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org/IECR Article

Numerical and Experimental Research on a Kaibel Divided-Wall

Column: Design and Steady-State and Dynamic Operation
Hui Pan, Feng Ju, Guichun He, Jigang Zhao, Hui Sun, Jichang Liu, and Hao Ling*
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ABSTRACT: This work investigated the full design, startup, operation,

and control of a Kaibel divided-wall column (KDWC) for a laboratory-
scale KDWC. The KDWC is designed to separate mixtures of methanol,
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ethanol, n-propanol, and n-butanol on the basis of a rigorous model.

Effective steady-state and dynamic operation strategies are then proposed
to control the practical operation of the KDWC. The proposed startup
operation strategy, including total reflux, batch rectification, and
continuous rectification procedures, leads to a steady state, and the
steady-state design method is verified through steady-state experiments.
The dynamic control strategy including a four-temperature control loop
is further proposed and shows effective and precise dynamic control
performance, recovering the four products to the specified values in the
presence of ±20% feed disturbances. This work provides deep insight
into the realization and control of a practical KDWC and will increase the possibility of industrial achievement and optimal operation
of the KDWC.

1. INTRODUCTION Agrawal column),8 and the Kaibel column, a four-product DWC

An n-component mixture is separated into n pure single
components by (n − 1) conventional distillation columns with
multiple condensers and reboilers. However, the multiple-
component system can be operated through a divided-wall
column (DWC) with only one condenser and reboiler, thereby
resulting in reductions in both capital cost and operation cost as
well as required space compared with conventional distillation
columns. Within approximately 30% cost reduction in capital
and operation,1,2 DWC technology has been widely applied and
achieved clear progress with regard to multicomponent
separation in the chemical industry.3−5
The lateral mixing of liquid and vapor in the central region is
prevented by the introduction of a divided wall into the
cylindrical distillation column, and additional separate feed and
outlet sections can also be incorporated. This creative method
was first proposed by Petyluk for separating ternary mixtures and
then further developed by Kaibel, Agrawal, and others.6−11 With
numerous efforts applied to the use of a DWC to separate
ternary components during recent decades,12−22 many three-
product DWCs have been implemented industrially around the
world. For instance, more than 100 DWCs23,24 are operated
industrially by the BASF of Germany. A decrease of 50% in
energy expenditure25 has been achieved with the operation of a
xylene recovery DWC in ExxonMobil. Furthermore, the
feasibility of DWCs has recently been extended to azeotropic
DWC,26−28 extractive DWC,29,30 reactive DWC,31−34 multi-
purpose DWC,35 DWCs with two partitioning walls (e.g.,
with only one partitioning wall.7
The Kaibel divided-wall column (KDWC) that separates a
four-component mixture with a single wall was first proposed in
19877 and attracted increasing academic interest until Skogestad
et al.36 numerically investigated the control of a Kaibel column
through model-predictive control (MPC) in 2010 due to its high
complexity. Obviously, larger potential benefits, including
capital and operation costs, can be gained with a KDWC than
with conventional direct and indirect distillation sequences.37,38
Furthermore, KDWC is the simplest physical structure in four-
component mixture separation DWCs. DWCs with two
partitioning walls (e.g., Agrawal column) exhibit significant
advantages in energy saving;8,10 however, their complicated
topological structures greatly restrict their development and
industrial implementation. KDWC exhibits a great potential
industrial application prospect for the separation of a four-
component mixture because of its relatively simple structure and
cost savings. Thus, great efforts have focused on the operability
and controllability of the KDWC.39−50 Strandberg et al.39
investigated the stabilizing control of a KDWC by maximizing
Received: March 7, 2020
Revised: May 12, 2020
Accepted: June 11, 2020
Published: June 11, 2020

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the product purity with fixed energy usage, and the liquid split
ratio was found to have an impact on the column’s sensitivity to
disturbances. Two operating schemes, minimizing the vapor
flow rate at fixed product purities (J = V) and maximizing the
product purities with fixed boilup rate (J = D(1 − xD) + S1(1 −
xS1) + S2(1 − xS2) + B(1 − xB)), were compared to control a
KDWC in Ghadrdan et al.’s work.38 The first operation scheme
was found to be more difficult to operate because of multiplicity
issues and a narrow operating region. They further numerically
studied the influence of vapor split manipulation for the control
of a KDWC and concluded that the KDWC may not maintain
minimum energy operation at the fixed vapor split ratio when
facing feed disturbances.40 To handle the dynamic control of the
KDWC, researchers numerically investigated the control
performance of various control structures. Qian et al.41
investigated various control schemes for the dynamic control
of a KDWC. One control structure set the temperature as a
controlled variable, and two others set the composition as a
controlled variable. The results showed that simple temperature
control structure is capable of dynamically controlling a KDWC.
Subsequently, based on temperature as a controlled variable, the
dynamic control performance of three control schemes that
considered fixed split ratios and active liquid and vapor split
ratios as manipulated variables was evaluated.42 The results
showed that better control behavior is discovered with active
liquid and vapor split ratios than with fixed liquid and vapor split
ratios. Additionally, a pressure-compensated temperature
control strategy was proposed to solve the large offset of the
lower sidestream product when facing large feed disturbances in
a KDWC.43 In addition to the traditional single-loop PID
controller used in the aforementioned literature, model-
predictive control (MPC) was also applied to KDWC control.36
Furthermore, a two-layer control structure that combines PID
and MPC and fast model-predictive control (FMPC) were
utilized for KDWC control.44 Skogestad’s group45 built a
laboratory-scale KDWC and experimentally studied its steady-
state operation. The experimental data were compared with
model values for operation under two optimal modes, which
showed that steady-state operation was close to the optimal
scenario, although the upper side and lower side products had
low purity. In addition, the dynamic behavior of the Kaibel
column when facing a +20% disturbance in feed rate was
investigated, and good performance was achieved. They further
evaluated the possibility of manipulating the vapor split ratio in
the industrial operation of a KDWC.46
The complicated configuration and practical operation of the
KDWC present a formidable combinatorial issue; thus, the
emphasis of most published work on the KDWC has been
theoretical, and the aforementioned experimental study mainly
focused on the steady-state operation of a KDWC. Unlike the
DWC, the industrial applications of the KDWC are not
widespread worldwide because of the lack of a proven and
manifest design method.51,52 Additionally, attention to the
challenging practical operation and control of the KDWC, which
is of great importance for the industrial implementation of the
KDWC, is rare and not publicly available. The purpose of this
article is to investigate the full design, startup, operation, and
control of the KDWC through the practical implementation of a
laboratory-scale KDWC. Therefore, in this work, an exper-
imental KDWC device is designed first on the basis of the
numerical results of a steady-state simulation. Then, through
steady-state experiments, the steady-state design method is
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verified. Finally, the feasibility and effectiveness of the practical
operation and control strategy of the KDWC are analyzed
through dynamic experiments.
2. STEADY-STATE SIMULATION AND DESIGN OF A
KDWC
A methanol, ethanol, n-propanol, and n-butanol (MEPB)
mixture with approximate relative volatilities of 6.98, 4.55,
2.17, and 1, respectively, is taken as a case study. The liquid
composed of equimolar components is considered for the feed.
Its flow rate is set to 4.0 kg/h at 356 K. In addition, the product
purities of the four components are set to 90 mol %. The column
is operated at atmospheric pressure. The “virtual four-column”
model is simulated rigorously with the Wilson thermodynamic
model through the RADFRAC modules in ASPEN PLUS (see
Figure 1). The minimum of total annual cost (TAC) is achieved
Figure 1. “Virtual four-column” model of the KDWC.
through the optimization of the steady-state simulations. The
optimization procedure53 is presented in the Supporting
Information, and the final optimal KDWC data are listed in
Table 1.
Figure 2 reveals composition profiles of the liquid phase in the
KDWC. Obviously, the withdrawals of ethanol on stage 17 and
n-propanol on stage 27 occur as their compositions reach the
maximum values in the main column. Furthermore, the mole
fraction of ethanol at the lower end of the partition wall is
approaching zero, which ensures that few ethanol go over the
partition wall to affect the purity of n-propanol in the lower
sidestream. Similarly, the mole fraction of n-propanol at the top
of the partition wall is approaching zero, which ensures that few
n-propanol go over the partition wall to affect the purity of
ethanol in the upper sidestream. The remixing of ethanol and n-
propanol can be discovered in the prefractionator. In a three-
component DWC, the remixing of the intermediate is avoidable
due to the detouring route of the intermediate.37 However, the
detouring route cannot be obtained for every single intermediate
(ethanol and n-propanol) because the sharp split of ME/PB is
performed in the prefractionator.
The experimental KDWC is designed with a height of 6.41 m
packing with 6 mm × 6 mm θ rings through the steady-state
numerical simulation. The internal diameters of the prefractio-
nator, rectifying, stripping, and sidestream sections are 70, 90,
90, and 60 mm, respectively (see Figure 3a). The whole KDWC
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Table 1. Final Optimal KDWC Data human−computer interaction interface is realized with the help
of the Windows Control Center (WinCC). Figure 4 illustrates
descriptions values
the main interface of the KDWC through WinCC in the
stage number in prefractionator C11 24 experimental test, which includes six buttons. As observed in this
stage number in stripping section C23 7 figure, in addition to the “Exit” button, “Press” can be used to
stage number in rectifying section C21 8 refresh the current process interface. “Trend”, “Table”, “Alarm”,
stage number in side section C22 24 and “Tune” can switch to online variable monitoring, online
vapor split ratio βVa 0.600 variable recording, PID parameter tuning, and warning
liquid split ratio βLa 0.343 interfaces, respectively. The middle of the interface shows the
reflux ratio 5.33 main process area of the experimental KDWC, including the
reboiler heating required, kW 3.09 condenser, reboiler, feed tank, product tank, pipelines, and
condenser cooling required, kW 3.00 temperature, pressure, and flow rate readings.
boilup ratio 5.45
flow rate of feed (stage 20), kmol/h 0.18 3. STEADY-STATE OPERATION STRATEGY
feed composition, mol % M/E/P/B = 25/25/25/25
flow rate of distillate stream, kmol/h 0.0477
3.1. Verification of the Vapor Split Ratio. The vapor split
distillate composition, mol % M/E = 90/10
ratio is affected by the liquid−vapor distribution and pressure
flow rate of upper sidestream S1 (stage 17), 0.0421
drop during the operation. The vapor split ratio can be adjusted
kmol/h through the valve in our setup but is kept constant to facilitate
S1 composition, mol % M/E/P = 4.96/90/5.04 control of the system in the experiments. Because the
flow rate of lower sidestream S2 (stage 27), 0.0423 intercepting device located at the feed and discharge positions
kmol/h affects the gas and liquid flow behavior in the column, there may
S2 composition, mol % E/P/B = 5.47/90/4.53 be deviation between the actual vapor ratio and the simulation
flow rate of bottom stream, kmol/h 0.0479 result. Hence, the vapor split ratio must be verified before the
bottom composition, mol % P/B = 10/90 operation of the experimental KDWC.
a
The vapor split ratio (βV) is defined as the fraction of the vapor fed The verification of the vapor split ratio is achieved through the
to the prefractionator to the total vapor leaving the top tray in the total reflux operation of the experimental KDWC. During the
stripping section, and the liquid split ratio (βL) is defined as the total reflux operation, as the value of the vapor split ratio equals
fraction of the liquid fed to the prefractionator to the total liquid the liquid split ratio, the prefractionator and the sidestream
leaving the bottom tray in the rectifying section.
sections have the same liquid−vapor ratio ( L ) and theoretical
V
stages, resulting in the same temperature distribution for these
has 15 temperature sensors, of which 5 temperature sensors are two sections. Hence, in practical total reflux operation, the liquid
located at the prefractionator, and 10 temperature sensors are split ratio is adjusted until the prefractionator and the sidestream
located at the main column (see Figure 3b). The raw material is sections have the same temperature distribution. The liquid and
preheated by the feed heater and fed into the prefractionator vapor split ratios have the same value. Figure 5 illustrates the
section. The total condenser is installed on the column top measured temperature in the prefractionator and the sidestream
through water cooling, part of the liquid reflux becomes the top sections with various liquid split ratios in the total reflux
product, and the rest returns into the tower. The kettle-type operation. The vapor split ratio is in the range of 0.600−0.667,
reboiler has a 12 L capacity, and the input voltage is utilized to and equal temperature can be achieved when the vapor split ratio
adjust its heating power. The manipulation of the liquid flow is approximately 0.63.
time between the prefractionator and the main column controls 3.2. Steady-State Operation. As mentioned, the KDWC is
the liquid split ratio. The withdrawal of sidestream products, operated under atmospheric pressure. The feed is composed of
including ethanol and n-propanol, into a liquor-collecting equimolar components, namely, methanol, ethanol, n-propanol,
container is achieved through a peristaltic pump. Figure 3c and n-butanol, at 356 K within a 4.0 kg/h flow rate. In addition,
shows a solid view of the experimental KDWC. the analyses of the component purities are accomplished with a
In the control setup, to achieve stable control of the KDWC, SHIMADZU gas chromatograph (GC1120) equipped with a
the experimental device uses SIMATIC s7-300 to monitor the flame ionization detector. The separation was conducted with a
data at each measurement point. The PLC logic control program capillary column PEG-20M 30 m × 0.32 mm × 0.5 mm under
is written in Step 7, and the configuration of the upper computer 343.15 K. The injector and detector temperatures were 433.15

Figure 2. Liquid composition profiles in the KDWC: (a) methanol and ethanol; (b) n-propanol and n-butanol.

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Figure 3. Designed laboratory-scale KDWC: (a) design drawing of the KDWC; (b) location of the temperature sensors; (c) solid view of the
experimental KDWC.

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Figure 4. Main operation interface of the KDWC.
Figure 5. Measured temperature in the prefractionator and the sidestream sections with various liquid split ratios in the total reflux operation: (a) βL =
0.400, (b) βL = 0.500, (c) βL = 0.600, (d) βL = 0.667, and (e) βL = 0.714.
and 473.15 K, respectively. The injection volume was 1 μL. In
steady-state operation, three main procedures, total reflux, batch
rectification, and continuous rectification, are performed to
ensure stable operation of the KDWC. First, the vapor−liquid
phase circulation in the whole column needs to be established
through the total reflux procedure. The batch rectification
procedure starts after the column is heated to form a liquor
condenser in the total reflux procedure. The excessive light
component accumulated in the column during the total reflux
procedure can be removed in the batch rectification procedure.
In this period, the distillate product withdrawal is initially
controlled manually until the purity of the distillate product
reaches 90 mol %. Similarly, the upper sidestream product is
withdrawn until the upper sidestream product purity reaches the
designed value. Then, the lower sidestream product withdrawal
is controlled manually, and the n-butanol purity is analyzed. The
withdrawal of the lower sidestream product is stopped if the
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purity achieves the set value. Subsequently, the feed mixtures are
fed into the KDWC, and the steady-state operation enters the
continuous rectification procedure. To decrease the large
temperature disturbance caused by the feed inlet, the feed
capacity can be raised gradually to the required feed amount. In
the continuous rectification procedure, the withdrawal of
distillate, upper sidestream, and lower sidestream products are
opened simultaneously and controlled manually to ensure the
purity of the MEPB. During these three procedures, the four
product purities are analyzed through the SHIMADZU gas
chromatograph (GC1120) every 13 min. The instantaneous
mole fractions of the four products for the three procedures are
shown in Figure 6.
The period from 0 to 1.5 h includes the total reflux and batch
rectification procedures. At the batch rectification procedure,
the light component is gradually removed from the KDWC, and
the heavy component in the bottom region of the column rises
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Figure 7. Comparison of steady-state numerical results and steady-state

Figure 6. Instantaneous mole fractions of the four products for the
three procedures.
gradually to the upper region. Therefore, at the top of the
column, the mole fraction of ethanol gradually increases while
the purity of methanol decreases to the designed value.
Similarity, in the upper sidestream, the purity of the ethanol
first increases because of the decrease of the mole fraction of
methanol and then decreases to the designed value because of
the increase of the mole fraction of n-propanol. Additionally, the
n-propanol purity in the lower sidestream shows a rising trend
due to the gradual decrease of the mole fraction of ethanol. In
the bottom region, the purity of n-butanol increases due to the
decrease of the mole fraction of n-propanol. The continuous
rectification procedure occurs from 1.5 to 3.5 h. It is obvious that
the purities of the four components remain at approximately 90
mol %, although the mole fraction of n-propanol fluctuates
slightly, indicating that the steady-state operation strategy is
efficient and leads to a stable state. We further compare the
steady-state simulation results with the experimental data to
evaluate the validity of the steady-state design model in terms of
the product purities and temperature profiles. The product
purities for the steady-state experimental data with the modeling
results are compared in Table 2. Obviously, the content of the
impurities in the sidestreams varies slightly between the
modeling and experimental results. However, the simulated
mole fractions of M, E, P and B in the top, upper sidestream,
lower sidestream, and bottom stream, respectively, agree well
with the experimental results. Figure 7 displays the temperature
profiles of the main column and prefractionator predicted by the
model with the experimental results. As shown in the figure, for
the prefractionator, a larger temperature difference between the
simulation and experimental results is observed in the bottom
region than in the top region, mainly because of the enrichment
of n-butanol in the bottom of the prefractionator section rather
than in the stripping section in the model. As shown in Table 2,
the modeled content of n-butanol in the lower sidestream is
higher than the experimental value. Similarly, the mole fraction
of n-propanol in the upper sidestream and n-butanol in the lower
sidestream predicted by the model are higher than the
experimental values (see Table 2); thus, the predicted
experimental data on column temperature.
temperature is slightly higher than the measured temperature
in Figure 7. The difference in the content of the impurities leads
to a slight difference in the temperature distribution between the
model and experimental results, but nevertheless, the simulated
temperature distribution for the main column and prefractio-
nator is in good agreement with the experimental data.
4. DYNAMIC CONTROL OPERATION STRATEGY
4.1. PID Parameter Tuning. A four-temperature control
structure based on the conventional proportional-integrator
(PI) controller that can be easily implemented in industry is
used for the dynamic control of the KDWC in this work (see
Table 3). The quick and accurate responses of the temperature
Table 3. Dynamic Control Structure and the Corresponding
Tuning Parameters
control loop controlled variable manipulated variable gain (%) TI (s)
TC1 TM1 D 150 60
TC2 TM6 S1 65 10
TC3 TM10 S2 280 100
TC4 TP5 QR 30 540
control loops for manipulating variables according to the
measured control variables are the key to ensuring the dynamic
control performance of the KDWC, which, however, is greatly
affected by the PID tuning parameter. In this work, the PID
parameters of the four control loops are first tuned manually in
the experiments, and the PID parameter tuning processes of the
temperature control loop for the prefractionator are demon-
strated in Figure 8. We first introduce a feed disturbance into the
steady-state system of the KDWC and adjust the temperature
setting value (TSV) of the reference stage in the prefractionator
from 367 to 366.5 K. The step change in the temperature setting
point changes the temperature current value (TCV) of the
reference stage due to the influence of the control loop. As
shown in the figure, the transient oscillations and offset of the
TCV initially decrease and then increase with increasing gain
value and constant integral time (TI), and thereby the optimal

Table 2. Comparison of Steady-State Experimental and Simulated Compositions

D S1 S2 B
component feed exp. sim. exp. sim. exp. sim. exp. sim.
methanol (mol %) 25.0 90.68 90.68 7.10 5.27 0 0 0 0
ethanol (mol %) 25.0 9.32 9.32 89.91 89.95 8.75 4.08 0 0
n-propanol (mol %) 25.0 0 0 2.99 4.78 90.55 90.67 9.91 9.87
n-butanol (mol %) 25.0 0 0 0 0 0.69 5.25 90.09 90.13

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Figure 8. PID parameter tuning processes of the temperature control

loop for the prefractionator.

gain value is determined to be 540. Subsequently, the TI value is

tuned downward while maintaining the optimized gain value to
reduce the oscillating amplitude and change cycle of the TCV.
Obviously, the oscillation amplitude of the TCV decreases
gradually with decreasing TI value. Furthermore, the TCV
gradually returns to the temperature set point as the TI value
decreases to 30, which indicates the elimination of the steady-
state error of the system. Similarly, the gain value and TI for the
other three control loops are tuned through the same method.
The corresponding tuning parameters within the dynamic
control structure in this work are summarized in Table 3.
4.2. Dynamic Operation. The dynamic control perform-
ance of the experimental KDWC is evaluated by introducing
±20% feed composition disturbances for the four components.
Specifically, the feed mole fraction for one of the components is
increased or decreased by 20%, while the mole fractions of the
other three components are changed equidistantly to ensure a
constant sum of the mole fractions of the four components. To
introduce the disturbed feed into the system, the control loops Figure 9. Dynamic responses for ±20% changes in feed composition:
for the KDWC are changed from auto to manual mode. The (a1) +20% methanol composition disturbance, (a2) −20% methanol
composition disturbance, (b1) +20% ethanol composition disturbance,
control loops are returned to auto mode after feeding is
(b2) −20% ethanol composition disturbance, (c1) +20% n-propanol
complete. Notably, the auto mode of the control loops for the composition disturbance, (c2) −20% n-propanol composition
KDWC is turned on after the steady-state operation described disturbance, (d1) +20% n-butanol composition disturbance, and (d2)
above. Every 15 min the four product purities are analyzed until −20% n-butanol composition disturbance.
new stabilization has been achieved after feed composition
disturbances are introduced into the KDWC.
Figures 9a, 9b, 9c, and 9d show the dynamic responses to temperature control loop for the lower sidestream shows
±20% changes in the feed composition for M, E, P, and B, weakened control of the purity of P.
respectively. The results clearly illustrate that this four- 4.3. Dynamic Simulation. A dynamic control model in
temperature control structure provides stable regulatory control ASPEN DYNAMICAS is further proposed based on the four-
for the separation of the four components. Additionally, all temperature control loops used in the experiments. In the four-
products return nearly to their specified values within temperate control structure, the manipulation of the distillate
approximately 1−3 h. The product purities range between product flow (D), upper sidestream flow rate (S1), lower
0.8817 and 0.9399 during the dynamic operation, indicating that sidestream flow rate (S2), and reboiler duty (QR) are applied to
the deviations of the product purity are all less than 0.5%, which control the temperature of the reference stages from the
shows that the four-temperature control structure is capable of rectifying section (stage 2 in the main column), the upper region
handling feed disturbances. Furthermore, the largest purity of the sidestream section (stage 21 in the main column), the
deviation is observed in the lower sidestream product P lower region of the sidestream section (stage 39 in the main
(approximately a 4.43% offset), and the control of P purity column), and the prefractionator stage 30 in the prefractiona-
exhibits greater difficulty because stronger transient oscillations tor), respectively. The tuning parameters of the PID controller
and larger offsets are discovered with larger settling times. This for the four temperature control loops are listed in Table 2.
pattern arises because the pressure also has a non-negligible Figure 10a and 10b display the dynamic control model and the
influence on the component composition in the lower region of scheme of four temperature control loops for the KDWC,
the column.53 Specifically, the composition of the lower respectively. Model verification is achieved by comparing the
sidestream product is affected by both temperature and pressure simulated and experimental temperature profiles when facing
rather than only temperature as the pressure changes feed disturbances. Figure 11 compares the simulated and
substantially in the column lower region. Therefore, the only experimental axial temperature distributions facing ±20%
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Figure 10. Dynamic control model for the KDWC: (a) the “virtual four-column” dynamic model; (b) the dynamic control structure.
Figure 11. Comparisons of the axial temperature distributions as facing
±20% disturbances in feed composition between the dynamic model
results and dynamic experimental data: (a1) +20% methanol
composition disturbance, (a2) −20% methanol composition disturb-
ance, (b1) +20% ethanol composition disturbance, (b2) −20% ethanol
composition disturbance, (c1) +20% n-propanol composition dis-
turbance, (c2) −20% n-propanol composition disturbance, (d1) +20%
n-butanol composition disturbance, and (d2) −20% n-butanol
composition disturbance.
disturbances in the feed composition of M, E, P, and B. It is
worth noting that the measured experimental temperature
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profiles are collected as the distillation system reaches
stabilization again after the disturbed feed is introduced. The
x-axis in Figure 11 presents the theoretical stages in the model,
numbered from top (1) to bottom (39). The numerical axial
temperature is in positive agreement with the temperature
measured experimentally through temperature sensors,
although some temperature differences are discovered in the
lower region of the prefractionator. The numerical data in the
lower region of the prefractionator with a −20% E composition
change are clearly higher than the experimental values in Figure
11b2, which results from the predicted content from the
simulation exceeding the experimental value (see Table S3 in the
Supporting Information). Similarly, in Figure 11c1, the
temperature predicted by the dynamic model is slightly higher
than the experimental value in the lower region of the
prefractionator, possibly because the predicted mole fraction
of n-butanol in this region is higher than the actual value.
Notably, the experimental impurity in the lower sidestream is
0.68 mol %, while the predicted value is 5.40 mol % (see Table
S4 in the Supporting Information). Thus, in the lower region of
the prefractionator, the predicted n-butanol content is higher
than the experimental value, thereby resulting in a higher
predicted temperature. In summary, the dynamic temperature
control model in ASPEN DYNAMICS closely matches the
experimental data, which suggests that the proposed dynamic
model is useful for studying the dynamic operation and design of
the Kaibel column.
5. CONCLUSIONS
The complex configurations and operation strategy of the
KDWC greatly restrict its wide industrial application compared
with the DWC. In this work, a laboratory-scale KDWC is
designed based on a rigorous steady-state model to separate a
four-component mixture. The practical control of the KDWC is
then conducted through the proposed steady-state and dynamic
operation strategies. Furthermore, a proposed dynamic control
model based on the dynamic control loops utilized in the
experiments is verified. The numerical and experimental
research on the laboratory-scale KDWC reveals that
(1) The steady-state of the KDWC that provides good quality
products can be achieved through total reflux, batch
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Industrial & Engineering Chemistry Research
rectification, and continuous rectification of these three
procedures. Meanwhile, the steady-state model results
closely match the steady-state experimental data, which
further verifies the effectiveness of the design method.
(2) For the practical control of the KDWC based on a single-
loop (decentralized) PI controller, the PID tuning
parameter is crucial and greatly influences the dynamic
control performance. It is suggested to be tuned manually
in the experiments to maintain the effectiveness of the
proposed dynamic control strategy.
(3) The single four-temperature dynamic control structure
provides effective and precise dynamic control perform-
ance when facing larger ±20% feed disturbances that four
products recover to the specified values. Furthermore, a
dynamic model is proposed and verified by comparing the
simulated and experimental temperature profiles, which
suggests that the proposed dynamic model is useful for
studying the dynamic operation and design of the Kaibel
column.
In conclusion, this work comprehensively investigated the
KDWC numerically and experimentally and illustrates that the
preliminary design method is the basis and the control strategies
including steady-state and dynamic ones are the key for the
implementation of the KDWC. Additionally, if a single-loop
(decentralized) PI controller is applied, the PID parameter is
suggested to be tuned manually. Furthermore, good dynamic
control performance can be achieved without a component
control scheme. The full design, startup, operation, and control
of the KDWC through the practical realization of a laboratory-
scale KDWC is demonstrated in this work, and the results will
promote the realization and control of a practical KDWC.
Although simple temperature control structure is widely used
due to its great industrial prospect, it may lead to a steady-state
deviation54 for the control of DWCs. More advanced temper-
ature control structures were proposed and studied for the
dynamic control of DWCs (e.g., asymmetrical temperature
control, double temperature difference control, and pressure-
compensated temperature control structures),21,22,43 and the
application of these advanced temperature control schemes to
handle the industrial control of the KDWC need to be further
studied in the future due to more complex issues, like pressure
disturbance in the column, impurity sources, and higher control
requirement.
■
ASSOCIATED CONTENT
*
sı Supporting Information
The Supporting Information is available free of charge at
https://pubs.acs.org/doi/10.1021/acs.iecr.0c01168.
Optimization procedure of the KDWC and the
comparisons of dynamic experimental data and model
results of products composition as facing ±20% feed
composition disturbances (PDF)
■ AUTHOR INFORMATION
Corresponding Author
Hao Ling − State Key Laboratory of Chemical Engineering, School
of Chemical Engineering, East China University of Science and
Technology, Shanghai 200237, P. R. China; Phone: +86-21-
64252328; Email: linghao@ecust.edu.cn; Fax: +86-21-
64252160
I https://dx.doi.org/10.1021/acs.iecr.0c01168
pubs.acs.org/IECR Article
Authors
Hui Pan − State Key Laboratory of Chemical Engineering, School
of Chemical Engineering, East China University of Science and
Technology, Shanghai 200237, P. R. China; orcid.org/0000-
0002-5643-6546
Feng Ju − State Key Laboratory of Chemical Engineering, School of
Chemical Engineering, East China University of Science and
Technology, Shanghai 200237, P. R. China
Guichun He − State Key Laboratory of Chemical Engineering,
School of Chemical Engineering, East China University of Science
and Technology, Shanghai 200237, P. R. China
Jigang Zhao − State Key Laboratory of Chemical Engineering,
School of Chemical Engineering, East China University of Science
and Technology, Shanghai 200237, P. R. China; orcid.org/
0000-0002-2773-7200
Hui Sun − State Key Laboratory of Chemical Engineering, School
of Chemical Engineering, East China University of Science and
Technology, Shanghai 200237, P. R. China; orcid.org/0000-
0002-8544-756X
Jichang Liu − State Key Laboratory of Chemical Engineering,
School of Chemical Engineering, East China University of Science
and Technology, Shanghai 200237, P. R. China; orcid.org/
0000-0002-5295-1778
Complete contact information is available at:
https://pubs.acs.org/10.1021/acs.iecr.0c01168
Notes
The authors declare no competing financial interest.
■ ACKNOWLEDGMENTS
The authors thank the National Natural Science Foundation of
China (No. 21908056) and the Shanghai Sailing Program (No.
19YF1410800) for supporting this work.
■ NOTATION
B bottom stream
D distillate stream
gain gain value of the controller
L liquid flow rate
J cost function
QR reboiler duty, kW
R reflux ratio
S1 upper sidestream
S2 lower sidestream
T temperature
TM,i temperature of stage i in the main column
TMi the ith temperature point in the main column, i = 1, 2, 3, 4,
5, 6, 7, 8, 9, and 10
TPi the ith temperature point in the prefractionator,i = 1, 2, 3,
4, and 5
TP,i temperature of stage i in the prefractionator
TI integral time, s
V vapor flow rate
xB product purity in the distillate stream
xD product purity in the bottom stream
xS1 product purity in upper sidestream
xS2 product purity in lower sidestream
Greek Symbols
βL liquid split ratio
βV vapor split ratio
Subscripts
mai main column
Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
Industrial & Engineering Chemistry Research
pre prefractionator
■
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K https://dx.doi.org/10.1021/acs.iecr.0c01168
Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX