China Petroleum Processing and Petrochemical Technology

Simulation and Optimization 2015, Vol. 17, No. 2, pp 101-108 June 30, 2015

A Novel Thermally Coupled Reactive Distillation

Column for the Hydrolysis of Methyl Acetate
Zhai Jian1; Liu Yuliang1; Sun Lanyi1; Wang Rujun2
(1.State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Qingdao 266580;
2. China Petroleum Engineering Co., Ltd., Beijing Company, Beijing 100085)

Abstract: A different pressure thermally coupled reactive distillation column (DPT-RD) for the hydrolysis of methyl acetate
(MeAc) is developed, and its design and optimization procedures are investigated. The sensitivity analysis is carried out to
minimize the energy consumption, which is associated with the total annual cost (TAC). The influence of the proposed DPT-
RD scheme on energy consumption and economic efficiency are evaluated in comparison with the conventional reactive
distillation column (CRD). Both the DPT-RD and CRD are simulated with the Aspen Plus®, and it can be observed that for
the DPT-RD the energy consumption and the TAC are reduced, and the thermodynamic efficiency is increased as compared
with the CRD process.
Key words: different pressure thermally coupled distillation; reactive distillation; thermodynamic efficiency; energy sav-
ings; total annual cost

1　Introduction the energy consumption could be reduced by 92.3% and

Distillation columns are widely used in the petrochemi-
cal process, but they are also well-known for their high
energy consumption and low thermodynamic efficiency.
As a result, the process intensification becomes an im-
portant trend in chemical industry, which can improve
process efficiency and decrease energy consumption by
linking different separation units together or integrating
with other processes[1]. Many kinds of energy integration
techniques have been developed, such as the dividing
wall column[2-3], the internally heat-integrated distillation
column[4-6], the heat pump-assisted distillation column[7-8],
etc. The different pressure thermally coupled distillation
(DPT-CD) column is an example of internally thermally
coupled distillation technology developed to achieve
energy conservation[9]. In this technology, a distillation
column is divided into two columns operating under dif-
ferent pressures. The top stream from the high-pressure
column is used as the heat source for the reboiler of the
low-pressure column. In this way, the thermally coupled
process is realized. Li, et al.[9] analyzed the energy saving
of DPT-CD by taking the separation of propane-propylene
and C4 hydrocarbons as an example, and found out that
upon comparing with ordinary distillation technologies,
87.1% in these two DPT-CD processes, respectively.
Reactive distillation is an innovative process with numer-
ous applications in the petroleum and chemical indus-
tries. It combines the reaction and separation operations
together, which can reduce the energy consumption and
capital costs[10-11]. This technique is specifically applied
to the equilibrium-limited reactions such as esterification
and ester hydrolysis reactions. The conversion rate can be
increased far beyond what is expected due to the continu-
ous removal of reaction products from the reactive zone.
Researchers’ results[12-13] showed that reactive distillation
has great economic and environmental advantages. Gao
Xin, et al.[14] proposed a new process based on the catalyt-
ic distillation for MeAc hydrolysis, and the energy saving
for this process is 28.6%. Fuchigami[15] applied reactive
distillation to the hydrolysis of MeAc by using reactive
column packing made of ion-exchange resin molded with
polyethylene powder in a furnace, investigated the influ-
ence of operating variables on the conversion of MeAc,
and finally found out that the total energy requirement of
Received date: 2014-12-14; Accepted date: 2015-04-06.
Corresponding Author: Professor Sun Lanyi, Telephone: +86-
13854208340; Fax: +86-532-86981787; E-mail: sunlanyi@upc.edu.cn.

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 Zhai Jian, et al. China Petroleum Processing and Petrochemical Technology, 2015, 17(2): 101-108
the optimum process was only about 50% as much as that
of the conventional process. Han, et al.[16] proposed add-
ing a pre-reactor before the reactive distillation column,
and got a great improvement in MeAc throughput com-
pared with the traditional process. Lee, et al.[17] proposed
a novel process for MeAc hydrolysis, in which the reflux
drum of the distillation column was used as the fixed bed
reactor packed with solid acid catalysts.
The different pressure thermally coupled reactive distil-
lation column (DPT-RD) proposed in this article com-
bines DPT-CD and reactive distillation to form a new
process intensification technology. Gao Xin and co-
workers[18] investigated this novel configuration in the
process for tert-amyl methyl ether synthesis. The results
showed that the total annual cost (TAC) of this process
was by about 6.6% lower than the conventional reactive
distillation column (CRD) process. As a typical ester hy-
drolysis reaction, the hydrolysis of MeAc is investigated
in this paper. The design and optimization procedures of
the DPT-RD proposed are evaluated and the thermody-
namic efficiency and economic performance of the DPT-
RD are studied.
2　Process Description
2.1　Conventional reactive distillation column
Upon considering the conversion of MeAc and the need
of subsequent separation process, the process flow dia-
gram in Figure 1 is supposed as the conventional process
in this work.
The CRD column has 27 stages, which can be divided
into three sections, namely the rectifying section, the
Figure 1　Conventional reactive distillation process for
MeAc hydrolysis
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stripping section and the reactive section (6 th to 17 th
stage). The separation occurs in all sections. In the reac-
tive section, the MeAc hydrolysis reaction takes place:
MeAc+H 2 O ←
→ HAc+MeOH (1)
The reaction is rate controlled with a liquid holdup of
0.063 m 3 in the reactive section. The NKC-9 ion ex-
change resin is chosen as the catalyst, and Quan Xia, et
al.[19] provided the reaction kinetics equations which are
shown as follows:
R = k f xMeAc xH2O − kr xMeOH xHAc (2)
7 4
k f = 1.543 × 10 exp(−5.974 ×10 / RT ) (3)
5 4
kr = 4.013 × 10 exp(−4.270 × 10 / RT ) (4)
where R is the reaction rate, L/(mol·h); xi is the molar
fraction of component i; and kf and kr are reaction kinetic
constants of the forward and reverse reaction, respec-
tively, L/(mol·h). The reactive section is packed with acid
catalyst. The assumptions are made as follows: the cata-
lyst loading occupies half of the tray holdup volume, and
the tray holdup is determined by assuming a weir height
of 50 mm with a tray spacing of 0.6 m.
A mixture of MeAc and methanol (65:35 in molar ratio)
is fed to the bottom of reactive zone with a flow rate of
76.92 kmol/h, and water is routed to the top of column
with a flow rate of 250 kmol/h. The vapor condensed at
the top of the column is totally recycled. The reflux ratio
(reflux ratio=FL/FD as shown in Figure 2) of the CRD is
specified at 10 and the top stage/condenser pressure is
0.112 1 MPa with a stage pressure drop of 0.000 7 MPa.
The flow sheet of CRD implemented in the Aspen Plus
is shown in Figure 2, and Table 1 gives its design pa-
rameters.
Figure 2　Flow sheet of CRD implemented in Aspen Plus
 Zhai Jian, et al. China Petroleum Processing and Petrochemical Technology, 2015, 17(2): 101-108

Table 1　Design parameters of CRD umn with higher pressure. As the hydrolysis of MeAc
Design parameters Values is an endothermic reaction, high pressure and tempera-
Molar ratio of MeAc to methanol 65/35 ture is in favor of positive reaction, and a configura-
tion of the reaction taking place in the high-pressure
Flow rate of MeAc+methanol, kmol/h 76.92
column is chosen in this work. The model of DPT-RD
Flow rate of H2O, kmol/h 250
in the platform of the Aspen Plus is shown in Figure 3.
Number of stages 27 DPT-RD mainly contains a high-pressure column (T1),
Location of the top of reactive zone 6 a low-pressure column (T2), a compressor (COMPR),
Location of the bottom of reactive zone 17 a main heat exchanger (HE1), an assisted reboiler
(HE3) and an assisted condenser (HE2). The reactive
Column diameter, m 2
zone of DPT-RD is wholly placed in the high-pressure
Column height, m 25.8
column (T1).
3
Liquid holdup, m 0.063 The feedstocks and products of DPT-RD are identical
Feeding stage of F 17 with CRD to keep the comparability of the two processes.
Feeding stage of H2O 4 The design parameters of DPT-RD are detailed in Table
2. In this study, the split fractions of splitters SP1 and SP2
Top flow rate, kmol/h 60
are defined as
Reflux ratio 10
Split fraction of SP1=FT1D-CR/FT1D-1 (5)
Top pressure, MPa 0.112 1
Split fraction of SP2= FT2B-P/FT2B (6)

2.2　Different pressure thermally coupled reactive where FT1D-CR, FT1D-1, FT2B-P, and FT2B are the flow rate of
distillation column T1D-CR, T1D-1, T2B-P and T2B in Figure 3, respec-
DPT-RD contains an atmospheric column and a col- tively.

Figure 3　Flow sheet model of DPT-RD implemented in Aspen Plus

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Table 2　Design parameters of DPT-RD Table 3　Properties of azeotropic mixtures obtained during
Design parameters Column T1 Column T2 hydrolyzation of MeAc

Molar ratio of MeAc to methanol 65/35 MeAc-Methanol MeAc-Water

Items Calculated Literature Calculated Literature
Flow rate of MeAc+methanol, kmol/h 76.92
values values values values
Flow rate of H2O, kmol/h 250.00
Temperature, ℃ 53.60 53.67 56.64 56.90
Number of stages 19 8

Top pressure, MPa 0.273 6 0.101 3 Molar fraction of

0.661 8 0.661 0 0.910 7 0.894 0
MeAc
Stage pressure drop, MPa 0.000 7 0.000 7
Molar fraction of
0.338 2 0.339 0 0 0
Location of the top of reactive zone 6 - MeOH

Location of the bottom of reactive zone 17 - Molar fraction of

0 0 0 0
HAc
3
Liquid holdup, m 0.063 -
Molar fraction of
0 0 0.089 3 0.106 0
Feeding stage of F 17 - water

Feeding stage of H2O 4 -

Discharge pressure of compressor, MPa 0.273 6
Split fraction of SP1 0.43
Split fraction of SP2 0.40
3　Design and Simulation
There are three steps for the development of DPT-RD:
shortcut design, rigorous simulation and optimization.
The design method of the DPT-RD is based on the CRD.
The feed conditions, product specifications and column
operating conditions are available from either the plant or
the given examples depending on the situation.
The simulation of the DPT-RD is carried out using the
rigorous distillation module RadFrac of Aspen Plus®.
The UNIQUAC method is adopted for the calculation of
the activity coefficients in liquid phase and the Hayden-
O’Conell equation of state is used to describe the vapor
phase behavior. The predicted azeotropic temperatures
and compositions agree well with experimental results[20],
as shown in Table 3.
The shortcut design of the DPT-RD can be obtained by
dividing a CRD into two columns with different pressures
and by exchanging heat between the top stream from the
high-pressure column and the bottom stream of the low-
pressure column. And a compressor is adopted to provide
the upward vapor for the high-pressure column.
The RadFrac module of Aspen Plus®, a rigorous model
for simulating all types of multistage vapor-liquid frac-
tionation operations, is selected for the simulation of the
flowchart as shown in Figure 3. The UNIQ-HOC physical
property method is adopted when the simulation is imple-
mented using the Aspen Plus. Rigorous simulation used in
the present study is based on the equilibrium-stage model,
which uses the mass, equilibrium, summation of molar
fractions and enthalpy (MESH) equations for each stage.
The stage numbers of the whole column and reaction
section in DPT-RD are the same as those of CRD respec-
tively, with the purpose of comparing the performance of
the two processes. And for both of DPT-RD and CRD, the
stages are numbered in a downward direction.
According to the features of DPT-RD (Figure 3), many
sensitivity tests have been carried out in the optimiza-
tion process to adjust the design and operating variables.
Here, the design variables considered are the top pressure
of T1, the compression ratio, the feeding stages of water
and MeAc, the split fraction of SP1, and the split fraction
of SP2. By keeping the input conditions identical for both
distillation schemes, the variables of the DPT-RD are sys-
tematically adjusted to obtain the conditions that meet the
product specifications.
3.1　Selection of top pressure of T1
Here, the heat transfer temperature difference refers to
the difference between the top temperature of T1 and the
bottom temperature of T2. Only after the heat transfer
temperature difference reaches a specific value, the DPT-
RD then can operate effectively, which is very crucial for
the good performance of DPT-RD. Figure 4 illustrates
how the top pressure of T1 affects the heat transfer tem-
perature difference of DPT-RD. It shows that, along with
the increase in the top pressure of T1, the top temperature

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 Zhai Jian, et al. China Petroleum Processing and Petrochemical Technology, 2015, 17(2): 101-108
of T1 would increase while the bottom temperature of T2
remains nearly unchanged, and the temperature difference
would enlarge finally. When the heat duty keeps constant,
the heat-exchange area should increase with the reduction
of the temperature difference. Upon considering the cost
of heat exchanger and the normal operation of DPT-RD,
the top pressure of T1 was set at 0.233 0 MPa.
Figure 4　Effect of pressure on heat transfer temperature
difference
■—Top Temperature of T1; ●—Bottom Temperature of T2
3.2　Selection of compression ratio
The influence of compression ratio on product purity and
energy consumption of DPT-RD is presented in Figure
5 with other variables remaining unchanged. Obviously,
as the compression ratio increases, the molar fraction of
MeAc in the product stream drawn from the bottom of
T2 slightly decreases. However, the energy consumed by
the compressor significantly increases with an increasing
compression ratio. Finally, the compression ratio is se-
lected as 2.5 to meet the product specification.
Figure 5　Effect of compression ratio on product purity and
energy consumption
●—Molar fraction of MeAc in product stream; ■—Compressor duty
3.3　Selection of feeding stage of water
The influence of the feeding stage of water on the product
purity and energy consumption is displayed in Figure 6.
This simulation experiment is performed with the values
of other variables fixed. It can be concluded that the feed-
ing stage of water has little impact on product purity and
energy consumption. The 6th stage (numbered from top
downward) is chosen as the stage of water feeding, where
the molar fraction of MeAc in product stream and the
compressor duty would change relatively quickly.
Figure 6　Effect of feeding stage of water on product purity
and energy consumption
●—Molar fraction of MeAc in product stream; ■—Compressor duty
3.4　Selection of feeding stage of MeAc and methanol
The feeding stage of MeAc and methanol has been varied
from 8th to 19th (numbered from top downward), while the
values of other variables remain the same as those shown in
Table 3. Figure 7 shows how the feeding stage of MeAc and
methanol affects the product purity and energy consumption
Figure 7　Effect of feeding stage of MeAc and methanol on
product purity and energy consumption
●—Molar fraction of MeAc in product stream; ■—Compressor duty
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 Zhai Jian, et al. China Petroleum Processing and Petrochemical Technology, 2015, 17(2): 101-108

of DPT-RD. Both of the molar fraction of MeAc and the fraction of SP2 can be selected as 0.55.
compressor duty nearly remain constant before the feeding
stage moves to the 16th stage, but when the feeding stage
continues to move downward, the compressor consumes
more energy and the product purity drops sharply. The
stream of MeAc and methanol is fed at 16th stage here-
upon to achieve the desired product purity in this work.

3.5　Selection of split fraction of SP1

Figure 8 shows the effect of split fraction of SP1 on prod-
uct purity and energy consumption, with other variables
remaining constant. It’s clear that, when the split fraction
Figure 9　Effect of split fraction of SP2 on product purity
of SP1 increases, the product purity also increases, but
and energy consumption
the energy consumption increases constantly as well. This
●—Molar fraction of MeAc in product stream; ■—Compressor duty
happens because of the increase in the flow rates inside
the column. To save energy as much as possible, the split Based on the aforementioned work, the optimum pa-
fraction of SP1 is chosen as 0.43. rameters of DPT-RD for the hydrolysis of MeAc can be
obtained, and the simulation results of DPT-RD under
optimal conditions are shown in Table 4.

Table 4　The simulation results of DPT-RD under

optimal conditions
Design parameters Column T1 Column T2

Number of stages 19 8

Top pressure, MPa 0.273 6 0.101 3

Stage pressure drop, MPa 0.000 7 0.000 7

Top temperature, ℃ 76.9 46.6

Figure 8　Effect of split fraction of SP1 on product purity Bottom temperature, ℃ 86.3 64.4
and energy consumption Location of the top of reactive zone 10 -
●—Molar fraction of MeAc in product stream; ■—Compressor duty Location of the bottom of reactive zone 16 -

Column diameter, m 1.5 1.5

3.6　Selection of split fraction of SP2
Column height, m 16.5 9
The top pressure of T1, the compression ratio, the feeding
Discharge pressure of compressor, MPa 0.253 3
stage of water, the feeding stage of MeAc and methanol,
Split fraction of SP1 0.43
and the split fraction of SP1 are specified at 0.233 0 MPa,
Split fraction of SP2 0.55
2.5, 4, 17, and 0.43, respectively, as required by the test
process. When the split fraction of SP2 varies, the corre- Molar flow rate of T2B-P, kmol/h 326.9

sponding product purity and energy consumption profiles Methanol 23.5

are presented in Figure 9. As the split fraction of SP2 Composition of T2B-P, Water 61.2
increases, the product purity at first remains unchanged mol% Acetic acid 15.3
and then drops quickly, while the energy consumption
MeAc 0.001
decreases continuously. This happens because the hydro-
Compressor duty, kW 513.3
lysis of MeAc is an equilibrium-limited reaction, and the
Main reboiler duty, kW 2 950.7
continuous removal of reaction products facilitates the
conversion of MeAc. From this sensitivity test, the split Side condenser duty, kW 640.6

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 Zhai Jian, et al. China Petroleum Processing and Petrochemical Technology, 2015, 17(2): 101-108

4　Results and Discussions 5　Conclusions

There are many references for the calculation of thermody-
namic efficiency and total annual cost (TAC)[21-22]. The ther-
modynamic analysis results and TAC of CRD and DPT-RD
for the hydrolysis of MeAc are summarized in Table 5.
Table 5　Thermodynamic analysis results and TAC of CRD
and DPT-RD for the hydrolysis of MeAc
DPT-RD
Parameters CRD
Column T1 Column T2
In this study, the hydrolysis of MeAc is studied using a
CRD and a different pressure thermally coupled reactive
distillation column (DPT-RD). The design configura-
tion and optimization of this technology are investigated.
The optimal design flow sheet of DPT-RD is obtained by
minimizing the total energy consumption of the process
by means of the sensitivity analysis. The results show
that the proposed DPT-RD can achieve significant en-

Total heat duty, kW 6 638.5 2 441.1

ergy savings and improve the thermodynamic efficiency
by around 2.9%, and its TAC is reduced by 41.3% in
Compressor duty, kW - 813.7
comparison with the CRD. Obviously, the DPT-RD pro-
Thermodynamic efficiency, % 6.18 9.04
vides advantages in terms of higher energy savings and
Total reboiler heat transfer area, m2 357.3 149.3
a lower TAC.
Total condenser heat transfer area, m2 560.6 54.1 Acknowledgements: This work was supported by the Na-
Total capital cost, 103 $ 1 566.0 3 498.9 tional Natural Science Foundation of China (Grant Nos.
3
Total operating cost, 10 $/a 1 925.0 547.8 21276279, 21476261); the Key Technologies Development
3
TAC, 10 $/a 2 238.2 1 314.0 Project of Qingdao Economic and Technological Develop-
ment Zone (Grant No. 2013-1-57); the Fundamental Research
It can be seen that the CRD requires a heat duty of Funds for the Central Universities (No. 14CX05030A; No.
7 062.3 kW while the energy consumption of the DPT-RD 14CX06108A). Furthermore, the authors are grateful to the
is 2 441.1 kW, which shows that the DPT-RD can save editor and the anonymous reviewers for their helpful com-
the energy by 36.1% compared to the CRD. The total ments and constructive suggestions with regard to the revi-
heat transfer area of the reboilers of the CRD is 357.3 m2, sion of the paper.
while that of the DPT-RD is 149.3 m2, which can achieve
a reduction of 58.2%. The reduction in total heat trans-
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