Journal of the Indian Chemical Society 100 (2023) 100795

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Journal of the Indian Chemical Society

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Batch distillation for separating the acetone and n-heptane binary

azeotrope mixture: Optimization and simulation
Pravin Kale a, Siddhesh Pujari a, Jotiram G. Gujar a, *, Renuka Sontakke b, Ejaz I. Haddadi b,
Shriram S. Sonawane c
a
Department of Chemical Engineering, Sinhgad College of Engineering, Vadgaon, Pune, MS, 411041, India
b
Equinox Software and Services Pvt. Ltd. Pune, MS, 411009, India
c
Visvesvaraya National Institute of Technology, Nagpur, MS, 440010, India

A R T I C L E I N F O A B S T R A C T

Keywords: A batch distillation column is one of several approaches that have been developed to improve the distillation
Batch distillation process’s performance. Batch and specialty chemical industries require quick and reliable process simulations to
Azeotropic mixture predict the extent of separation of mixtures such as volatile natural compounds. Acetone and n-Heptane found in
Entrainer
wastewater are usually associated with solvents from the pharmaceutical industry. At 329.11 K, acetone and n-
MBDS™ thermodynamic Models
Heptane easily combine to form an azeotropic mixture. The different distillation and separation techniques were
Purity
used to separate the azeotropic mixture which requires several plates and columns. In the current work, batch
distillation was used to study the separation of the azeotropic mixture (Acetone and n-Heptane).
It was observed that the desired separation was not possible for the Acetone and n-Heptane system. To
overcome this, a third component such as Butyl propionate or Benzene is added to the mixture of Acetone and n-
Heptane system. This system was simulated using Equinox Software and Services Pvt. Ltd. licensed Multi Batch
Distillation Software (MBDS™).
Different thermodynamic models have been studied for the azeotropic mixtures, such as NRTL, UNIFAC I,
UNIFAC II, and UNIFAC III. The batch distillation system for separating the Acetone and n-Heptane was opti­
mized. Various operating factors such as the number of plates, reflux ratio, batch times, and distillate rates were
investigated. Based on simulation studies, the optimal parameters were determined to be a reflux ratio of 2.2, 19
number of plates, and a total time of 1 h to separate >99 wt % Acetone purity from the azeotropic mixture.

1. Introduction boiling point entrainer, 1-chlorobutane (1-CB) and butyl propionate

A batch distillation is widely used in the fine chemical, specialty
polymer, biochemical, pharmaceutical, and food industries. A single
column is required for multi-component separation in batch distillation.
However, extractive distillation systems may require multiple columns.
As a result, a single column for batch distillation can quickly handle
different feed compositions, different amounts of components, and
different separation difficulties, providing great process flexibility [1].
Due to its functional flexibility, batch distillation is an important
technology in the pharmaceutical and specialty chemical sectors.
Acetone (ACT) and n-heptane (HEP) are the main compounds used as
solvents for organic synthesis in the pharmaceutical industry [2]. In one
trial, Zhang et al. [3] used extractive distillation to separate the binary
azeotropic combination of acetone and n-heptane. As medium and high
(BP) were used. Due to increasing economic incentives and environ­
mental regulatory constraints, several batch distillation processes may
be required to separate a binary mixture. Separating the system from the
azeotrope, on the other hand, is difficult and time-consuming. This
means that distillation separation beyond azeotropic composition
cannot be achieved with ease, regardless of the use of the number of
plates and the reflux ratio. Several studies have been conducted to
overcome the difficulties in the conceptual and design phases of azeo­
tropic batch distillation. However, they limited the entrainer providing
the azeotropic binary mixture to a homogeneous mixture, which
severely limits the flexibility and number of process options available.
Heterogeneous batch distillation was a batch system treatment that
involved adding a third ingredient to a ternary system and causing a
liquid-liquid phase between the binary mix components in several

* Corresponding author.
E-mail address: jggujar.scoe@sinhgad.edu (J.G. Gujar).

https://doi.org/10.1016/j.jics.2022.100795
Received 2 August 2022; Received in revised form 19 September 2022; Accepted 4 November 2022
Available online 5 November 2022
0019-4522/© 2022 Indian Chemical Society. Published by Elsevier B.V. All rights reserved.
P. Kale et al.
configurations (Fig. 1). It is required to widen possibilities and enable
azeotropic separations, which are difficult to do with homogeneous
systems. The first step is to modify all the existing designs and formalize
approaches for heterogeneous constant distillation. Researchers
demonstrated that similar to homogeneous systems, the construction of
batch distillation procedures for separating non-ideal mixtures using a
heterogeneous entrainer includes examining a residue contour map
[4–6].
Residue curve maps were quite useful when it comes to the design
and assessment of separation methods, particularly purification pro­
cedures. Fig. 1 shows the appropriate configuration for extractive
distillation using a residue curve map and a univolatility collection. In
batch distillation, introducing a solvent effective in significantly
changing the mixture’s relative volatility is essential. Based on the sol­
vent screening guidelines, BP was selected as the most suitable solvent to
separate the azeotrope combination under investigation. Because of its
solvent’s low vapor pressure, perfect mixing efficiency, and tolerable
odour, it has been taken into consideration [8–10].
The non-volatile curve intersection point with the ACT/BP binary
side can be used for solvent capacity. Acetone boiling point can be uti­
lized to assess the entrainers capability [11]. The efficiency was assessed
using ternary stage representation. This can be integrated along with
consecutive iterative optimization sequences as well as multi-objective
optimization formula [12]. The presence of an entrainer ensures that
solvent usage is reduced, separation will be more effective, and energy
costs will be reduced [13].
According to RCM curve determination, the residue curve map with
an univolatility line has the optimal method for batch distillation,
showing that BP can perform as a solvent for the ACT/HEP separation.
To analyze the solvent’s volatility, one can use the intersection of the
univolatility curve with the binary side of ACT/BP. The solvent’s ability
can be evaluated at the point where the univolatility curve intersects
with the binary side of ACT/BP. Low solvent use and improved sepa­
ration efficiency are indicated by an intersection of its ACT [7,14].
The concept of thermodynamics, as well as molecular properties,
were used to examine the separation technique and find the best en­
trainers. Extractive dividing-wall columns, as well as pervaporation (PV)
technology, were also used to lower the amount of energy used in the
heating process. In the separation of azeotropes, it was observed that the
PV-extractive distillation technique had significant advantages over the
basic procedure [15].
Bernot et al. [16] addressed the selection of an appropriate entrainer
Fig. 1. A residue curve map was used to create univolatility line for the ACT/
HEP/BP system with the help of UNIQUAC thermodynamic model at 101.325
kPa [7].
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Journal of the Indian Chemical Society 100 (2023) 100795
for homogeneous batch distillation. They have recently designed an
extensive collection of requirements for choosing a suitable entrainer to
separate minimal and even optimal temperature level azeotropic binary
system and close boiling mixture with homogeneous batch purification,
as their conditions do not cover all possible scenarios [17,18]. Bernot
[19] and Dussel [20] were the first to solve this challenge for homoge­
neous batch azeotropic distillation. They have no specific entrainer se­
lection requirements were given for heterogeneous batch distillation.
Heterogeneous batch distillation is composed of an element that causes a
liquid-liquid separation in various configurations. Recent studies have
provided a comprehensive set of guidelines for selecting homogeneous
and heterogeneous entrainers to separate the minimal or maximum
optimum temperature level of azeotropic binary mixtures. Based on the
investigation of ternary residue curve diagrams (Fig. 1) under the as­
sumptions of a significantly larger quantity of an actual number of trays
and reflux ratio, relative volatility components were also reduced [21].
The chemical industry has critical and difficult challenges related to
the separation of binary azeotropes with low cost and low energy con­
sumption [22]. This type of mixture, which is characterized by it being
at the end of the low-pressure column and at the top of the high-pressure
column, may be easily distinguished using an unconventional
pressure-swing distillation configuration. This configuration includes
vapor recompression and an inside heat-integrated purification column,
in accordance with this important technology for increasing power ef­
ficiency [23].
As the trend of manufacturing small-volume, high-value chemicals
continue, batch handling is becoming increasingly important in many
chemical industries. Batch distillation offers the benefit of producing a
wide range of products using a single column. When compared to
continuous distillation, batch distillation consumes more energy. It
provides more flexibility while requiring fewer resources. A single col­
umn may also handle extensive configurations, components, and sepa­
ration problems. Batch distillation is typically preferred for this product
because energy costs are not as significant in small-volume, higher
market value products [24]. In the chemical and petrochemical in­
dustries, the use of computer models for process design is an established
best practice for process development and optimization. The batch
distillation system of Acetone and n-Heptane separation was studied and
optimized.
In this work, MBDS™ software was used to carry out the simulation
procedure. It has a graphical user interface (GUI), advanced thermo­
dynamics calculations, and theoretical component production capabil­
ities. MBDS™ is capable of simulating steady-state, vapor-liquid, and
vapor-liquid-liquid thermodynamic designs. This research looks at
azeotropic systems and the most effective entrainer. In this study,
modeling approaches and simulation on MBDS™ to examine the batch
distillation purity of an azeotropic combination were studied. It also
includes the complete examination of a binary azeotropic mixture to
enhance purity by using an entrainer. MBDS™ provide a quick and
efficient method to conceptualize, evaluate, screen, and optimize the
separation problem. The purpose of this work was to compare extractive
and batch distillation techniques. In this comparison, we observed that
batch distillation needs lesser plates and a lower reflux ratio. This
research presents a breakthrough in the use of simulation for evaluating
industrial separation problems.
1.1. Entrainer
Distillation is one of the most widely used methods for separating
fluid mixtures and is based on differences in relative volatility of the
constituent components [25,26]. It is, however, impossible to separate
azeotropic combinations and even close-boiling systems in a single
continuous distillation column [27]. Various components (entrainer,
solvent, and even a mass separating agent) were utilized to adjust the
relative volatility of the components to be separated in such scenarios
[28,29]. Entrainer is explicitly chosen to aid separation by making the
P. Kale et al. Journal of the Indian Chemical Society 100 (2023) 100795

most of non-ideal movements. Liquid-liquid separation, azeotropic
distillation (AD), and extractive distillation (ED) are separation pro­
cesses that use entrainers. Azeotropic distillation separates azeotropes,
forming various compounds, and uses the existing one to achieve a
chosen separation [30,31].
An azeotropic ternary representation may undoubtedly be used to
screen distillation limits and purification zones. As a result, separating a
binary mixture may need multiple batch distillation processes and may
even be impracticable. One way to avoid an azeotrope was to separate
by using an entrainer that interacts with binary components. The se­
lection of a suitable entrainer was critical since it significantly influences
the duration of the treatment and its environmental impact. It describes
the order of batch distillation operations that allows for separating the
initial components and the desired purity.
The fundamental advantage of using entrainer is its capacity to
separate mixtures that cannot be separated cost-effectively by conven­
tional distillation (e.g., Acetone and n-Heptane system with azeotropes),
thereby increasing the costs. Table 1 describes azeotropic pair of com­
ponents with an entrainer based on boiling point.
2. Methodology
Batch distillation of an azeotropic mixture is a sophisticated dynamic
process (the holdup and composition of the result vary over time during
operation), and the complexity of batch distillation increases with
increasing design precision, numerous components, and a various
number of trays. Analyzing and optimizing several variables simulta­
neously requires the use of modeling and simulation technology.
3. Process optimization: Literature reveals many separations tech­
nique such as continuous distillation, binary distillation, extraction
distillation etc. But in this, all techniques required different param­
eters like some required more no. of plate, more reflux etc. that’s why
recently innovative technique batch distillation is studied for azeo­
tropic mixture separation. My most important advantage is to reduce
capital costs in industry and find out good Purity. Another important
factor justifying the use of batch distillation is the ability to achieve
good product integrity; each batch of product may be properly
defined in terms of feeds utilized and processing conditions. This is
important in industries such as food and medicine. The purpose of
this work was to compare extractive and batch distillation tech­
niques. In this comparison, we observed that batch distillation needs
lesser plates, a lower reflux ratio, and many more parameters to
separate this mixture than extractive distillation. Finding the opti­
mum value is referred to as solving a parameter optimization prob­
lem or objective parameter. The paper’s overall purpose is to provide
a particular solution with a good or best result, considering the time
and resources available. The main objectives of this project are to use
the software tool MBDS™ to simulate the effects of an entrainer to
find the optimum separation parameters in terms of reflux ratio
(energy requirement), number of stages, and product purities of 99
wt% Acetone.
4. Process evaluation: The purpose of this work was to compare
extractive and batch distillation techniques. In this comparison, we
observed that batch distillation needs lesser number of plates and a
lower reflux ratio to separate the mixture compared to extractive
distillation.

1. Conceptual/initial design: As indicated in the fresh feed flowrate
and composition were taken from the work of Maripuri et al. [39] for
the purpose of accurate comparison, which contains 100 kg/hr of
Acetone (50 wt%), n-Heptane (10 wt%), and Butyl propionate (10 wt
%). As for the design variables, our literature review revealed that
the common design variables include the entrainer to number of
Plates, fresh feed, entrainer feed, and Reflux Ratio. During the con­
ceptual design, these design variables are varied until all the product
purities can be met. In all cases, the pressure of all the columns is set
at atmospheric pressure (i.e. 1 atm) for the sake of easier operation
[7,14,40].
2. Solvent selection: Based on the solvent screening guidelines, BP was
selected as the most suitable solvent to separate the azeotrope
combination under investigation. Because of its solvent’s low vapor
pressure, perfect mixing efficiency, and tolerable odour, it has been
taken into consideration [8–10].
Table 2 shows extractive column design parameters for Acetone and
n-Heptane which were used as a reference in the present work. A solvent
that can significantly alter the relative volatility of the binary compo­
sitions is necessary for batch distillation. The first stage in batch puri­
fication is to select various solvents. Based on solvent testing standards
[8,9], the boiling points of all likely solvents were chosen to isolate the
azeotrope combination in this investigation. Fig. 2 shows the flow dia­
gram of the batch distillation process for ACT/HEP separation.
Table 2
Extractive column design parameters for Acetone and n-Heptane system.
Sr. No. Parameters Condition
1 Number of Plates 26
2 Azeotropic Temperature 329.11 K
3 Reflux ratio 2

Table 1
Azeotropic pair of components with entrainer.
Component Pure compound boiling Azeotropic Entrainer References
point (K) temperature (K)

Ethanol 351.3 351.15 Benzene, ethylene glycol glycerol [32]

Water 373.45
Tetrahydrofuran 338.95 337.05 Ethylene glycol, glycerol [33]
Water 373.45 Dimethyl sulfoxide
Isopropyl 355.65 353.45 Dimethyl sulfoxide [34]
alcohol
Water 373.45
Acetonitrile 354.55 349.75 Benzene Ammonium-based deep eutectic solvent [35]
Water 373.45
Tert-butanol 355.15 352.55 Glycerol,1-Butyl-3-methylimidazolium thiocyanide [C4MIM][SCN], and 1-pentyl-3-meth­ [36]
Water 373.45 ylimidazolium thiocyanide [C5MIM][SCN].
Acetone 329.15 328.15 Dimethyl sulfoxide [37]
Methanol 337.35
Toluene 383.25 336.35 DMF Ethylbenzene Chlorobenzene Aniline [38]
Methanol 337.35
Acetone 329.15 329.05 Butyl propionate [7]
n-Heptane 371.55 Benzene

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P. Kale et al. Journal of the Indian Chemical Society 100 (2023) 100795

3.1.1. Effect of number of plates

The total number of plates shows a significant factor in the design
and optimization of distillation systems. Tables 3–7 shows Acetone pu­
rity (wt. %) based on the number of plates at a temperature of 329.11 K
for various reflux ratio. The result shows that as the distillate rate in­
creases, the purity of Acetone decreases for the same number of plates.
As the number of plates increased, the purity also increased. An opti­
mum number of plates to achieve high Acetone purity was found to be in
the range of 18–19. As a result, this optimum was chosen to provide the
maximum Acetone purity with the lowest energy consumption.
When there are more than 19 stages, it is evident that the composi­
tion of the distillate is not considerably affected. The results indicate that
the column operating at a reflux rate of 2.2 with 19 stages provides
maximum Acetone purity. Similar results were found in extractive
distillation by Mahsa Kianinia [7].

3.1.2. Effect of reflux ratio

Fig. 2. Process flow diagram of the Batch distillation process for ACT/
HEP Sepration
3. Results and discussion
This work includes the results of the simulation models developed for
batch distillation, consisting of liquid composition profile, purity,
number of plates, reflux ratio, thermo-package, temperature profile, and
total condenser duty to the still from the condenser at the end of batch
time.
The effects of various process variables on the performance of binary
and multi-component batch distillation processes have been studied. All
the results have been taken from the simulation developed using
MBDS™. The total temperature and the liquid composition profiles of
various methods and variables have been presented.
3.1. Effect of process variables on the performance of an azeotropic
component of batch distillation
The impact of adjusting the reflux ratio on the separation of Acetone
from an azeotropic mixture using a batch distillation method was
investigated at 329.11 K. As the reflux ratio rises, the top product be­
comes even purer. However, a minimum number of reflux ratio must be
retained to have a cost-effective distillation column. This is because a
greater reflux ratio will result in a larger reboiler and condenser duty
consumption.
Fig. 3 illustrates that Acetone mass fraction varies with reflux ratio
based on the different number of plates at a constant distillate rate 10
kmol/h.
Fig. 4 illustrates that Acetone mass fraction varies with reflux ratio
based on the different number of plates at a constant distillate rate of 20
kmol/h. It is seen that the purity of Acetone improves at the same reflux
ratio as the number of plates increases.
Fig. 5 illustrates that Acetone purity varies with reflux ratio based on
the different number of plates at a constant distillate rate of 30 kmol/h.
At the same reflux ratio, the purity of Acetone increases as the number of
plates increases.
Fig. 6 illustrates that Acetone mass fraction varies with reflux ratio
based on the different number of plates at a constant distillate rate of 40
kmol/h. According to Fig. 5, the purity of Acetone increases as the
number of plates increases while maintaining the same reflux ratio.
Fig. 7 shows how the mass fraction of acetone fluctuates with the
reflux ratio depending on the number of plates used at a constant
distillation rate of 50 kmol/h. Figs. 3–7 depict the variance in the
number of plates for the same reflux ratio. Acetone purity increased as
the reflux ratio increased. However, the number of plates for the same
reflux ratio gradually increased in purity. Following the further expla­
nation, it is observed that for the initial number of the plate at reflux
ratio 1, the Acetone purity was 88 wt %. As the reflux ratio increases, the
Acetone purity also increases. It also shows that the best Acetone purity
was obtained when the reflux ratio was between 2 and 2.2. At reflux
ratios greater than 2.2, the Acetone mass percentage in the distillate
falls. High reflux dilutes the liquid phase, which must be BP-rich. As a
result, the optimal point was chosen to provide the maximum Acetone

The effect of various operating parameters can be predicted from the

simulation of batch distillation. The model can predict the composition, Table 3
temperature, the number of plates, reflux ratio, and batch time. To test Acetone Purity (wt. %) based on number of plates for reflux ratio (R) = 1 and
the validity of the simulation findings, the initial conditions utilized in temperature: 329.11 k
this simulation were the same as those used in the problem statement for Reflux Ratio = 1
the supplied azeotropic combination Acetone-n-Heptane and Butyl Number Distillate Distillate Distillate Distillate Distillate
propionate. The effect of each process variable was studied as a function of plates rate = 10 rate = 20 rate = 30 rate = 40 rate = 50
of another specified variable; for example, when changing the batch kmol/h kmol/h kmol/h kmol/h kmol/h
time, reflux ratio, and the number of plates, the distillate rate was kept 5 88.01 87.74 87.45 87.13 86.75
constant. 10 90.58 90.44 90.29 90.14 89.98
15 91.62 91.54 91.44 91.34 91.24
18 91.97 91.91 91.82 91.74 91.63
19 92.06 92.01 91.92 91.84 91.74

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P. Kale et al. Journal of the Indian Chemical Society 100 (2023) 100795

Table 4
Acetone Purity (wt. %) based on number of plates for reflux ratio (R) = 1.3 and
temperature: 329.11 K
Reflux Ratio = 1.3

Number Distillate Distillate Distillate Distillate Distillate

of Plates rate = 10 rate = 20 rate = 30 rate = 40 rate = 50
kmol/h kmol/h kmol/h kmol/h kmol/h

5 89.76 89.50 89.22 88.90 88.52

10 93.02 92.86 92.76 92.58 92.40
15 94.40 94.25 94.09 93.97 93.89
18 94.89 94.73 94.55 94.45 94.38
19 95.02 94.85 94.67 94.57 94.49

Fig. 3. Acetone Purity (wt. %) Vs Reflux Ratio (Distillate Rate (D) = 10 kmol/
Table 5 h; temperature: 329.11 K).
Acetone Purity (wt. %) based on number of plates for reflux ratio (R) = 1.6 and
temperature: 329.11 K
Reflux Ratio = 1.6

Number Distillate Distillate Distillate Distillate Distillate

of Plates Rate = 10 Rate = 20 Rate = 30 Rate = 40 Rate = 50
kmol/h kmol/h kmol/h kmol/h kmol/h

5 91.04 90.78 90.51 90.20 89.81

10 94.74 94.62 94.49 94.36 94.18
15 96.30 96.13 96.01 95.93 95.84
18 96.85 96.69 96.58 96.52 96.45
19 97.00 96.83 96.73 96.67 96.58

Table 6
Acetone Purity (wt. %) based on number of plates for reflux ratio (R) = 2.0 and Fig. 4. Acetone purity (wt. %) Vs Reflux Ratio (Distillate Rate (D) = 20 kmol/h;
temperature: 329.11 K temperature: 329.11 K).

Reflux Ratio = 2

Number Distillate Distillate Distillate Distillate Distillate

of Plates Rate = 10 Rate = 20 Rate = 30 Rate = 40 Rate = 50
kmol/h kmol/h kmol/h kmol/h kmol/h

5 92.27 92.02 91.76 91.45 91.06

10 96.34 96.23 96.12 95.99 95.81
15 97.94 97.87 97.85 97.80 97.54
18 98.52 98.49 98.48 98.45 98.00
19 98.68 98.66 98.65 98.62 98.05

Table 7
Acetone purity (wt. %) based on number of plates for reflux ratio (R) = 2.2 and
temperature: 329.11 k Fig. 5. Acetone Purity (wt. %) Vs Reflux Ratio (Distillate Rate (D) = 30 kmol/
Reflux Ratio = 2.2
h; temperature: 329.11 K).

Number Distillate Distillate Distillate Distillate Distillate

of Plates Rate = 10 Rate = 20 Rate = 30 Rate = 40 Rate = 50
kmol/h kmol/h kmol/h kmol/h kmol/h

5 92.74 92.50 92.24 91.94 91.55

10 96.92 96.82 96.71 96.59 96.41
15 98.50 98.47 98.44 98.39 98.02
18 99.06 99.05 99.03 99.00 98.30
19 99.20 99.20 99.18 99.15 98.37

purity with the least amount of energy.

3.1.3. Effect of distillate rate

The effect of change on the separation of Acetone from an azeotropic
mixture using a batch distillation process was first considered. For the
given system, a simulation was performed at 329.11 K.
For a high purity column, i.e. one with high reflux, it can be proved
that the distillate composition is sensitive to the distillate flow but
insensitive to the reflux rate. Therefore, the aforesaid control method­
ology is utilized for a high purity column. It should be noticed that the
reflux rate must be used to maintain effective control over the level in
the reflux drum. Fig. 8 illustrates that Acetone mass fraction varies with
distillate rate based on different reflux ratios at a constant number of
Fig. 6. Acetone Purity (wt. %) Vs Reflux Ratio (Distillate Rate (D) = 40 kmol/
h; temperature: 329.11 K).
plates 5.
Fig. 9 illustrates that Acetone mass fraction varies with distillate rate
based on different reflux ratios at a constant number of plates 10. It has
been discovered that when the reflux ratio increases, the purity of
Acetone increases at the same distillation rate.
Fig. 10 illustrates that Acetone mass fraction varies with distillate

5
P. Kale et al.
Fig. 7. Acetone Purity (wt. %) Vs Reflux Ratio (Distillate Rate (D) = 50 kmol/
h; temperature: 329.11 K).
Fig. 8. Acetone Purity (wt. %) Vs Distillate Rate (kmol/h) (Number of Plates =
5; temperature: 329.11 K).
Fig. 9. Acetone Purity (wt. %) Vs Distillate Rate (kmol/h) (Number of Plates =
10; temperature: 329.11 K).
rate based on different reflux ratios at a constant number of plates 15.
Fig. 11 illustrates that Acetone mass fraction varies with distillate
rate based on different reflux ratios at a constant number of plates 18. It
also shows that as the reflux ratio increases, so does the purity of
Fig. 10. Acetone Purity (wt. %) Vs Distillate Rate (kmol/h) (Number of Plates
= 15; temperature: 329.11 K).
6
Journal of the Indian Chemical Society 100 (2023) 100795
Acetone at the same distillation rate.
Fig. 12 illustrates that Acetone mass fraction varies with distillate
rate based on different reflux ratios at a constant number of plates 19. It
can be concluded that as the reflux ratio increases, the purity of Acetone
also increases at the same distillate rate.
Figs. 8–12 represents the contrast of the reflux ratio for the same
distillate rate. As the distillate rate increases, the Acetone purity de­
creases. However, increasing the reflux ratio for the same distillate rate
gradually resulted in increased purity. It can be concluded that as the
distillate rate increases, the purity decreases. The highest Acetone purity
was obtained at a distillate rate of 30 kmol/h - 40 kmol/h. In addition to
condenser duties, the reflux ratio influences distillate composition. As a
result, depending on the number of plates and distillation rate, the best
parameters were chosen to have the highest Acetone purity. The opti­
mization flow chart is shown in Fig. 13. The effect of various parameters
like number of plates, reflux ratio, distillate rate was studied in the
manuscript. Table 8 shows the optimized operating parameter of the
batch distillation process..
3.2. Effect of time
The time factor was significant in batch distillation due to its un­
steady nature. It is observed that the operating time for getting the
maximum purity of Acetone was between 0.5 h and 1 h. As additional
time was increased, the distillate purity of Acetone decreased. Baelen
et al., 2010 [41] studied the separation of isopropyl alcohol recovered
by hetro-azetropic batch distillation. They obtained about 99.96 wt %
purity by using hetreazetropic batch distillation by simulation and about
97.60 wt % is obtained by experiments. Fig. 14 illustrate that Acetone
Purity (wt. %) varies with time based for optimization parameters such
as reflux ratio, number of plates and distillate rate.
3.3. Computational procedure
3.3.1. Semi-rigorous model
In this paper, an MBDS™ simulation was used to solve the semi-
rigorous behavior of an optimal number of plates and reflux ratio. The
shortcut column is used to separate multi-component solvent mixtures.
It uses a simplified approach FUG (Fenske-Underwood-Gilliland) with
the Kirkbride equation to determine the optimal feed plate. The semi-
rigorous governing equations can be solved instantaneously, whereas
most other known techniques require repeated calculations to create a
relatively accurate and practical design.
This semi-rigorous formulation uses substantially less computer
memory than rigorous techniques. Because the relevant assumption data
for the semi-rigorous model is available, the simulation was performed
using the semi-rigorous model. For a column with a low holdup, the
semi-rigorous method is implemented.
Fig. 15 depicts the purity of acetone determined using various
models such as NRTL, UNIFAC I, UNIFAC II, and UNIFAC III. It is
Fig. 11. Acetone Purity (wt. %) Vs Distillate Rate (kmol/h) (Number of Plates
= 18; temperature: 329.11 K).
P. Kale et al. Journal of the Indian Chemical Society 100 (2023) 100795

Fig. 12. Acetone Purity (wt. %) Vs Distillate Rate (kmol/h) (Number of Plates
= 19; temperature: 329.11 K).

Fig. 14. Acetone Purity (wt. %) Vs Time (h) (Number of Plates = 19; Distillate
rate = 30 kmol/h; temperature: 329.11 K).

Fig. 15. Acetone Purity (wt. %) Vs Thermodynamic model (Number of Plates

= 19; Distillate rate = 30 kmol/h; temperature: 329.11 K; batch time = 1 h,
reflux ratio = 2.2).

4. Conclusion
Fig. 13. Optimization flowchart.
This work reviews recent developments in batch distillation, such as
unique column designs and alternative analysis techniques. A batch
Table 8 distillation system can lead to the most promising and flexible column
Optimization results of the batch distillation process. arrangement with the most acceptable operating strategy and condi­
Parameter Optimum Parameter tions. At the outset, entrainer selection criteria and novel techniques for
breaking azeotropes with an entrainer that was partially miscible with
Reflux ratio 2 to 2.2
Number of plates 18 to 19 one of the binary mixture components were reviewed.
Time 0.5–1 h In this study, we simulated and optimized the operating parameters
Distillate rate 20–30 kmol/h of a batch distillation to separate an azeotrope of acetone and n-heptane
Acetone purity 99.182 wt % and a combination of butyl propionate. Sensitivity analysis was per­
Condenser duty 12.209 KW
Reboiler duty 12.514 KW
formed to investigate the influence of different operating parameters
such as distillation rate, number of trays, reflux rate, and batch distil­
lation time on the results.
observed that the UNIFAC II thermodynamic model gives maximum As the MBDS™ simulation results show, the reflux rate has one of the
Acetone purity (99.18 wt %) for the simulation of a system separating most significant effects on energy consumption and is an important
Acetone, n-Heptane, and Butyl propionate mixture. Table 9 shows the parameter for optimization. The simulated result shows that a reflux
comparative study of Acetone purity based on literature (extractive ratio of 2–2.2, distillate rate of 20–30 kmol/h, number of plates of
distillation), theoretical calculation, and simulation of MBDS™ with 18–19, and a batch temperature of 329.11 K were found to be optimal
different entrainers. parameters for separation using batch distillation. For azeotropic mix­
In this study, the UNIFAC II thermodynamic model was used as a tures, various thermodynamic models, such as NRTL, UNIFAC I, UNIFAC
suitable fluid package to simulate batch distillation. The UNIFAC II II, and UNIFAC III, have been investigated. It is observed that the UNI­
model predicts pseudo-binary vapor-liquid equilibrium data of azeo­ FAC II thermodynamic model provides the highest Acetone purity
tropic mixtures. This figure demonstrates that the acetone-n Heptane (99.18 wt %) for the simulation of a system separating a mixture of
system was simulated with UNIFAC-II model and the results were Acetone, n-Heptane, and Butyl propionate.
compared (Fig. 16).

7
P. Kale et al. Journal of the Indian Chemical Society 100 (2023) 100795

Table 9
Comparison of Azeotropic Mixture Binary Batch Distillation Component Purity with entrainer.
Component Boiling Point Azeotropic Temperature Entrainer Boiling Point Purity (wt.%)
Mixture (K) (K) (K)
Literature [7] Theoretical MBDS™
Calculation Simulation

Acetone 329.32 329.11 Butyl 419.15 99.5 97.82 99.18

n-Heptane 371.46 propionate
Acetone 329.32 329.11 Benzene 353.25 99.5 97.06 99.28
n-Heptane 371.46

Fig. 16. Pseudo-binary Y− X diagram for the Acetone + n Heptane system.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgment
The author would like to thank Equinox Software and Services Pvt.
Ltd. Pune, India for providing the software facility.
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