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Reactive Distillation for Producing n-Butyl Acetate: Experiment and


Simulation

Article  in  Chinese Journal of Chemical Engineering · October 2012


DOI: 10.1016/S1004-9541(12)60426-1

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PROCESS SYSTEMS ENGINEERING AND PROCESS SAFETY
Chinese Journal of Chemical Engineering, 20(5) 980ü987 (2012)

Reactive Distillation for Producing n-Butyl Acetate: Experiment and


Simulation

TIAN Hui (ජ᡿)1, HUANG Zhixian (ܻᄦບ)2, QIU Ting (௎භ)2, WANG Xiaoda (ฆ໋Ӓ)2
and WU Yanxiang (๑ཀྵີ)2,*
1
College of Chemistry and Chemical Engineering, Yantai University, Yantai 264005, China
2
College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China

Abstract In this paper, a reactive distillation (RD) column was applied for synthesis n-butyl acetate from
n-butanol and acetic acid. The Langmuir-Hinshelwood-Hougen-Watson (LHHW) kinetic model and an equilibrium
stage model for separation were employed to study the RD process. The results obtained from the equilibrium stage
model agreed well with the experiments. The effects of operating variables on the n-butanol conversion and n-butyl
acetate purity were further investigated. The optimal column configuration for the production of n-butyl acetate was
designed with 5 rectifying stages, 8 reaction stages and 13 stripping stages by the simulation study. According to the
simulation results, n-butanol conversion and n-butyl acetate purity all reached greater than 96%.
Keywords reactive distillation, esterification, n-butyl acetate, simulation

1 INTRODUCTION with 26 theoretical stages. The high purity product


(>99%) could be obtained by simple separation from
The conception of Reactive Distillation (RD) was the raw product in this paper, which decreased the energy
firstly reported by Backhaus in 1921 [1], and has re- obviously. Based on the computer simulation, Steini-
ceived more and more attentions, especially for the geweg and Gmehling [8] carried out the pilot plant test
equilibrium-limited reversible reactions. RD had be- to study the RD process for producing n-BuAc using
came an attractive unit operation due to the following the strongly acidic ion exchange resin (Amberlyst-15)
reasons: (1) enhancing conversion and selectivity for as the catalyst, and both the thermodynamic and the
equilibrium reaction, (2) breaking the composition of kinetic aspects of the system were investigated. While
azeotropic mixtures, (3) reducing the energy con- they used the RD column with 30 theoretical stages,
sumption and the number of equipments [24]. the product purity could come to 96%. Gangadwala et
n-Butyl acetate (n-BuAc) is one of the most com- al. [9] explored various RD configurations for the pro-
mon solvents, which is used in lacquer and coating duction of n-BuAc in order to eliminate the by-product
manufacture and other branches in large quantity. The di-butyl ether, but they did not validate the model re-
consumption of n-BuAc grows in the last decade be- sults experimentally. Jimenez and Costa-Lopez [10]
cause it is of low toxic and environment-friendly using methyl acetate and n-BuOH produced n-BuAc
compared with other esters [5]. n-BuAc is synthesized and methanol, while three columns were used to ob-
through esterification by acetic acid (HAc) and tain high purity n-BuAc product, and the RD column
n-butanol (n-BuOH) with acid catalyst. Because the had 43 theoretical stages. Qiu et al. [11] investigated
reaction is reversible, the conversion of n-BuOH is lim- the kinetic model of the esterification reaction by
ited by the chemical equilibrium. Removing the prod- n-BuOH and HAc catalyzed by Amberlyst 36 Wet, and
ucts during the reacting is beneficial for enhancing the the Langmuir-Hinshelwood-Hougen-Watson (LHHW)
conversion. Thus, an integrated RD process is desirable. model was proposed to describe the reaction.
The information about n-BuAc synthesis in a RD The aim of this study was to investigate the per-
column is plentiful in the literature. In China, Liao and formance of RD for the production of n-BuAc from
Tong [6] studied the synthesis of n-BuAc by RD using HAc and n-BuOH in more detail. Experimental stud-
the cation exchange resin as the catalyst primeval, and ies were performed in our lab and simulation studies
the conversion of HAc could reach 94%. Meanwhile were carried out using the ASPEN PLUS simulator.
the conversion of HAc and n-BuOH were all above Emphasis was placed on analyzing the effects of key
96% at the optimized condition in their study. Hanika parameters such as the height of rectifying, reaction
et al. [7] studied the n-BuAc synthesis through RD in a and stripping sections, and also the feed location, on
packed column experimentally, and the computer simu- the conversion of n-BuOH and n-BuAc purity.
lation was performed to evaluate the experimental data.
But three columns were used to obtain high purity 2 EXPERIMENTAL MATERIAL AND THE ANAL-
(>99%) n-BuAc product, and the RD column had 50 YSIS METHORD
theoretical stages, while the n-BuAc product (>96%)
was obtained in this paper using one RD column only HAc (purity >99%, by mass) was supplied by

Received 2011-06-07, accepted 2012-03-14.


* To whom correspondence should be addressed. E-mail: wuyx@fzu.edu.cn
Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012 981

Shenbo Chemical CO., and n-BuOH (>99.8%) was ters K are expressed as
supplied by Merck. The catalyst used in the present K a exp(b / RT ) (3)
experiment was cation exchange resin Amberlyst 36
Wet, produced by Rohm and Haas, and the parameters All the parameters of the LHHW kinetic model
were given in Table 1. were taken from the Ref. [11] for the esterification
catalyzed by Amberlyst 36 Wet ion-exchange resin.
The average relative error was less than 2%, and the
Table 1 Physical properties of Amberlyst 36 Wet
kinetic parameters were given in Table 2.
physical form opaque beads
ionic form as shipped hydrogen Table 2 Parameters of the LHHW kinetic model
concentration of acid sites ı1.95 mol·L 1 for n-BuAc reaction system [11]
ı5.4 mol·kg1 Parameter a/kmol·kg1·s1 b/J·mol1
moisture holding capacity 51% to 57% (H+ form) ka 1.23×103 1.96×103
shipping mass 800 g·L1 (50 lbs·ft3) kf 1.45×10 4
6.45×103
fines content <0.425 mm: 0.5% max Ks,HAc 6.44×101 5.41×103
coarse beads >1.180 mm: 4.0% max Ks,BuOH 2.84×10 7
4.80×104
2 1
surface area 33 m ·g Ks,BuAc 2.86×103 2.47×104
average pore diameter 24 nm K s,H2O 3.88×10 4
2.92×104
maximum operating temperature 150°C (300 °F)

4 REACTIVE DISTILLATION EXPERIMENT


Both titration and gas chromatography were used AND SIMULATION
for the analysis of the reaction mixtures. The gas
chromatograph (Varian CP-3900, USA) equipped with 4.1 Experimental setup
a hydrogen flame detector. A CP-8907 column was
used with nitrogen as the carrier gas at a flow rate of A RD column containing solid catalyst was used
1 ml·min1. Injector and detector temperature were for the synthesis of n-BuAc. The strong cation ex-
523.15 K and 573.15 K, respectively. The water in or- change resin (Amberlyst 36 Wet) was used as the
ganic phase was measured by means of the Karl-Fischer catalyst. The experimental setup was given in Fig. 1.
instrument. The concentration of free HAc was deter- The setup included a RD column with internal diame-
mined through titrating with standard 0.1 mol·L1 so- ter of 32 mm in addition to a fixed-bed reactor with
dium hydroxide solution, and phenolphthalein was internal diameter of 20 mm with the height of 600 mm
used as the indicator. for fulfilling part of the load of reaction. The rectify-
ing section and the stripping section of the RD column
3 KINETIC MODEL were packed with bulk  packing (2.5 mm) while
catalyst-bundles containing cation exchange resin
catalyst were packed in the middle of the column as
In this work, the Langmuir-Hinshelwood- Hougen- the reaction zones [12]. The height of the rectifying
Watson (LHHW) kinetic model was used to describe section, the reaction section, and the stripping section
the reaction occurring in the RD column. The reaction were 550 mm, 1050 mm, and 600 mm, respectively. In
of synthesis n-BuAc from HAc and n-BuOH in the order to describe the RD column separation efficiency
reactive zone can be written as follows: quantitatively, the number of theoretical stages (TS) of
ZZX H 2 O  n - BuAc
HAc  n - BuOH YZZ (1) RD column was estimated by using the Fenske
method through separating a mixture of ethanol and
The rate of reaction for the LHHW model can be isopropyl alcohol [13]. The results indicated that the
written as follows: separation efficiencies of rectifying section, reactive
section, and stripping section were equivalent to 8, 6,
rBuOH M cat K f K s,HAc K s,BuOH u and 9 theoretical stages, respectively. The temperature
CHAcCBuOH  CBuAcCH O / Ka u
2
was measured at eight points in the column while the
samples were taken from top, bottom and along the
1  Ks,HAc CHAc  Ks,BuOH CBuOH  column (as shown in Fig. 1). The theoretical stages
were numbered from the top of the column to the
K s,BuAc  K s,H O CH O
2
2 2
(2) column bottom (reboiler), and the relationship be-
tween sampling and the number of theoretical stage
where r is the reaction rate (mol·s1); Ci is the concen- were shown in Table 3.
tration (mol·L1); Mcat is the catalyst mass (g); Kf is During the production of n-BuAc by this setup,
the reaction rate constant (mol·g1·s1); Ks and Ka are the equimolar n-BuOH-HAc mixture was fed to the
chemical reaction equilibrium constant and adsorption first reactor which was packed with ion exchange resin.
equilibrium constant, respectively. All of the parame- The temperature in the fixed-bed was maintained at
982 Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012

Figure 1 Reactive distillation experimental setup

Table 3 The relationship of sampling and thermometers stage model is often applied with great success for the
location with number of theoretical stage simulation of RD column [14]. Therefore, the RADFRAC
Sampling Number of module, based on the rigorous equilibrium stage model
Thermometers location containing the mass balance, phase equilibrium, summa-
point theoretical stage
a T2 3
tion and energy balance (MESH) equations, was used to
describe the multistage vapor-liquid separation in the
b T3 5 RD. To simplify the calculation, the low pressure drop
c T4 10 along the column (about 2 kPa) was neglected accord-
d T5 12 ing to some researches [15, 16], for the whole equip-
ment was supposed to operate at atmospheric pressure.
e T6 18
The selection of the physical property method
f T7 22 was very important due to the highly non-ideal nature
of the quaternary system, and the phase equilibrium of
this system was complex because of the existence of
358.15K. The effluent from the fixed-bed reactor, azeotropes. Because of the non-ideal vapor-liquid
which almost achieves the chemical equilibrium, en- equilibrium (VLE) and possible vapor-liquid-liquid
tered the RD column above the reactive zone. n-BuAc, equilibrium (VLLE) for the quaternary system, the
whose boiling point was the highest in this system, UNIQUAC activity coefficient model was adopted [9],
was withdrawn from the bottom of the column. The and the model equation came from the Aspen Plus
overhead distillate was mainly n-BuOH, HAc, water, user manual 11.1. The Hayden-O’Conell model with
and a small amount of n-BuAc. The overhead vapor association parameters was used to account for the
was condensed and cooled to liquid at room tempera- dimerization and trimerization of HAc in the vapor
ture at first and then introduced to a decanter for phase phase [17]. The Aspen Plus built-in association parame-
separation. While the organic phase was completely ters were used to compute the fugacity coefficients.
refluxed back to the column, the aqueous phase which The binary interaction parameters of the UNIQUAC
might still contain small amount of the organic com- model came from the built-in Aspen Plus Databanks
pounds (i.e., n-BuAc, unreacted n-BuOH and HAc) and Ref. [17]. The azeotropes for the four components
was withdrawn from the system. system [HAc-(n-BuOH)-(n-BuAc)-H2O] calculated at
the atmospheric pressure were listed in Table 3. From
Table 4, the calculated azeotropic composition and
4.2 Modeling and simulation
temperature were compared with the literature values,
and the maximal error was less than 1%, showing the
The RD was a complex process, which contains selection of the thermodynamic model was reliable.
not only the mass transfer process but also the separa- Since the available built-in reaction kinetic model
tion and reaction processes. In this paper, simulation in Aspen Plus 11.1 was power law and defined on the
of the synthesis of n-BuAc in a RD column was car- basis of mass or mole fraction, the reaction kinetics
ried out by using Aspen Plus 11.1. The equilibrium model for n-BuAc system based on LHHW [Eq. (2)]
Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012 983

Table 4 The compositions and temperatures of the azeotropes at atmospheric pressure


Data from Ref. [17] Calculated results
Azeotrope n-BuOH n-BuAc H2 O T n-BuOH n-BuAc H2O T
/% (by mass) /% (by mass) /% (by mass) /K /% (by mass) /% (by mass) /% (by mass) /K
(n-BuAc)-H2O 0.00 27.66 72.34 364.34 0.00 28.22 71.78 364.07
(n-BuOH)-H2O 57.50 0.00 42.50 366.11 53.77 0.00 46.23 366.91
(n-BuOH)-(n-BuAc) 70.74 29.96 0.00 389.30 69.96 30.04 0.00 390.00
(n-BuOH)-HAc 51.61 0.00 0.00 395.84 51.73 0.00 0.00 396.38
(n-BuOH)-(n-BuAc)-H2O 8.95 20.41 70.64 363.81 4.82 24.01 71.16 363.98
(n-BuOH)-(n-BuAc)-HAc 20.00 34.00 0.00 394.45 21.27 29.49 0.00 395.08

Table 5 The detailed specification of the BuAc RD column in simulation


Total no. Rectifying Reactive Stripping Feed Catalyst loading Mole feed ratio of HAc Space velocity of
of stages section section section stage per stage/g to n-BuOH n-BuOH/m3·h1·m3
24 18 stage 914 stage 1524 stage 9th stage 27.5 (914 stages) 1Ή1 0.2348

(a) Space velocity: 0.2348 m3·h1·m3 (b) Space velocity: 0.4375 m3·h1·m3
Figure 2 Temperature profile in the RD column
simulation;Ƶexperimental

was incorporated into the process simulator using an for simulating the RD column, the model was used to
additional subroutine written in FORTRAN, and the predict the temperature distribution and vapor composi-
different catalyst concentrations and the efficiency of tion along the RD column, and the predictions were
the catalyst-bundle [18] in the RD column were con- compared with the experimental data obtained in the
sidered. The simulation was run and fitted to the present study. The temperature and concentration profiles
available experimental data by adjusting the Murphree obtained from the experiment and simulation results
stage efficiency (from 0.5 to 0.8), and the value of were shown in Figs. 2 and 3. The experimental values
which is reasonable [15]. were all came from the average value of three experi-
According to the experimental setup, the theo- ments and the relative errors were all less than 2.0%.
retical stages were numbered from the column to the Figure 2 demonstrated the calculated temperature
column bottom (reboiler). The process parameters of profile was similar to the experimental values and the
the experiment and the specification of the RD column maximum relative error was 1.1%, which was accept-
for process simulation were listed in Table 5. able. From Fig. 3, it can be seen that the vapor com-
positions in 6 sampling points were in good agreement
with the simulation results. The errors mainly came
4.3 Model validation
from the equilibrium stage model not accounting for
transport phenomena. The conversion of n-BuOH as
In order to check whether the model was suitable defined as
984 Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012

(a) Space velocity: 0.2348 m3·h1·m3 (b) Space velocity: 0.4375 m3·h1·m3
Figure 3 Experimental and predicted concentration profiles in the sampling location
Ʒ BuOH experimental; BuOH simulation; ƹ BuAc experimental; Ƶ H2O experimental; H2O simulation; BuAc
simulation; HAc experimental

n-BuOH conversion

(4)

was calculated to compare the performance of the RD.


Experimental and simulation results at different
space velocity and HAc concentration were listed in
Figs. 4 and 5. The experimental values were all came
from the average value of three experiments and the
relative errors were all less than 1.0%. From Fig. 4,
n-BuOH conversion reduced gradually along with the
Figure 5 Experimental and simulation results at different
space velocity increase because of the limit of the re- HAc concentration
active section capacity. n-BuOH conversion reduced ƹexperimental; simulation
gradually along with the reducing of the HAc concen-
tration. It was evident that the experimental data agreed 5 DISCUSSION
very well with the results of the numerical model, and
the equilibrium stage model could describe well the
RD column profiles. Due to the constraints and limitations in the ex-
perimental study, some of the important RD design
parameters could not be studied experimentally. The
important design variables considered include the num-
ber of rectifying, reaction and stripping stages and the
feed stage location. So a series of analysis were con-
ducted to determine the effects of the design variables
on conversion of n-BuOH and the purity of n-BuAc.
The conditions of the base case simulation study were
the same as shown in Table 5. From the base case, a
series of sensitivity studies were performed to study
the RD column performances.

5.1 Number of reaction stages

Figure 4 Experimental and simulation results at different Increasing the number of reaction stages was not
space velocity always a better option because that will affect the
ƹexperimental; simulation column separation performance, thereby changing
Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012 985

compositions in the reactive zone. For equilibrium


limited systems, increasing the number of reaction
stages will lead to the enhancement of temperature and
concentration which would favor the reversion reac-
tion, causing the product decomposition [19, 20]. Fig. 6
shows the influence of the number of reaction stages
on the RD column performance. All other design and
operating variables such as the number of rectifying,
stripping stages and feed conditions were kept at the
values of the standard condition and the mixture
which was close to chemical equilibrium being from
the fixed-bed reactor is still fed at the top of the reaction
section. The simulated results shown that by using Figure 7 Effects of rectifying stages on n-BuOH conver-
more reaction stages both the conversion of n-BuOH sion and n-BuAc purity
and the purity of n-BuAc were increased, and the heat ƻn-BuAc purity;Ƶn-BuOH conversion;Ʒheat duty
duty of the reboiler also increased. This was to be ex-
pected as the reactive zone in the column could be
analogous to the series of reactors. The number of could be concluded that the contribution of the in-
reactors in the series increased as the height of the crease of rectifying stages to the column performance
reactive zone increased and therefore that provided became progressively small and therefore the number
sufficient residence time for higher conversion. The of rectifying stages of 5 was used as the column con-
number of reaction stages of 8 was used as one of the figurations for the following simulations.
column configurations for the following simulations.
5.3 Number of stripping stages

In the RD, the number of stripping stages should


be adjusted to achieve a satisfactory separation. The
main function of the stripping section was to maintain
favorable reaction conditions by removing n-BuAc
from the reactive zone, purifying the n-BuAc product
in the residue, and minimizing the loss of n-BuOH in
the product of n-BuAc. It could be seen from Fig. 8
that the n-BuOH conversion, n-BuAc purity and the
heat duty of the reboiler increased as the number of
stripping stages was increasing from 2 to 15 stages.
Increasing the number of stripping stages decreased
Figure 6 Effects of reaction stages on n-BuOH conversion the concentration of n-BuAc in the reaction zone,
and n-BuAc purity shifting the equilibrium of the etherification forward
ƻn-BuAc purity;Ƶn-BuOH conversion;Ʒheat duty
n-BuAc. Therefore, the optimum configuration was 13
stripping stages.
5.2 Number of rectifying stages

The rectification section of the RD column for


n-BuAc synthesis should remove light components
from the reaction zone, and recycle the unreacted re-
actants back to the reaction section in the RD column.
The effects of the number of the rectifying stages on
the purity of n-BuAc, the conversion of n-BuOH and
the heat duty of the reboiler were demonstrated in Fig. 7.
It was found that the purity of n-BuAc, the conversion
of n-BuOH and the heat duty of the reboiler increased
slightly with the increase of the number of rectification
stages from 2 to 11 stages. This could be explained by
the fact that with the increase of the rectifying stages, Figure 8 Effects of stripping stages on n-BuOH conver-
water and the lightest component were more removed sion and n-BuAc purity
ƻn-BuAc purity;Ƶn-BuOH conversion;Ʒheat duty
from the reaction section, decreasing the concentration
of water in the reaction zone. This caused the equilibrium
of reaction (1) to shift forward and thus, the conversion 5.4 Feed stage location
of n-BuOH and the purity of n-BuAc became higher,
both reached at 96.5% and 96.4%, respectively. It The RD column could be treated as a tubular reactor
986 Chin. J. Chem. Eng., Vol. 20, No. 5, October 2012

Table 6 Compare of the experiment and simulation value of n-BuOH conversion and n-BuAc purity
n-BuOH conversion Relative n-BuAc purity/mass fraction Relative
Number
Experiment Simulation error/% Experiment Simulation error/%

1# 0.9581 0.9628 0.47 0.9675 0.9653 0.23


2# 0.9636 0.9628 0.09 0.9601 0.9653 0.54
3 1 3
results of Section 4.3 with 0.2348 m ·h ·m 0.9432 0.9588 1.65 0.9723 0.9673 0.52
different space velocity 0.4375 m3·h1·m3 0.9426 0.9583 1.66 0.9615 0.9671 0.58

cascaded with separation units, while the reactive zone was capable of modeling the n-BuAc synthesis rela-
of a RD column could be viewed as a cascade-type tively accurately. The simulation results shown that
two-phase reactor with the reaction temperature deter- the experimental data agreed with the simulation results
mined from the bubble-point temperature of the tray well. The equilibrium stage model could describe the
liquid phase composition. The composition and tem- column profiles quantitatively. The effects of some
perature profiles could affect the performance of the important process parameters were investigated with
reactive zone, and the feed tray location appear to be the aid of simulation studies and the optimal parameters
one of the most important variables for these profiles were obtained: the optimal design variables for the RD
redistribution [21, 22]. The right choice for feed location were 5 rectifying stages, 8 reaction stages and 13
ensured high concentrations of reactants in the reactive stripping stages, and the best feed location was the 6th
zone. Fig. 9 presented the effects of the feed location theoretical stages. According to the simulation results,
on n-BuOH conversion, n-BuAc purity and the heat the RD column was changed to 5 rectifying stages, 8
duty of the reboiler. It was found that feeding equilib- reaction stages and 13 stripping stages based on the
rium reaction mixture at the 5th TS offered the highest experimental setup. n-BuOH conversion and n-BuAc
conversion of n-BuOH (96.83%) and the highest purity purity were all greater than 96% at this condition.
of n-BuAc (96.71%).
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