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Frontiers of Chemical Science and Engineering

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Front. Chem. Sci. Eng.    2020, Vol. 14 Issue (5) : 913-927    https://doi.org/10.1007/s11705-019-1877-1
RESEARCH ARTICLE
Combining extractive heterogeneous-azeotropic distillation and hydrophilic pervaporation for enhanced separation of non-ideal ternary mixtures
Eniko Haaz1, Botond Szilagyi1, Daniel Fozer1, Andras Jozsef Toth1,2()
1. Environmental and Process Engineering Research Group, Department of Chemical and Environmental Process Engineering, Budapest University of Technology and Economics, Budapest H-1111, Hungary
2. Institute of Chemistry, University of Miskolc, Miskolc H-3515, Hungary
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Abstract

The separation of non-ideal mixtures using distillation can be an extremely complex process and there continues to be a need to further improve these techniques. A new method which combines extractive heterogeneous-azeotropic distillation (EHAD) and hydrophilic pervaporation (HPV) for the separation of non-ideal ternary mixtures is demonstrated. This improved distillation method combines the benefits of heterogeneous-azeotropic and extractive distillations in one column but no added materials are needed as is usually the case with pervaporation. The separation of water-methanol-ethyl acetate and water-methanol-isopropyl acetate mixtures were investigated to demonstrate the accuracy of the combined EHAD/HPV technique. There is not currently an established treatment strategy for the separation of the second mixtures in the literature. These separation processes were rigorously modelled and optimized using a professional flowsheet. The objective functions were total cost and energy consumption and heat integration was also investigated. The verification of the process modelling was carried out using laboratory-scale measurements. Extractive heterogeneous-distillation combined with methanol dehydration was found to be more efficient than conventional distillation for the separation of these highly non-ideal mixtures.
Keywords hydrophilic pervaporation      non-ideal mixture      modelling      extractive heterogeneous-azeotropic distillation      heat integration     
Corresponding Author(s): Andras Jozsef Toth   
Online First Date: 06 March 2020    Issue Date: 25 May 2020
 Cite this article:   
Eniko Haaz,Botond Szilagyi,Daniel Fozer, et al. Combining extractive heterogeneous-azeotropic distillation and hydrophilic pervaporation for enhanced separation of non-ideal ternary mixtures[J]. Front. Chem. Sci. Eng., 2020, 14(5): 913-927.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-019-1877-1
https://academic.hep.com.cn/fcse/EN/Y2020/V14/I5/913
Fig.1  Schematic diagram of extractive heterogeneous-azeotropic distillation [5].
Azeotrope Boiling point
/°C		 Component (i)
/wt-%		 Component (j)
/wt-%		 UNIQUAC
I J Type Uij−Ujj Uji−Uii
EtAc MeOH Homo 62.3 53.2 46.8 773.59 ?147.599
Water EtAc Hetero 70.4−72.3 7.9−8.6 91.4?92.1 151.64 757.59
IpAc MeOH Homo 64.3 74.4 25.6 5319.32 ?1027.46
Water IpAc Hetero 81.7−82.8 12.2–16.2 83.8–87.8 245.7977 813.2316
Tab.1  Binary azeotropes of the investigated mixtures [24−26]
Fig.2  Laboratory apparatus for investigation of extractive heterogeneous-azeotropic distillation [28].
Fig.3  Method I flowsheet for mixtures I and II.
Fig.4  Method II flowsheet for mixtures I and II.
EHAD column Feed Modelling results Experimental results
Mixture I Water D?u.p. W D?u.p. W
Water/wt-% 6 100 5.3 93.2 6.1 92.8
MeOH/wt-% 24 0 0.1 6.7 0.14 7.2
EtAc/wt-% 70 0 94.6 0.1 93.76 0
Stream/(kg?h?1) 0.5 2.5 0.36 2.60 0.36 2.58
Temperature /°C 20 20 70.9 94.6 69.3 96.0
Tab.2  Comparison of simulated and measured data for Mixture I with EHAD (Column I)
EHAD column Feed Modelling results Experimental results
Mixture II Water D?u.p. W D?u.p. W
Water/wt-% 6 100 2.07 96.1 2.2 95.9
MeOH/wt-% 24 0 0.07 3.8 0.1 4.1
IpAc/wt-% 70 0 97.87 0.1 97.7 0
Stream/(kg?h?1) 0.5 3.0 0.35 3.15 0.35 3.13
Temperature /°C 20 20 76.5 95.3 76.1 96.1
Tab.3  Comparison of simulated and measured data for Mixture II with EHAD (Column I)
Fig.5  Calculated equilibria and operating lines of EHAD (Mixture I).
Fig.6  Calculated equilibria and operating lines of EHAD (Mixture II).
Fig.7  Influence of the number of stages and reboiler duties on the TAC in the separation of Mixture I.
Fig.8  Influence of the number of stages and reboiler duties on the TAC in the separation of Mixture II.
Fig.9  Reboiler duty and minimal water consumption in the function of total stages (Mixture I, Column I).
Fig.10  Reboiler duty and minimal water consumption in the function of total stages (Mixture II, Column I).
Mixture I?Method I Column I Column II Column III
NTotal 10 20 30
NFeed 5 10 20
NExtractive agent 1
pFeed /Pa 105 3×105 105
Reflux ratio (RR) 1.0 0.5 2.0
Q-DISTCondenser /(MJ?h?1) ?582 ?1112 ?1532
Q-DISTReboiler /(MJ?h?1) 702 1250 1654
QPost cooler /(MJ?h?1) ?59 ?321
Mixture I?Method I F F F
Water/wt-% 4.5 7.9 69.8
MeOH/wt-% 24.8 5.9 30.1
EtAc/wt-% 70.7 86.3 0.1
Mixture stream/(kg?h?1) 1000 811 639
Extractive agent stream/(kg?h?1) 500 0 0
Temperature /°C 40.0 70.0 80.0
Mixture I?Method I D D D
Water/wt-% 11.5 10.1 0.2
MeOH/wt-% 6.5 7.7 99.5
EtAc/wt-% 82.1 82.2 0.3
Mixture stream/(kg?h?1) 861 622 191
Temperature/°C 74.6 101.9 64.2
Mixture I?Method I W W W
Water/wt-% 69.8 0.5 99.5
MeOH/wt-% 30.1 0.0 0.5
EtAc/wt-% 0.1 99.5 0.0
Mixture stream/(kg?h?1) 639 189 448
Temperature/°C 81.3 112.2 99.1
Tab.4  Final optimized parameters for Method I with Mixture I
Mixture I?Method II Column I Column II Column III PV
NTotal 10 20 6 ?
NFeed 5 10 3
NExtractive agent 1
pFeed /Pa 105 3×105 105 3×105
RR 1.0 0.5 0.1
Effective membrane area /m2 40
Q-DISTCondenser /(MJ?h?1) ?582 ?1112 -302
Q-DISTReboiler /(MJ?h?1) 702 1250 320
QPost cooler /(MJ?h?1) ?59 ?324 ?53
Q-PVFeed cooler /(MJ?h?1) ?5
Q-PVRetentate heating /(MJ?h?1) 202
Q-PVPermeate cooler /(MJ?h?1) ?37
Mixture I?Method II F F F F
Water/wt-% 4.5 7.9 69.8 9.9
MeOH/wt-% 24.8 5.9 30.1 90.0
EtAc/wt-% 70.7 86.3 0.1 0.1
Mixture stream/(kg?h?1) 1000 811 639 211
Extractive agent stream/(kg?h?1) 500 0 0 0
Temperature /°C 40.0 70.0 81.3 70.0
Mixture I?Method II D D D P
Water/wt-% 11.5 10.1 9.9 99.1
MeOH/wt-% 6.5 7.7 90.0 0.8
EtAc/wt-% 82.1 82.2 0.1 0.1
Mixture stream/(kg?h?1) 861 622 211 20
Temperature/°C 74.6 101.9 66.4 56.8
Mixture I?Method II W W W R
Water/wt-% 69.8 0.5 99.5 0.5
MeOH/wt-% 30.1 0.0 0.5 99.5
EtAc/wt-% 0.1 99.5 0.0 0.0
Mixture stream/(kg?h?1) 639 189 428 191
Temperature /°C 81.3 112.2 99.1 69.5
Tab.5  Final optimized parameters for Method II with Mixture I
Mixture II?Method I Column I Column II Column III
NTotal 16 12 40
NFeed 8 6 30
NExtractive agent 1
pFeed /Pa 105 105 105
RR 0.5 4.0 5.0
Q-DISTCondenser/(MJ?h?1) ?743 ?1357 ?1706
Q-DISTReboiler/(MJ?h?1) 946 1374 1747
QPost cooler/(MJ?h?1) ?42 ?219
Mixture II?Method I F F F
Water/wt-% 6.3 5.1 80.6
MeOH/wt-% 25.7 11.1 19.3
IpAc/wt-% 68.0 83.8 0.1
Mixture stream/(kg?h?1) 1000 835 765
Extractive agent stream/(kg?h?1) 700 0 0
Temperature /°C 40.0 70.0 80.0
Mixture II?Method I D D D
Water/wt-% 15.6 11.6 0.4
MeOH/wt-% 11.7 24.5 99.5
IpAc/wt-% 72.7 63.9 0.1
Mixture stream/(kg?h?1) 935 369 146
Temperature/°C 79.9 73.8 64.2
Mixture II?Method I W W W
Water/wt-% 80.6 0.0 99.5
MeOH/wt-% 19.3 0.5 0.4
IpAc/wt-% 0.1 99.5 0.1
Mixture stream/(kg?h?1) 765 466 620
Temperature /°C 85.7 87.8 99.0
Tab.6  Final optimized parameters for Method I with Mixture II
Mixture II?Method II Column I Column II Column III PV
NTotal 16 12 8 ?
NFeed 8 6 4
NExtractive agent 1
pFeed /Pa 105 105 105 3×105
RR 0.5 4.0 0.5
Effective membrane area /m2 35
Q-DISTCondenser /(MJ?h?1) ?743 ?1357 ?439
Q-DISTReboiler /(MJ?h?1) 946 1374 497
QPost cooler /(MJ?h?1) ?42 ?352 ?46
Q-PVFeed cooler /(MJ?h?1) ?4
Q-PVRetentate heating /(MJ?h?1) 195
Q-PVPermeate cooler /(MJ?h?1) ?29
Mixture II? Method II F F F F
Water/wt-% 6.3 5.1 80.6 9.9
MeOH/wt-% 25.7 11.1 19.3 90.0
IpAc/wt-% 68.0 83.8 0.1 0.1
Mixture stream/(kg?h?1) 1000 835 765 161
Extractive agent stream/(kg?h?1) 700 0 0 0
Temperature/°C 40.0 70.0 80.0 70.0
Mixture II?Method II D D D P
Water/wt-% 15.6 11.6 9.9 99.1
MeOH/wt-% 11.7 24.5 90.0 0.8
IpAc/wt-% 72.7 63.9 0.1 0.1
Mixture stream/(kg?h?1) 935 369 161 15
Temperature/°C 79.9 73.8 66.4 62.3
Mixture II?Method II W W W R
Water/wt-% 80.6 0.0 99.5 0.5
MeOH/wt-% 19.3 0.5 0.45 99.5
IpAc/wt-% 0.1 99.5 0.05 0.0
Mixture stream/(kg?h?1) 765 466 605 146
Temperature/°C 85.7 87.8 99.1 69.5
Tab.7  Final optimized parameters for Method II with Mixture II
Mixture Method Q-DISTReboiler/(MJ?h?1) Q-DISTCondenser/(MJ?h?1)
Basic HI Diff./% Basic HI Diff./%
Mixture I Method I 4484 3606 ?20 ?3923 ?3226 ?18
Method II 2764 2272 ?18 ?2368 ?1996 ?16
Mixture II Method I 4567 4067 ?11 ?4312 ?3806 ?12
Method II 3132 2817 ?10 ?2887 ?2539 ?12
Tab.8  Energy savings due to heat integration (HI)
Mixture I (10 years amortization) Method I Method II
1000 $·y−1 % 1000 $·y−1 %
Investment cost
Column 53 34
Reboiler 47 29
Condenser+ LLVF+ post cooler 15 12
PV-membrane modules 37
PV-feed cooler 6
PV-retentate heating 22
PV-permeate cooler 2
Total 115 12 142 21
Operating cost
Steam 823 505
Water 40 32
PV-membrane change 10
Total 863 88 547 79
TAC 978 ? 689 ?
Tab.9  Comparison of the cost elements of the two methods for Mixture I
Mixture II (10 years amortization) Method I Method II
1000 $·y−1 % 1000 $·y−1 %
Investment cost
Column 62 40
Reboiler 52 32
Condenser+ LLVF+ post cooler 20 16
PV-membrane modules 32
PV-feed cooler 5
PV-retentate heating 20
PV-permeate cooler 2
Total 134 13 147 20
Operating cost
Steam 834 542
Water 42 34
PV-membrane change 8
Total 876 87 584 80
TAC 1010 731 ?
Tab.10  Comparison of the cost elements of the two methods for Mixture II
A Membrane transfer area, m2
B Constant in pervaporation model
D Distillate product
D‾i Transport coefficient of component i, kmol?m?2?h?1
F Feed
NF Number of mixture feed stage
NT Number of total stages
p Pressure, bar
pi0 Pure i component vapor pressure, bar
pi1 Partial pressure of component i on the liquid phase membrane side, bar
pi3 Partial pressure of component i on the vapor phase membrane side, bar
P Permeate
Q Heat of duty, MJ?h?1
R Retentate
U UNIQUAC parameter
W Bottom product
x Concentration of component, wt-%
xi1
y		 Concentration of component i in the feed, wt-%
Year
Greek letters
a ˜¯i Average activity coefficient of component i
  
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