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Procedia Engineering 42 (2012) 1202 – 1213

20th International Congress of Chemical and Process Engineering CHISA 2012

25 – 29 August 2012, Prague, Czech Republic

Modeling, design and control of cyclic distillation systems

I. Liţăa, C. Sorin Bîldea a*, A. A. Kissb
a
University Politehnica of Bucharest, Department of Chemical Engineering, Str. Polizu 1-7, 011061 Bucharest, Romania
b
Web: www.tonykiss.com, E-mail: tonykiss@gmail.com

Abstract

Cyclic distillation can bring new life in old distillation columns, by using a cyclic operation mode that leads to key
benefits, such as: increased column throughput, lower energy requirements and higher separation performance. The
literature reveals experimental and theoretical studies carried out so far, including several models for simulating
cyclic distillation. However, the accuracy of these models is limited due to the linear equilibrium assumption.
Moreover, these models can be used for rating studies only and no design method exists up to now, for the general
case of nonlinear equilibrium. This paper fills this gap by presenting a novel approach for the design of cyclic
distillation systems and an insightful comparison against conventional distillation. The complete model, an innovative
graphical design method, and a case study proving the good controllability of cyclic distillation are also presented.

© 2012 Published by Elsevier Ltd. Selection under responsibility of the Congress Scientific Committee
(Petr Kluson) Open access under CC BY-NC-ND license.

Keywords: Cyclic distillation; design method; non-linear equilibrium; operating lines; comparison with classic distillation

1. Introduction

Process intensification in distillation systems received much attention during the last decades, with the
aim of increasing energy and separation efficiency. Various techniques, such as internal heat-integrated
distillation, dividing-wall columns and reactive distillation were studied [1,2]. Cyclic operation is
considered as an innovative method for operating existing distillation columns, leading to increased
throughput, lower energy requirements and higher separation performance.

* Corresponding author. Tel.: +40 21 402 3903

E-mail addresses: s_bildea@upb.ro, tonykiss@gmail.com

1877-7058 © 2012 Published by Elsevier Ltd. Open access under CC BY-NC-ND license.
doi:10.1016/j.proeng.2012.07.512
 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213 1203

Nomenclature
B bottoms (kmol/cycle)
D distillate (kmol/cycle)
L reflux (kmol/cycle)
F feed (kmol/cycle)
M holdup (kmol)
NF feed stage
NT total number of stages
t time
tvap duration of the vapor-flow periond
V vapor flow rate
x mole fraction, liquid phase
y mole fraction, vapor phase

Superscripts
(V) end of the vapor-flow period
(L) end of the liquid-flow period

Subscripts
k stage number (1 – condenser, NT – reboiler)
F feed
D distillate
B bottoms

The cyclic operating mode consists of two parts: (1) a vapor-flow period, when vapor flows upward
through the column, while liquid remains stationary on each plate, and (2) a liquid-flow period, when
vapor flow is stopped, reflux and feed are supplied to the column, while the liquid holdup is dropped from
each tray to the tray below [3]. This mode of operation can be easily achieved by using perforated trays,
without downcomers, combined with sluice chambers located under each tray. If the vapor velocity
exceeds the flooding limit, the liquid does not overflow from tray to tray during the vapor-flow period.
When the vapor supply is interrupted, the liquid drops down by gravitation to the sluice chamber. When
the vapor supply is started again, the sluice chambers open and the liquid is transferred to the tray below.
The principle of cyclic operation is schematically illustrated in Fig. 1.
Although the advantages of cyclic operation have been demonstrated experimentally, the information
about modelling and designing cyclic distillation columns is rather limited. The idea of cyclic operation in
the fields of distillation, liquid-liquid extraction and particle separation was introduced by Cannon [4] and
tested in tray [5] and packed columns [6]. Afterward, Sommerfeld et al. [7] used computer simulation to
investigate the theoretical effects of various parameters on the separating ability of a controlled cycling
column. Analytical results were also presented for certain simplified cases assuming constant composition
in the reboiler, and a linear equilibrium relationship. Moreover, an analogy with classic distillation was
developed. Analytical expressions describing the dynamics of a distillation column operated in controlled
cyclic fashion were derived for linear equilibrium assumption and considering an average value for the
liquid composition during one operating cycle. Also, an iterative procedure was proposed to handle the
case of nonlinear equilibrium [8]. Based on a model assuming linear equilibrium and straight operating
line, Robinson and Engel [9] suggest replacing the distance-axis composition profiles found in a
conventional column with a composition profile along the time axis.
1204 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213

Vapour-flow period Liquid-flow period

to condenser to condenser

Liquid Liquid

Feed Feed

Vapour Vapour

to reboiler to reboiler

Fig. 1. Schematics illustrating the working principle of cyclic distillation

Schrodt et al. [10] describes a plant-scale cyclic column (19 in. diameter) for separation of water-
acetone mixture, proving that a 240% capacity increase is possible. Gel'perin et al. [11] created a cyclic
regime using electromagnetic valves. A 200% efficiency increase proved again the beneficial effect of
cycling regime An empirical model was used to predict the performance. Soon after, Rivas [12] derived
simple analytical equations that can be used to calculate the ideal number of trays for cyclic counter-
current processes such as cyclic distillation, absorption, and stripping. However, this applies better to
absorption than to distillation, due to the linear-equilibrium assumption. For a benzene-toluene mixture
and 95% product purity, a 50% reduction in number of stages compared to conventional distillation was
observed. The importance of liquid plug-flow down the column was emphasized by Baron et al. [13]. An
analytical solution of balance equations in cycling operation was obtained [14], under the assumptions –
among others – of constant vapor concentration entering the bottom stage, condenser without holdup and
again linear equilibrium. This was used for studying the effect of feed tray location, reboiler volume,
relative volatility, stage efficiency, number of trays and reflux number on the separation performance. The
assumption of linear equilibrium was relaxed. Matsubara et al. [15,17] used cycling operation as an
example to emphasize the advantages of relay feedback periodic control compared to the forced
oscillation scheme. Further energy saving was achieved by combining cycling and stepwise operation
modes [16,17]. The cycling operating mode was demonstrated experimentally on a five-stage water-
methanol mixture. Up to 50% energy reduction was observed, compared to conventional continuous
column.
 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213 1205

An efficient algorithm for dynamic simulation of cyclic processes, without the need of repeatedly
evaluating a large number of steps, was applied to cyclic distillation[18]. Dynamic optimization was used
to find the optimal profiles of flow rates of feed, product streams, reflux and vapor in order to reduce the
energy demand [19].
A more recent study [3] gives an overview of previous work on cyclic distillation and presents a novel
model of a theoretical stage with perfect displacement. Equilibrium and operating lines (assuming linear
equilibrium) diagrams are used to illustrate the principle of cyclic operation. Two relevant case-studies
illustrate the theoretical findings and applications. Application of cyclic operation to batch distillation was
recently reviewed by Flodman and Timm [20].
The literature review clearly proves the advantages of cyclic operation as compared to conventional,
steady state operation of distillation. Several models are available to simulate the behaviour of the cyclic
distillation columns. When the assumption of linear equilibrium is employed, it is indeed possible to
derive analytical solutions of the model equations. However, although these analytical expressions could
be used to design cyclic operation columns, the accuracy of the results is limited due to the linear
equilibrium assumption. Moreover, these models can be used for rating studies only and no design method
exists up to now, for the general case of nonlinear equilibrium. This paper fills this gap by presenting a
novel approach for the design of cyclic distillation systems and an insightful comparison against
conventional distillation. The complete model and an innovative graphical method similar to the McCabe-
Thiele diagram are also presented hereafter. Finally, the good controllability of cyclic distillation columns
is demonstrated.

2. Modelling approach

2.1. Assumptions

The model of the cyclic distillation column is derived under the following assumptions:
x Binary (mixture) distillation
x Ideal stages (vapor-liquid equilibrium is reached)
x Equal heat of vaporization (this implies constant molar holdup and vapor flow rate)
x Perfect mixing on each stage
x Negligible vapor holdup
x Saturated liquid feed
Note that in contrast to the previously cited papers, no assumptions are made here with regard to the
linearity of vapor-liquid equilibrium, infinite reboiler holdup or zero condenser holdup.

2.2. Operational constraints

From the condenser and reboiler mass balance, written for one operating cycle:
V ˜ tvap D  L (1)
LF V ˜ tvap  B (2)
the following feasibility condition follows:
L  V ˜ tvap  L  F (3)

2.3. Model of the vapor-flow period

The following equations describe the evolution in time of stage holdup and composition, during the
vapor-flow period:
1206 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213

dM 1 dx1
Condenser: V; M1 V  y2  x1  (4)
dt dt

dM k dxk
Trays: 0; Mk V  yk 1  yk  (5)
dt dt
dM NT dx
Reboiler: V ; M NT NT V  xNT  yNT  (6)
dt dt
Initial conditions: At t = 0,  M , x   M   , x  
L L
(7)

Integration from t=0 to t = tvap gives the state of the system at the end of the vapor flow period,
 M   , x  
V V

2.4. Model of the liquid-flow period

The following equations give the stage holdup and composition at the end of the liquid-phase period:
M1  M1   D  L ; x1  x1 
L V L V
Condenser: (8)
M k
L
xk
L
xk 1
V
Trays, rectifying section: L; (9)
V 
  L  L LxNF  FxF
Feed tray: M NF L  F ; xNF (10)
1 1
L  F 
M k
L
xk
L
xk 1
V
Trays, stripping section: LF ; (11)
 L V  V 
Reboiler: M NT M NT  B  M NT 1

 L
xNT
 M    B  x   M  
V
NT
V
NT
V V 
x
NT 1 NT 1
(12)
 L
M NT

2.5. Solution method

Equations (4)-(7) and (8)-(12) can be written in the following condensed form, where )V  and ) L  are
mappings relating the state at the start and the end of the vapor- and liquid-flow periods, respectively.
 M   , x  
V V
)V   M , x  (13)

 M   , x  
L L
) L   M , x  (14)
Periodicity condition requires:
 M   , x  
L L

) L )V  M  L , x L  (15)

A straightforward solution of equation (15) can be obtained by considering an initial state and applying
relationships (13) and (14) until the difference between two iterations becomes small. However, the
convergence can be accelerated by applying algebraic equations numerical methods (for example Newton
or Broyden). The model can be conveniently solved in Mathworks Matlab or any other similar software.
 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213 1207

3. Comparison with classic distillation

Fig. 2. compares the vapor / feed ratio versus the product purity (xD = 1 - xB) in conventional
distillation and cyclic distillation employing different number of trays: 24 trays for conventional
distillation and 12-24 trays for the cyclic distillation. Separation of an equimolar mixture benzene -
toluene was considered.
It can be observed that the energy requirements – which are directly proportional with the vapor flow
rate – are greatly reduced, especially for high purity products. Moreover, the number of trays required by
cyclic distillation is almost half as compared to the conventional distillation, when the same purity is
obtained with the same vapor flow rate.

1.8 14
12 Classic distillation
NT = 24
1.6
V /F

16
1.4 20

1.2 NT = 24

1
0.0001 0.001 0.01 0.1
1 - xD
Fig. 2. Comparison of energy requirements in cyclic distillation vs conventional distillation

4. Design of cyclic distillation

4.1. Design methodology

x Initial data. Given the feed (F, xF) and the required performance (xD, xB) solve the mass balance over
one operating cycle, to find the product flow rates (D, B):
F DB (16)
F ˜ xF D ˜ xD  B ˜ xB (17)

x Hydrodynamics. Specify the vapor flow rate V and the duration of the vapor-flow period, tvap, and
calculate the amount of liquid transferred from condesnser to the top tray:
L V ˜ tvap  D (18)

Tray holdups are Mk = L (rectifying section) and Mk = L + F (stripping section).

Check the hydrodynamics (column diameter, vapor velocity, pressure drop)
1208 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213

x The state of the reboiler at the end of the vapor-flow period, specified as follows:
- holdup, MNT(tvap). The result of the design procedure is independent of this value, whose specification
is nevertheless necessary.
- composition, xNT(tvap) = xB. At the end of vapor-flow period, the reboiler is richer in the heavy
component, therefore this is the moment to take out the bottom product.

x Integrate the reboiler equations (6), from t = tvap to t = 0, to find the holdup and reboiler composition at
the beginning of the vapor-flow period, MNT(0), xNT(0).

x Find the state of the last tray (stage NT-1) at the end of the vapor-flow period, using the mass balance
for the liquid-flow period:
M NT 1  tvap  L  F (19)

xNT 1  tvap 
 
M NT  0  ˜ xNT  0   M NT  tvap   B ˜ xNT  tvap 
(20)
LF

x Find the state of reboiler and last tray at the beginning of the vapor flow period by integrating
equations (5) and (6) from t = tvap to t = 0

x Add one more tray, whose state at the end of the vapor-flow period is
M NT  2  tvap  L  F (21)
xNT  2  tvap  xNT 1  0  (22)
and integrate the resulting set of equations from t = tvap to t = 0. Repeat until the feed composition is
reached for the tray NF+1.

x Find the state of the feed tray at the end of the vapor-flow period:
M NF  tvap  L (23)
M NF 1 ˜ xNF 1  0   F ˜ xF
xNF  tvap  (24)
M NF
and integrate the resulting set of equations from t = tvap to t = 0.

x Similarly, repeat addition of one tray, finding its state at the end of vapor-flow period and integration
of the resulting equations until the distillate composition is reached.

The first three steps of the design procedure are illustrated in Fig. 3.
x(tvap) x(0)
Tray
x(tvap) x(0) x(tvap) x(0)
Tray Tray
x(tvap) x(0) x(tvap) x(0) x(tvap)
xB Reboiler Reboiler x(0)
Reboiler

Fig. 3. First steps of the design procedure

 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213 1209

4.2. Results of case study

The following model system is used to demonstrate the procedure:

- Ideal binary mixture, relative volatility D = 3.5 (the large volatility is chosen for a clear graphical
illustration of the results)
- Feed: F = 0.375 kmol/cycle; xF = 0.5
- Distillate: D = 0.1875 kmol/cycle; xD = 0.995
- Bottoms: B = 0.1875 kmol/cycle; xB = 0.005
- Vapor flow: V = 2.21 kmol/min; tvap= 0.2 min (0.442kmol/cycle)

stage

1 NT-7
NT-6

NT-5
0.8

NT-4
0.6
x

0.4 NT-3

0.2 NT-2

NT-1

0
0 0.25 0.5 0.75 1
t / [min]

Fig. 4. Evolution of liquid-phase mole fraction over four operating cycles. Tray number are indicated on the right side (condenser
not shown). The coloring of the lines indicate the flow of the liquid from one tray to another.

Fig. 4 shows the evolution of the liquid phase composition over four vapor flow - liquid flow cycles,
for the model system. Tray numbers are indicated on the right, while the line coloring suggests the flow
of the liquid from tray to tray (the liquid-flow period). The feed is on the tray NT-4, as the composition at
the end of vapor-flow period / beginning of the liquid-flow period matches the feed composition, xF = 0.5.
If the vapor flow rate is set to 2.21 kmol/min, nine separation stages are needed to perform the required
separation (reboiler, 7 trays, condenser). The bottom mole fraction is xB = 0.005, while the distillate purity
xD=0.9993 exceeds the specification.
It is useful to present the results in a plot similar to the McCabe-Thiele diagram (Fig. 5). The diagram
contains the equilibrium line and the operating line. The coordinates of the points on the operating line
are the liquid mole fraction on the tray k, xk(t), and the vapour mole fraction on the tray below, yk+1(t).
As the time varies between 0 and tvap, one segment corresponds to each tray k. Additionally, these
segments are connected because, at the end of the vapour-flow period, liquid from tray k is moved to tray
k+1, therefore:
xk  0  xk 1  tvap  (25)
and
yk 1  0  yk  tvap  (26)
1210 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213

The dotted lines represent the operating lines for the classic distillation corresponding to the same
reflux and vapor flow. Clearly, fewer trays are required in cyclic operation. Moreover, Fig. 5 illustrates
the existence of a minimum vapor-flow rate – corresponding to an infinite number of trays – and also a
minimum number of trays, corresponding to an infinite vapor flow.
After the number of trays is found, the cyclic operation mode is simulated and the vapor flow rate is
adjusted such that the purity specifications are exactly matched. For the test case, the new vapor flow rate
is V = 2.12 kmol/min.
NT-7

1 V ·t vap =0.35 kmol/cycle

NT-6

NT-5

Equilibrium line
0.8 NT-4

x NT-3(t vap) = x NT-2(0) Operating line

yNT-3(t vap)=y NT-3(0) NT-3 V ·t vap =0.442 kmol/cycle
0.6
x NT-3(0) V·t vap =4 kmol/cycle
y

y NT-2(0)
0.4 D = 3.5
NT-2 F = 0.375 kmol/cycle
x NT-3(t vap) = x NT-2(0) x F = 0.5
0.2 yNT-2(t vap)
x D = 0.995
NT-1
x B = 0.005

0
0 0.2 0.4 0.6 0.8 1
x
Fig. 5. Representation of the cyclic operation mode using equilibrium and operating lines

Condenser stage 2
0.9951 1

0.995
0.98
0.995

0.9949 0.96
0 0.5 1 1.5 0 0.5 1 1.5
time / [min] time / [min]
stage 4 stage 6
1 0.5
0.9
0.4
0.8
0.3
0.7
0.2
0 0.5 1 1.5 0 0.5 1 1.5
time / [min] time / [min]
stage 8 -3 Reboiler
x 10
0.1 6

5.5
0.05
5

0 4.5
0 0.5 1 1.5 0 0.5 1 1.5
time / [min] time / [min]

Fig. 6. Evolution of liquid composition in condenser, reboiler and selected trays, over several operation cycles
 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213 1211

Fig. 6 shows the evolution of liquid mole fraction in condenser, reboiler and selected trays over several
operating cycles. It should be observed that a stationary periodic state is reached. Moreover, at the end of
vapour-flow period, the reboiler and condenser mole fractions are equal to the bottoms and distillate
specifications.

5. Control considerations

The design procedure described in the previous section was applied for separation of an equimolar
mixture of benzene and toluene. The feed flow rate was set to 0.375 kmol/cycle, while the distillate and
bottoms composition were set to 0.995 and 0.005, respectively. The cyclic distillation column has 14
stages in total, with the feed located on stage 7. The required vapor and liquid flows were set to V = 0.496
kmol/cycle and L = 0.312 kmol/cycle, respectively.

The control strategy measures the reboiler and condenser compositions at the end of the vapor-flow
period and uses the discrete PI-algorithm to adjust the values of the vapor and reflux, according to:

uk 1 uk  D ˜ H k 1  E ˜ H k (27)

where u and H are the manipulated and control errors, respectively, while D and E are the control tuning
parameters.
In addition, the bottoms and distillate amounts are used to control the reboiler and condenser holdups
(e.g. level control). The performance of the control system was tested for a 10% increase of the feed flow
rate, as well as for a change of the feed composition from xF = 0.5 to xF = 0.6. The results presented in
Fig. 7 and Fig. 8 show that the product purities can be indeed kept to their set points. Remarkable, the
disturbances in the feed flowrate and composition are rejected successfully with short settling times and
low overshooting – this proving indeed the good controllability of cyclic distillation.
1 0.01

0.999 0.009

0.998 0.008

0.997 0.007

0.996 0.006
xB
xD

0.995 0.005

0.994 0.004

0.993 0.003

0.992 0.002

0.991 0.001

0.99 0
0 20 40 60 80 100 0 20 40 60 80 100
time / [min] time / [min]

Fig. 7. Performance of the control system for a 10% increase of the feed amount
1212 I. Li__ et al. / Procedia Engineering 42 (2012) 1202 – 1213

1 0.01

0.999 0.009

0.998 0.008

0.997 0.007

0.996 0.006
xD

xB
0.995 0.005

0.994 0.004

0.993 0.003

0.992 0.002

0.991 0.001

0.99 0
0 20 40 60 80 100 0 20 40 60 80 100
time / [min] time / [min]

Fig. 8. Performance of the control system for a change of the feed composition from xF = 0.5 to xF = 0.6

6. Conclusions

Cyclic distillation can bring new life in old distillation columns, providing key benefits, such as: high
column throughput, low energy requirements and high separation performance. However, the cyclic
distillation models reported in literature can be used for rating studies only and no design method exists
up to now, for the general case of nonlinear equilibrium. This study successfully fills this gap by
proposing a novel approach for the design of cyclic distillation systems, and presenting an insightful
comparison against conventional distillation. The key findings of this work are the following:
x The energy requirements for cyclic distillation are greatly reduced especially for high purity products.
Moreover, the number of trays required by cyclic distillation is almost half as compared to the
conventional distillation, when the same purity is obtained with the same vapor flow rate.
x In cyclic distillation, a minimum vapor-flow rate exists – corresponding to an infinite number of trays
– as well as a minimum number of trays, corresponding to an infinite vapor flow.
x Cyclic distillation columns can be easily controlled by adjusting the reflux and the vapor flow rate, in
order to keep the required product purities. Remarkable, disturbances in the feed flowrate and
composition are successfully rejected with low settling times and low overshooting.

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