Separation and Purification Technology 272 (2021) 118887

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Separation and Purification Technology

journal homepage: www.elsevier.com/locate/seppur

Novel energy-saving methods to improve the three-column extractive

distillation process for separating ethyl acetate and ethanol using furfural
Cong Duan , Chunli Li *
National-Local Joint Engineering Laboratory for Energy Conservation in Chemical Process Integration and Resources Utilization, School of Chemical Engineering and
Technology, Hebei University of Technology, Tianjin 300130, China

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

Keywords: A mixture of ethyl acetate and ethanol is difficult to separate because of a minimum-boiling homogeneous
Vapor–liquid coupling azeotrope. The characteristics of the ethyl acetate/ethanol system are analyzed. The energy-saving potential of a
Heat integration three-column extractive distillation process to separate the system is explored. The effects of the distillate
Partial condensation
composition of pre-concentrator, the temperature of solvent feed and operating pressures are studied. Energy-
Extractive distillation
Energy saving
saving processes including heat pump distillation, heat integration and partial condensation are proposed. A
Ethyl acetate/ethanol novel way of partial condensation is proposed and compared with the conventional way. An innovative method
of vapor–liquid coupling between the per-concentrator and the extractive column is then proposed. It is more
economical and energy-efficient than the above processes. Besides, based on the vapor–liquid coupling process,
two further improvements are proposed through heat integration and through compressors. All processes are
optimized using the sequential iterative optimization procedure with the minimum total annual cost as the
target. Compared with the conventional process operated at 101.3 kPa, the two improved processes can reduce
total annual cost by more than 52%, reduce energy consumption by more than 60%, and reduce CO2 emissions
by more than 61%.

emissions and high total annual cost (TAC) [15]. Therefore, it is

1. Introduction
Ethyl acetate (EA) is not only an important raw material and solvent
[1], but a popular product in organic synthesis [2]. During the synthesis
process of EA, a mixture of EA and ethanol is difficult to separate
because of a minimum-boiling homogeneous azeotrope [1] with a
composition of 53.5 mol % EA at 101.3 kPa as given in Fig. 1. Many
methods have been studied to separate EA and ethanol including
pressure-swing distillation [3–5], extractive distillation (ED) [1,6,7],
and liquid–liquid extraction [8]. In this work, ED with furfural as the
entrainer [9–11] is studied.
ED is widely used to separate binary close-boiling/azeotropic mix­
tures by introducing a solvent to change the relative volatility between
the feed components [12]. When the feed composition is dilute and far
from the azeotropic composition, a three-column extractive distillation
(TCED) process is usually used. The three columns are pre-concentrator
(C1), extractive column (C2) and solvent recovery column (C3) [13]. As
a kind of special distillation [14], ED not only has the advantages in
operation and control, but also has the disadvantage of high energy
consumption. High energy consumption is accompanied by high CO2
necessary to explore energy-saving processes for the TCED.
In the literature, many methods and techniques have been used to
reduce energy consumption and intensify the process for the ED process,
including optimization process improvement [16,17], heat integration
[18,19], heat pump [20,21], partial condensation [22,23], column
combination [9,24,25], etc.
Among all the optimization variables, distillate composition of the
C1 (xD1) is an important one [13,26]. Operating pressure of a column is
getting more and more attention. It has an influence on the phase
equilibrium [16,17,27], entrainer selection [10], and the diameter of the
columns.
There are two cases of heat integration in the ED process, one of
which is double-effect heat integration. The double-effect heat integra­
tion includes two columns with different pressures. The overhead vapor
of the high-pressure column is used as the heat source in the reboiler of
the low-pressure column [28]. The other case is to use economizers to
preheat the feed streams with the hot solvent from the C3 base [29]. A
partial heat-integrated TCED scheme to separate acetonitrile/water
proposed by Qi et al. [19] could reduce energy consumption by 36.92%,
and reduce TAC by 27.26% compared with the conventional TCED

* Corresponding author.
E-mail address: lichunli_hebut@126.com (C. Li).

https://doi.org/10.1016/j.seppur.2021.118887
Received 11 January 2021; Received in revised form 20 April 2021; Accepted 29 April 2021
Available online 9 May 2021
1383-5866/© 2021 Elsevier B.V. All rights reserved.
C. Duan and C. Li Separation and Purification Technology 272 (2021) 118887

Nomenclature P electric power, kW

P1 operating pressure for the pre-concentrator, kPa
Abbreviations P2 operating pressure for the extractive column, kPa
COP coefficient of performance P3 operating pressure for the solvent recovery column, kPa
EA ethyl acetate PC-1 the process in which a partial condenser is installed in the
ED extractive distillation pre-concentrator.
NRTL non-random two-liquid PC-2 the process in which a partial condenser is installed in the
TCED three-column extractive distillation extractive column
TAC total annual cost, k$/y Q energy consumption, kW
VLE vapor–liquid equilibrium QW reboiler duty, kW
QW1 the reboiler duty of the pre-concentrator, kW
Symbols QW2 the reboiler duty of the extractive column, kW
C1 pre-concentrator QW3 the reboiler duty of the solvent recovery column, kW
C2 extractive column QD condenser duty, kW
C3 solvent recovery column QD1 the condenser duty of the pre-concentrator, kW
C% carbon content QD2 the condenser duty of the extractive column, kW
D distillate rate, kmol/h QD3 the condenser duty of the solvent recovery column, kW
S solvent flowrate, kmol/h Qh the heat rejected at high temperature, kW
hProc the enthalpy of the utility steam used in the process, kJ/kg RR reflux ratio
hwater,373.15K the enthalpy of water at 373.15 K, kJ/kg Ts the temperature of solvent feed, K
HP-1 heat pump distillation process for the pre-concentrator TFTB the theoretical flame temperature, K
HI-12 heat integration process between the pre-concentrator and Tstack the stack temperature, K
the extractive column T0 ambient temperature, K
Nt1 the number of the theoretical stages of the pre- ΔT temperature difference, K
concentrator ΔTm the minimum temperature difference, K
Nt2 the number of the theoretical stages of the extractive VLC-12 the vapor–liquid coupling process between the pre-
column concentrator and the extractive column
Nt3 the number of the theoretical stages of the solvent recovery VLC-HI the improved VLC-12 process by heat integration
column VLC-C the improved VLC-12 process by a compressor
Nf1 the feed stage location of the pre-concentrator W the work input for the compressor, kW
Nf2 the feed stage location of the extractive column xD1 distillate composition of the pre-concentrator
Nfs the feed stage location of solvent x liquid molar fraction of ethyl acetate
Nf3 the feed stage location of the solvent recovery column y vapor molar fraction of ethyl acetate
NHV the net heating value of fuel, kJ/kg
Opt the process that optimizing more variables

without heat integration. Another two-column ED process with optimal

Fig. 1. T–xy diagram for EA/ethanol at 101.3 kPa.
partial heat integration to separate acetone and methanol [30] could
reduce energy consumption by 32.2% and reduce TAC by 24.4%
compared with the base case without heat integration.
The energy can also be reduced by upgrading low-temperature waste
heat to a higher temperature with a heat pump [31]. CO2 emissions can
be greatly reduced in this way. A partial vapor recompression heat pump
process to separate acetone and water by two-column ED can reduce
CO2 emissions by 55.92%, despite an 18.12% increase in TAC (3-year
payback period) compared with the case without heat pump [30]. Cui
et al. [32] shown that using heat pumps in the ED process to separate
EA/isopropanol/water allowed for a 37.16% reduction in CO2 emis­
sions, and a 34.78% reduction in TAC.
Partial condensers can also be used for the TCED to provide a vapor
feed to reduce the energy. Errico et al. [22] proposed various alternative
sequences for bioethanol production and showed the energy-saving
potential of partial condensers. Zhang et al. [23] replaced the C1 and
its partial condenser with a pre-stripper. Using a pre-stripper in TCED
could save TAC by 23.6% and 14.4% compared with using a pre-
concentration column with a total condenser for acetonitrile/water/
(ethylene glycol) system and N-propanol/water/(N-methyl-2-pyrroli­
done) system respectively (note that the brackets indicate the solvent).
Column combination [9,24,25] is also very popular in the ED pro­
cess. For the TCED, C1 and C2 can be combined [9], or C1 and C3 can be
combined [24]. Liang et al. [24] combined C1 and C3 for a conventional
TCED process and showed that the column combination could save TAC
by 12.1% and 14.7% for separating acetonitrile/water/(ethylene glycol)

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C. Duan and C. Li
Fig. 2. The sequential iterative optimization procedure.
system and isopropanol/water/(dimethyl sulfoxide) system respec­
tively. An et al. [9] proposed two conventional TCED processes at at­
mospheric pressure and their corresponding energy-saving processes in
which C1 and C2 were combined. They showed that the column com­
bination could save TAC by 15.2% and 17.6% for separating EA/
ethanol/(furfural) system and N-propanol/water/(N-methyl-2-pyrroli­
done) system respectively.
It is worth mentioning that for many systems such as ethanol/water/
(ethylene glycol) system and acetonitrile/water/(dimethyl sulfoxide)
system, the separation in the extractive column becomes easier with a
decreasing pressure. Moreover, the light key component is the overhead
product of the extractive column. However, the separation of EA and
ethanol using furfural is different, which will be discussed in this work.
Based on an above conventional TCED process to separate the EA/
ethanol system [9], the purpose of this work is to explore its energy-
saving potential.
The effects of some key variables are analyzed. The characteristics of
the EA/ethanol/(furfural) system are obtained. Several energy-saving
processes including a heat-pump distillation process, a heat-integrated
process, a conventional partial-condensation process, a novel partial-
condensation process and an innovative vapor–liquid coupling process
are proposed. Based on the innovative vapor–liquid coupling process,
further improvements through heat integration and vapor recom­
pression are explored. All the processes are optimized using the
sequential iterative optimization procedure with minimum TAC as the
target. After the optimal processes are obtained, the CO2 emissions and
energy consumption are also calculated for the processes.
2. Methods of simulation, optimization and evaluation
In this work, all the simulations and optimizations are carried out
using Aspen Plus V11 software. The sequential iterative optimization
procedure is selected for process optimization. The optimization target is
to minimize TAC. Therefore, TAC is the objective function for every
process. After the optimal processes with the minimum TAC are
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Separation and Purification Technology 272 (2021) 118887
obtained, energy consumption, CO2 emissions and coefficient of per­
formance (COP, if there is a heat pump in the process) will be also
calculated to evaluate the processes.
2.1. Thermodynamic model
Thermodynamic model is very important in predicting vapor–liquid
equilibrium (VLE) in the simulation, which affects the accuracy of the
calculation results [33]. According to the work by An et al. [9], non-
random two-liquid (NRTL) model is selected for this system. The bi­
nary parameters of NRTL model have been slightly modified based on
the literature [9]. The source of the binary parameters for EA/furfural
system was changed from VLE-IG to NIST-IG. The Table A1 in Supple­
mentary material shows the three sets of binary parameters used for
NRTL model. The accuracy of the binary parameters is verified by the
experimental data [34–38]. Fig. A1 (a)− (c) shows that the experimental
data fits well with the model for the three binary systems.
2.2. Optimization procedure
During the optimization, the objective function is TAC and the target
is to minimize the TAC. Optimization variables include three operating
pressures (P1, P2, P3), three total numbers of the theoretical stages (Nt1,
Nt2, Nt3), three feed stage locations (Nf1, Nf2, Nf3), the feed stage
location of solvent (Nfs), the solvent flowrate (S), xD1, and the solvent
feed temperature (Ts).
The sequential iterative optimization procedure [9,19,24] is used in
this work. Fig. 2 shows the procedure, where the three columns are
optimized in the sequence of C1, C2, C3, C1… until the TAC is the
minimum. The detailed steps and some special cases are in the Supple­
mentary material.
2.3. Economic evaluation
TAC is calculated from:
C. Duan and C. Li Separation and Purification Technology 272 (2021) 118887

Fig. 3. Base case: the conventional TCED process at 101.3 kPa proposed by An et al.[9]

capital cost
TAC = + operating cost (1) [CO2 ]Emiss = QFuel ⋅FuelFact (3)
payback period
Eq. (3) shows that the CO2 emissions are related to the amount of fuel
The capital cost, payback period and operating cost are calculated
burnt QFuel and the effect of the fuel FuelFact.
according to the formulas listed in Table A2, assuming an annual
operating time of 8000 h. The costs of pumps, valves and reflux drums QProc ( ) TFTB − T0
QFuel = hProc − hwater,373.15K (4)
are ignored at the conceptual design stage [39]. The coefficient M&S is λProc TFTB − TStack
1638.2 (2018) [40,41].
The formulas to calculate the vacuum system costs are from the book where λProc (kJ/kg) and hProc (kJ/kg) represent the latent heat and the
of Seider et al. [42]. Liquid-ring pumps are selected due to the lower cost enthalpy of the utility steam used in the process, respectively. The
than that of steam-jet electors. An isentropic compressor model is used theoretical flame temperature (TFTB) of 2073.15 K, the stack tempera­
in the simulation with an isentropic efficiency of 0.4 and a mechanical ture (TStack) of 433.15 K and the ambient temperature of 293.15 K are
efficiency of 0.92 to calculate the power of the liquid-ring pump. The used in Eq. (4). QProc is the heat duty required by the process. The boiler
amount of air leakage is estimated from the equation in the Table A1. feedwater is assumed to be at 373.15 K with an enthalpy of 419 kJ/kg.
When the air leakage is added to the overhead vapor, a flash model is ( α )( C% )
used in the simulation. It gives a vapor leaving the reflux drum and FuelFact = (5)
NHV 100
entering the vacuum system. The flash is set at a temperature of 323 K
and a pressure drop of 5 kPa. where α (=3.67) is the ration of molar masses of CO2 and C, while NHV
represents the net heating value of a fuel with a carbon content of C%.
2.4. Energy consumption evaluation Heavy fuel oil is used in this work. The NHV and C% are 39771 kJ/kg
and 86.5, respectively [30].
Energy consumption (Q, kW) is mainly composed of thermal energy The CO2 emissions of electricity are 51.1 kg CO2/GJ according to the
consumption (reboiler duty (QW, kW)) and electrical energy consump­ article [46]. Using enthalpy data from Aspen V11 and using the equa­
tion. Considering the thermoelectric efficiency, it is assumed that elec­ tions from (3) to (5), the calculated CO2 emissions of LP steam, MP steam
tric power (P, kW) can be converted into the equivalent thermal energy and HP steam are 98.44 kg CO2/GJ, 104.53 kg CO2/GJ and 135.75 kg
by a factor of 3 [43,44]. So, the energy consumption is calculated from: CO2/GJ, respectively.

Q = QW + 3P (2)
2.6. Heat pump performance evaluation

2.5. CO2 emissions evaluation The heat pump performance is evaluated by the COP, which is pro­
posed by Bruinsma and Spoelstra [47]. It is the ratio of the heat rejected
CO2 emissions are considered for environmental impact [23]. The (Qh) at high temperature to the work input of the compressor (W):
hot utility of the reboiler is the steam which is produced by steam boilers Qh
from the combustion of fuel. The CO2 emissions from the steam boilers COP = (6)
W
are calculated from [45]

Table 1
Optimal design results.
Optimization results Base case Opt HP-1 HI-12 PC-1 PC-2 VLC-12 VLC-HI VLC-C

Capital cost (k$) 3315 3059 4855 2975 2558 2856 2400 2547 2567
Energy cost (k$/y) 3685 2476 1402 1698 2585 2189 1662 1425 1293
Q (kW) 8531 6176 4211 4092 6500 5387 4004 3221 3393
CO2 (kg/h) 3359 2220 1136 1520 2326 1961 1485 1293 1138
TAC (k$/y) 4790 3496 3021 2690 3437 3141 2462 2274 2148
Q saving* – 27.6% 50.6% 52.0% 23.8% 36.9% 53.1% 62.2% 60.2%
CO2 reduction* – 33.9% 66.2% 54.7% 30.8% 41.6% 55.8% 61.5% 66.1%
TAC saving* – 27.0% 36.9% 43.8% 28.2% 34.4% 48.6% 52.5% 55.2%
*
Compared with the base case, which is from the reference article [9].

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C. Duan and C. Li
Fig. 4. x–y diagram for EA/ethanol at 101.3, 50, and 200 kPa.
Fig. 5. x–y diagram for pseudo EA/ethanol system at 101.3, 50, and 200 kPa
with furfural as the solvent (the composition of furfural is 75%).
Plesu et al. [48] proposed that when the COP was higher than 10, the
heat pump was clearly recommended; when the COP was between 5 and
10, a detailed evaluation should be carried out.
3. Results and discussion
3.1. Base case
Fig. 3 shows the conventional flowsheet for the TCED process pro­
posed by An et al. [9]. The product specifications are 99.5 mol% EA and
99.5 mol% ethanol. The feed is a saturated liquid with a composition of
25 mol% EA and a flow rate of 300 kmol/h. The operating pressure of
each column is set at 101.3 kPa. The xD1 is specified to be 45.0 mol% EA,
which near the azeotropic composition. The Ts is specified to be 343.15
K. Using the above conditions for simulation, the recalculated results are
shown in Column base case in Table 1, which are used as the basis for
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Separation and Purification Technology 272 (2021) 118887
Fig. 6. x–y diagram for ethanol/furfural at 101.3, 50, and 200 kPa.
Fig. 7. x–y diagram for EA/furfural at 101.3, 50, and 200 kPa.
comparison in this work.
3.2. VLE analysis
Fig. 4 shows the x–y diagram for the EA/ethanol system at different
pressures. It can be clearly seen that the pressure has effects on the
relative volatility and azeotropic composition. Since the feed in this
work is 0.25 mol% EA, which is less than the azeotropic composition, the
C1 bottom product will be ethanol while the distillate product will be a
mixture of ethanol and EA. Moreover, in the region where x is less than
the azeotropic point, the VLE curve deviates more from the diagonal line
at a lower pressure, and the azeotropic composition is greater at a lower
pressure. Therefore, a lower pressure is more helpful for the separation
in the C1.
Fig. 5 shows the entrainer-free basis equilibrium curves at 101.3, 50
and 200 kPa. The molar composition of the furfural in the feed stream is
C. Duan and C. Li
Fig. 8. The optimal three-column process without heat integration (Opt).
0.75. In Fig. 4, x is the liquid molar fraction of EA without computing
furfural while y is the vapor molar fraction of EA without computing
furfural. The Fig. 5 can reflect most of the separation process (extractive
section and stripping section) in the C2. The VLE curves are below the
diagonal line, which means the volatility of ethanol is greater than that
of EA. Therefore, the distillate of the C2 is ethanol. Moreover, the VLE
curve deviates more from the diagonal line under a higher pressure,
indicating a higher pressure is more helpful for the separation. However,
higher pressures mean higher bottom temperatures and more expensive
energy sources [49]. Therefore, there is a trade-off on selecting an
operating pressure.
The separation process of the solvent recovery section in the C2 can
be reflected in Fig. 6, which shows the x–y diagram for the ethanol/
furfural system at different pressures. Fig. 7 shows the x–y diagram for
the EA/furfural system at different pressures. It can reflect the separa­
tion process in the C3. The separation is very easy for the two systems
due to the very fat curves. Moreover, as the pressure decreases from 200
kPa to 50 kPa, the VLE curve becomes fatter, so the separation becomes
easier.
From the VLE analysis and Fig. 1, three important features of the
system are obtained. (1) The separation becomes easier as the pressure
increases when using furfural as the solvent in the C2, while in the other
two columns, the separation becomes easier as the pressure decreases.
(2) At 101.3 kPa, the difference of boiling points between the two
components is only 1.1 K, and the difference between the boiling points
and the minimum azeotropic point is less than 6.5 K. (3) The C1 bottom
product is the same with the C2 overhead product when the feed
composition is lower than the azeotropic composition.
Fig. 9. (a) Effects of P1 on capital cost, energy cost and TAC; (b) effects of P3 on capital cost, energy cost and TAC.
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Separation and Purification Technology 272 (2021) 118887
3.3. Process improvement by optimizing more variables (Opt)
Among all the variables in the design and optimization of the TCED,
xD1, Ts and operating pressures are important. However, in the base
case, optimization is performed with the fixed xD1, Ts, P1, P2 and P3,
and without calculating the pressure drop. According to the first feature
of the system in Section 3.2, the pressure has effects on the three col­
umns and these effects are different. Therefore, the base case can be
improved by varying P1, P2, P3 as well as xD1, Ts. The pressure drop for
each stage is added and set at 0.6 kPa for the columns at atmospheric
pressure and high pressure. The tray pressure drop in a vacuum column
is set at 0.2 kPa according to the paper by Luyben [27].
As the pressure increases, the condenser temperature and the
reboiler temperature both increase. In this work, a minimum reflux-
drum temperature of 323 K is selected so that the heat sink used in
the condenser can be cooling water [27]. However, the minimum tem­
perature difference (ΔTm) for reboilers is set to 20 K so that thermosi­
phon reboilers can be used. The bottom temperature should be
controlled so that heat source used in the reboilers can be steam.
Fig. 8 shows the process in which P1, P2, P3, xD1 and Ts are included
in the optimization variables. This process is named Opt process. During
the optimization (mainly when optimizing Nt2), it is not conducive to
practical application due to too many trays. Moreover, as the Nt2 in­
creases, the impact of it on TAC is small after more than 70 stages.
Therefore, the upper limit of the Nt2 is set at 70 in this work. The
optimal results are listed in Column Opt in Table 1. The effects of the
variables on TAC are studied as follows.
For the C1 and C3, the separation is favored by a lower pressure as
C. Duan and C. Li Separation and Purification Technology 272 (2021) 118887

Fig. 10. (a) Effects of P2 on QW2 and QW3; (b) effects of P2 on capital cost, energy cost and TAC.

Fig. 11. (a) Effects of xD1 on heat duty distribution; (b) effects of xD1 on energy cost, capital cost and TAC.

shown in Figs. 4 and 7. Therefore, as the pressure increases, energy costs
will increase while the column diameter and the vacuum pump costs
(capital cost and operating cost) will decrease. As the pressure increase
causes the temperature difference (ΔT) in the reboiler to decrease, the
capital cost of the reboiler will increase. Meanwhile, as the pressure
increases, the ΔT in the condenser increases and the capital cost of the
condenser will decrease. All the effects are added together as shown in
Fig. 9. The optimal P1 is 48 kPa, and the optimal P3 is 52 kPa.
For the C2, as analyzed in Section 3.2, the separation is more favored
by a higher pressure. Therefore, as P2 increases, the energy cost de­
creases. The important thing is that not only the C2 but also the C3 that
causes the reduction in energy as shown in Fig. 10 (a). This is because
the thermal conditions of the C2 bottom stream have changed, leading to
changes in the feed conditions of C3, which affects the C3 reboiler duty
(QW3). Meanwhile, the equipment cost of the reboiler increases due to
the higher bottom temperature. The column diameter decreases due to
the reduced vapor density. The total capital cost increases due to the
overall effects. In addition, when the pressure is greater than 393 kPa,
the bottom temperature exceeds 437 K. In order to ensure a ΔT of 20 K,
the heat source (middle-pressure steam, $14.19/GJ, 457 K) needs to be
replaced with the high-pressure steam ($17.70/GJ, 537 K). Therefore,
the energy cost suddenly increases, while the equipment cost suddenly

Fig. 12. (a) Effects of Ts on the C2; (b) effects of Ts on energy cost, capital cost and TAC.

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C. Duan and C. Li
Fig. 13. Flowsheet of heat pump distillation (HP-1).
decreases due to an increased ΔT in the reboiler. As a result, the TAC
increases suddenly. Fig. 10 (b) shows the effects of P2 on the costs.
Fig. 11 (a) shows the effects of xD1 on heat duty distribution. As xD1
increases, the reboiler duty of the C1 (QW1) increases because the
separation becomes more difficult when xD1 approaches the azeotropic
composition (0.613 at 48 kPa). However, the reboiler duty of C2 (QW2)
decreases. This is because the composition of EA in the C2 feed is getting
higher and the feed flowrate is getting smaller. The QW3 remains un­
changed. Therefore, the total QW of the three columns first decreases
and then increases. The change in the condenser duty is similar to the
change in the reboiler duty as shown in Fig. 11 (a). When xD1 equals
0.55, QW has the minimum values. Fig. 11 (b) shows the effects of xD1 on
the energy cost, capital costs and TAC. The change trend of the TAC is
similar to the change trend of the energy cost, and is similar to the trend
of QW in Fig. 11 (a). Therefore, when xD1 equals 0.55, the TAC is also the
minimum.
Fig. 12 (a) shows the effects of Ts on the C2 in terms of the condenser
duty and the reboiler duty. As Ts increases, the QW2 decreases hardly,
but the C2 condenser duty (QD2) increases rapidly. The heat sink in the
condenser is inexpensive cooling water (0.354 $/GJ) which is much
cheaper than middle-pressure steam (14.19 $/GJ) used as the heat
source in the reboiler. The Ts has little effect on the reboiler duty,
Fig. 14. Flowsheet of heat integration between the C1 and the C2 (HI-12).
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Separation and Purification Technology 272 (2021) 118887
resulting in little effect on the energy cost as shown in Fig. 12 (b).
Meanwhile, the Ts has a major impact on the condenser duty. Therefore,
as Ts increases, the capital cost of the condenser increases. However, the
capital cost of the cooler decreases. The decrease is more than the in­
crease. As a result, the capital cost and TAC decrease slowly. The TAC is
the minimum when the Ts is the maximum. Therefore, the cooler is
removed and the high-temperature solvent is directly fed to the C2 as
shown in Fig. 8.
After the optimization, TAC could be reduced by 27.0% compared
with the base case. Meanwhile, energy consumption could be reduced by
27.6% and CO2 emissions could be reduced by 33.9%. This process is
even more energy-efficient (6176 kW) compared with the energy-
efficient combined-column process (7177 kW) in the literature [9].
The results show that adding an economizer and performing a
comprehensive optimization are very effective energy-saving measures
for this system.
3.4. Process improvement by heat-pump distillation
Based on the Opt process, it is considered to use heat pump distil­
lation for the C1 (HP-1) due to a low overall column temperature [30] in
C1 (the second feature of the system from Section 3.2). The HP-1 process
C. Duan and C. Li
Fig. 15. Flowsheet of no condensation for the C1 (PC-1).
is shown in Fig. 13. The C1 overhead vapor is fed to a compressor to
increase the pressure and the temperature. Therefore, it could provide
heat for the C1 reboiler. At the same time, it is condensed. After reducing
pressure through a valve, part of it is refluxed to the top of the column,
while the other part is taken out as the overhead product. Usually, an
auxiliary reboiler or an auxiliary condenser needs to be installed when
the heat is not so matched [50].
The COP value for this heat pump is 7.5, which indicates that
whether a heat pump should be used requires further evaluation. The
other detailed results are shown in Table 1. It achieves a 36.9% reduc­
tion in TAC, a 50.6% reduction in energy consumption, and a 66.2%
reduction in CO2 emissions compared with the base case. Therefore, the
heat-pump distillation process is recommended for the system.
Fig. 16. Flowsheet of installing a partial condenser for the C2 (PC-2).
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Separation and Purification Technology 272 (2021) 118887
3.5. Process improvement by heat integration between the C1 and the C2
(HI-12)
In the Opt process in Fig. 15, both the C1 and the C3 are operated at a
vacuum pressure, while the C2 is at a high pressure. According to Luy­
ben’s paper, if the C2 condenser temperature is sufficiently larger
(20–30 K) than the C1 reboiler temperature, a heat exchanger can serve
as both a condenser and a reboiler [51].
Due to the coupling of QD2 and QW1, the parameters that affect QD2
and QW1 are important. All the variables should be analyzed and
optimized with the minimum TAC as the target. During the optimiza­
tion, if |QD2| is greater than QW1, an auxiliary condenser is needed for
the C2. If |QD2| is less than QW1, an auxiliary reboiler is necessary for
the C1. After the comparison, it is found that the former is more
economical. However, the auxiliary condenser duty is very small (0.1
kW), which means an almost complete coupling.
The optimal results are listed in Column HI-12 in Table 1. The
C. Duan and C. Li Separation and Purification Technology 272 (2021) 118887

Fig. 17. Flowsheet of the vapor–liquid coupling between the C1 and the C2 (VLC-12).

flowsheet is shown in Fig. 14. TAC could be reduced by 43.8%, energy
consumption could be reduced by 52.0%, and CO2 emissions could be
reduced by 54.7% compared with the base case.
Heat integration between C1 and C2 is very suitable for this system
because of the natural ΔT.
3.6. Process improvement by partial condensation
3.6.1. Partial condensation (or no condensation) for the C1 (PC-1)
In a partial condenser, only the reflux stream is condensed, while the
distillate stream is in the vapor phase. Energy can be saved when this
vapor product is fed to the next column. Using a partial condenser in­
volves the problem of vapor feed. To avoid using a compressor, the
pressure difference between the vapor stream and the feed stage is at
least 15 kPa considering the resistance loss of pipelines and valves.
During the optimization process, it is found that it is more economical to
remove the condenser when the reflux ratio (RR) is very small. The
absence of a condenser is considered an extreme case of partial
condensation. So, in order to describe this method, even if there is no
condenser, the name of the method is still called partial condensation.
The process of installing a partial condenser for the C1 to produce a
vapor product which is fed to the C2 (Fig. 15) is considered first. In this
way, the capital cost of the C1 condenser and the energy cost of the C2
reboiler are greatly reduced.
The vapor feed makes the concentration of the entrainer in liquid
phase more constant which is beneficial to the separation in the C2.
The partial condenser for the C1 can be removed due to the small RR.
Therefore, the C1 is replaced by a pre-stripper [23]. This process can
reduce TAC by 28.2%, reduce energy consumption by 23.8%, and
reduce CO2 emissions by 30.8% compared with the base case.

Fig. 18. Flowsheet of vapor–liquid coupling between the C1 and the C2 and heat integration between the C1 and the C3 (VLC-HI).

10
C. Duan and C. Li
Fig. 19. Flowsheet of vapor–liquid coupling between the C1 and the C2 and installing a compressor between the C1 and the C2 (VLC-C).
3.6.2. A novel way of partial condensation (PC-2)
Because the third feature analyzed in Section 3.2 is that the C2
overhead product and the C1 bottom product are both ethanol, another
way to install a partial condenser is innovatively proposed. Based on the
direct steam injection method [52], a partial condenser can be installed
for the C2 to produce a vapor stream which could be directly fed to the
C1 bottom to provide some direct heat input. In this way, the capital cost
of the C2 condenser and the energy cost of the C1 reboiler are greatly
reduced.
Fig. 16 shows the optimal PC-2 process and Table 1 shows the results.
Installing a partial condenser for the C2 can reduce TAC by 34.4%,
reduce energy consumption by 36.9%, and reduce CO2 emissions by
41.6% compared with the base case.
The TAC, energy consumption and CO2 emissions of PC-2 are all
reduced compared to those of the PC-1 process Therefore, installing a
partial condenser for C1 is not so good as installing a partial condenser
for C2. This is mainly because the optimum pressures of the C1 and the
C2 are too different. The C1 and the C2 are operated at their respective
optimum pressures in the PC-2, but not in the PC-1.
The latent heat recovered by the PC-2 process is less than that of HI-
12 due to the reflux in the C2. So, HI-12 is more energy efficient, more
ecological and more economical than PC-2.
3.7. Process improvement by a novel energy-saving method of
vapor–liquid coupling
3.7.1. Vapor-liquid coupling between the C1 and C2 (VLC-12)
In order to increase the amount of latent heat recovered in PC-2, the
C2 condenser is removed so that all the vapor can be fed to the C1
bottom. Part of the C1 bottom product is refluxed to the C2. The amount
of the reflux is also one of the optimized variables. In this way, C2
overhead vapor can be fully utilized without partial condensation.
During the optimization process, it is found that as QW1 decreases, TAC
decreases. So, the reboiler is finally removed. The optimal process is
shown in Fig. 17, and the optimal results are shown in Table 1. It ach­
ieves a 48.6% reduction in TAC, a 53.1% reduction in energy con­
sumption, and a 55.8% reduction in CO2 emissions compared with the
base case. Comparing the above processes, it is found that VLC-12 is the
most economical process.
Compared with the HI-12 process, it is found that in the VLC-12
process, a condenser and a reboiler are saved, and the purity of the C2
11
Separation and Purification Technology 272 (2021) 118887
overhead product is lower, resulting in a lower energy consumption.
Therefore, VLC-12 is better than HI-12.
3.7.2. Further improvement based on the VLC-12 process through heat
integration (VLC-HI)
In Section 3.7.1, we have found the most economical process, namely
VLC-12. However, energy saving potential can still be explored for this
process. The first way is heat integration. As shown in Fig. 18, the C3
condenser is thermally integrated with the C1 reboiler. The high-
temperature solvent from the C3 bottom is used as a heat source to
preheat the C2 feed.
In the thermal integration process, when QW1<|QD3|, an auxiliary
condenser is installed in the C3. When QW1>|QD3|, an auxiliary
reboiler is installed in the C1. It is found that the former scheme is more
economical after the calculation. However, just like the HI-12 process,
the auxiliary condenser is also vary small (0.03 kW). In this way, TAC is
reduced by 7.6%, energy consumption is reduced by 19.6%, and CO2
emissions are reduced by 12.9% compared with those of the VLC-12
process.
3.7.3. Further improvement based on the VLC-12 process through a
compressor (VLC-C)
In addition to heat pump distillation, there are other ways to use
compressors. Base on the VLC-12 process in Section 3.7.1, a partial
condenser is installed in the C1 to produce a vapor stream. This vapor
stream then enters a suitable location of C2 after being pressurized by a
compressor as shown in Fig. 19. In this way, capital cost of C1 condenser
and costs of C2 reboiler are all reduced despite a large increase in the
equipment cost and operating cost of the compressor. Therefore, TAC is
reduced by 12.8%, energy consumption is reduced by 15.3%, and CO2
emissions are reduced by 23.4% compared with those of the VLC-12
process. Compared with the HP-1, the VLC-C process can save TAC by
28.9%, and save energy by 19.4%, despite a very small increase (0.2%)
in CO2 emissions.
As shown from Fig. 8 and Figs. 13–19, all the processes have different
optimal values of xD1, Ts and pressures. Therefore, these parameters
should not be fixed but should be re-analyzed and re-optimized in
different processes. Table 1 lists the optimal results of all the processes.
As shown in Table 1, the most economical process is VLC-C. VLC-C is not
as good as VLC-HI in terms of energy saving, but better than VLC-HI in
terms of reducing carbon emissions.
C. Duan and C. Li
4. Conclusions
Based on the VLE analysis, the characteristics of using furfural to
separate EA and ethanol in a TCED process are obtained. Eight energy-
saving processes are proposed and optimized with the minimum TAC as
the target. The optimal results show that they are all more energy-
efficient than the energy-saving combined-column process (7177 kW)
in the reference article [9]. Among the optimization variables, the
operating pressures, xD1 and Ts are all key variables for the TCED pro­
cess especially for the processes that use energy-saving methods.
Heat pump distillation, heat integration, two kinds of partial
condensation, and vapor–liquid coupling methods are all very suitable
for the EA/ethanol/(furfural) system. The novel way of partial
condensation is better than the conventional way in terms of TAC, en­
ergy and CO2 emissions. The novel vapor–liquid coupling energy-saving
method is more economical than the others.
The VLC-12 process can be further improved by additional heat
integration or vapor recompression. The VLC-C process, where a
compressor is installed for the C1 in the VLC-12 process to generate a
vapor feed for the C2, is the most economical process. It can achieve a
55.2% reduction in TAC. It can also achieve a 60.2% reduction in energy
consumption and a 66.1% reduction in CO2 emissions.
The PC-2, VLC-12, VLC-HI, and VLC-C processes proposed in this
work are applicable to other systems whose characteristic is that the
distillate product of C2 and bottom product of C1 are the same.
CRediT authorship contribution statement
Cong Duan: Conceptualization, Data curation, Investigation, Meth­
odology, Software, Writing - original draft, Writing - review & editing.
Chunli Li: Supervision, Validation, Funding acquisition, Writing - re­
view & editing.
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.
Acknowledgements
This work was supported by the National Key R&D Program of China
[grant number 2017YFB0602500], and the Central Committee Guides
Local Science and Technology Development Special Project [grant
number 19944507G].
Appendix A. Supplementary material
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.seppur.2021.118887.
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