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Article history:
Received 29 January 2015
Received in revised form
25 April 2015
Accepted 2 May 2015
Available online 9 May 2015
In extractive distillation, the addition of entrainer may reverse the relative volatility of the feed
components causing the component with higher-boiling point to be removed as the distillate from the
extractive column. In this study, the energy saving possibility of a three-column extractive distillation
system was studied when this phenomenon occurred. Based on a three-column conventional extractive
distillation system, an innovative energy-saving extractive distillation process with lower capital
investment was developed by combining preconcentration column and extractive distillation column.
Two important case studies were investigated to verify the above-mentioned energy and economic
advantages: the separation of n-propanol-water using N-methyl-2-pyrrolidone (NMP) as entrainer and
the separation of ethyl acetateethanol using furfural as entrainer. In order to separate these two
mixtures, rst a three-column extractive distillation sequence including a preconcentration column was
applied to diluted fresh feedstock. Then, based on this three-column conventional extractive distillation
system, an innovative energy-saving distillation process was developed. For the two separated mixtures,
based on the method of global economic optimization, a scheme with optimum design variables was
developed for both of the conventional distillation and the new proposed distillation processes. Results
revealed that the new process offered 22.76% and 17.25% energy-savings respectively. Similar percentage
of reduction in total annual costs (TAC) can also be obtained when compared to the conventional
distillation process.
& 2015 Elsevier Ltd. All rights reserved.
Keywords:
Extractive distillation
Energy-saving
Process design
1. Introduction
Distillation is by far the most important separation process in
chemical engineering, and it exploits the relative volatility
http://dx.doi.org/10.1016/j.ces.2015.05.003
0009-2509/& 2015 Elsevier Ltd. All rights reserved.
the azeotropic composition is not sufciently sensitive to pressure, and some complexities of dealing heterogeneous azeotropic
distillation, such as multiple steady states, parametric sensitivity
that were clearly illustrated by many authors which consequently
make the design and control challenging (Doherty and Malone,
2001; Seader and Henley, 1998; Widagdo and Seider, 1996).
Extractive distillation is the most widely used form of homogeneous azeotropic distillation due to the low energy consumption
and exible selection of the possible entrainers (Lei et al., 2003;
Sucksmith, 1982). In extractive distillation, a heavier entrainer that
has different interaction with the azeotropic components is added
to alter the relative volatility of the components, thereby effectively breaking the azeotrope. Nowadays, extractive distillation
with ionic liquids or the mixture of ionic liquids and solid
inorganic salt as entrainers attracted more and more attention
(Lei et al., 2014a, 2014b).
An important and special aspect of extractive distillation is that
we are not free to pick which of the components in the feed will be
the distillate from the extractive column. For a given entrainer, one
and only one of the feed components can be recovered in the
distillate from the extractive column, and it is not always the
component with the lowest boiling point. For example, the separation of methanol and acetone using chlorobenzene causes higherboiling methanol to be recovered as the distillate from the extractive
column, and the lower-boiling acetone to leave in the bottom stream
with chlorobenzene. Other entrainers, such as water, dimethyl
sulfoxide (DMSO) causes acetone to be recovered as the distillate
from the extractive column (Kossack et al., 2008; Luyben, 2008a,
2008b; Kotai et al., 2007; Modla and Lang, 2012, 2011; Langston et
al., 2005; Gil et al., 2009). It is important to know which of the feed
components will appear in the distillate stream from the extractive
column in order to design the equipment. Isovolatility curve and
pseudo-binary (entrainer-free) equilibrium diagram are reliable
ways. (Doherty and Malone, 2001; Hsu et al., 2010).
Extractive distillation is widely used in a number of processes
(Lladosa et al., 2011; Pacheco-Basulto et al., 2012; Arin and Chien,
2008; Abushwireb et al., 2007; Wang et al., 2012; Gil et al., 2012; Xu
and Wang, 2006; Hsu et al., 2010), but it is still energy intensive,
different methods to overcome the drawback of energy intensive
have been reported. Process integration is a useful option and it has
been proven that the process integration leads to a signicant
reduction in energy consumption compared to conventional process
with no integration. Doherty et al. (Knapp and Doherty, 1990)
developed thermally-integrated extractive distillation sequences for
the separation of ethanol from water using ethylene glycol as
167
MAKEUP
S
D1
D2
D3
F
A+B
B1
B2
B3
B
Preconcentration
column
Extractive distillation
column
Entrainer recovery
column
168
F
A+B
Preconcentration
section
D1
D2
A
B
MAKEUP
S
Extractive
distillation
section
B1
B2
A+S
Combined
preconcentration/extractive
column
Entrainer
recovery
column
For the new process, the rst column is a special column with
complex conguration. From Figs. 1 and 2 the path from conventional process to the new process, it is clear to know that when the
combined preconcentration/extractive distillation column is
decomposed, it should be exactly the PDC and EDC in the
conventional extractive distillation system. Thus, after we get the
optimal design variables of the conventional extractive distillation
system, the optimum design variables of the conventional extractive distillation system can be directly applied to the new process.
Therefore, the original optimal congurations are all kept the same
in the new process (Errico et al., 2014a, 2014b).
3.1. Process design
In this work, the commercial software Aspen Plus V7.1 was
used in the steady state simulations. The desired product quality
requirements were achieved by the Design Spec/Vary feature in
Aspen Plus. In all cases, the reux ratio and distillate rate were
used as the operation variables of each column.
The PDC and the ERC are all simple columns with one feed
stream and two product streams. It's easy to design these two
columns. The EDC with two feed streams and two product streams,
it is more complicated. There are some very simple and reliable
tools can be used. Residue curve maps that allow us to determine
whether the entrainer is feasible and they can be used as simple
method to analysis and design feasible extractive distillation
sequence (Doherty and Malone, 2001; Doherty and Caldarola,
1985). It is important to know which of the feed components will
appear in the distillate stream from the extractive column in order
to design the equipment. Isovolatility curve is a reliable way, plot the
isovolatility curve on the composition triangle. If the curve intersects the A-S edge, then component A will be the distillate from the
extractive column, otherwise component B will appear in the
distillate stream (Doherty and Malone, 2001; Hsu et al., 2010). A
relative volatility at various feed ratios plot is a useful tool to
demonstrate the effectiveness of the entrainer. The feed ratio is a
very important design variable. In fact, there is a minimum value of
feed ratio where the minimum and maximum reux ratios occur
simultaneously. Below this value, we are unable to get the desired
purity of the product. With the sensitivity analysis tool in Aspen
Plus, it can clearly show the feasible range of feed ratio and reux
ratio. It can help us choose the appropriate feed ratio and reux
ratio to meet the product specications.
3.2. Economical optimization
Once a base-case design is developed, the next step is to
optimize the design variables. It is conventional to use the total
annual cost (TAC) as the objective function to be minimized to
screen process candidates, which including annualized capital
costs and operating costs (Douglas, 1988; Muoz et al., 2006;
Kraemer et al., 2009; Harwardt and Marquardt, 2012). The following objective function was used to carry out a global economic
optimization.
TAC 103 $=year C v ir FCI
1
Table 1
Utility prices.
Utility
Price ($/GJ)
169
where FCI is the xed capital investment. In this paper, just major
pieces of equipment were concerned, which are the three distillation column vessels (including column internals), three reboilers,
and four condensers. The tray sizing function in Aspen Plus was
used to calculate the diameter of column vessels and sieve plate is
selected in all columns. An overall heat transfer coefcient and a
differential temperature driving force in each heat exchange were
used to calculate the required heat transfer area. Here the overall
heat transfer coefcient and differential temperature for the
condenser and reboiler were all taken from Luyben (2006). A cost
estimation program CAPCOST of Turton was used to estimate all
the major equipment costs (Turton et al., 2009). ir is the xed
capital recovery rate, it is assumed to be 0.3. Cv is the operating
cost, which includes mostly utilities consumption (steam, cooling
water). The utilities consumption costs can be calculated from the
heat duties of reboilers and condensers. High pressure steam with
pressure of 41 barg (254 1C), medium pressure steam with pressure of 10 barg (184 1C) and low pressure steam with pressure of
5 barg (160 1C) and cooling water with temperature of 30 1C are
supposed to be available in the plant. The utility prices taken from
CAPCOST are listed in Table 1 (Turton et al., 2009).
The design variables need to be optimized in the conventional
process include the total stages of the PDC (NT1), the EDC (NT2),
and the ERC (NT3), fresh stream feeding location of the PDC (NF1),
entrainer and fresh streams feeding locations (NFE and NF2) of the
EDC, and the feeding location of the ERC (NF3) and the entrainer
ow rate (S). As so many design variables need to be optimized, a
calculation sequence was established to facilitate the optimization.
Such sequential iterative optimization procedure is clearly demonstrated in Fig. 3 (Liang et al., 2014).
170
Fig. 3. Sequential iterative optimization procedure for the conventional extractive distillation system.
Table 2
Specications for streams.
Stream
Conditions
Feed
n-Propanol product
H2O product
NMP entrainer recycle
Saturated liquid
Saturated liquid
Saturated liquid
90.0 1C
Table 3
The binary interaction parameters for the Aspen plus NRTL model.
Binary parameters
n-Propanol (i)
H2O(j)
n-Propanol (i)
NMP(j)
H2O(i)
NMP(j)
Aij
Aji
Bij/K
Bji/K
Cij
0.0
0.0
181.2160
927.9748
0.4687
0.0
0.0
234.2208
205.8249
0.3000
0.0
0.0
120.5810
288.7615
0.3055
H2O (100.02 C)
2.5
Relative Volatility
0.9
0.8
0.7
87.65 C
0.6
0.5
0.4
0.3
0.2
NMP
2.0
1.5
1.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
0.1
(203.99 C)
171
C3H8O-01
(97.20 C)
1.000
0.999
S=310kmol/h
0.998
S=300kmol/h
0.997
S=290kmol/h
0.996
0.995
S=280kmol/h
0.8
1.0
1.2
1.4
1.6
1.8
2.0
Fig. 4. (a) Residue curve map with isovolatility curves for the N-propanol-H2O-NMP system at 1 atm. (b) Relative volatility at various feed ratios.
0.005
0.004
S=280kmol/h
S=290kmol/h
0.003
S=300kmol/h
0.002
S=310kmol/h
0.001
0
0.8
1.0
1.2
RR2
1.4
1.6
1.8
2.0
RR2
Fig. 5. (a) Effect of RR2 and entrainer ow rate S in extractive column (NT2 58) on H2O purity. (b) Effect of RR2 and entrainer ow rate S in extractive column (NT2 58) on
impurity of n-propanol.
998.0
TAC(x1000$/year)
the NMP will have a very bad inuence on the water purity. A heat
exchanger must be placed between the EDC and the ERC to cool
the NMP temperature. In this case, the temperature of the
entrainer NMP was cooled to be 90.0 1C. This is because Knight
and Doherty (1989) suggested that the entrainer feed temperature
to the EDC should be 515 1C below the boiling temperature of the
distillate product from the EDC.
997.5
997.0
NT1=9 with the
optimum NF1=6
996.5
996.0
995.5
995.0
994.5
10
11
NT1
Fig. 6. TAC vs NT1 with the optimum NF1 plot for the PDC.
172
3340
NFE=5
NFE=6
NFE=7
2371.5
3335
2371.0
QR2/kW
TAC(x1000$/year)
2372.0
2370.5
2370.0
3330
3325
2369.5
2369.0
320
330
340
350
3320
43
44
45
46
NF2
TAC(x1000$/year)
2375
2374
2373
2372
2371
2370
2369
54
56
58
60
NT2
TAC(x1000$/year)
Fig. 7. (a) TAC plot at various entrainer ow rate S for the EDC. (b) QR2 vs NFE and NF2 for S 330 kmol/h, NT2 58 plots for the EDC. (c) TAC vs NT2 for S 330 kmol/h plot for
the EDC.
1302
1301
1300
1299
1298
1297
25
26
27
28
29
30
NT3
Fig. 8. TAC vs NT3 with the optimum NF3 plot for the ERC.
173
Fig. 9. (a) The optimum process ow diagram for the new combined preconcentration/ extractive column system. (b) The optimum process ow diagram for the
conventional extractive distillation system.
Table 4
Comparision between the optimum conventional design and corresponding new
two-column design.
Conventional process
Heat duty
QRT (kW)
QCT(kW)
Economical data
TIC (103 $)
TOC (103 $/year)
TAC (103 $/year)
New process
Table 5
Specications for streams.
Stream
Conditions
Feed
Ethyl acetate product
Ethanol product
Furfural entrainer recycle
Saturated liquid
Saturated liquid
Saturated liquid
70.0 1C
(%) Difference
6925.3
6876.9
5349.4
5301.0
22.76
22.92
4605.3
3371.4
4753.0
3885.3
2752.4
3918.0
15.63
18.36
17.57
174
section for the rst column of the new process respectively. The
nal optimum process ow diagram for the conventional extractive distillation system design and the new process design is
shown in Fig. 15.
acetate/ethanol system is less effective than NMP to the npropanol/water system. Fig. 11b shows the effects of changing
the ow rate of furfural and RR2 on the impurity of ethyl acetate
of the EDC. The bottom composition of the ERC was set at
99.999 mol% furfural. A heat exchanger must be placed between
the ERC and the EDC. In this case, the temperature of the entrainer
furfural was cooled to be 70.0 1C.
Table 6
The binary interaction parameters for the Aspen plus NRTL model.
Binary parameters
Ethanol (i)
Ethyl acetate (j)
Ethanol (i)
Furfural (j)
Aij
Aji
Bij/K
Bji/K
Cij
0.0
0.0
216.3048
95.0457
0.3000
0.0
0.0
139.6013
425.8981
0.30000
0.0
0.0
548.0231
257.2865
0.30000
Relative Volatility
0.9
0.8
0.7
0.6
72.14 C
0.5
0.4
0.3
0.2
0.1
FURFURAL
(161.35 C)
C4H8O-01
(77.20 C)
2.8
2.6
2.4
2.2
2.0
1.8
1.6
1.4
1.2
1.0
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
Fig. 10. (a) Residue curve map with isovolatility curves for the ethanol-ethyl acetate-furfural system at 1 atm. (b) Relative volatility at various feed ratios.
0.998
175
0.010
0.997
0.996
S=410kmol/h
0.995
0.994
S=400kmol/h
0.993
S=390kmol/h
0.992
S=380kmol/h
0.991
0.009
0.008
S=380kmol/h
0.007
S=390kmol/h
0.006
S=400kmol/h
0.005
0.004
S=410kmol/h
0.003
0.002
1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0
0.990
1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0
RR2
RR2
Fig. 11. (a) Effect of RR2 and entrainer ow rate S in extractive column (NT2 46) on ethanol purity. (b) Effect of RR2 and entrainer ow rate S in extractive column (NT2 46)
on impurity of ethyl acetate.
1457
TAC(x1000$/year)
TAC(x1000$/year)
1911
1910
1909
1908
1907
1906
25
26
27
28
29
30
1456
NT3=25 with the
optimum NF3=11
1455
1454
24
31
25
1927.0
3250
1926.5
3248
QR2/kW
TAC(x1000$/year)
27
Fig. 14. TAC vs NT3 with the optimum NF3 plot for the ERC.
Fig. 12. TAC vs NT1 with the optimum NF1 plot for the PDC.
1926.0
1925.5
1925.0
1924.5
525
26
NT3
NT1
NFE=7
NFE=8
NFE=9
3246
3244
3242
3240
530
535
540
545
550
3238
30
555
31
32
33
NF2
TAC(x1000$/year)
1932
1930
1928
1926
1924
42
44
46
48
NT2
Fig. 13. (a)TAC plot at various entrainer ow rate S for the EDC. (b) QR2 vs NFE and NF2 for S 540 kmol/h, NT2 46 plots for the EDC. (c) TAC vs NT2 for S 540 kmol/h plot for
the EDC.
176
F
300.000 kmol/hr
0.750 Ethanol
0.250 EA
S MAKEUP
0.100 kmol/hr
1.000 Furfural
2415.6 kW
2
11
26
225.758kmol/hr
1908.4 kW 0.995Ethanol
0.00454 EA
0.000460Furfural
56
B2
536.721kmol/hr
1.2334E-16 Ethanol
1E-05 EA
0.99999 Furfural
S
1atm
3391.8 kW MAKEUP
RR1=1.066
11
26
Preconcentration
column
2028.3 kW
1atm
1481.4kW
1atm
1344.6kW
RR2=0.507
31
45
B1
134.831kmol/hr
0.995 Ethanol
0.005 EA
3399.6kW
2
8
0.1kmol/hr
1.000 Furfural
D1
165.169 kmol/hr
0.550 Ethanol
0.450 EA
24
Entrainer recovery
column
Combined preconcentration/extractive
column
D2
74.347 kmol/hr
0.00499 Ethanol
0.995 EA
0.00001 Furfural
11
D1
165.169kmol/hr
0.550Ethanol
0.450 EA
5.0696E-21Furfural
33
B1
611.068kmol/hr
0.000607Ethanol
3239.9kW 0.121 EA
0.878Furfural
300.000 kmol/hr
0.750 Ethanol
0.250 EA
RR2=1.012
RR1=1.068
70
1atm
1340.9kW
1atm
3395.5kW
3239.2 kW
D2
90.926 kmol/hr
0.995 Ethanol
0.004 EA
0.001 Furfural
B2
614.248 kmol/hr
0.000604 Ethanol
0.120 EA
0.879 Furfural
RR3=1.018
11
24
2033.7kW
Extractive distillation
column
D3
74.342 kmol/hr
0.00499 Ethanol
0.995 EA
0.00001 Furfural
B3
539.906kmol/hr
1.226E-16 Ethanol
1E-05 EA
0.99999 Furfural
2429.9kW
Entrainer recovery
column
Fig. 15. (a) The optimum process ow diagram for the new combined preconcentration/ extractive column system. (b) The optimum process ow diagram for the
conventional extractive distillation system.
conventional extractive distillation process and the new process were presented. For the two case studies-the separation of
n-propanol/water and ethyl acetate/ethanol, the results show
that the new process leads to energy savings of 22.76% and
17.25% respectively and a similar reduction in capital investment and the total annual costs. In the new process, an
intermediate reboiler was used to meet the energy requirement in the preconcentration section.
Conict of interest
The authors declare no competing nancial interest.
Table 7
Comparision between the optimum conventional design and corresponding new
two-column design.
Heat duty
QRT (kW)
QCT(kW)
Economical data
TIC (103 $)
TOC (103 $/year)
TAC (103 $/year)
Conventional process
New process
(%) Difference
8672.5
8647.8
7176.6
7151.9
17.25
17.30
5448.0
3748.7
5383.1
4680.0
3163.2
4567.2
14.10
15.62
15.16
Nomenclature
NRTL
E-DWC
PDC
EDC
ERC
NF1
NFE
NF2
NF3
NTn
QCn
QRn
QCT
QRT
NMP
EA
RRn
TAC
TIC
TOC
Acknowledgment
The authors thank for the support by the Programme of
Introducing Talents of Discipline to Universities (No: B06006)
and the assistance from the staffs in the State Key Laboratories
of Chemical Engineering (Tianjin University).
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