the top. Increase in tray temperature
will lead to an increase in the HAC concentration at
the top after a while. The measure is taken to decrease
the top HAC concentration by increasing the reflux
flow. On the other hand, less feed flow will lead to a
decrease in the bottom HAC concentration. The
measure is taken to increase the bottom HAC concentration by decreasing the reflux flow.
In conclusion, reflux flow is an important manipulating variable in industrial operation and temperature is also important to the HAC concentration.
Increase of reflux flow decreases top HAC concentration to prevent the loss of HAC at the top, with bottom
HAC concentration decreased. Feed flow does not
affect top HAC concentration, but changing bottom
HAC concentration. In practical operation, reflux flow
is adjusted when tray temperature changes. According
to the above simulation result and analysis, some control scheme is implemented. Table 2 is the specification for the azeotropic distillation column. Fig. 18 gives
the control strategy as follows: using reflux flow FC1504
to control temperature TC1503 and using the heat flow
of reboiler FC1507 to control temperature TC1501. The
above control strategy is consistent with the industrial
control strategy, verifying our analysis results.

Feed temperature/K

Feed pressure/kPa

Reboil duty/kW

333

120

13061.2

temperature is derived. Dynamic analysis is presented.

The comparison between the simulation and industrial
values shows that the model and algorithm are particularly effective for the separation of HAC and water
with NBA. Based on this model, advanced process
control, online optimization, performance monitoring,
and production evaluation can be implemented.
ACKNOWLEDGEMENTS

Some helpful suggestions are from Engineering

Research Center of Intelligent Process System Engineering( Ministry of Education) of Beijing University of Chemical Technology.
NOMENCLATURE
B
C
D
Ej
F
H
K
M
n
p
Q
T
t
u
V, L
x, y

amount of product in tower bottom

the number of components
amount of product in tower top
energy hold up on tray j, J
feed flow, kmolh1
enthalpy, kJkmol1
equilibrium constant
holdup, kmol
the number of tower tray
pressure, kPa
heat duty, kJh1
temperature, K
time, s
liquid holdup, kmol
flow of vapor and liquid phases, kmolh1
mole fraction of liquid and vapor phases
phase separation parameter

Superscripts
l
ll
v

the first liquid phase

the second liquid phase
vapor phase

Subscripts
f
i
j

feed
index of component
index of tray

REFERENCES
Figure 18

Schematic diagram of control structure

CONCLUSIONS
2

This work introduces an improved model and

algorithm for the dynamic simulation of industrial
PTA solvent dehydration tower. A new model for

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