Chemical Engineering and Processing 50 (2011) 1128–1136

Contents lists available at SciVerse ScienceDirect

Chemical Engineering and Processing:

Process Intensification
journal homepage: www.elsevier.com/locate/cep

Dynamic control analysis for manufacturing ethanol fuel via reactive distillation
Shiqing Lu, Zhen Lei, Jiang Wu, Bolun Yang ∗
Department of Chemical Engineering, State Key Laboratory of Multiphase Flow in Power Engineering, Xi’an Jiaotong University, Xi’an, Shaanxi 710049, China

a r t i c l e i n f o a b s t r a c t

Article history: Reactive distillation process for removing water from bio-ethanol by the hydration using C4 olefin cut in
Received 10 November 2010 the present of the ␤ molecular sieve catalyst is proposed and described in this work. Simulation based on
Received in revised form 26 April 2011 the MESH equations is developed using the simulation package Aspen Plus 10.2. The sensitivity analysis
Accepted 10 September 2011
for steady states of this process is performed to obtain the optimal column operation conditions and
Available online 29 September 2011
the most sensitive operation parameters. The dynamic open-loop transient responses are investigated
with Aspen Dynamics 10.2 to find the manipulated variables that might have significant effects on the
Keywords:
control object. The control system of reactive distillation column is established and evaluated with Aspen
Ethanol fuel
Bio-ethanol
Dynamics 10.2 to make sure that the process runs well. With the proposed control system, the final
Reactive distillation product is composed of ethanol (43.3%), ethyl tert-butyl ether (48.2%), tert-butyl alcohol (8.3%) and water
Dynamic analysis (0.2%) in mass percentage.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction gasoline. As a result, the combined reaction system of hydration

Ethanol (EtOH) fuel receives increasing attentions since it is eas-
ily obtained by the bio-fermentation process and having higher
blending octane number. Many countries make laws for the utiliza-
tion of this environmental friendly automobile fuel. Presently, there
are a lot of reports on the techniques of manufacturing ethanol fuel,
while most of them are mainly focused on rectifying bio-ethanol to
the azeotropic concentration, then using enhanced separation pro-
cess to separate remaining water as to obtain anhydrous ethanol,
and finally mixing with conventional gasoline in a volumetric ratio
of 1:9 [1]. However, these enhanced separation processes are not
cost-effective enough and show the drawbacks of high energy con-
sumption.
A novel technique has been reported that it uses chemical reac-
tion to separate some components that are difficult to be treated
with conventional methods. The technique has been successfully
applied in several separation processes [2]. With this technique,
water can be removed from EtOH by some suitable reaction pro-
cess, which is known as hydration of isobutene (IB) with water. It
could cause the formation of tert-butyl alcohol (TBA) in the present
of some catalysts [3–5]. The TBA shows a blending octane number
as high as EtOH does. Thus, this reaction can be employed to remove
water from EtOH. Although the etherification between IB and EtOH
is always combined, the product of ethyl tert-butyl ether (ETBE) is
a fuel additive with high octane number [6–9]. The product is con-
sisted of EtOH, TBA and ETBE and thus can be directly added into
∗ Corresponding author. Tel.: +86 29 82663189; fax: +86 29 82668789.
E-mail address: blunyang@mail.xjtu.edu.cn (B. Yang).
and etherification of IB can be developed to obtain a mixture of fuel
additive. Great efforts have been made on the individual hydra-
tion or etherification of IB [10–13]. Dirk-Faitakis and Chuang [14]
reported to remove water from azeotropic ethanol by etherifica-
tion and hydration, however, their study was limited to the steady
state case.
For this combined process of reaction with separation, both the
two main reactions, IB hydration to form TBA and IB etherification
to form ETBE, are exothermic, reversible and equilibrium limited.
Thus, applying the reactive distillation technique in this process
could yield following advantages: (1) selectivity and conversion
can be improved by continuous removal of products from the reac-
tion zone, (2) the direct heat integration could reduce the demand
on heat, especially for strong exothermic reaction, so the hot spot
can be avoided, (3) combination of the reaction and separation into
one unit might save a significant amount of capital and (4) when
the feed point is located below the reaction zone, catalyst poison-
ing can be avoided, resulting in a longer catalyst life than in the
conventional systems.
Due to the interaction between chemical reaction and distilla-
tion, reactive distillation exhibits intricate nonlinear phenomena,
which poses a formidable challenge to the design and control
of the system. Previous research on reactive distillation mainly
focused on steady-state design and open-loop dynamic along
with the existence of multiplicity phenomena, while only a few
papers discussed the closed-loop control [15–18]. Recently, the
control of reactive distillation has been received more attention.
Selection of control configurations and the application of robust
proportional-integral (PI) [19–24], linear [25–27], nonlinear
[28] and near-linear [29] control strategies have been applied

0255-2701/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2011.09.006
 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136 1129

Table 1 Table 2
Standard molar Gibbs free energy (r G ), standard molar enthalpy (r H ), appar- Initial values of operating parameters used in steady states simulation.
ent rate constants (k), activation energies (Ea ) of different reactions, and inhibition
coefficient (K) of different compounds [32]. Key operating parameters Unit Value

Total number of stages 15

Expression Unit Activity energy, Ea
Reaction stages 4–7
(kJ mol−1 )
Feed stage location 7
r1 G = −5.65 kJ mol−1 Type of condenser Total
r2 G = −10.08 kJ mol−1 Type of reboiler Kettle
r3 G = −4.43 kJ mol−1 Feed composition (EtOH:water:IB) Mass ratio 19:1:14
r1 H  = −35.03 kJ mol−1 Feed pressure Pa 5 × 105
r2 H  = −21.27 kJ mol−1 Feed flow kg s−1 0.13
r3 H  = 13.76 kJ mol−1 Column pressure Pa 1 × 105
k1 = exp(20.10 − 9429.90/T) mol kg−1 s−1 78.4 Water mass concentration of bio-ethanol feed % 5
k1 = exp(28.72 − 12689.0/T ) mol kg−1 s−1 105.5 Molar ratio of IB to water in feed – 1
k2 = exp(22.15 − 9069.04/T) mol kg−1 s−1 75.4 Molar reflux ratio – 1
k2 = exp(31.18 − 12039.03/T ) mol kg−1 s−1 100.1 Catalyst weight kg 0.5
k3 = exp(17.77 − 8154.92/T) mol kg−1 s−1 67.8 Reboiler duty kW 12
k3 = exp(23.20 − 10031.27/T ) mol kg−1 s−1 83.4
KH2 O = exp(−21.41 + 6824.64/T ) – –
KEtOH = exp(−15.10 + 4943.45/T) – – The rate equation and reaction rate constant are summarized in
KTBA = exp(−12.39 + 3180.01/T) – – Table 1 and expressed as Eqs. (4)–(6).
k1 ˛IB ˛H2 O − k1 ˛TBA
r1 = (4)
for different reactive distillation systems. However, dynamic (1 + KH2 O ˛H2 O + KEtOH ˛EtOH + KTBA ˛TBA )2
control of reactive distillation for hydration and etherification k2 ˛IB ˛EtOH − k2 ˛ETBE
of IB to obtain a mixture of fuel additive has not been reported r2 = (5)
yet. (1 + KH2 O ˛H2 O + KEtOH ˛EtOH + KTBA ˛TBA )2
For the design of a reactive distillation process control system, k3 ˛TBA ˛EtOH − k1 ˛ETBE ˛H2 O
it is important to investigate the column response to the changes r3 = (6)
(1 + KH2 O ˛H2 O + KEtOH ˛EtOH + KTBA ˛TBA )2
in manipulated variables. Aspen Dynamics is a powerful tool for
dynamic simulation, which is tightly integrated with AspenTech’s where ˛i is the activity of component i.
steady-state simulator Aspen Plus. With Aspen Plus, a process can The Wilson thermodynamic model is used to describe the
be evaluated in terms of the steady state energy consumption, yield vapor–liquid equilibrium with gas phase fugacity coefficient cal-
improvement and process alternatives. Using Aspen Dynamics, the culated by the virial equation. Aspen Plus built-in thermodynamic
same process model can be used for dynamic process analysis such model parameters are used in the simulation. The standard molar
as examining process operability, control, evaluating plant safety Gibbs free energy and molar enthalpy for different reactions
and troubleshooting operational problems. Al-Arfaj and Luyben obtained from our previous paper [32] are shown in Table 1.
[30] reported the control of an ethylene glycol reactive distilla-
tion column using Aspen Plus and Aspen Dynamics. Zeng et al. [31] 2.2. Reactive distillation experiments
investigated the design and control of a reactive distillation column
system for the production of butyl acrylate using Aspen Plus and A numerical controlled column with 0.025 m inner diameter and
Aspen Dynamics. 1.5 m effective height was used, which was once used for ethanol
In this work, a process simulation model is established by fuel production by ethanol–water mixture near azeotropic con-
Aspen Plus 10.2 with the supplementary reaction kinetics FOR- centration and C4 olefin cut in previous work [33]. Cylindrical ␤
TRAN subroutine. The sensitivity of the manipulated variables is molecular sieves were packed in the column up to the height to
analyzed to obtain the optimal column manipulated conditions 0.5 m in the reaction zone. The stripping section and the rectifying
and the most sensitive operation parameters. Dynamic open-loop section were packed with stainless steel ␪ rings.
responses are investigated using Aspen Dynamics 10.2 to find out In each experimental run, ethanol–water mixture was fed above
the operation conditions that might have significant effects on the the reaction zone while liquid IB was fed under the bottom of
control object. Finally, a group of close-loop transient responses are the reaction zone. The hydration reaction changed water into TBA,
tested for the control system stability of this process using Aspen while the etherification reaction changed a part of EtOH into ETBE
Dynamics 10.2. in the reaction. The TBA, ETBE and excess EtOH were split to bot-
tom of the column, while IB was distilled to top of the column. The
2. Basic procedure for dynamic analysis bottom product could be added into gasoline. The concentration of
each component was analyzed in a gas chromatograph with a 3-m
2.1. Reaction kinetics and thermodynamics column of Gaskuropack 54 as packing material at 463 K using a TCD
detector. Hydrogen at 0.12 MPa was used as the carrier gas.
The catalyst used in this process is the cylindrical ␤ molecular
2.3. Dynamic analysis method
sieve (3 mm × 10.5 mm) provided by Nankai University Catalyst Co.,
Ltd., China. The reactions occurred in the reaction zone are shown
The basic steps for dynamic analysis of reactive distillation pro-
as follows:
cess using Aspen Plus and Aspen Dynamics are described in Fig. 1.
i-C4 H8 (IB) + H2 O ⇔ i-C4 H9 OH(TBA) (1) The reactive distillation column model is established by the
equilibrium module, RadFrac, which is included in Aspen Plus.
i-C4 H8 (IB) + C2 H5 OH(EtOH) ⇔ i-C4 H9 –O–C2 H5 (ETBE) (2) The specification of column design and manipulated conditions
such as components, property method, feed conditions (flow rate,
composition and thermal state), operating pressure, column con-
i-C4 H9 OH(TBA) + C2 H5 OH(EtOH) ⇔ i-C4 H9 –O–C2 H5 (ETBE) + H2 O
figuration (number of stages, feed location, reaction stage, types
(3) of condenser and reboiler), two operating parameters and reaction
1130 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136
Fig. 1. Basic procedure for dynamic analysis.
type are required in Aspen Plus. The two operating parameters can
be chosen from a set of parameters such as reflux ratio, distillate
rate, bottoms rate, reboiler duty and condenser duty. All the ini-
tial values of operating parameters, shown in Table 2, are input
to the process model. “Kinetics” is chosen from the reaction types
listing in Aspen Plus, because this choice is closest to the experi-
mental results compared with other choices such as “equilibrium”
and “conversion”. A reaction kinetic subroutine powered by Visual
FORTRAN 6.5 is linked to the RadFrac module with the help of Aspen
Plus simulation Engine.
It is specified that all the initial estimates for every step are reini-
tialized during the sensitivity analysis. In this case, simulations are
first slightly converged to the lowest value of the feasible manipu-
lated parameter, and then the parameter varies continuously with
a small step towards the highest one. This procedure keeps repeat-
ing until all the interested operation parameters are investigated.
After the solution curves are observed and analyzed, the optimal
column manipulated condition and the most sensitive operation
parameters are obtained.
All the optimal manipulated parameters must be specified for
the steady state model to replace the initial guess to ensure the col-
umn under the optimal conditions. After the model is reinitialized
and converged to the values of optimal parameters, dynamic data
such as condenser and reboiler geometry, heat transfer data, tray
or packing geometry are introduced into the steady state model.
Then, the simulation is conducted to guarantee convergence and
exporting the enhanced model as a flow driven simulation to the
dynamic analysis software.
3. Results and discussion
3.1. Sensitivity analysis and optimization of manipulated
variables
The water content of the fuel ethanol must be less than 1% to
meet the blending demand with gasoline [35]. The first step of the
Fig. 2. Effects of the column pressure (molar feed ratio of IB to water: 1:1; feed water
concentration: 5 wt%; reboiler duty: 12 kW; molar reflux ratio: 1; catalyst weight:
0.5 kg).
simulation is varying the values of key manipulated conditions, and
researching the effects of those variations on hydration selectivity,
water conversion and water content of the bottom product. All the
interesting key manipulated conditions are analyzed as follows.
3.1.1. Effects of column pressure
Operating pressure is a key operating parameter of a distilla-
tion column. The column pressure sets the lower and upper bounds
of the temperature within the column. The operating pressure
should be chosen within a range so that water can be used as a
coolant for the overhead condenser and that steam can be used
as a heating medium for the reboiler. Within this range, the reac-
tion temperature is close to the boiling point of the liquid phase
flowing around the catalyst. Thus, the reaction temperature will
increase with climbing operating pressure. Fig. 2 shows the effects
of the column pressure on hydration selectivity, water conversion
and water content of the bottom product. As the pressure increases
from 1 × 105 Pa to 10 × 105 Pa, water content of the bottom prod-
uct decreases monotonously. That is because increasing pressure
brings on the increasing amount of liquid IB in the reaction zone,
which forces hydration and etherification shift to the product side.
However, a higher column pressure causes a higher operation
capital and water content of the bottom product decreases slowly
after 5 × 105 Pa. Thus, 5 × 105 Pa is chosen as the best column head
pressure.
3.1.2. Effects of IB/water feed molar ratio
As well known, increasing the reactant concentration may force
the reaction shift to the product side, the stoichiometric ratio of IB
to water in the feed stream should be considered as a key manipu-
lated variable. Fig. 3 shows the effects of IB/water feed molar ratio
on water content of the bottom product, water conversion and
hydration selectivity. It is obvious that, water content of the bottom
product decreases and reaches a minimum as the ratio increases to
4:1. In addition, other two curves reach an extreme value at that
ratio. It indicates that too much IB may decrease water conversion,
as the decreasing temperature in the reaction zone.
3.1.3. Effects of feed water concentration
Fig. 4 shows the result of strong nonlinear phenomenon with
increasing water concentration of feed stream from 5 wt% to
100 wt%. The three curves may be caused by the competitive
adsorption of water and ethanol on the catalyst surface. However,
too much water in feed stream will reduce the octane number of
bottom product since the octane number of TBA is lower than that
 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136
Fig. 3. Effects of the molar feed ratio of IB to water (column pressure: 1 × 105 Pa;
feed water concentration: 5 wt%; reboiler duty: 12 kW; molar reflux ratio: 1; catalyst
weight: 0.5 kg).
of ETBE. What is more, although water concentration drops from
15 wt% to 10 wt%, the cost of bio-ethanol feed does not increase
significantly. To take all these factors into account, the region of
water concentration available is 5–30 wt%. Thus, the optimal water
concentration of feed stream is 10 wt%.
3.1.4. Effects of reboiler duty
As shown in Fig. 5, with increasing reboiler duty from 12 kW to
96 kW, the water conversion and hydration selectivity decreases
monotonically and water content of the bottom product increases
linearly, which indicates that water content of the bottom prod-
uct may also decline as the reboiler duty decreases. It is obvious
that increasing reboiler duty may decrease the mount of liquid IB,
not conducive to hydration reaction. Thus, a lower reboiler duty is
favored.
3.1.5. Effects of molar reflux ratio
The reflux ratio is intended to increase the concentration of the
component in condenser to be concentrated. The effects of reflux
ratio on water content of the bottom product, water conversion
and hydration selectivity are shown in Fig. 6. With increasing reflux
ratio from 1 to 20, the hydration selectivity firstly increases up to a
maximum, and then keeps constant. In contrast, water conversion
reaches its minimum when the reflux ratio is 5. However, there is
almost no change in water content of the bottom product. It can
Fig. 4. Effects of the feed water concentration (column pressure: 1 × 105 Pa; molar
feed ratio of IB to water: 1:1; reboiler duty: 12 kW; molar reflux ratio: 1; catalyst
weight: 0.5 kg).
1131
Fig. 5. Effects of the reboiler duty (column pressure: 1 × 105 Pa; molar feed ratio
of IB to water: 1:1; feed water concentration: 5 wt%; molar reflux ratio: 1; catalyst
weight: 0.5 kg).
be guessed that increasing reflux ratio mainly results in liquid IB
increasing in the reaction zone, when it is less than 5. However,
when it is more than 5, increasing reflux ratio mainly results in
temperature decreasing in the reaction. Thus, the best reflux ratio
is designated as 5.
3.1.6. Effects of catalyst weight
Fig. 7 shows the effects of the catalyst weight on water conver-
sion, water content of the bottom product and hydration selectivity.
As the amount of catalyst increases in the reaction zone, the water
conversion increases as well. When the catalyst weight is more
than 0.5 kg, water conversion increase slowly, and the hydration
selectivity and water content of the bottom product seem to keep
constant, these facts indicate that the reaction is close to the equi-
librium state. Thus, the best catalyst weight is 0.5 kg.
3.2. Simulation optimization and determination of sensitive
manipulated variables
After the sensitivity analysis of the key operating variables, an
optimal column manipulated configuration is developed based
on steady-states simulation, as shown in Table 3. Other operation
conditions such as feed location, reaction stage number and
reaction stage location are obtained from the experiments in
our previous paper [33]. For most reactive distillation process,
the reactive distillation column should run under an invariable
Fig. 6. Effects of the reflux ratio (column pressure: 1 × 105 Pa; molar feed ratio of
IB to water: 1:1; feed water concentration: 5 wt%; reboiler duty: 12 kW; catalyst
weight: 0.5 kg).
1132 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136

Table 3
Simulation optimization results of steady state.

Key operating parameters Optimal value Objective functions Initial value Optimal value

Column pressure (Pa) 5 × 105 Water conversion (%) 5.7 46.9

Water content in bio-ethanol feed (wt%) 10 Water content of the bottom product (wt%) 4.4 1.8
Molar ratio of IB to water in feed 4 Hydration selectivity (%) 17.9 16.0
Molar reflux ratio 5
Catalyst weight (kg) 0.5
Reboiler duty (kW) 48

pressure. If the column is built up, it will not be easy to change
the amount of the catalyst. Thus, the two operation conditions
cannot be determined as sensitive variables. Additionally, it can
be inferred from Fig. 6 that water content of the bottom product
increases slightly with the change in reflux ratio if the molar reflux
ratio is higher than 5. Thus, the reflux ratio is not adequately
sensitive, either. The other three operation parameters, namely
molar feed ratio of IB to water, water concentration of feed stream
and reboiler duty, are considered as sensitive variables. However,
the feed IB rate can be controlled more easily than the feed ratio
of IB to water and have the same control effect as that of feed ratio
of IB to water. In this respect, the feed rate of IB thus is selected
as the first sensitive variable. What is more, the feed pressure is
considered as the fourth sensitive variables since it is susceptible
to the disturbance from the pump around the column.
to a 5% decrease in IB feed rate is observed. As shown in Fig. 8a,
the response direction of the test objective is reverse. The water
concentration of the bottom product deviation is 6.22%, which is
probably caused by the decrease of IB in the reaction zone shown
in Fig. 8b, as a decrease in the reactant concentration may force the
reaction balance shift to the reactant side.
3.2.1.2. Effects of a step change in feed pressure. In a certain case of
process run, the feed pressure may show a 5% step decrease due
to the power decreasing of the pump around the column. The step
decrease will force the feed pressure to move closer to the stage
pressure where the feed stream enters. Consequently, the water
conversion of the reaction zone increases whereas the water con-
tent of the bottom product decreases as shown in Fig. 9. The test
object deviation is 0.86%, and the direction of response is direct.

3.2.1. Open-loop transient responses of sensitive variables 3.2.1.3. Effects of a step change in feed water concentration. Fig. 10
The dynamic open-loop responses for a group of step changes shows the transient response of an important manipulated vari-
are tested for some disturbances critical to the system: (1) able step change during this manufacturing process. The 5% step
feed IB rate decrease, (2) feed pressure decrease, (3) feed
water concentration increase and (4) reboiler duty decrease.
Despite that the step changes are large enough to have a sig-
nificant effect on the column operation, their magnitude do
not reach to the extent that the column stability would be
compromised. In each of the open-loop tests, the overhead pres-
sure, liquid level of reboiler and reflux rate are assumed to be
constant. The objective of dynamic open-loop responses is to
investigate the dynamic behavior of the column on the control
object including response direction, time delay, stabilization time,
etc. and to guide the tuning of PID controller. The test object is water
mass concentration of the bottom product.

3.2.1.1. Effects of a step change in IB feed rate. Under certain cir-

cumstances, the power of feed IB pump decreases, which in turn
leads to a step decrease IB feed rate. Thus, the transient response

Fig. 7. Effects of the catalyst weight (column pressure: 1 × 105 Pa; molar feed ratio Fig. 8. (a) Open-loop response to a 5% step decrease in IB feed rate. (b) Liquid
of IB to water: 1:1; feed water concentration: 5 wt%; reboiler duty: 12 kW; molar composition profiles in the column before and after a 5% step decrease in IB feed
reflux ratio: 1). rate.
 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136
Fig. 9. Open-loop response to a 5% step decrease in feed pressure.
Fig. 10. Open-loop response to a 5% step increase in feed water content.
increase in feed water content is unquenchable due to the strong
absorbency of ethanol. Without any change in other manipulated
conditions, the increase in feed water content usually causes an
increase in water content of the bottom product. Thus, the response
direction of this open-loop test is reverse. In addition, the transient
response deviation is 5.00%.
3.2.1.4. Effects of a step change in reboiler duty. The transient
response to a 5% decrease is probably caused by a sudden decrease
in the heating steam flow rate of the reboiler, as shown in Fig. 11.
There is a fast initial decrease response to the water content
of bottom product, which then disappeared as the permanent
Fig. 11. Open-loop response to a 5% step decrease in reboiler duty.
1133
Fig. 12. Dynamic model of reactive distillation.
changes are asserted. As mentioned in Section 3.1, reduction of
the reboiler duty may lead to a decrease of in the water content
of bottom product. Thus, the response direction is direct, and the
test objective deviation is 2.22%.
According to the open-loop transient response analysis, there is
no delay in all the response of any step changes in the manipulated
variables. Compared with the test object step change response devi-
ation, IB feed flow rate seems to be the most sensitive manipulated
variable. The response directions of all the manipulated variables
were obtained. The transition of all the manipulated variables lasts
for almost 400 min.
3.2.2. Close-loop PID control
3.2.2.1. Control objectives and controller configuration. As assumed
in all the open-loop tests, column pressure, liquid level of reboiler
and reflux rate were kept constant. Hereby, to achieve that assump-
tion, three PID controllers (i.e., PC1, LC2 and LC3) are used as shown
in Fig. 12. Moreover, due to the strict limited water content of bot-
tom, a controller of bottom product composition is involved. As
a result, there are four control objectives involved in this process,
which are column head pressure, liquid level of reboiler, reflux rate
and water content of the bottom. The previous three of the control
objectives are intended to keep the stability of reactive distillation
process, while the last one is to maintain the product quality.
The Ziegler–Nichol close-loop technique is one of the most
popular methods for controller’s configuration [34]. It gives an
approximate evaluation of the controller gain, integral time and
derivative time required for a one-quarter amplitude response. In
this work, the Ziegler–Nichol technique is employed for configuring
all the controllers, and the control effect is tested by close-loop tran-
sient response to step changes of several manipulated variables.
The controller settings are shown in Table 4.
3.2.2.2. Close-loop process stability test. A stochastic step change of
the column manipulated variable is employed to test the stability of
Table 4
Controller settings.
Controller Gain (%/%) Integral time (min) Derivative time (min)
PC1 20 12 0
LC2 10 10,000 0
LC3 10 10,000 0
QC4 20 12 0
1134 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136
Fig. 13. Close-loop response of head pressure controller.
Fig. 14. Close-loop response of reflux level controller.
the first three objectives. The responses of the three control objec-
tives are shown in Figs. 13–15, respectively. As shown in Fig. 13, the
dash line illustrates the set point of the controller obtained from the
optimal manipulated variables of a steady state model, the solid line
demonstrates the actual control result which is head pressure here,
and the dash dot line indicates the change in controller output. As
the step change, the column head pressure initially presents a dis-
tribution but disappears at the 350 min. The deviation distortion is
0.05%. The transition time is 350 min. Fig. 14 shows the responses
of the reflux level while the dash line shows the set point obtained
from the steady state simulation. Similarly, the solid line indicates
actual control results and the dash dot line indicates controller out-
put. The deviation distortion is 0.75% and transition time is 400 min.
Fig. 15 shows the same expression of the three lines. There is a 0.11%
of deviation distortion of the control result and 350 min of transi-
tion time. Therefore, it can be concluded that the three controllers
is capable of maintaining the stability of the process and verifying
the assumption above-mentioned.
Table 5
Close-loop test results of the PID product quality controller.
Step change variable Step change direction
Feed pressure Decrease
Reboiler duty Decrease
Feed water contraction Increase
Fig. 15. Close-loop response of reboiler level controller.
Fig. 16. Close-loop test result to a 5% step decrease in feed pressure.
3.2.2.3. Close-loop test of the PID product quality controller. The
open-loop transient response analysis suggests that the IB feed rate
is the most sensitive manipulated variable under a same percent-
age of step change. Accordingly, the water concentration is set as
the product quality controller (QC4) input, the IB feed rate is set as
its output, while the set point is obtained from the optimal result
of steady state simulation. After the configuration of gain, integral
time and derivative time of the QC4 using Ziegler–Nichol technique,
a group of close-loop transient response analysis is carried out.
Figs. 16–18 show the responses under a 5% step change of feed
pressure decrease, feed water content increase and reboiler duty
decrease, respectively. The major control result is summarized in
Table 5. The results suggest that, under different distributions, the
QC4 can decrease the transient response deviation and the devia-
tion distortion without increasing the transition time.
Simulation results with the proposed control system are com-
pared with the experimental results shown in Table 6 to validate
the simulation. It can be observed that water content in the product
in simulation is lower than that in experiment, which can meet the
blending demand with gasoline. The product quality is under good
control.
Transition Transient response Deviation
time (min) deviation (%) distortion (%)
400 0.14 0.08
400 1.11 0.84
400 0.33 0.22
 S. Lu et al. / Chemical Engineering and Processing 50 (2011) 1128–1136 1135

Acknowledgements

Financial support for this work from the National Basic Research
Program of China (973 Program, 2009CB219906), National Natural
Science Foundation of China (20976144).

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