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Article history:
Received 23 April 2011
Received in revised form
27 December 2011
Accepted 12 January 2012
Available online 21 January 2012
Keywords:
Ethanol dehydration
Extractive distillation
Glycerol
Entrainer
Distillation control
a b s t r a c t
In this paper, an investigation of the design and control of an extractive distillation process to produce
anhydrous ethanol using glycerol as entrainer is reported. The extractive distillation process receives the
azeotropic mixture ethanolwater that is fed into a dehydration column in one of the intermediate stages
while at the same time glycerol is fed into one of the top stages. As overhead product high purity ethanol
is withdrawn and in the bottom stream a mixture of water/glycerol is sent to a recovery column. The
effects of the entrainer to feed molar ratio, reux ratio, feed stage, feed entrainer stage and entrainer feed
temperature were studied to obtain the best design with minimal energy requirements. A control scheme
is developed in order to maintain stable operation for large feed disturbances. Dynamic simulations show
that is possible to use only one temperature control to hold the purity specications.
2012 Elsevier Ltd. All rights reserved.
1. Introduction
Distillation processes represent a high percentage of the separation operations used in the rening and chemical industries.
Distillation, in addition to being a very common operation, has
a strong impact on energy consumption of the processes and it
is used in the purication steps, where the products will have a
higher added value and specications are more rigorous, which is
the case of dehydration step in the anhydrous ethanol production.
Anhydrous ethanol is widely used in the chemical industry as a
raw material in chemical synthesis of esters and ethers, and as solvent in production of paint, cosmetics, sprays, perfumery, medicine
and food, among others. Furthermore, mixtures of anhydrous
ethanol and gasoline may be used as fuels, reducing environmental contamination and improving gasoline octane index, mainly
due to the addition of ethanol (Barba, Brandani, & Di Giacomo,
1985; Black, 1980; Chianese & Zinnamosca, 1990; Meirelles, Weiss,
& Herfurth, 1992). Among the most popular processes used in
ethanol dehydration, heterogeneous azeotropic distillation uses
solvents such as benzene, pentane, iso-octane and cyclohexane;
extractive distillation with solvents and salts as entrainers; adsorption with molecular sieves; and, processes that use pervaporation
130
1,0
105
Temperature (C)
0,8
y Ethanol
EtOH-Water T-x
EtOH-Water T-y
EtOH-Water T-x
EtOH-Water T-y
100
0,6
0,4
0,2
95
Exp.
Exp.
Est. NRTL
Est. NRTL
90
85
80
x-y Exp.
x-y Est. NRTL
0,0
75
0,0
0,2
0,4
0,6
0,8
1,0
0,0
0,2
x Ethanol
0,6
0,8
1,0
0,8
1,0
x-y Ethanol
1,0
290
250
Temperature (C)
0,8
y Water
0,4
0,6
0,4
0,2
210
170
130
Water-Gly T-x Exp.
Water-Gly T-y Exp.
Water-Gly T-x Est. NRTL
Water-Gly T-y Est. NRTL
90
x-y Exp.
x-y Est. NRTL
50
0,0
0,0
0,2
0,4
0,6
0,8
0,0
1,0
0,2
0,4
0,6
x-y Water
x Water
1,0
290
250
Temperature (C)
y Ethanol
0,8
0,6
0,4
0,2
210
170
130
90
x-y Exp.
x-y Est. NRTL
0,0
50
0,0
0,2
0,4
0,6
0,8
1,0
x Ethanol
0,0
0,2
0,4
0,6
0,8
1,0
x Ethanol
Fig. 1. T-xy and xy experimental and predicted diagrams at 1 atm for the ethanolwater, waterglycerol and ethanolglycerol systems (Carey & Lewis, 1932; Chen &
Thompson, 1970; Coelho, dos Santos, Mafra, Cardozo-Filho, & Coraza, 2011).
131
Fig. 2. Txy and xy experimental and predicted diagrams at 1 atm for the ethanolwater and waterglycerol systems (Carey & Lewis, 1932; Chen & Thompson, 1970). (a)
Residue curve map, (b) pseudo-binary vaporliquid equilibrium for ethanolwaterglycerol system (Lee & Pahl, 1985).
2008) as entrainers has been reported. However, there are no studies that report ethanol dehydration using glycerol as entrainer and
considering at the same time the control strategy required to produce high purity ethanol and recover totally the glycerol stream.
The purpose of this work is to design and control an extractive
distillation process to produce anhydrous ethanol using glycerol
as entrainer. This is a new alternative for dehydrate ethanol taking
into account that glycerol is available at low costs as consequence of
the high production of this substance in the biodiesel process. Additionally, it has been demonstrated the potential effect of glycerol in
modifying the vaporliquid equilibrium of the ethanolwater mixture eliminating the azeotrope. The steady state design involves the
selection of the appropriate thermodynamic model and the study
of the effect of the main design variables. The control strategy considers the control of only one temperature on each column in order
to be used for wider industrial applications and to provide good
product quality control.
2. Thermodynamic model
Ethanolwater mixture at atmospheric pressure has a
minimum-boiling homogeneous azeotrope at 78.1 C of composition 89 mol% ethanol. Thus, this mixture cannot be separated
in a single distillation column and if it is fed to a column operating
at atmospheric pressure, the ethanol purity in the distillate cannot
exceed 89 mol% while high purity water can be produced out from
the bottom. The NRTL physical property model (Renon & Prausnitz,
1968) is used to describe the nonideality of the liquid phase and
the vapor phase is assumed to be ideal. The complete NRTL model
binary parameters are taken from Aspen Plus database.
The thermodynamic model prediction is validated with experimental data from Carey and Lewis (1932), and Chen and Thompson
(1970) for ethanolwater and waterglycerol mixtures, respectively. The yx and Txy vaporliquid equilibrium plots are shown
in Fig. 1, where it can be seen that the model ts the experimental
132
Fig. 4. Effect of RR and EFS on ethanol purity and reboiler energy consumption of extractive distillation column.
data very well for the case of ethanolwater mixture and with some
difculties for the case of waterglycerol mixture in the zone of
lower water composition.
Ternary-phase diagrams with residue curves, distillation
boundaries and tie lines, provide very useful tool into the constraints encountered in the highly nonideal systems and they can
be used as simple method for identifying and designing feasible
extractive distillation sequences. Fig. 2a gives the residue curve
map for the ethanolwaterglycerol system calculated using Aspen
Split at 1 atm and Fig. 2b shows the pseudo-binary vaporliquid
equilibrium diagram for the same system with the experimental data reported by Lee and Pahl (1985). In Fig. 2b it is evident
that glycerol modies the vaporliquid equilibrium curve, eliminating the azeotrope and allowing obtaining high purity ethanol.
Lee and Pahl (1985) report that the glycols used as solvents eliminate the ethanolwater azeotrope and change the VLE curve.
Ethylene glycol is well known as solvent in extractive distillation of ethanolwater mixtures with a good performance results.
Fig. 5. Effect of RR and E/F on ethanol purity and reboiler energy consumption of extractive distillation column.
133
Fig. 6. Effect of EFT and RR on ethanol purity and reboiler energy consumption of extractive distillation column.
200
Ethanol
0,9
Temperature (C)
180
160
140
120
100
80
Water
0,8
Glycerol
0,7
0,6
0,5
0,4
0,3
0,2
0,1
60
0
0
10
Stage
15
20
10
Stage
15
20
134
210
Temperature (C)
0,9
160
110
60
0,8
0,7
Ethanol
0,6
Water
0,5
Glycerol
0,4
0,3
0,2
0,1
0
10
0
Stage
Stage
E/F ratio at 0.3, and increasing values of the reux ratio until a
distillate composition equivalent to the one obtained in the previous variation is reached; the increase in energy consumption was
30%. Consequently, the reux ratio must be operated in the lowest
possible value, so the ratio E/F ratio can be manipulated to reach
the distillate composition without high energy consumption, and
reminding that high E/F ratios increase the energy consumption in
reboiler of the recovery column. Also, Figs. 4 and 5 show that the
change in reux molar ratio (RR) has a greater effect on the reboiler
energy consumption than that of the entrainer feed stage (EFS) and
entrainer to feed molar ratio (E/F). To achieve the desired 99.5 mol%
of ethanol in D1, the entrainer to feed molar ratio must be about
0.45 at a low reux molar ratio of about 0.35.
Entrainer feed temperature (EFT) has an important effect on
the distillate composition and the reboiler energy consumption.
Several authors recommend considering EFT as design variable
15
+5%
-5%
1
0
-1
-2
-3
+5%
135
10
-5%
5
0
-5
-10
-15
-4
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Stage
Stage
Fig. 10. Sensitivity analysis for 5% changes in extractive and recovery reboiler duties.
distillation is fullled in eliminating water going into the rectifying section. Entrainer is fed on stage 3 and the azeotropic feed is
introduced on stage 10. Fig. 9 shows the nal owsheet for this system. It is important to observe that the overhead temperature in the
entrainer recovery column corresponds to 16 C. Therefore, cooling water cannot be used as cooling medium and a more expensive
cooling medium must be used instead.
4. Control strategy design
The development of the control strategy requires the conversion
of the steady state model in a dynamic one in order to evaluate the
effect of the main disturbances to the extractive distillation system.
108,00
195,00
107,50
194,00
136
107,00
106,50
106,00
87 mol % Ethanol
105,50
85 mol % Ethanol
193,00
192,00
191,00
190,00
105,00
87 mol % Ethanol
85 mol % Ethanol
189,00
104,50
188,00
0
10
Time (h)
10
Time (h)
0,99300
0,99700
0,99680
0,99200
XD2 (water)
0,99640
0,99620
0,99600
0,99100
0,99000
0,98900
0,99580
87 mol % Ethanol
87 mol % Ethanol
0,98800
85 mol % Ethanol
0,99560
0,99540
85 mol % Ethanol
0,98700
0
10
Time (h)
90,00
61,00
89,00
60,00
10
59,00
B1 (kmol/h)
D1 (kmol/h)
Time (h)
88,00
87,00
86,00
85,00
58,00
57,00
56,00
55,00
84,00
83,00
87 mol % Ethanol
54,00
87 mol % Ethanol
85 mol % Ethanol
53,00
85 mol % Ethanol
82,00
52,00
0
10
Time (h)
10
Time (h)
15,00
45,30
45,25
14,00
45,20
13,00
B2 (kmol/h)
D2 (kmol/h)
XD1 (ethanol)
0,99660
12,00
11,00
87 mol % Ethanol
45,10
85 mol % Ethanol
45,05
45,00
87 mol % Ethanol
10,00
45,15
85 mol % Ethanol
44,95
9,00
44,90
Time (h)
10
Time (h)
Fig. 12. Dynamic responses for feed composition disturbances in the control strategy 1.
10
114,00
200,00
112,00
198,00
110,00
108,00
106,00
104,00
102,00
Azeotropic Feed = +20%
100,00
137
196,00
194,00
192,00
190,00
Azeotropic Feed = +20%
188,00
186,00
98,00
0
10
10
Time (h)
Time (h)
0,99710
0,99000
0,99700
0,98800
0,98600
0,99680
XD2 (water)
XD1 (ethanol)
0,99690
0,99670
0,99660
0,99650
0,98400
0,98200
0,98000
0,99640
0,99630
0,97800
0,99620
0,97600
0
10
Time (h)
10
Time (h)
110,00
70,00
105,00
65,00
100,00
60,00
B1 (kmol/h)
95,00
D1 (kmol/h)
90,00
85,00
80,00
75,00
55,00
50,00
45,00
40,00
70,00
65,00
35,00
60,00
30,00
0
10
Time (h)
10
Time (h)
66,00
14,00
13,00
56,00
B2 (kmol/h)
D2 (kmol/h)
12,00
11,00
10,00
9,00
46,00
36,00
26,00
8,00
16,00
7,00
6,00
6,00
Time (h)
10
Time (h)
Fig. 13. Dynamic responses for feed ow disturbances in the control strategy 1.
10
138
139
196,00
107,50
195,00
107,00
106,50
106,00
105,50
87 mol % Ethanol
85 mol % Ethanol
194,00
193,00
192,00
191,00
190,00
87 mol % Ethanol
189,00
105,00
85 mol % Ethanol
188,00
104,50
187,00
0
10
Time (h)
10
Time (h)
0,99690
0,99300
0,99680
0,99200
0,99100
XD2 (water)
0,99660
0,99650
0,99640
0,99630
0,99620
0,99000
0,98900
0,98800
87 mol % Ethanol
87 mol % Ethanol
0,99610
85 mol % Ethanol
0,98700
85 mol % Ethanol
0,99600
0,99590
0,98600
0
10
Time (h)
10
Time (h)
90,00
64,00
89,00
62,00
B1 (kmol/h)
D1 (kmol/h)
88,00
87,00
86,00
85,00
60,00
58,00
56,00
84,00
87 mol % Ethanol
83,00
87 mol % Ethanol
54,00
85 mol % Ethanol
82,00
85 mol % Ethanol
52,00
0
10
Time (h)
10
Time (h)
15,00
48,00
14,00
47,50
47,00
13,00
B2 (kmol/h)
D2 (kmol/h)
XD1 (ethanol)
0,99670
12,00
11,00
46,50
46,00
45,50
87 mol % Ethanol
87 mol % Ethanol
10,00
45,00
85 mol % Ethanol
9,00
85 mol % Ethanol
44,50
0
Time (h)
10
Time (h)
Fig. 15. Dynamic responses for feed composition disturbances in the control strategy 2.
10
114,00
198,00
112,00
197,00
140
110,00
108,00
106,00
104,00
102,00
196,00
195,00
194,00
193,00
192,00
100,00
191,00
98,00
190,00
0
10
Time (h)
0,99900
0,99000
0,99850
0,98000
XD2 (water)
0,99750
0,99700
10
0,97000
0,96000
0,95000
0,99650
Azeotropic Feed = +20%
0,99600
0,94000
0,99550
0,93000
0
10
Time (h)
10
Time (h)
110,00
70,00
105,00
65,00
100,00
60,00
B1 (kmol/h)
95,00
D1 (kmol/h)
Time (h)
0,99800
XD1 (ethanol)
90,00
85,00
80,00
75,00
55,00
50,00
45,00
40,00
70,00
65,00
35,00
60,00
30,00
0
10
Time (h)
10
Time (h)
14,00
66,00
13,00
56,00
B2 (kmol/h)
D2 (kmol/h)
12,00
11,00
10,00
9,00
46,00
36,00
26,00
8,00
16,00
7,00
6,00
6,00
0
Time (h)
10
Time (h)
Fig. 16. Dynamic responses for feed ow disturbances in the control strategy 2.
10
1.568
4.2 min
0.4902
9.24 min
2.727
4.8 min
0.8523
10.56 min
6.77
0.59 min
0.6 min
0.13
0.899 min
Luyben (2002) Kc = 0.5 and I = 0.3 min and a lter time constant
F = 0.1 min. The two temperature control loops for the columns are
closed loop tested for determining the ultimate gains and periods,
and TyreusLuyben tuning rule (Tyreus & Luyben, 1992) is used. For
the cooler temperature control loop, open loop tests are performed
for determining the PI tuning constants following the IMC-PI tuning rule (Chien & Fruehauf, 1990). The results of those calculations
and the nal controller tuning parameters are shown in Table 1.
Extractive distillation process is the nal step in the ethanol production. The dehydration column is fed with azeotropic ethanol
coming from a rectication column. Changes in the operating
conditions of this column could originate disturbances in the
feed composition to the extractive distillation system, particularly
diminishing the concentration of stream to lower values of ethanol
mole fraction. Here have been considered two ethanol composition disturbances to test the control strategy from 89 to 87 mol%
ethanol and from 89 to 85 mol% ethanol at time = 2 h. Additionally,
feed ow disturbances of 20% also have been considered. Figs. 12
and 13 show the closed-loop results for these disturbances applied
to the control strategy 1.
Analyzing the results for the feed composition disturbances presented in Fig. 12, in the two top plots the temperature control point
on each column works well in rejecting disturbances and the temperatures back to their setpoints. The variation in temperature is
not higher than 3 C in extractive column and 5 C in the recovery column, but the system rapidly achieves the steady state. In
parallel, the results for the feed ow rate disturbances presented
in Fig. 13 show that temperature control points vary 10 and 12 C
for extractive and recovery column, respectively. This is due to the
most important effect that has the feed ow rate on the energy
required for the separation. Product purities are held quite close
to their specications and they are mainly affected by changes in
the feed composition, however the quality of ethanol stream never
is negatively affected and the control strategy ensures the quality
product. Inventory control loops are stabilized rapidly. In particular,
when the feed ow rate increases, the cascade controller increases
the entrainer ow rate fed to the extractive column making the base
level of the recovery column begins to drop. Because the ow rates
of entrainer and feed to the extractive column have increased the
material balance is adjusted increasing the feed to the recovery column, which brings the base level back up. However, good results
only are obtained augmenting the holdup time in the base level
which implies increase the size of the sump level of the recovery
column to achieve good controllability and compensate the loop
poor dynamics.
In order to improve the dynamic performance an alternative control strategy 2 is proposed modifying slightly the control
141
5. Conclusions
This article presents the design and control of an ethanol
dehydration process via extractive distillation using glycerol as
entrainer. The design owsheet is simulated using the NRTL thermodynamic model which describes appropriately the experimental
vaporliquid equilibrium data and supports on a solid thermodynamic basis the simulation results. From the sensitivity analysis
is possible to establish the main operating conditions of the system and to determine the effect of the design variables. Reux
ratio on the extractive distillation column has the greatest effect
on the energy consumption and it must be operated at low values.
Entrainer to feed molar ratio is useful in compensating changes
in some operating conditions without affecting the energy consumption in an important manner compared with the effect of
the reux ratio. Glycerol is an interesting candidate entrainer in
142
extractive distillation taking advantage of its low cost, high availability and great effect on azeotropic mixtures to improve the
relative volatility. The only possible drawback for ethanol dehydration via extractive distillation is that the two columns need to be
operated at higher temperatures demanding high pressure steam
to be used in the two reboilers.
Two control structures are developed and tested, providing
effective quality and production rate control. Control strategy 1
which uses the entrainer makeup ow rate to control the base level
in the recovery column has good control performance rejecting for
the disturbances in feed ow rate and feed composition, however,
it is necessary to adjust the size of sump level in order to obtain
good controllability and additionally the perturbations in temperature of the control point of each column are important. On the
contrary, control strategy 2 which uses the entrainer makeup ow
rate to control the entrainer feed ow rate to the extractive column allows to achieve a soft-regulating control with a minimal
changes in the temperature prole for both columns and maintaining the high purity of the products. Therefore, control strategy
2 is recommended for the extractive distillation of ethanol.
Acknowledgment
This work is supported by the Departamento Administrativo de
Ciencia, Tecnologa e Innovacin Colciencias under grant research
project code 1101-452-21113.
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