Science and Technology for Energy Transition 77, 2 (2022)

Ó The Author(s), published by EDP Sciences, 2022

https://doi.org/10.2516/stet/2021002

Available online at:

stet-review.org

REGULAR ARTICLE

Constant distillate composition of batch distillation column with

variable reflux mode based on still pot concentration
Naseer A. Alhaboubi*

Chemical Engineering Dept., Al-Nahrain University, Baghdad 10071, Iraq

Received: 27 April 2021 / Accepted: 20 December 2021

Abstract. The objective of this work is to control the constant distillate composition of batch distillation
column xD. A new correlation developed involved the instant reflux ratio value R with a composition of the
remaining mixture in the bottom pot (boiler) xB. Also adding the dynamic time as ahead time (+dt) to the
control algorithm to increase the R to anticipate the changes in xD. +dt was calculated using an electroconduc-
tive tracer that was injected both in the bottom pot and in the top tray to estimate the upward and the down-
ward dynamic time. The proposed correlation was successfully applied as a control strategy on a glass batch
distillation pilot plant that has 5 cm diameter, 1 m long, eight sieve trays, and Methanol–Water mixture as
a system. The real-time experimental runs of the suggested control algorithm applied by manipulating the
reflux stream that affects the changes that happened in the top composition product to keep it constant.
The proposed procedure shows a quick and stable response for distillate product composition during the oper-
ating time that minimizes and saves the energy supplied to the boiler. Moreover, the system gives a straight,
smooth linear constant distillate product even in case of disturbing the system.

1 Introduction allows for handling different feed compositions and product

specifications; Also, a wide range of different mixtures can
Batch Distillation (BD) is one of the oldest separation be separated using the same batch column. This is a big
units, historical development from the first applications advantage with the ever-changing product specification
more than 5000 years ago in Mesopotamia (today is known requirements in the market today. Moreover, BD often
as Iraq) [1]. BD is one of the most important unit operations means a simpler process and lower capital cost than contin-
and the most widely used separation process in industrial uous distillation [5].
separation chemicals used in small-scale production. BD is In BD, the researcher’s concern for the last decades
preferred to continuous distillation where small quantities about: the design of alternative and suitable column config-
of high-tech and high value-added chemicals and biochem- urations, the development of mathematical models, the
icals can be separated. The batch unit requires less capital formulation and solution of dynamic optimization problems
to separate relatively pure components. The most notable for optimal design, control, and operation [6].
feature of BD is its versatility, so distillation is widely used The use of BD despite the industry’s competitiveness
in the pharmaceutical industry to purify and recover high- has increased over the past years, which makes the interest
value liquid components. It has better operational flexibility in process modelling and the use of this model to optimize
as well as reduces equipment costs when compared to con- and reduce energy requirements (which means, in practice,
tinuous distillation [2, 3]. minimizing production time) and product loss, and always
Generally, the distillation column is operated normally maintaining High purity requirements [7].
either in continuous or batch mode. The column is operated It is this flexibility and the inherent unsteady nature of
by the continuous method in a steady state after the start- the process which pose challenging design and operation
up period until it is closed. On the other hand, in batch problems. There are two methods of operating BD columns:
mode, the column states change continuously over time variable reflux and constant reflux, resulting in constant
resulting in non-linear and non-stationary [4]. product composition and variable product composition at
Also, the advantage of BD has of being much more flex- distillate of the key component, respectively (Bogart [8] pre-
ible than continuous distillation, as it has more degrees of sented the first analysis of the variable reflux for a binary
freedom (e.g., temperature, flow rate, pressure). Flexibility system).
* Corresponding author: [email protected]

This is an Open Access article distributed under the terms of the Creative Commons Attribution License (https://creativecommons.org/licenses/by/4.0),
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2 The Author(s): Science and Technology for Energy Transition 77, 2 (2022)

Diwekar and Madhavan [6] added a third operating mode Concerning the extended Kalman Filter (KF) algorithm,
to the BD, in addition to the previous two modes (fixed reflux this nonlinear observer configuration is known as Extended
rate with variable distillate composition, and variable reflux Luenberger Observer (ELO) for control to achieve a con-
rate with fixed distillate composition) which is an optimal stant concentration of the distillate for the BD. Also
reflux rate with an optimal distillate composition. Defined showed a benefit of the methodology using a regular propor-
the last operating mode like the one leading to the most prof- tional plus integral controller. In any case, they detailed
itable operation. Compared with other traditional operating that the ELO exactness was likely to degrade if the tray
modes, their optimal reflux rate was also a policy of increas- hydraulic was taken into account, and the observer was
ing reflux policy led to the shortest batch time. considered. The utilization of a stochastic estimator like a
Sørensen [9] studied the cyclic operation and its useful Kalman Filter (KF) was suggested when a lot of noise
execution in BD. It comprises of an alternation of three was expected [4].
assignments: a reflux drum filling arranged underneath the Li et al. [16] considered the ordinary BD and center ves-
condenser, complete distillate evacuation into a tank, and sel BD by modified variable and constant reflux operations
total reflux from the reflux drum with differing hold-up. in the traditional BD. For two control strategies one of
Also, built up a heuristic equation utilizing the which was mentioned the composition control strategy with
gPROMS software for tracking down the total number of an adjusted level-set point, and the other was mentioned
cycles to contemplate the cyclic working policy for a BD the flowrate-restricting control strategy. Subsequently, the
column arrangement. It was tracked down that a cyclic center vessel BD had the option at the same time to sepa-
policy could altogether decrease the all-out working time rate the parts of the ternary mixture. Contrasting the
for mixtures with a low measure of light key components. two control strategies showed that the flowrate-restricting
But, more clear rules for different mixtures were hard to control strategy was superior to the composition control
form, because the investigation relies upon the mixture, of strategy with an adjusted level-set point regarding their
the column number of trays and the purity of distillate applicability. Also, Li et al. in 2019 [17] designed double col-
and recovery specifications. umn batch column to separate ternary azeotropes system
Peng et al. [10] applied Sørensen’s system focusing “tetrahydrofuran, methanol, water” to separate such distil-
on the reflux drum hold-up and the plate hold-up dynamics late mixtures based on the residue curve maps.
during the operating time. The researcher showed by All above observations show the control distillate with a
simulation and experiments what these hold-up dynamics constant composition is very challenging even for a binary
affecting on optimal product composition for a given mixture system due to continuous changes over time results
number of cycles. Prior, Sørensen and Skogestad [11] pro- in high nonlinearity and non-stationary for distillate pro-
posed an optimal reflux strategy dependent on cycles and duct xD. The present study, we suggest to adopted relation
saw that the number of cycles increases as the batch time for the reflux ratio at specific time related within bottom
decline. concentration in the pot xB based on material balance, mod-
Stojkovic et al. [12] examined the distillate optimal con- ified by using a new control methodology considering BD
trol issue of BD for the non-ideal binary zeotropic systems. dynamics time. The dynamic time is the sum of the time
The describe equation depends on full column dynamics for vapor flow toward the top tray and the time for con-
and manipulating the distillate flow rate to be used as a densed liquid flow gotten back from the top tray to the boi-
control variable rather than the reflux, where the purity ler (pot). The modified relation considers the delay time to
of distillate composition is taken as another state variable. anticipate quick and stabilize the response of overhead con-
Noda et al. [13] examined the optimal working strategy, centration despite the decreasing bottom concentration
which limits the energy utilization in complete reflux with time. To calculate this time, we use electroconductive
neglecting both hold-up dynamics and constant vapor flow tracer (KCl) injected the bottom pot and the top tray.
rate. The researcher showed that the maximum perfor- The modified relation implemented with controller
mance was accomplished by optimizing the reflux flow timing loop using LabView on BD column by manipulating
rate, subsequently changing the reboiler and reflux drum solenoid valve (controls the reflux rate) gives pre timing
hold-ups with time. In a composition control, most early during the operation to maintain control of the distillate
researchers studied the implementation of a controller composition with quick response. And overcome the delay
incorporated with an assortment of a state estimator in time that occurs for the relation involves both compositions
which compositions in all column plates were measured. of the reboiler and reflux rate to keep constant distillate
In 1998, Barolo and Berto [14] proposed a control tech- composition along operating time. A modified relation with
nique dependent on modified Nonlinear Internal Model dynamic time control gives a good result, as compared with-
Control (NIMC) structure combined with an Extended out adding the dynamic as pre-time (+dt).
Luenberger Observer (ELO) is utilized for nonlinear
Single-Input Single-Output (SISO) systems. The state
transformation relation with the nonlinear observer sanc- 2 Theoretical work
tioned structure was created by Zeitz, in 1987 [15].
It can be using the eigenvalue operator to dimension a The steps involved in the calculation procedure keep the
nonlinear observer without solving the nonlinear partial dif- product concentration constant with Variable Reflux Mode
ferential equations for the transformation if the transformed for a binary system. We suggest the following equations
nonlinearities are linearized about the reconstructed state. from Bauerle and Sandall [18] relying upon the mathemat-
 The Author(s): Science and Technology for Energy Transition 77, 2 (2022) 3

ical model of the reflux strategy need to use as a control

variable (R).
Overall mole balance for the BD system in equation (1):
dB ¼ dD: ð1Þ

A material balance for the light component

dðx B B Þ ¼ x D dD: ð2Þ

Combining equations (1) and (2) results in

dB=B ¼ ðdx B Þ=ðx D  x B Þ: ð3Þ

Equation (3) may be integrated between the initial

charge conditions, x B1 and B1 and some later conditions,
x B2 and B2.

dB=B ¼ ðdx B Þ=ðx D  x B Þ: ð4Þ Fig. 1. Vapor–liquid equilibrium for a methanol–water system
with the adapted operating line at constant concentration 0.9.
Equation (4) relates the total moles in the still at any time,
B2, to the mole fraction of the light component in the still
(boiler), x B2 . This is the basic design equation that describes Solve equation (7) and equation (10) gives equation (11)
the separation that the column can achieve. For the con- which represent reflux effect on top and bottom concentra-
stant distillate composition mode of operation, xD is con- tions with the time of the separation process. The instanta-
stant and equation (4) can readily be integrated. neous value of xD as a function of xB [18]:
A differential balance around the condenser leads to
½ðR þ 1Þax B  Rx B  Rx 2B ða  1Þ
xD ¼ : ð11Þ
dV ¼ dL þ dD ð5Þ ½1 þ x B ða  1Þ

rearranged In solving equation (11) for average relative volatility a

(methanol–water 4.02) and a constant distillate composi-
dV ¼ dD=ðð1  dL=dV ÞÞ; ð6Þ tion (xD = 0.9) to find the relationship of instantaneous
value xB as a function reflux ratio for a constant distillate
where dL/dV is the instantaneous slope of the operating
composition mode operation as shown in Table 1.
line Figure 1, which may be related to the external reflux
ratio.
A differential balance around the condenser leads to
Table 1. Value of the reflux ratio at a specific time that
keeps the distillate concentration constant at 0.90.
dL=dV ¼ R=ððR þ 1ÞÞ: ð7Þ
Methanol conc. in the pot (xB) Reflux ratio
For the constant distillate composition mode of operation,
the material balance relation, equation (4), may be inte- 0.5 0.333
grated directly to give: 0.45 0.424
0.4 0.53
B 2 ðx D  x B1 Þ 0.35 0.662
¼ ; ð8Þ
B 1 ðx D  x B2 Þ 0.3 0.81
0.25 1.022
Z v
0.2 1.33
V ¼ f ðx ÞdV
0 0.18 1.5
Z x w2
dx B 0.16 1.716
¼ B 1 ðx D  x B 1 Þ : ð9Þ 0.14 2
x w1 ððx D  x B Þ2 ð1  dL=dV ÞÞ
0.12 2.35
To integrate equation (9) for the vapor requirement it is 0.1 2.85
necessary to relate the instantaneous slope of the operating 0.08 3.6
line, dL/dV, to the mole fraction in the still, xB.
0.07 4.14
Substitution of relative volatility results in
0.06 4.86
dL ðx D  x D x B ða  1Þ  ax B Þ 0.05 5.86
¼ : ð10Þ 0.04 7.36
dV ðx D  x B Þð1 þ x B ða  1ÞÞ
4 The Author(s): Science and Technology for Energy Transition 77, 2 (2022)

3. At this point, the expected bottom concentration xB

could be determined by fitting 8 trays between the
operating line and the equilibrium line.
4. Meanwhile finding the minimum reflux Rmin
(R = 2.0 Rmin) required to achieve the distillate com-
position as shown in Figure 1.

The proposed correlation of xB and R considering the

calculated dynamic time +dt to increase the response for
xD at the desired constant mode. To build a typical predic-
tive control for a distillation column for a fast, stable, and
constant distillate composition technique is by finding the
time required to make changes in the reflux rate to antici-
Fig. 2. Theoretical minimum reflux ratios vs. still pot concen- pate the concentration drop in the bottom vessel (pot).
tration xB are required for a constant distillate composition of In other words, when reading the xB the controller must
90% methanol. change R to keep the system run with a constant xD. There-
fore, there is a time required to make it happen for the
response of change to make it happen for the vapor to rise
Making correlation xB with R from data taken for each from the bottom vessel through the trays to the final desti-
case using the following procedure draw the equilibrium line nation in the condenser (t1). Also, the downtime required to
for the system (methanol–water) and locating the desire return back to the vessel by the reflux flow (t2).
concentration of distillate (dome concentration). These periods (t1, t2) were estimated by using a tracer
For a BD, an increase of the reflux ratio R is to accom- dose of KCl solution (10 gm/L) that was injected both into
plish the desired distillate quality. So, it can obtain the rela- the bottom pot and the top tray with reflux. The tracer dis-
tionship between the instant reflux ratio R and the tribution across the column was monitored by conductivity
corresponding composition of the remaining liquid in the measurement. Taken time for the column used in this study
pot xB keeping XD constant. Figure 2 shows the results from was t1 7.21 min and for t2 5.4 min as shown in Figures 3a
mathematical simulations concerning the present study and 3b, the total time t1 + t2 represents the dynamic time
relation of R with xB give a regression equation (12). (+dt) that is considered to predict the varying in reflux
ratio based on the composition of pot at the specific control
R ¼ 0:1837  1:178x B : ð12Þ time.
From all above, a mathematical model based on mole
balance and equilibrium vapor–liquid equation has been
3 Calculation and applying the mathematical developed for xB with R to overcome the delay time for a
model change to take place as a model to predict action map that
used in LabView to achieve the goal that runs the BD at xD
To derive the relation between reflux ratio R and boiler in a constant mode.
composition xB, use McCabe-Thiele graphical method is
shown in Figure 1. Several values of (R) were selected,
operating lines were drawn through the fixed point at distil- 4 Experimental works
late composition (xD, xD) with slope dL/dV = (R/R + 1),
and steps were drawn between the operating line and the The distillation column was in 5 cm diameter with 8 sieve
equilibrium curve to obtain the bottom composition xB. trays and 1 m long as shown in Figure 4. The boil-up rate
This recursive scheme is repeated until the desired stopping was kept constant by controlling the heating mantle
criterion is met, thus xB can be found at each value of the surrounding the boiler (still pot) with a heat duty of
reflux ratio R. 1000 W. The column works at atmospheric pressure, where
While R (L/D) was changed as shown in Figure 1, the the reflux ratio was controlled by a solenoid valve at the
slope of the operating line keeps changing with the fixing top. The system mixture was methanol-water, initial com-
point of the intersect xD. Solving for a constant number position 50% mole of methanol and 50% mole of water in
of trays to find the relation of xB with R to keep xD con- all experiments runs. Temperature sensors (thermocouples)
stant, to make this process worked it should be taken by were placed at each distillation tray.
control through manipulating reflux ratio R at a specific The boiler (still pot) was charged and heated up under
time. The correlation of composition (xB) with R from data total reflux until the steady-state conditions were achieved.
taken for each case using the following procedure: After, the reflux ratio R was turned from infinity to the
finite reflux ratio, and the product was withdrawn at the
1. Draw the equilibrium line for the system (methanol– top of the column.
water). During the column operations, the distillate flowrate
2. Locating the desire concentration of distillate compo- profile, the concentration profiles of the liquid phase along
sition (dome conc.) in our case we take constant distil- the column, and the temperature profiles were measured
late composition at 90% of methanol. for all trays, pot, and condenser was interfaced to the
 The Author(s): Science and Technology for Energy Transition 77, 2 (2022) 5

Fig. 3. (a) The response time required for the tracer injected into the pot to achieve the distillate accumulator. (b) The required time
for the tracer that injected in the distillate accumulator to achieve the still pot.

Fig. 5. Overhead concentration at setup points at 0.9 with/

without adding dynamic-time (+dt).

specific point, these are input as a data signal from temper-

ature sensors where the output signal controls the solenoid
valve that involves changes for reflux rate.
A dynamic model based on equilibrium stages correla-
Fig. 4. Schematic diagram for the batch distillation column (1 – tions implemented in LabViewÒ and validated for a
Vessel; 2 – Still Pot (boiler); 3 – Heating mantle; 4 –
multi-tray column operating under a varying reflux ratio
Temperature sensors; 5 – Condenser; 6 – Product receiver; 7 –
to separate a methanol/water mixture.
Solenoid valve; 8 – Conductivity; 9 – DAQ; 10 – PC.
Figure 5 shows applying the protocol described above as
pre-time determined using the tracer method to anticipate
computer. The computer interface used was NI USB-6211 the delay in the process due dynamic time in the
data acquisition card which can support 16 Analog LabViewÒ, the model agreed with the simple equation
inputs for temperature sensors and 2 Analog output chan- (14). Considering the case of methanol-water in a batch
nels that’s control the heat rate of heating mental and a column with N = 8 plates, the pre-time in control loop time
Solenoid valve was used to control the reflux rate. The policy was compared with instantaneous time equation (13)
complete experimental controlled distillation column is and increasing purity as step change of the distillate compo-
shown in Figure 4. sition as a final product:
Rðt Þ ¼ f ðx B ðt ÞÞ; ð13Þ

5 Results and discussion Rðþdt Þ ¼ f ðx B ðt ÞÞ: ð14Þ

A model equation has been written with LabVIEW to run On the other hand, when taking into account equation (14)
the whole process of batch distillation column at constant and working on it within the control program, we notice the
distillate composition mode due to its equilibrium at a stability of the response. Furthermore, we can believe that
6 The Author(s): Science and Technology for Energy Transition 77, 2 (2022)

To check the Validation for the suggested model and its

stability and the operability of the batch distillation, we dis-
turb the system by changing the setpoint of the distillate
composition as an example from 0.85 to 0.9 and vice versa
to the system checking reading the response for xD as shown
in Figure 7.
The control policy for the reflux flow rate (Fig. 8) is
approximated as a succession of reflux at time t with reflux
at time +dt with the same duration. Compare both soft-
ware in terms of control variable reflux and constant distil-
late composition response for Batch Column.

6 Conclusion
Fig. 6. Bottom concentration vs. variable reflux that maintains
constant distillate concentration at 0.90. Literature works noticed that complexity controlling
distillate composition in batch distillation control problem.
In this work, the proposed batch column separates a binary
mixture (methanol–water) in two different methods to con-
trol the distillate composition by varying reflux rate based
on the boiler concentration. First is the instant time control
of the distillate with varying reflux rates. The second
method is modified by considering the time delay due to
the dynamic behaviour. Time for both vapor upstream
through the trays and refluxed liquid downstream through
the trays to the bottom column using an electroconductive
tracer. However, the mathematic relation for the reflux rate
with bottom concentration was implemented easily using
LabVIEW software to control the operation. The corre-
sponding experiments confirm that the improved reflux
policy column (adding the predicted time) is practicable
and easy to implement, operate, and of great practical
Fig. 7. Overhead concentration for setpoints at 0.85, and 0.9 importance in controlling distillate products. Reduces the
with dynamic-time (+dt). separation time required for the distillation process, thus
reducing the operating energy consumed. Finally, we
believe that further research in this field should address
the problem of selecting the best method to measure the
dynamic time required for the R changes to keep xD con-
stant, when the system is complicated. In the case of sepa-
ration multicomponent mixtures, the proposed control
strategy can be easily extended to control the desired distil-
late purity. The dynamic time delay for the batch column
used in this study was about 12 min was estimated by
adding a conductive tracer both to the boiler and the reflux
accumulator. Add the dynamic time delay within the
equation relations of reflux ratio and boiler concentration
as predicting the change in reflux rate policy to obtain
the desired constant distillate composition. To overcome
the delay problem for a response and keep distillate product
Fig. 8. Overhead concentration disturbance from 0.85 to 0.9
with the desired purity using pre-time is more performant
with dynamic-time (+dt).
for variable reflux R[+dt] was prompted to get a quick
response for the desired constant xD. This leads to distillate
concentration stabilized by manipulating the reflux rate.
the light component xD more stable along the operation For example, keep xD = 0.9 when working with the control-
time, and the production phase is fast and smooth in the ling program using equation (14) it can notice the loss of
case of adding dynamic time, and the composition control control after a period due to accumulated errors as a result
is tight until the end of the operation. Figure 6 shows the of the delay time when sensing to the concentration of xB
real-time relationship between the xB reading and the and the change of the value of reflux responded to get a
amount of R needed to control the constant distillate com- fixed xD. Manipulating the reflux without taking effect of
position mode as an output value. the delayed time, leads to accumulating error on the
 The Author(s): Science and Technology for Energy Transition 77, 2 (2022) 7

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