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Recent Advances in Extractive Distillation

Article in Engineering Proceedings · October 2023

DOI: 10.3390/ASEC2023-15261

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Proceeding Paper
Recent Advances in Extractive Distillation †
Althea Francesca Aquilon 1 , Diana Mae Cargullo 1 , Jeremay Onayan 1 , Jgiordana Sarno 1 , Vea Marie Molino 1
and Edgar Clyde R. Lopez 2,3, *

1 Chemical Engineering Department, College of Engineering, Adamson University, Ermita, Manila 1000,
Philippines; althea.francesca.aquilon@adamson.edu.ph (A.F.A.);
diana.mae.cargullo@adamson.edu.ph (D.M.C.); jeremay.onayan@adamson.edu.ph (J.O.);
jgiordana.sarno@adamson.edu.ph (J.S.); vea.marie.molino@adamson.edu.ph (V.M.M.)
2 Nanotechnology Research Laboratory, Department of Chemical Engineering, University of the Philippines
Diliman, Quezon City 1101, Philippines
3 Department of Chemical Engineering, University of Santo Tomas, España Blvd., Sampaloc,
Manila 1015, Philippines
* Correspondence: edgarclydelopez09@gmail.com
† Presented at the 4th International Electronic Conference on Applied Sciences, 27 October–10 November 2023;
Available online: https://asec2023.sciforum.net/.

Abstract: Distillation is widely recognized as the preferred method for separation due to its opera-
tional and control benefits. Traditional distillation processes, however, cannot successfully separate
azeotropic mixtures with near boiling points. Numerous special distillation processes have been
developed to address this limitation. Extractive distillation, in particular, has gained significant
popularity in the chemical, petrochemical, pharmaceutical, and refining industries. This review
examined the state-of-the-art advances in extractive distillation. The importance of the proper se-
lection of a solvent was discussed. Several configurations of extractive distillation processes were
presented. Additionally, alternative extractive distillation systems have been elaborated. However,
significant research gaps remain, such as the need for an exhaustive investigation of various control
variables, the impact of certain entrainers on distillation processes, and cost comparisons across
specialized distillation systems. Furthermore, process intensification strategies require additional
research to solve complexity and operability issues. The integration of energy-efficient technologies,
developments in renewable energy consumption, and the development of cost-effective reactive or
split distillation columns will shape the future of distillation operations. These advances will help
the chemical process sector achieve improved energy efficiency, lower environmental impact, and
increased sustainability.
Citation: Aquilon, A.F.; Cargullo,
Keywords: extractive distillation; azeotrope; entrainer
D.M.; Onayan, J.; Sarno, J.; Molino,
V.M.; Lopez, E.C.R. Recent Advances
in Extractive Distillation. Eng. Proc.
2023, 56, 11. https://doi.org/
10.3390/ASEC2023-15261 1. Introduction

Academic Editor: Manoj Gupta

The benefits of distillation in terms of operation and control make it the most preferred
separation method. However, some systems with close boiling points, commonly referred
Published: 26 October 2023 to as azeotropic mixtures, cannot be separated using traditional distillation. This is where
special distillation processes like azeotropic distillation, catalytic distillation, extractive
distillation, pressure-swing distillation, etc., were developed [1,2]. Among these distil-
lation methods, extractive distillation is commonly used in the chemical, petrochemical,
Copyright: © 2023 by the authors.
pharmaceutical, and refining sectors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
Conventional extractive distillation involves at least two columns wherein one of
distributed under the terms and
the components will go overhead, and the other will go either overhead or at the bottom
conditions of the Creative Commons column, depending on the volatilities of the components. The choice of solvent is a
Attribution (CC BY) license (https:// significant additional aspect to consider. It must have a boiling point greater than the
creativecommons.org/licenses/by/ components that need to be separated. It must also be miscible and not form an azeotrope.
4.0/).

Eng. Proc. 2023, 56, 11. https://doi.org/10.3390/ASEC2023-15261 https://www.mdpi.com/journal/engproc

Eng. Proc. 2023, 56, 11 2 of 15

The high energy demand for extractive distillation technology, like other distillation
methods, has an adverse economic and environmental impact [3]. Additionally, improving
the extraction method is motivated by the desire to raise the cost, quality, and yield
of the extraction process. Numerous improvements have been made over time, either
by combining different extraction procedures into a single process, adding more useful
techniques, or changing the original methodology.
The ability of extractive distillation to separate azeotropic mixtures and mixtures
with low relative volatility in various fields has highlighted its significance, resulting in
numerous studies. While some processes reduce energy consumption and improve the
economy, they frequently complicate the process, making operability and control more
challenging. Because feasibility is still a problem, this review paper will thoroughly discuss
and evaluate recent advancements in extraction distillation.

2. Selection of Appropriate Solvent

The extractant or solvent is one of the most important parts of extractive distillation.
One of the parameters in choosing the perfect extractant includes its effect on the azeotropic
system’s relative volatility, the intermolecular forces at atmospheric temperature and
pressure, and electrostatic potential. The perfect extractant can be easily chosen using these
parameters; an extractant should be able to increase the relative volatility of the system; in
terms of this article, an extractant that has stronger attraction to the undesired substance
and weaker attraction to the desired substance is ethanol and ETBE, respectively.
The solvent to be used determines how well an extractive distillation process works.
The selected solvent needs specific properties that increase the process’s feasibility by
lowering energy and solvent consumption [4,5]. However, some commonly used solvents
have not performed well with mixtures exhibiting azeotropes, hence the utilization of ionic
liquids (ILs). A low vapor pressure, melting point, and considerable chemical and thermal
stability are just a few of the remarkable physicochemical characteristics of ILs. Moreover,
there is a need for green technologies using non-hazardous solvents or renewable natural
resources while retaining high-quality, safe extracts.
Distinct solvents and flow rates have distinct impacts on the components’ vapor–liquid
equilibrium and volatility order. This may be used to assess solvents’ performance and
flow rate.
Consider the ternary mixture of acetonitrile, methanol, and benzene, which has three
binary azeotropes. Possible solvents include aniline (AN) and chlorobenzene (CB). The
equilibrium between vapor and liquid in the pairwise combinations of three components
is shown. The vapor–liquid equilibrium curves alter upon the introduction of solvents.
Methanol, benzene, and acetonitrile are volatile compounds in decreasing order of light
to heavy when using AN as the solvent; methanol, acetonitrile, and benzene are volatile
compounds when using CB.

2.1. Supercritical Fluid Extraction (SFE)

Advanced extraction techniques were developed to attain high quality and extraction
yield. Supercritical Fluid Extraction (SFE) enhances the conventional extraction method
by reducing the amount of organic solvent used. SFE starts by heating and pressurizing
the fluid to its critical state before entering the reactor. The solute can readily be sorted
out by gravity. Therefore, the extracted component can be collected at the bottom of the
separator, and the gas can be recycled or released. Despite being more appealing than
other organic solvents like acetone, ethanol, or hexane because of its capacity to surpass
conventional extraction methods, SFE has a disadvantage because it needs high pressure,
which increases the operating cost due to additional safety requirements.

2.2. Extractive Distillation Using Ionic Liquids (ILs)

Various research has been conducted in the study of the behavior of ILs when they are
used as a solvent for extractive distillation because of their properties. The separation of
Eng. Proc. 2023, 56, 11 3 of 15

benzene and cyclohexane, which have similar boiling points and are inclined to combine
into an azeotropic mixture, is one of the most difficult operations in the petrochemical in-
dustry. Adsorption, pervaporation, and liquid–liquid extraction are only a few examples of
the many separation procedures that have been attempted. However, extractive distillation
employing organic solvents as solvents is discovered to be the most effective method.
Ionic liquids are used as solvents, especially in the separation of hydrocarbons, because
they possess a non-volatile nature and high selectivity around aromatic compounds. The
performance of seven ionic liquids for C6 H6 and C6 H12 separation by ED was investigated.
The optimum solvent for this separation has been determined to be the [4bmpy][TCM].
The C6 H12 /C6 H6 , the relative volatility of this ionic liquid, is at its peak at 363.2 K, and
even though it is at its lowest at 403.2 K, it is sufficient to carry out the separation satisfac-
torily. Adding these ionic liquids increases the C6 H12 /C6 H6 relative volatility, reaching
values approximating 15, and breaking the azeotrope. The 1-Ethyl-3-methyl-imidazolium-
dicyanamide was selected as the solvent in the EDC due to the IL’s strong influence on the
relative volatility of aromatic–aliphatic mixtures and its high thermal stability. According
to the results, liquid–liquid extraction and extractive distillation do not separate.
Some compounds used for various industrial applications require a certain purity
level as raw materials. An instance of this is ethanol, which requires 99.5% purity before it
can be used for industries such as paint, cosmetics, and perfumery. The use of ILs shows
the potential to decrease energy consumption. Compared with conventional extractive
distillation, ionic liquid-based extractive distillation (ILED), which produces anhydrous
ethanol, uses less energy. The TAC value of $0.73 × 106 illustrates how the ILED discovered
during the sensitivity analysis for the least energy consumption outperformed alternative
setups.
Additionally, much study has been done to compare which IL best suits a spe-
cific system. As solvents, 1-Butyl-3-methylimidazolium trifluoromethanesulfonate or
[BMIM][CF3 SO3 ], 1-Ethyl-3-methylimidazolium tetrafluoroborate or [EMIM][BF4], and
1-Ethyl-3-methylimidazolium methanesulfonate or [EMIM][MeSO3 ] are used. The best
option among all these ILs for extractive distillation is the stripper with 1-Ethyl-3- methylim-
idazolium methanesulfonate, or [EMIM][MeSO3 ]. The researchers used three methods: an
extractive distillation column, a flash tank, and a stripper. At the EDC, IL raises the relative
volatility of ethanol acetate compared to ethanol. Additionally, it causes the ethanol to flow
downward and the ethyl acetate to go upward. Due to the lower volatility of the IL, it just
flows down the column, leaving the bottom product.
One study employed [MMIM][DMP], 1,3-dimethylimidazolium, to separate the
isopropanol–water mixture. The approach using [MMIM][DMP] as a solvent reduced
TAC by 7.92%, as opposed to the process using a normal solvent, it was discovered. Be-
cause of their outstanding qualities, ILs can be used as better solvents. The success of the
ED processes was examined considering the effects on the economy, energy efficiency, and
environment using the thermodynamic efficiency index, CO2 emissions, and TAC [6].
The separation process is generally optimized to improve the EDC’s operating condi-
tions and design parameters. Due to a broad selection of potential solvents, extractive distil-
lation works effectively in the chemical industry to separate binary or multiple azeotropes,
but it has several drawbacks, including energy consumption. This study offered two
solutions as to how to do this. The first is process intensification using heat-integrated dis-
tillation, divided wall columns, the thermal coupling of columns, and heat pump-assisted
distillation. The second method involves using a green solvent with great selectivity.
Triethylene glycol (TEG) and the solvents [EMIM][Cl] were used in studies that used
the t-butanol dehydration method. According to the findings, utilizing [EMIM][Cl] as an
entrainer as opposed to TEG could lower the total annual cost (TAC) by 13.9% [6].

2.3. Ionic Liquid-Based Mixed Solvents

Conventional ternary extractive distillation (CTED) uses different solvents, such as
EG and ionic liquids. EG and ionic liquids are the common solvents used in extractive
Eng. Proc. 2023, 56, 11 4 of 15

distillation, wherein EG significantly impacts relative volatility. Energy consumption and

operating costs are one of the disadvantages of extractive distillation. An entrainer was
recently developed, combining ionic liquids with another solvent in one shell, which uses a
dividing wall column. Conventional ternary extractive distillation (CTED) using EG and
ionic liquid solvents provide a good outcome, but ionic liquid-based mixed results are
better. Conventional ternary extractive distillation, dividing wall column, and extractive
distillation column reduce energy consumption and operating costs, but extractive dividing
wall column ternary extractive distillation is the most effective in saving energy, as it
reduces up to 7.81% [7].

3. Optimized Configurations for Extractive Distillation

Since different types of systems can be separated, researchers have studied various
kinds of strategies over the years, and the separation process is not a type of process that
applies to all kinds of systems; therefore, all of these strategies are efficient in different
ways for different kinds of systems [8]. These methods use innovative techniques to
provide a more effective way of recovering desired materials without the constraints that
are encountered using conventional ways [9].
Different methods for achieving energy efficiency are being developed as distillation
process designs grow more energy conscious. Some of the processes used in distillation to
become energy efficient are feed flashing, multi-effect distillation, vapor compression, and
heat-integrated distillation column. Feed flashing incorporates a feed-splitting vessel that
creates a two-phase feed directed to their respective feed plates; this reduces the energy
requirement and allows for flexibility in variations in thermodynamic modeling. Heat
integration can be employed in various ways, such as heat exchange between the feed and
rundown or pump-around to optimize heat recovery. Multi-effect distillation integrates the
condenser and reboiler of two columns with different operating pressures. This method
uses the heat the high-pressure condenser releases to operate the low-pressure reboiler.
This method saves 40% of energy costs. Heat-integrated distillation columns operate in
a single unit that consists of a high-pressure section (top/rectifying) and a low-pressure
section (bottom/stripping); this difference in pressure allows for heat transfer between
the columns [10,11]. This type of method reduces reboiler and condenser duties and
significantly reduces energy consumption down to 50% [12].
Other ways of lowering energy requirements are by intensifying the process of dis-
tillation. These include reactive distillation, dividing wall column utilization, and hybrid
separation processes. The wall columns separate the feed, side stream, and product streams.
The product is extracted at the top of the column, and the feed and side streams are on each
side of the wall, preventing contamination. This intensification method reduces capital
costs and energy by up to 45%. A hybrid separation method combines two distinct units
into a single process. This is applied to a design wherein one unit overcomes the limitation
of the other working in a mutually beneficial relationship [13]. In azeotropic distillation,
commonly used methods include extractive and pressure-swing distillation, which are
energy-intensive processes. In these cases, hybrid distillation is recommended.

3.1. Classic, Modified, and Intensified Extractive Distillation

Several separation techniques can be identified while concentrating on extractive
distillation, which is thought to be the most researched type of distillation employed in the
manufacture of bioethanol [8]. The classic extractive distillation configuration is shown in
Figure 1.
 Eng. Proc.
Eng. Proc. 2023,
2023, 56,
56, 11
11 55 of
of 16
16

Eng. Proc. 2023, 56, 11 5 of 15

manufacture of
manufacture of bioethanol
bioethanol [8].
[8]. The
The classic
classic extractive
extractive distillation
distillation configuration
configuration is
is shown
shown in
in
Figure 1.
Figure 1.

Figure 1.
Figure
Figure 1. Classic
1. Classic extractive
extractive distillation.
distillation. Reprinted
distillation. Reprinted with
Reprintedwith permission
withpermission from
permissionfrom [8].
from[8]. Copyright
[8].Copyright (2022)
Copyright(2022) Else-
(2022)Else-
Elsevier.
vier.
vier.
There are alternatives to the classic ED that had a higher recovery by using a recycle
stream There
There are solvent
are
in the alternatives
alternatives to the
to
recoverythe classic
classic
column. ED (Figure
ED that had
that had2).
aa higher
higher recovery
This recovery by using
by using aa recycle
set of configurations recycle
was the
stream in the
stream inpoint
starting solvent
the solvent recovery
recovery
for creating column.
column.
various (Figure 2).
(Figuredesigns.
complex This set
2). This set of configurations
of configurations
Thermally coupledwas was the start-
the start-
systems and ex-
ing
ing point
point for
for creating
creating various
various complex
complex designs.
designs. Thermally
Thermally coupled
coupled
tractive divided wall columns (DWC) were produced from these. These types of extractive systems
systems and
and extractive
extractive
divided wall
divided wall columns
columns (DWC)(DWC) werewere produced
produced from these.these. These
These types
types ofof extractive
extractive distil-
distil-
distillation have been studied since 2012, andfrom reports and comparative analyses have been
lation have
lation have been studied
been 3studied since 2012, and reports and comparative analyses have been writ-
written. Figure showssince 2012, andofreports
an example and comparative
intensified extractive analyses
divided have
wall been writ-
configuration
ten. Figure
ten. Figure 33 shows
shows an an example
example of of intensified extractive
extractive divided
divided wall wall configuration
configuration
wherein it utilizes a reduced numberintensified
of columns compared to the classic configuration,
wherein it
wherein it utilizes
utilizes aa reduced
reduced number
number of of columns
columns compared
compared to to the
the classic
classic configuration,
configuration,
which uses three columns; the intensified DWC uses only two or one. In a two-column
which uses
which uses three
three columns;
columns; the the intensified
intensified DWC
DWC uses uses only
only two
two or or one.
one. In
In aa two-column
two-column
configuration,
configuration, the
the separation
separationand
the separation
andsolvent
solvent recovery
recovery occur
occur
occur on
on
on the
the second
the second
second column
column
column using
using
using an
an
an
configuration, and solvent recovery
extractive DWC;
extractive DWC;
DWC; the the distillate
the distillate
distillate is is collected
is collected
collected in in
in the the partition
the partition
partition and and
and flows flows
flows throughthrough a
through aa recycle recycle
recycle
extractive
stream
stream back
back toto the first
to the
the firstcolumn.
column.This Thisconfiguration
configuration ensures
ensures there
there are are no ethanol
no ethanol
ethanol losses
losses and and
stream back first column. This configuration ensures there are no losses and
provides a higher
provides aa higher recovery.
higher recovery. Moreover,
recovery. Moreover,
Moreover, it it reduces
it reduces capital
reduces capital
capital costs costs
costs by by
by 23% 23%
23% while while
while havinghaving
having thethe the
provides
same energy consumption as a regular
same energy consumption as a regular configuration. configuration.
same energy consumption as a regular configuration.

Figure 2. Modified extractive distillation. Reprinted with permission from [8]. Copyright (2022)
Figure 2.2.Modified
Modifiedextractive
extractivedistillation.
distillation.Reprinted
Reprintedwith
with permission from
Figure permission from [8].[8]. Copyright
Copyright (2022)
(2022) Elsevier.
Elsevier.
Elsevier.
3.2. Assisted Single-Column Extractive Distillation with a Heavy Entrainer
Figure 4 proposes an extractive distillation with one column and a heavy entrainer
(FT-SCED) [14]. It allows for pure light and heavy compounds to be produced from the
flash tank and column overheads. In this review study, we will concentrate on the proposed
design in the first case, which is the separation of an ethanol and water mixture with a
heavy entrainer, ethylene glycol. In comparison to extractive dividing wall columns and
conventional two-column extractive distillation, it was determined that the new process
had high energy efficiencies and low investment costs. A control study also revealed
that the FT-SCED process could be effectively managed. When ±20% feed flow rate and
±10% composition disturbances were introduced, the purities of the product returned to
its original setting for about 10 h, indicating its effectiveness.
 Eng.Proc.
Eng. Proc.2023,
2023,56,56,
1111 6 of 16 6 of 15

Figure 3. Intensified extractive distillation. Reprinted with permission from [8]. Copyright (2022)
Elsevier.

3.2. Assisted Single-Column Extractive Distillation with a Heavy Entrainer

Figure 4 proposes an extractive distillation with one column and a heavy entrainer
(FT-SCED) [14]. It allows for pure light and heavy compounds to be produced from the
flash tank and column overheads. In this review study, we will concentrate on the pro-
posed design in the first case, which is the separation of an ethanol and water mixture
with a heavy entrainer, ethylene glycol. In comparison to extractive dividing wall columns
and conventional two-column extractive distillation, it was determined that the new pro-
cess had high energy efficiencies and low investment costs. A control study also revealed
that the FT-SCED process could be effectively managed. When ±20% feed flow rate and ±
Figure 3. Intensified
10% composition extractive distillation.
disturbances Reprinted
were introduced, the with permission
purities from [8].
of the product Copyright
returned to its(2022)
Elsevier.
original
Figure setting for
3. Intensified about distillation.
extractive 10 h, indicating its effectiveness.
Reprinted with permission from [8]. Copyright (2022)
Elsevier.

3.2. Assisted Single-Column Extractive Distillation with a Heavy Entrainer

Figure 4 proposes an extractive distillation with one column and a heavy entrainer
(FT-SCED) [14]. It allows for pure light and heavy compounds to be produced from the
flash tank and column overheads. In this review study, we will concentrate on the pro-
posed design in the first case, which is the separation of an ethanol and water mixture
with a heavy entrainer, ethylene glycol. In comparison to extractive dividing wall columns
and conventional two-column extractive distillation, it was determined that the new pro-
cess had high energy efficiencies and low investment costs. A control study also revealed
that the FT-SCED process could be effectively managed. When ±20% feed flow rate and ±
10% composition disturbances were introduced, the purities of the product returned to its
original setting for about 10 h, indicating its effectiveness.

Figure 4. Proposed single-column extractive distillation. Reprinted with permission from [14].
Copyright (2023) Elsevier.

3.3. Ternary Extractive Distillation

Conventional distillation (CD) systems are inefficient in terms of energy due to the
remixing of the components [7]. Numerous research has recommended the use of thermo-
couples to address this issue. The first column of the distillation is then proposed to be
managed by thermally coupled systems with side rectifiers and dividing-wall columns.
Operating issues are unavoidable; hence, a modified extractive distillation structure with
thermal couplings (TCD) was proposed to address probable issues.

3.3.1. Alternative Extractive Distillation Systems

Extending the previously mentioned ideas, which are depicted in Figure 5a, an alter-
native system (AD) was proposed, which is depicted in Figure 5b and does not have a
thermocouple. In the alternative configuration, a second column with one feed was used
in the place of the vapor–liquid interface, and a stripping section was added to the side
 managed by thermally coupled systems with side rectifiers and dividing-wall columns.
Operating issues are unavoidable; hence, a modified extractive distillation structure with
thermal couplings (TCD) was proposed to address probable issues.

Eng. Proc. 2023, 56, 11 3.3.1. Alternative Extractive Distillation Systems 7 of 15

Extending the previously mentioned ideas, which are depicted in Figure 5a, an alter-
native system (AD) was proposed, which is depicted in Figure 5b and does not have a
thermocouple. In the alternative configuration, a second column with one feed was used
rectifier to complete the separation process. While the second column (C2) creates the
in the place of the vapor–liquid interface, and a stripping section was added to the side
intermediate as the top stream, the first column (C1) becomes the side stream column,
rectifier to complete the separation process. While the second column (C2) creates the in-
termediate as the
where light
the top component
stream, the firstis eliminated
column as the distillate.
(C1) becomes The column,
the side stream solventwhere
is then recycled
the light component is eliminated as the distillate. The solvent is then recycled to the
to help with the separation and is present in the bottom streams from helpC1 and C2.
Thermally coupled and conventional distillation are reported to
with the separation and is present in the bottom streams from the C1 and C2. Thermally have five parts; however,
coupled and conventional distillation are reported to have five parts; however, the alter-designated
the alternative system has six sections. The goal of this additional section,
nativeas S5 inhas
system Figure 5b, is the
six sections. Thesame
goal as the additional
of this task of thesection,
bottomdesignated
part of the
asTCD
S5 in system,
Fig- which
ure 5b,isispurification.
the same as the task of the bottom part of the TCD system, which is purification.

Eng. Proc. 2023, 56, 11 8 of 16

(a)

(b)
Figure 5.Figure
(a) Extractive distillation
5. (a) Extractive system with
distillation thermal
system coupling
with thermalsystem and side
coupling rectifier
system and (b)
sidePro-
rectifier (b) Pro-
posed alternative extractive distillation system. Reprinted with permission from [3]. Copyright
posed alternative extractive distillation system. Reprinted with permission from [3]. Copyright
(2017) Elsevier.
(2017) Elsevier.
The new alternative system was applied to three case studies to prove its efficiency:
The new alternative system was applied to three case studies to prove its efficiency:
ethanol dehydration, heptane–toluene–aniline mixture, and acetone–methanol–water sys-
ethanol dehydration, heptane–toluene–aniline mixture, and acetone–methanol–water sys-
tem. In the first case, it was determined that AD is advantageous to CD and TCD because
tem. In the
it saves 13.50% more first case,resulting
energy, it was determined
in a 12.40%that AD isin
reduction advantageous to cost.
the total annual CD and TCD because
Also,
CO2 emissions are reduced by 10.60% compared to the CD and 3.20% compared to TCD. cost. Also,
it saves 13.50% more energy, resulting in a 12.40% reduction in the total annual
Similar outcomes were also seen in the other two cases, demonstrating that AD can be
more energy efficient and offer a more sustainable alternative when compared to CD and
TCD.
A structure that implements heat integration between columns for additional energy
 Eng. Proc. 2023, 56, 11 8 of 15

CO2 emissions are reduced by 10.60% compared to the CD and 3.20% compared to TCD.
Similar outcomes were also seen in the other two cases, demonstrating that AD can be more
energy efficient and offer a more sustainable alternative when compared to CD and TCD.
A structure that implements heat integration between columns for additional energy
and CO2 emissions saving was also proposed [3]. It was implemented in AD and CD, as
seen in Figure 6. The results showed that the AD system had superior potential for energy
integration, since it resulted in a reduction in energy consumption compared to the CD
system and a reduction compared to the conventional system with heat integration. Such an
effect leads to a decreased annual total cost. When heat integration between AD columns is
Eng. Proc. 2023, 56, 11 used, CO2 emissions are reduced by 11% compared to the CD with heat. This 9 ofis16
equivalent
to a 39% reduction compared to the CD that is not integrated for extractive distillation.

(a)

(b)
Figure 6. Heat
Figure 6. integration: (a) Conventional
Heat integration: system; system;
(a) Conventional (b) Alternative system. Reprinted
(b) Alternative with permis-
system. Reprinted with permis-
sion from [3]. Copyright (2017) Elsevier.
sion from [3]. Copyright (2017) Elsevier.

3.3.2. Three-Column Extractive Distillation

A three-column extractive distillation (TCED) is usually used to separate azeotropic
mixtures. TCED processes work in two types: XYX and XXY. The difference between the
two types is shown in Figures 7 and 8, wherein D3 and B1 are equal for XYX, and D3 and
B1 for XXY are not equal. As shown in both figures, condenser 1 has many roles.
 Eng. Proc. 2023, 56, 11 9 of 15

3.3.2. Three-Column Extractive Distillation

A three-column extractive distillation (TCED) is usually used to separate azeotropic
mixtures. TCED processes work in two types: XYX and XXY. The difference between the
Eng. Proc. 2023, 56, 11 two types is shown in Figures 7 and 8, wherein D3 and B1 are equal for XYX, and D3 and 10 of 16
Eng. Proc. 2023, 56, 11 10 of 16
B1 for XXY are not equal. As shown in both figures, condenser 1 has many roles.

Figure7.7.XYX
Figure XYX Type.
Type. Reprinted
Reprinted withwith permission
permission from from [15]. Copyright
[15]. Copyright (2022) Elsevier.
(2022) Elsevier.
Figure 7. XYX Type. Reprinted with permission from [15]. Copyright (2022) Elsevier.

Figure 8. XXY Type. Reprinted with permission from [15]. Copyright (2022) Elsevier.
Figure8.8.XXY
Figure XXYType.
Type. Reprinted
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with permission
permission fromfrom
[15]. [15]. Copyright
Copyright (2022) (2022) Elsevier.
Elsevier.
The feed split method is developed to help the distillate flow, feed flow, and the role
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3.3.3.
3.3.3.Comparison
Comparisonof of
Conventional Ternary
Conventional Extractive
Ternary Distillation
Extractive and VRHP
Distillation and VRHP
3.3.3.Conventional
Comparisonternary of Conventional Ternary Extractive
extractive distillation (CTED) works Distillation and VRHP
directly (DCED) and indi-
Conventional ternary extractive distillation (CTED) works directly (DCED) and indi-
rectlyConventional
(ICED). These two CTEDs
ternary are usually
extractive used to separate
distillation (CTED) the
worksbinary azeotrope,
directly (DCED) which
andwhich
indi-
rectly
is
(ICED).
considered
These two
expensive.
CTEDs
Based on
are calculation
the
usually used in
to separate
this study,
the binary
economic and
azeotrope,
environ-
rectly (ICED). These
is considered two CTEDs
expensive. Based are usually
on the used to in
calculation separate
this the binary
study, economicazeotrope, which
and environ-
mental
ismental ICED performance
considered expensive. isBased
much better
on thethan DCED. Since
calculation in it is study,
this expensive, a new method
economic and environ-
known asICED a vapor performance
recompression is much
heat pumpbetter(VRHP)
than DCED.
is beingSince
studied it istoexpensive, a new method
improve economic
mental
knownICED as performance
a vapor is much better
recompression than DCED.
heat pump (VRHP) Since it is expensive,
is being studied toaDCED)
new method
improve eco-
efficiency and environmental performance [16]. VRHP works directly (VRHP-
known
nomic
and
as a vapor
efficiency
indirectly
recompression
and environmental
(VRHP-ICED).
heat
The calculation
pump
performance(VRHP)
for ICED and
is
[16].
CED
being
VRHP studied
does not works to improve
directly
correlate
eco-
with(VRHP-
nomic
DCED)efficiency
VRHP-DCED and and and (VRHP-ICED).
indirectly environmental
VRHP-ICED, wherein six performance
Thedifferent [16].
separation
calculation VRHP
for ICEDsequences
and works directly
for both
CED does VRHP (VRHP-
not correlate
DCED)
are
with and
determined.
VRHP-DCEDindirectly (VRHP-ICED).
For VRHP-DCED,
and VRHP-ICED, The
sequence calculation
V provides
wherein for ICED
the lowest
six different and CED
steam costs,
separation does not correlate
and fourfor both
sequences
with VRHP-DCED and VRHP-ICED, wherein six different
VRHP are determined. For VRHP-DCED, sequence V provides the lowest steam separation sequences for costs,
both
VRHP are determined. For VRHP-DCED, sequence V provides
and four sequences (I, II, III, IV) are much better in terms of annual cost than CED se- the lowest steam costs,
and four sequences
quences, (I, II, III,(I,
and four sequences IV)II, are much
III, IV) are better in terms
better for of annualefficiency.
environmental cost thanHowever,
CED se-
quences, and four sequences (I, II, III, IV) are better for environmental
II’ and IV’ made VRHP-ICED more environmentally efficient than CED sequences and I,’ efficiency. However,
Eng. Proc. 2023, 56, 11 10 of 15

sequences (I, II, III, IV) are much better in terms of annual cost than CED sequences, and
four sequences (I, II, III, IV) are better for environmental efficiency. However, II’ and IV’
made VRHP-ICED more environmentally efficient than CED sequences and I,’ IV,’ and VI’
sequences [17].

3.3.4. Extractive Distillation with Two Columns and Rectifier

The dynamics of a traditional three-column configuration are compared with a non-
conventional two-column configuration with a side rectifier since a conventional ternary
extractive process requires three columns, but thermally coupled side stream/rectifier
columns have demonstrated economic advantages. Furthermore, it is necessary to investi-
gate dynamic controllability because process disruptions are unavoidable and may affect
product quality, safety, and environmental concerns.
Both feed flow rate and feed composition disturbances are compared between the
conventional and non-conventional configurations. A 1-min dead time was employed, and
a disturbance of ±10% was introduced. The non-conventional process’s dynamic response
was observed to be inferior to the conventional process. It is possible to conclude that, al-
though the non-conventional process has a lower energy cost than the conventional process,
it still needs to be studied because of how poorly it responds dynamically to disturbances.

3.3.5. Comparison of Heterogeneous Azeotropic Distillation and Extractive Distillation

Methods for Ternary Azeotrope Ethanol/Toluene/Water Separation
Comparisons are made between two techniques for separating the ternary azeotrope
ethanol/toluene/water. These processes are extractive distillation and heterogeneous
azeotropic distillation. This study covered four solvents for extractive distillation, including
ethylene glycol, glycerol, N-propylbenzene, and n-butylbenzene. The authors’ solvent of
choice was glycerol. Due to the immiscibility of water and toluene, only two columns are
needed after selecting the solvent [18].
It was discovered that ED had a lower cost of energy than HAD—to be more precise,
18.8% and 39.3%, respectively [6]. Overall, it was found that in terms of economics, ED is
more desirable than partially heat-integrated HAD.

3.4. Hybrid Reactive-Extractive Distillation Configurations

Three processes were used in this study [19], namely the common process (CP),
reactive extractive dividing wall process (REDWP), and reactive extractive distillation
process (REDP). Process design optimization was created using a simulation software
called Aspen. The diagrams of each process discussed above are shown below, respectively.
The common process (Figure 9) utilizes three distillation columns. The REDP (Figure 10)
is a modified process of the classic one, where the distillation and reactor columns are
combined to form a device with azeotropic distillation. The REDWP (Figure 11) uses a
single column for the azeotropic and extractive distillation process. Economic optimization
results showed that the REDWP outperformed the REDP and CP, and it amounted to a total
cost of 15% and 9% less than the REDP and CP, respectively. In terms of environmental opti-
mization, REDWP again stood higher against its counterparts, showing overall remarkable
results regarding greenhouse gas emissions and water pollution as well as environmental
benefits such as lower biological toxicity. Regarding exergy losses, REDP and REDWP
showed that these processes had great thermodynamic efficiency and less exergy loss.
 tion results showed that the REDWP outperformed the REDP and CP, and it amounted t
a total cost of 15% and 9% less than the REDP and CP, respectively. In terms of environ
mental optimization, REDWP again stood higher against its counterparts, showing overa
remarkable results regarding greenhouse gas emissions and water pollution as well a
Eng. Proc. 2023, 56, 11 environmental benefits such as lower biological toxicity. Regarding exergy
11 oflosses,
15 RED
and REDWP showed that these processes had great thermodynamic efficiency and les
exergy loss.

Figure
Eng. Proc. 2023, 56, 11 Figure
9. Common 9. Common
process process ofether
of ethyl tert-butyl ethyl production.
tert-butyl ether production.
Reprinted Reprinted with
with permission frompermission
[19]. 12 from
of 1
Eng. Proc. 2023, 56, 11 [19]. Copyright (2022) Elsevier. 12 of 16
Copyright (2022) Elsevier.

Figure
Figure 10. Reactive 10. Reactive
extractive extractive
distillation distillation
process. process.
Reprinted withReprinted withfrom
permission permission from [19]. Copyrigh
[19]. Copyright
(2022)
Figure 10. Reactive Elsevier.
extractive distillation process. Reprinted with permission from [19]. Copyright
(2022) Elsevier.
(2022) Elsevier.

Figure 11. Reactive extractive dividing wall process. Reprinted with permission from [19]. Copy
Figure11.
Figure right
11. Reactive
Reactive (2022) Elsevier.
extractive
extractive dividing wall
dividing wall process.
process. Reprinted
Reprinted with
with permission
permissionfrom
from[19].
[19].Copy-
Copyright
right (2022) Elsevier.
(2022) Elsevier.
4. Research Gaps
4. Research Gaps
4. Research Gaps Reactive distillation, which combines chemical reaction and distillation into a sing
Reactive distillation,
Reactive distillation, which
unit, has emergedwhichcombines
combines chemical
as a promising chemical reaction
technology
reaction and
withdistillation
and the intointo
potential
distillation atosingle
transform
a single chemica
unit, has emerged as
processes.a promising
Reactive technology
distillation with
offers the potential
benefits such
unit, has emerged as a promising technology with the potential to transform chemical asto transform
enhanced chemical
yield, lower energy usag
processes. Reactive distillation offers benefits such as enhanced yield, lower
processes. Reactive distillation offers benefits such as enhanced yield, lower energy usage,processe
and streamlined process flows by integrating these two energy
usually usage,
independent
and streamlined
and streamlined process
Despite
process theflows by
byintegrating
advances
flows achieved these
integrating thetwo
inthese usually
field,
two there
usually independent
areindependent processes.
still significant research gaps tha
processes.
Despite the advances
must beachieved
addressed in in
theorder
field,tothere
fully are stillits
realize significant
promise research
and gaps
facilitate itsthat
widespread appl
Despite the advances achieved in the field, there are still significant research gaps that must
must be addressed
cationin order
in to fully realize its promise and facilitate its widespread appli-
industry.
be addressed in order to fully realize its promise and facilitate its widespread application
cation in industry. Although several authors have investigated various grounds for studying, som
in industry.
Although space
severalremains
authorslefthave investigated
for further various
research. grounds
For one, therefor studying,
is usually some
a lack of parameters t
Although several authors have investigated various grounds for studying, some space
space remains left
placeforunder
further research.
study. For one,the
For instance, there is usually process
optimization a lack of parameters
only focused on to a single facto
remains left for further research. For one, there is usually a lack of parameters to place
place under study.
suchFor instance, [20].
as pressure the optimization
Only one article process[21]only focused
reported on a single
on reduced factor,
capital costs by utilizin
under
such asstudy. For [20].
pressure instance,
Only the
oneoptimization
article [21] processon
reported only focused on a costs
single factor, such as
different configuration configurations ofreduced
extractive capital
distillationbycolumns.
utilizing One could fu
different configuration
ther obtain configurations of extractive
data and information distillation
on the differences columns. One controls,
in process could fur- parameters, an
ther obtain datadetailed
and information
information on ontherecovery.
differences In in process
[22], controls,
entrainer parameters,
selection is another andone that is di
detailed information
cussed;on recovery.
however, In [22],
there entrainer
is a lack selection
of research on howis another
a specificoneentrainer
that is dis-affects the distilla
cussed; however,tionthere is a lack
process [14].of research on how a specific entrainer affects the distilla-
Eng. Proc. 2023, 56, 11 12 of 15

pressure [20]. Only one article [21] reported on reduced capital costs by utilizing different
configuration configurations of extractive distillation columns. One could further obtain
data and information on the differences in process controls, parameters, and detailed
information on recovery. In [22], entrainer selection is another one that is discussed;
however, there is a lack of research on how a specific entrainer affects the distillation
process [14].
One study [23] showed that, even though computer-aided molecular design is a new
method for efficiency, two aspects must be considered in screening solvents: price and
source. Intensification and integration techniques are used for capital cost and energy
consumption but are much more complex than traditional processes. Another study [14]
discovered that a vapor recompression heat pump (VRHP) is better than conventional
ternary extractive distillation. As specialized distillations are created, a comparison of
specialized and vapor recompression heat pumps should be made regarding their financial
costs and environmental performances.
With regard to process intensification, a study [2] showed that, even though some
process intensification technologies increase economic efficiency and reduce energy con-
sumption, they also make the process more complex than it would otherwise be and make
it harder to operate and monitor. Another study [24] indicated that different special distil-
lations reduce energy consumption using inorganic salts as the entrainer. More research
should be conducted regarding thermally coupled distillation columns with inorganic salt
entrainers.
Another major research gap in reactive distillation is the development of comprehen-
sive kinetic models that adequately represent the complicated chemical processes that occur
within the distillation column. Many existing models are very simplistic, assuming perfect
performance and ignoring the influence of variables like as temperature and pressure
fluctuations down the column. More precise and thorough kinetic models are required for
improving reactor design, predicting product quality, and ensuring the reactive distillation
process’s stability.
In reactive distillation, the intricate interplay between mass transfer and chemical reac-
tion kinetics remains an extremely challenging field of research. Understanding how mass
transfer limitations impact reaction rates and selectivity is critical when designing efficient
reactive distillation columns. The influence of parameters such as catalyst distribution,
phase equilibrium, and column geometry on mass transfer within the reactive distillation
system should be studied.
A significant research gap exists in the behavior of multiphase systems within reactive
distillation columns. Understanding fluid dynamics, especially liquid-liquid and vapor-
liquid interactions, is critical for improving column design and operation. Current research
frequently falls short of the required depth in investigating the intricate fluid flow patterns
and phase distributions that influence the overall performance of reactive distillation
systems.
The lack of established design standards for reactive distillation is a significant problem
for both researchers and industry practitioners. Establishing thorough standards that take
into account varied reaction systems, feed compositions, and operating circumstances
is critical for guaranteeing consistency and dependability in reactive distillation process
design and scale-up. To close the research gap, academia and industry must work together
to establish globally applicable design concepts.
While reactive distillation has demonstrated promise in the laboratory, there is a
significant research gap in understanding the issues associated with scaling these processes
up for commercial applications. To aid the effective transition of reactive distillation from
the laboratory to full-scale production, factors such as heat and mass transfer restrictions,
potential equipment failures, and the effects of large-scale operation on reaction kinetics
must be extensively explored.
To summarize, while reactive distillation has immense promise for enhancing chemical
processing, various research gaps must be addressed before its full potential can be realized.
Eng. Proc. 2023, 56, 11 13 of 15

Researchers encounter several hurdles, ranging from the development of accurate kinetic
models to the understanding of fluid dynamics in multiphase systems. Bridging these gaps
necessitates multidisciplinary cooperation, novel techniques, and a collaborative effort
from academics and industry. By filling these research gaps, we can pave the road for
reactive distillation to become more widely used and contribute to the development of
more sustainable and efficient chemical processes.

5. Future Outlook
Technological breakthroughs are expected to affect the future of reactive distillation.
Process control and automation are two important areas of growth. Artificial intelligence
and machine learning algorithms in advanced control systems can optimize the operation
of reactive distillation columns in real-time. This not only improves process efficiency but
also increases reactive distillation’s responsiveness to changing feedstock compositions and
reaction conditions. Furthermore, the use of online sensors and advanced analytics will
be critical in monitoring and improving reactive distillation operations. These technolo-
gies allow for real-time data analysis, enabling for faster decision-making and proactive
modifications to maintain optimal performance and product quality.
The future of reactive distillation will most likely see an increase in R&D focusing on
developing and enhancing catalytic systems particularly designed for the unique conditions
within distillation columns. For reactive distillation operations to be as efficient as possible,
advanced catalysts with better stability, selectivity, and resistance to deactivation will
be required. Furthermore, research into multifunctional catalysts capable of catalyzing
numerous reactions at the same time might lead to more streamlined and varied processes.
This approach is consistent with the increased emphasis on sustainability since it allows for
the design of processes with fewer reaction stages and lower environmental impact.
As the global chemical industry shifts toward sustainability, the integration of renew-
able feedstocks is anticipated to become more important in the future of reactive distillation.
Because of the adaptability of reactive distillation, it can handle a wide range of feedstock
compositions, including those obtained from biomass or other renewable sources. This
transition toward sustainable feedstocks is consistent with the industry’s overall trend
toward green and circular chemistry. Furthermore, the development of reactive distillation
techniques for converting waste streams into useful products has the potential to contribute
to the circular economy. By utilizing reactive distillation’s capacity to simultaneously
execute reactions and separate products, the technique may play a critical role in converting
waste into a resource, minimizing environmental impact and increasing resource efficiency.
Because of its capacity to allow complicated reaction sequences and create high-purity
products, reactive distillation is poised to be an important player in the future of customized
and specialized chemical manufacturing. The technology’s flexibility enables the efficient
synthesis of a diverse spectrum of specialized compounds with specific features. This
customization is especially useful in sectors like pharmaceuticals, where precise control of
reaction conditions and product purity is critical. Reactive distillation may find more use
in pharmaceutical manufacture in the future, allowing for more efficient and sustainable
production procedures. This shift is being driven not just by economic reasons, but also
by a regulatory push in the pharmaceutical industry toward greener and more efficient
production techniques.
The integration of reactive distillation with other novel technologies offers a potential
development horizon. Hybrid processes that combine reactive distillation with techniques
such as membrane separation or sophisticated separation technologies have the potential
to improve overall process efficiency and minimize energy usage. Combining reactive
distillation with membrane technology, for example, can increase selectivity by selectively
permeating specific components, resulting in improved product purity. Exploring and
enhancing these hybrid techniques will be critical for tackling specific difficulties and
unlocking new potential for process intensification.
Eng. Proc. 2023, 56, 11 14 of 15

Ultimately, the future of reactive distillation is defined by a convergence of scientific

improvements, sustainability objectives, and growing industrial application. From im-
proved catalytic systems to the integration of renewable feedstocks and the development of
hybrid processes, the reactive distillation trajectory has considerable potential for transform-
ing the landscape of chemical processing. As the chemical industry moves toward more
ecological and efficient methods, reactive distillation stands out as a versatile and strong
technology capable of fulfilling future needs. The entire potential of reactive distillation
may be achieved via continued research, innovation, and cooperation, contributing to a
more sustainable and resilient chemical industry in the years to come.

Author Contributions: Conceptualization, E.C.R.L.; writing—original draft preparation, A.F.A.,

D.M.C., J.O., J.S. and V.M.M.; writing—review and editing, E.C.R.L.; supervision, E.C.R.L.; project
administration, E.C.R.L. All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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