Dynamic Behavior of Alternative Separation Processes For Ethanol Dehydration by Extractive Distillation

Subscriber access provided by Mississippi State University Libraries
Article
Dynamic Behavior of Alternative Separation Processes
for Ethanol Dehydration by Extractive Distillation
Cesar Ramírez-Márquez, Juan Gabriel Segovia - Hernández,
Salvador Hernández, Massimiliano Errico, and Ben-Guang Rong
Ind. Eng. Chem. Res., Just Accepted Manuscript • Publication Date (Web): 22 Nov 2013
Downloaded from http://pubs.acs.org on November 25, 2013
Just Accepted
“Just Accepted” manuscripts have been peer-reviewed and accepted for publication. They are posted
online prior to technical editing, formatting for publication and author proofing. The American Chemical
Society provides “Just Accepted” as a free service to the research community to expedite the
dissemination of scientific material as soon as possible after acceptance. “Just Accepted” manuscripts
appear in full in PDF format accompanied by an HTML abstract. “Just Accepted” manuscripts have been
fully peer reviewed, but should not be considered the official version of record. They are accessible to all
readers and citable by the Digital Object Identifier (DOI®). “Just Accepted” is an optional service offered
to authors. Therefore, the “Just Accepted” Web site may not include all articles that will be published
in the journal. After a manuscript is technically edited and formatted, it will be removed from the “Just
Accepted” Web site and published as an ASAP article. Note that technical editing may introduce minor
changes to the manuscript text and/or graphics which could affect content, and all legal disclaimers
and ethical guidelines that apply to the journal pertain. ACS cannot be held responsible for errors
or consequences arising from the use of information contained in these “Just Accepted” manuscripts.
Industrial & Engineering Chemistry Research is published by the American Chemical

Society. 1155 Sixteenth Street N.W., Washington, DC 20036
Published by American Chemical Society. Copyright © American Chemical Society.
However, no copyright claim is made to original U.S. Government works, or works
produced by employees of any Commonwealth realm Crown government in the course
of their duties.
Page 1 of 31 Industrial & Engineering Chemistry Research
1
2
3 Dynamic Behavior of Alternative Separation Processes for
4
5
6 Ethanol Dehydration by Extractive Distillation
7
8
9 César Ramírez – Márquez1, Juan Gabriel Segovia-Hernandez 1*, Salvador Hernández1,
10
11 Massimiliano Errico2, Ben-Guang Rong3
12
13
14
15
16
1 Universidad de Guanajuato, Campus Guanajuato, Division de Ciencias Naturales y
17
18 Exactas, Departamento de Ingenieria Quimica, Noria Alta S/N, Gto., Mexico 20256
19
20 2 Università degli Studi di Cagliari, Dipartimento di Ingegneria Meccanica, Chimica e
21
22 dei Materiali, Via Marengo 2, 09123 Cagliari, Italy
23
24 3 University of Southern Denmark, Department of Chemical Engineering,
25
26
27 Biotechnology and Environmental Technology, Niels Bohrs Allé 1, DK-5230 Odense
28
29 M, Denmark
30
31
32
33
34
35
36
37
38 *Corresponding author. Tel.: +52(473)7320006; E-mail: gsegovia@ugto.mx
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 1
ACS Paragon Plus Environment
Industrial & Engineering Chemistry Research Page 2 of 31
1
2
3
4
5
6
7
8
9
10 Abstract
11
12
13
Ethanol is attracting attention of researchers due to its potential in reducing the
14
15 dependence on crude oil together with the possible reduction in the pollution associated
16
17 with the combustion processes. The ethanol dehydration process is significant in terms
18
19 of its production cost. Recently new distillation sequences have been proposed for the
20
21
separation of pure ethanol from the fermentation broth. Extending the concept of
22
23
24 thermally coupled structures and column sections recombination, already successfully
25
26 applied to ideal mixtures, it was possible to generate new distillation sequences for
27
28 azeotropic mixtures. Those configurations are proved to exhibit lower energy
29
30 consumption together with reduced capital cost compared to the classical sequence
31
32
33
proposed in the literature. The aim of this work is the study of the controllability
34
35 properties under closed loop operation. Simulation results indicate that the presence of a
36
37 side stream in extractive distillation sequences does not necessarily provide operational
38
39 disadvantages; additionally results also suggest that control properties are ruled by the
40
41
kind of solvent used.
42
43
44
45
46 Keywords: extractive distillation, bioethanol, dynamic behavior, closed-loop operation.
47
48
49
50
51
52
53
54
55
56
57
58
59
60 2
1
2
3
4
5
6 1. Introduction
7
8 Renewable energy supply, climate change and environmental pollution have been the
9
10 main agenda in international dialogs and forums nowadays. Due to the political
11
12
13
instability in most of the oil-exporting countries, the price of the crude oil is escalating
14
15 to more than 96 US$ per barrel. The request of affordable and environmental friendly
16
17 energy sources is more than ever a necessity. Besides, the usage of fossil fuels such as
18
19 diesel and gasoline increases the greenhouse gases emission contributing to
20
21
environmental issues, like global warming, acid rain and human health deterioration.1
22
23
24 Hence, the use of new sources of energy, especially in the transport sector, has become
25
26 a priority. Bioethanol appears to be one of the most promising alternatives to fossil
27
28 derived fuels. Its production has increased all over the world in the last few years
29
30 through expansion of existing plants and construction of new facilities. 2 World fuel
31
32
33
ethanol production in 2003 was 32Mm3. The major producers of ethanol are Brazil and
34
35 the US, which together accounted for about 80% of world production. The U.S.
36
37 production of ethanol increased by an order of magnitude over the past 15 years,
38
39 reached 13 billion gallons (49 billion liters) in 2010, and grew at 15−20% per year over
40
41
the last two decades.3, 4 Although most of the ethanol is currently produced from corn
42
43
44 and other starch crops, the largest potential feedstock for ethanol is lignocellulosic
45
46 biomass, which includes materials such as agricultural residues (e.g., corn stover, crop
47
48 straws, sugar cane bagasse), herbaceous crops (e.g., alfalfa, switchgrass), forestry
49
50 wastes, wastepaper, and other wastes.
51
52
53 The ethanol concentration as obtained in the fermentation broth is about 5 wt %. To
54
55 reach a concentration of ethanol equal to 99.7 wt % as specified for the European Union
56
57 standards (EN 15376) or 98.7 wt % for the American Society for Testing and Materials
58
59
60 3
1
2
3 (ASTM) standards, significant amount of energy and high production cost are required.
4
5 5,6
Several energy demanding separation steps are required to reach the purity target,
6
7 mainly due to the presence of ethanol–water azeotrope (95.63 % wt ethanol at
8
9
10 atmospheric pressure). Different alternatives are available and described in the literature:
11
12 pervaporation, adsorption, pressure-swing distillation, extractive distillation, azeotropic
13
14 distillation, as well as hybrid methods combining these options. Although distillation
15
16 presents relatively high energy costs, it is still the preferred option in the case of large-
17
18
scale productions.7
19
20
21 One common industrial alternative for ethanol dehydration is extractive distillation.7-12
22
23 Extractive distillation performs the separation in the presence of a miscible, high boiling
24
25 point, relatively non-volatile component that does not form any azeotrope with the other
26
27 components in the mixture. For the extractive distillation of ethanol–water, ethylene
28
29
30 glycol remains the most commonly used entrainer, although glycerol, hyperbranched
31
32 polymers and ionic liquids were also proposed.7 As reported in Figure 1 the classical
33
34 extractive distillation sequence is composed by three columns.
35
36 The first, called pre-concentration or prefractionator, is used to concentrate ethanol from
37
38
5–12% up to 92.4–94% wt. In the second column the ethanol is dehydrated above the
39
40
41 azeotropic composition, then in the third one the solvent is recovered.
42
43 Extractive distillation is a promising separation opportunity and the aim of this paper is
44
45 to present a study about closed loop control policy, using PI controllers, for new
46
47 distillation sequences for the ethanol dehydration recently proposed by Errico and
48
49
50 Rong11. These new distillation configurations were obtained following the principles of
51
52 Process Intensification to save both energy and capital costs. The study of the control
53
54 properties represents the last step in the analysis of those new configurations.
55
56
57
58
59
60 4
1
2
3 Contrary to the conventional distillation process, the dynamic behavior of extractive
4
5 columns has been explored very little in published literature, although some authors
6
7 have approached this problem (Grassi II13, Yao et al.14, Arifin and Chien15, Gutierrez-
8
9
10 Guerra et al.16).
11
12 However, there are less studies focused on the dynamic behavior in extractive
13
14 conventional distillation to produce anhydrous ethanol using glycerol or ethylene glycol
15
16 as entrainer (Maciel and Brito17, Gil et al.18). The evaluation done by Maciel and Brito17
17
18
of the dynamic behavior of the extractive conventional distillation of ethanol using
19
20
21 ethylene glycol as the entrainer suggests good possibilities to control the process.19
22
23
24
25 Another important point is that the control properties in extractive distillation columns
26
27 are ruled by the kind of solvent used. The effect of the solvent in the control properties
28
29
30 has been discussed previously by Luyben20. A number of factors influence the selection
31
32 of solvent: selectivity, solvent power, boiling point, and heat of vaporization. Also,
33
34 controllability should be added to this list.
35
36
37
38
The purpose of this work is compare the dynamic behavior of alternative schemes of
39
40
41 extractive distillation proposed by Errico and Rong11, to produce anhydrous ethanol
42
43 using glycerol and ethylene glycol as entrainer. Taking advantage of these alternative
44
45 schemes characterized by a lower energy consumption compared to conventional
46
47 extractive distillation schemes.
48
49
50
51
52 2. Configurations Analyzed
53
54 Five sequences have been selected considering their low energy requirements and the
55
56 total annual cost.11 The first sequence called CLR and depicted in Figure 2a, consists on
57
58
59
60 5
1
2
3 a prefractionator, in which water-ethanol mixture is partially separated until a purity
4
5 close to the azeotrope is reached, followed by an extractive distillation column where,
6
7 using an entrainer, pure ethanol is obtained as distillate. Finally, the solvent is recovered
8
9
10 in the last column of the sequence. The distillate of the solvent recovery column
11
12 consists of a water-ethanol liquid mixture and is recycled back to the prefractionator.
13
14 The CVR configuration reported in Figure 2b has the same lay out of the previous one,
15
16 but the water-ethanol mixture is recovered in the solvent recovery column as a vapor.
17
18
Configurations CLR and CVR can be classified as conventional separation sequences.
19
20
21 The third configuration analyzed SSVR, reported in Figure 3, belongs to the category of
22
23 intensified sequences and consists of two columns. The prefractionator, followed by the
24
25 extractive distillation column with a side stream. In the extractive column, bioethanol is
26
27 obtained at the top, the solvent is recovered at the bottom and the vapor side stream
28
29
30 contains a mixture of water and ethanol, which is recycled to the prefractionator. The
31
32 fourth sequence, TCLR, consists of a DWC modeled considering its equivalent
33
34 thermally coupled configuration. As reported in Figure 4a, a liquid stream containing
35
36 water and ethanol, is recycled to the prefractionator. Ethanol is obtained as distillate of
37
38
the main column, while the solvent is recovered at the bottoms. The fifth sequence,
39
40
41 TCVR, reported in Figure 4b, is similar to the previous one, but the recycled mixture
42
43 ethanol-water is obtained in vapor phase.
44
45 Thus, the subspace of configurations under analysis includes the conventional
46
47 sequences, the two-column sequence with a side stream and the sequences with thermal
48
49
50 couplings. Additionally, the influence of the entrainer type is also considered.
51
52
53
54 3. Dynamic Analysis of Complex Sequences
55
56
57
58
59
60 6
1
2
3 For the closed-loop analysis, several issues must be defined first, such as the control
4
5 loops for each system, the type of process controller to be used, and the values of the
6
7 controller parameters. This analysis was based on proportional-integral (PI) controllers.
8
9
10 The choice of the type of controller was based on the ample use that the Proportional-
11
12 Integral (PI) mode has for distillation systems in the industrial practice. Several
13
14 alternatives exist for tuning up the controller parameters. We attempted a common
15
16 ground for comparison by optimizing the controller parameters, proportional gains (KC)
17
18
19 and reset times (τi), for each conventional and integrated scheme following the integral
20
21 of the absolute error (IAE) criterion.21
22
23
24
25 Therefore, for each loop, an initial value of the proportional gain was set; a search over
26
27
28
the values of the integral reset time was conducted until a local optimum value of the
29
30 IAE was obtained. The process was repeated for other values of the proportional gain.
31
32 The selected set of controller parameters was then the one that provided a global
33
34 minimum value of the IAE. Although the tuning procedure is fairly elaborated, the
35
36 control analysis is conducted based on a common tuning method for the controller
37
38
39 parameters. For the integrated arrangements, the procedure is particularly complicated
40
41 because of the interactions of the multivariable control problem. For these cases, the
42
43 tuning procedure was conducted taking one control loop at the time; the parameters thus
44
45 obtained were taken for the following control loop until all the loops were considered.
46
47
48
For the dynamic analysis, individual set point changes for product composition were
49
50 implemented for each of the two principal products streams: ethanol and water.
51
52
53
54 One of the key parts for the dynamic analysis is the selection of control outputs and
55
56
manipulated variables for each control loop. A well-known structure is based on energy
57
58
59
60 7
1
2
3 balance considerations, which yields to the so-called LV control structure in which the
4
5 reflux flowrate L and the vapor boilup rate V (affected directly by the heat duty
6
7 supplied to the reboiler) are used to control the distillate and bottom outputs
8
9
10 compositions (Häggblom and Waller22). It should be mentioned that such control loops
11
12 have been used with satisfactory results in previous studies on thermally coupled
13
14 systems.23-26 The manipulated variables for the distillation columns were the
15
16 corresponding reflux flowrates, reboiler heat duties or side stream flowrate for the
17
18
control composition of ethanol and water, (see for example Figure 5). Additionally, the
19
20
21 pairing of same manipulated and control variables was obtained using the relative gain
22
23 array method (RGA).
24
25
26
27 4. Case Study
28
29
30 A diluted ethanol-water solution hypothetically produced from a fermentation process
31
32 with a flowrate of 1694.24 kmol hr-1 and the composition reported in Table 1 is
33
34 considered as a feed for all the cases considered. The NRTL method was utilized to
35
36 evaluate the activity coefficients. Ethylene glycol was chosen as solvent. The ethanol
37
38
minimum purity was set to 0.999 on molar fraction basis to enable its use blended with
39
40
41 oil derived fuels. According to the work of Errico et al.27,28 the configurations
42
43 considered were first simulated utilizing the Winn-Underwood-Gilliland short-cut
44
45 method, then the design parameters were optimized minimizing the heat duty. A solvent
46
47 to feed ratio of 0.87 was employed in all the configurations simulated. The solvent
48
49
50 recovery column was designed in order to minimize the make-up flowrate. The
51
52 installation cost evaluation was performed with Aspen Plus Economic Analyzer. Some
53
54 representative designs are displayed in Tables 2 and 3. The energy consumptions, the
55
56 capital costs and the solvent makeup flowrate for the configurations reported in Figures
57
58
59
60 8
1
2
3 2-4, are summarized in Table 4. It is possible to notice that the divided wall
4
5 configurations are promising options to reduce the energy and capital costs even if,
6
7 considering their structure complexity, a dynamic analysis is essential. Another
8
9
10 interesting configuration is the SSVR. Analyzing the solvent makeup flowrate reported
11
12 in Table 4 it is evident that the SSVR has an high solvent consumption due to the
13
14 presence of the side stream. The convenience to employ this type of configuration can
15
16 be evaluated as a difference between the energy and capital costs saved compared to the
17
18
traditional sequences and the increase of the solvent consumption. For this reason the
19
20
21 configurations CVR and SSVR were simulated again considering glycerol as entrainer.
22
23 Glycerol is a cheaper solvent that can be obtained as a by-product from biodiesel plants.
24
25 The results, when glycerol is used as entrainer, are summarized in Table 5.
26
27
28
29
30 5. Results
31
32 The prediction of the transient response of a distillation column bears much importance
33
34 in the sense of the effective control of the separation process.29 Such resulting structures
35
36 obtained with the main target of the energy savings provided the configurations that
37
38
were subjected to the dynamic analysis. For all cases, two control loops were assumed
39
40
41 to operate under closed loop fashion. The performance of the sequences under analysis
42
43 was compared through the evaluation of IAE values for each test.
44
45
46
47 Table 6 shows the IAE values obtained for each composition control loop of the eight
48
49
50 cases considered using LV configuration in closed loop (see for example Figure 5).
51
52
53
54 The two-column sequence with a vapor side stream (SSVR-GL) exhibited the best
55
56 performances, based on the lowest values of IAE, for the control of the two product
57
58
59
60 9
1
2
3 streams. The conventional column sequence (CVR-GL) exhibit good dynamic
4
5 performance based in the IAE value for ethanol loop. However, it presents a worst
6
7 dynamic behavior in the water loop in comparison with SSVR-GL configuration (see
8
9
10 Figure 6). The worst performances are observed when ethylene glycol is used and the
11
12 conventional sequences (CLR-EG and CVR-EG) and the thermally coupled sequences
13
14 (DWC-TCVR and DWC-TCVR) based on the values of IAE (Table 6). An important
15
16 point to note is that for sequences SSVR and DWC-TCLR, using ethylene glycol as
17
18
entrainer, under the LV control structure and under the tuning methodology used in this
19
20
21 work was not possible to find the values of KC and τI to stabilize the dynamic response
22
23 for water.
24
25
26
27
28
To complete the study of the control properties, relative gain arrays (RGA) were
29
30 obtained for all sequences analyzed. Figure 7 show the RGA results and the schemes for
31
32 some representative sequences. As we can see, the complex sequence presents
33
34 interactions because positive values of the relative gains are greater than 1. Also, the
35
36 negative values cause negative interactions. In general, from relative gains arrays for all
37
38
39 cases of study, we can conclude that significant interactions are present in all distillation
40
41 sequences studied. We use the relative gain array method to fix other loops for the
42
43 control system. One representative case is showed in Table 7 is displayed a comparison
44
45 between loops proposed by LV and RGA study. The IAE values were reported for both
46
47
48
cases (LV and RGA control structure) in Table 8 for optimum control behavior. The
49
50 loops proposed by RGA structure, in the case of SSVR and DWC-TCLR, using
51
52 ethylene glycol as entrainer, are better than LV control loops. This shows that under this
53
54 configuration it was possible for these two sequences stabilize the control loop of water.
55
56
Recalling that it was not possible to stabilize this loop in the LV configuration.
57
58
59
60 10
1
2
3
4
5 The effect of the solvent in the control properties has been discussed previously by
6
7 Luyben20. Under these arguments is understandable that in our case study the kind of
8
9
10 solvent affects the dynamic performance and the selection of the loop configuration of
11
12 the systems.
13
14
15
16 In Table 8 a summary of the results obtained in this study is reported. It is important to
17
18
include both the toxicity (and cost) of the solvent and the amount of CO2 emissions
19
20
21 generated in the heating of reboiler of the columns, since they even pretend to have the
22
23 best integral design. Sometimes it is possible to get the best settings in dynamic
24
25 performance, but the design can be operating with high CO2 emissions levels or it might
26
27 also be using very toxic (or expensive) extracting agent. For those reasons it is
28
29
30 necessary to do a global analysis and selection of all parameters associated in the design
31
32 structure and dynamic behavior of the system.
33
34
35
36 The results from the dynamic behavior (based in IAE values) indicate that the presence
37
38
of a side stream does not necessarily provides operational disadvantages, as originally
39
40
41 expected due to the resulting complex structural design. Also, in general, configurations
42
43 with a side stream and the conventional sequences using glycerol as a solvent
44
45 outperformed the dynamic behavior of the DWC schemes, the energy consumption,
46
47 CO2 emissions, cost and toxicity of entrainer. The greenhouse emissions were calculated
48
49
50 as proposed by Gadalla et al. 30
51
52
53
54 6. Conclusions
55
56
57
58
59
60 11
1
2
3 A study on dynamic behavior of alternative extractive distillation sequences for the
4
5 purification of bioethanol has been presented. Results from closed loop fashion
6
7 indicated that, in general, configurations with a vapor side stream and the conventional
8
9
10 sequences using glycerol as solvent are the best options. One factor seems to affect the
11
12 optimal choice: the kind of solvent used as entrainer. The better performances of the
13
14 sequences with glycerol compare to the ethylene glycol promote even more the use of
15
16 sustainable solvents. In general, it is worth to notice that the presence of side streams
17
18
instead of deteriorating the dynamic behavior of extractive distillation systems, for this
19
20
21 case of study, may contribute positively to their dynamic properties. In general, those
22
23 alternative extractive distillation arrangements, with complex structures can be a good
24
25 option for industrial use, due to a good dynamic behavior and the reduction in energy
26
27 consumption.
28
29
30
31
32 Acknowledgements
33
34 This research project was supported by a project SAGARPA-CONACyT-174560,
35
36 (Universidad Michoacana de San Nicolás de Hidalgo and Universidad de Guanajuato,
37
38
México). Gratefully acknowledges Sardinia Regional Government for the financial
39
40
41 support (P.O.R. Sardegna F.S.E. Operational Programme of the Autonomous Region of
42
43 Sardinia, European Social Fund 2007-2013 - Axis IV Human Resources, Objective l.3,
44
45 Line of Activity l.3.1 “Avviso di chiamata per il finanziamento di Assegni di Ricerca”).
46
47
48
49
50
51
52 References
53
54
55
56
57
58
59
60 12
1
2
3 (1) Tan, K.T.; Lee, K.T.; Mohamed, A.R. Role of Energy Policy in Renewable Energy
4
5 Accomplishment: The Case of Second-Generation Bioethanol. Energy Policy 2008, 36,
6
7 3360.
8
9
10 (2) Karuppiah, R.; Peschel, A.; Grossmann, I, E.; Martín, M.; Martinson, W.; Zullo, L.
11
12 Energy Optimization for the Design of Corn-Based Ethanol Plants. AIChE J. 2008, 54,
13
14 1499.
15
16 (3) Kim, S.; Dale, B.E. Environmental Aspects of Ethanol Derived from No-Tilled Corn
17
18
Grain: Nonrenewable Energy Consumption and Greenhouse Gas Emissions. Biomass
19
20
21 and Bioenergy 2005, 28, 475.
22
23 (4) Wallington, T.J.; Anderson, J.E.; Mueller, S.A.; Kolinski Morris, E.; Winkler, S.L.;
24
25 Ginder, J.M. Corn Ethanol Production, Food Exports, and Indirect Land Use Change.
26
27 Environ. Sci. Technol. 2012, 46, 6379.
28
29
30 (5) Vane, L. M. Separation Technologies for the Recovery and Dehydration of Alcohols
31
32 from Fermentation Broths. Biofuels, Bioprod. Biorefin. 2008, 2, 553.
33
34 (6) Gudena, K.; Rangaiah, G.P.; Lakshminarayanan, S. HiGee Stripper-Membrane
35
36 System for Decentralized Bioethanol Recovery and Purification. Ind. Eng. Chem. Res.
37
38
2013, 52, 4572.
39
40
41 (7) Kiss, A.A. Novel Applications of Dividing-Wall Column Technology to Biofuel
42
43 Production Processes. J Chem Technol Biotechnol 2013, 88, 1387.
44
45 (8) Ravagnani, M.A.S.S.; Reis, M.H.M.; Maciel -Filho, R.; Wolf -Maciel, M.R.
46
47 Anhydrous Ethanol Production by Extractive Distillation: A Solvent Case Study.
48
49
50 Process Safety and Environment Protection 2010, 88, 67.
51
52 (9) Avilez – Martínez, A.; Saucedo – Luna, J.; Segovia - Hernández, J.G.; Hernández,
53
54 S.; Gómez – Castro, F.I.; Castro – Montoya, A.J. Dehydration of Bioethanol by Hybrid
55
56
57
58
59
60 13
1
2
3 Processes Liquid – Liquid Extraction / Extractive Distillation. Ind. Eng. Chem. Res.
4
5 2012, 51, 5847.
6
7 (10) Kiss, A.A.; Suszwalak, D.J.-P.C. Enhanced Bioethanol Dehydration by Extractive
8
9
10 Distillation in Dividing-Wall Columns. Separation and Purification Technology 2011,
11
12 86, 70.
13
14 (11) Errico, M.; Rong, B.-G. Synthesis of New Separation Processes for Bioethanol
15
16 Production by Extractive Distillation. Separation and Purification Technology 2012, 96,
17
18
58.
19
20
21 (12) Vázquez - Ojeda, M.; Segovia - Hernández, J.G.; Hernández, S.; Hernández –
22
23 Aguirre, A.; Kiss, A.A. Design and Optimization of an Ethanol Dehydration Process
24
25 Using Stochastic Methods. Separation and Purification Technology 2013, 105, 90.
26
27 (13) Grassi II, V.G. Process Design and Control of Extractive Distillation, in Practical
28
29
30 Distillation Control, Luyben, W.L. (ed). (Van Nostrand Reinhold, NY), 1992.
31
32 (14) Yao, J.Y.; Lin, S.Y. and Chien, I.L. Operation and control of batch extractive
33
34 distillation for the separation of mixtures with minimum-boiling azeotrope. J. Chin Inst
35
36 Chem Eng 2007, 38, 371.
37
38
(15) Arifin, S. and Chien, I.L. Design and control of an isopropyl alcohol dehydration
39
40
41 process via extractive distillation using dimethyl sulfoxide as an entrainer. Ind. Eng
42
43 Chem Res 2008, 47, 790.
44
45 (16) Gutiérrez-Guerra, R.; Segovia-Hernández, J.G. and Hernández, S. Reducing energy
46
47 consumption and CO2 emissions in extractive distillation. Chem Eng Res Des 2009, 87,
48
49
50 145.
51
52 (17) Maciel, M. R. W. and Brito, R. P. Evaluation of the Dynamic Behavior of an
53
54 Extractive Distillation Column for Dehydration of Aqueous Ethanol Mixtures. Comput.
55
56 Chem. Eng. 1995, 19 (Suppl. 1), 405−408.
57
58
59
60 14
1
2
3 (18) Gil, I. D.; Gómez, J. M.; Rodríguez, G. Control of an Extractive Distillation
4
5 Process to Dehydrate Ethanol Using Glycerol as Entrainer. Comput. Chem. Eng. 2012,
6
7 39, 129−142.
8
9
10 (19) Ramos, M. A.; García-Herreros, P. and Gómez, J. M. Optimal Control of the
11
12 Extractive Distillation for the Production of Fuel-Grade Ethanol. Ind. Eng. Chem. Res
13
14 2013, A-Q.
15
16 (20) Luyben W.L. Effect of solvent on controllability in extractive distillation. Ind. Eng.
17
18
Chem. Res. 2008, 47, 4425.
19
20
21 (21) Stephanopoulos, G. Chemical Process Control: An Introduction to Theory and
22
23 Practice. Prentice Hall, Englewood Cliffs, NJ, 1984.
24
25 (22) Häggblom, K.E.; Waller, K.V. Control Structures, Consistency, and
26
27 Transformations, in Practical Distillation Control. Edited by W.L. Luyben, Van
28
29
30 Nostrand Reinhold: NY, 1992.
31
32 (23) Jiménez, A.; Hernández, S.; Montoy, F. A.; Zavala-García, M. Analysis of Control
33
34 Properties of Conventional and Nonconventional Distillation Sequences. Ind. Eng.
35
36 Chem. Res. 2001, 40, 3757.
37
38
(24) Segovia-Hernández, J. G.; Hernández, S.; Jiménez, A. Control Behaviour of
39
40
41 Thermally Coupled Distillation Sequences. Trans IChemE 2002, 80, Part A, 783.
42
43 (25) Segovia - Hernández, J.G.; Hernández, S.; Rico – Ramírez V.; Jiménez, A. A
44
45 Comparison of the Feedback Control Behavior between Thermally Coupled and
46
47 Conventional Distillation Schemes. Comput. Chem. Eng. 2004, 28, 811.
48
49
50 (26) Segovia - Hernández, J.G.; Hernández, S.; Femat, R.; Jiménez, A. Control of
51
52 Thermally Coupled Distillation Sequences with Dynamic Estimation of Load
53
54 Disturbances. Ind. Eng. Chem. Res. 2007, 46, 546.
55
56
57
58
59
60 15
1
2
3 (27) Errico M.; Rong, B.-G.; Tola, G.; Spano, M. Optimal Synthesis os Distillation
4
5 Systems for Bioethanol Separation. Part 1: Extractive Distillation with Simple Columns.
6
7 Ind. Eng. Chem. Res. 2013 a, 52, 1619.
8
9
10 (28) Errico M.; Rong, B.-G.; Tola, G.; Spano, M. Optimal Synthesis os Distillation
11
12 Systems for Bioethanol Separation. Part 2: Extractive Distillation with Complex
13
14 Columns. Ind. Eng. Chem. Res. 2013 b, 52, 1626.
15
16 (29) Berber, R.; Karadurmus, E. Dynamic Simulation of a Distillation Column
17
18
Separating a Multicomponent Mixture. Chem. Eng. Comm. 1989, 84, 113.
19
20
21 (30) Gadalla, M.A.; Olujic, Z.; Jansens, P.J.; Jobson, M.; Smith, R. Reducing CO2,
22
23 Emissions and Energy Consumption of Heat-Integrated Distillation Systems. Environ.
24
25 Sci. Technol. 2005, 39, 6860.
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 16
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24 Figure 1. Classical extractive distillation process for ethanol dehydration.
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 17
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23 Figure 2. Conventional separation sequences: (a) CLR with liquid recycle, (b) CVR
24 with vapor recycle.
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 18
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22 Figure 3. Two-column sequence (SSVR) with vapor side stream.
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 19
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23 Figure 4. DWC/Thermally coupled sequence: (a) TCLR with liquid recycle, (b) TCVR
24 with vapor recycle.
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 20
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22 Figure 5. Loops LV: (a) Two-column sequence (SSVR) with vapor side stream, (b)
23 TCLR with liquid recycle.
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 21
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33 Figure 6. Dynamic responses: (a, b) SSVR sequence; (c, d) TCLR sequence.
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 22
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
Figure 7. Matrix and schemes by RGA method for Two-column sequence (SSVR) with
33
34 vapor side stream and DWC- TCLR with liquid recycle, with ethylene glycol as
35 entrainer.
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 23
1
2
3 Table 1. Mixture analyzed and component’s properties.
4
5 Component Feed composition Boiling point Critical Critical
6 (mol. fraction) (°C) temperature (°C) pressure (bar)
7 Ethanol 0.05 78.1 241 63
8 Water 0.95 100 373.94 220.58
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 24
1
2
3 Table 2. Design variables of SSVR.
4
5 Sections 1 to 3 Sections 4 to 8
6 Number of stages 44 36
7 Feed stage 30 25
8 Recycle stage 34 -
9 Extractant stage - 3
10 Distillate rate, kmol h−1 103.449 85.037
11 Bottom rate, kmol h−1 1609.178 51.145
Feed flowrate, kmol h−1 1694.24 103.449
12
Recycle flowrate, kmol h−1 18.387 -
13
Extractant flowrate, kmol h−1 - 51.12
14 Reflux ratio 2.011 0.189
15 Temperature of distillate, ◦C 78.212 78.308
16 Top pressure, bar 1 1
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 25
1
2
3 Table 3. Design variables of DWC –TCLR with ethylene glycol.
4
5 Sections 1 to 3 Dividing wall column
6 Section 4 Section 5 Section 6 and 7 Section 8
7 Number of stages 44 5 20 10 7
8 Feed stage 30 - 20 - -
9
Recycle stage 30 - - - -
10
Extractant stage - 5 - - -
11
Distillate rate, kmol h−1 100.200 84.165 - - -
12
Bottom rate, kmol h−1 1610.394 - - - 86.521
13
14 Feed flowrate, kmol h−1 1694.24 - 100.2 - -
15 Recycle flowrate, kmol h−1 16.354 - - - -
16 Extractant flowrate, kmol h−1 - 86.84 - - -
17 Reflux ratio 2.325 0.235 - - -
18 Temperature of distillate, ◦C 77.863 77.976 - - -
19 Top pressure, bar 1 1 - - -
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 26
1
2
3 Table 4. Energy requirements, capital costs and solvent makeup for the configurations
4 considered using ethylene ethylene glycol as entrainer.
5
6 CLR-EG CVR-EG SSVR-EG TCLR-EG TCVR-EG
7
Total condenser duty (kW) 4081.316 3871.042 3852.160 3970.814 3800.718
8
9
Total reboiler duty (kW) 5118.425 4907.893 4902.925 5005.800 4837.323
10 Solvent makeup (kmol hr-1) 0.004 0.004 0.619 0.004 0.004
11 Annualized capital cost (k$ yr-1) 132.8 133.1 107.8 102.3 102.6
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 27
1
2
3 Table 5. Energy requirements, capital costs and solvent makeup for the configuration
4 reported in Fig. 2(b) and in Fig. 3 using glycerol as entrainer
5
6 CVR-GL SSVR-GL
7
Total condenser duty (kW) 3820.645 3750.638
8
9
Total reboiler duty (kW) 5018.671 4934.136
10 Solvent makeup (kmol hr-1) 0.001 0.010
11 Annualized capital cost (k$ yr-1) 134.3 112.9
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 28
1
2
3 Table 6. Optimum closed loops LV
4
5 Component Kc Ti IAE
6 Ethanol 250.00 25.40 0.008570903
7 SSVR-GL
8 Water 25.00 3.00 4.90910E-04
9 Ethanol 20.00 68.00 0.014097702
10
SSVR-EG
Water - - -
11 Ethanol 250.00 22.76 0.008675855
12 CVR-GL
Water 175.00 8.75 0.002797684
13
14 Ethanol 250.00 55.00 0.010519718
CVR-EG
15 Water 150.00 100.00 0.015901120
16 Ethanol 250.00 51.25 0.010172300
17 CLR-EG
Water 10.00 139.75 0.050686177
18
Ethanol 225.00 58.25 0.010521612
19 DWC/TCVR-EG
20 Water - - -
21 Ethanol 250.00 52.00 0.011971880
22 DWC/TCLR-EG
Water 225.00 61.50 0.012179141
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 29
1
2
3 Table 7. Pairing loops by LV and RGA method in all sequences
4
5 LV RGA
6
7 xEthanol xWater(C1) xSolvent xWater xEthanol xWater(C1) xSolvent xWater
8 SSVR-GL R2 Fl Q2 Q1 Q2 Fl R2 Q1
9
10 SSVR-EG R2 Fl Q2 Q1 Fl Q2 R2 Q1
11 CVR-GL R2 R3 Q3 Q1 R2 R3 Q3 Q1
12 CVR-EG R2 R3 Q3 Q1 R2 R3 Q3 Q1
13
14 CLR-EG R2 R3 Q3 Q1 R2 R3 Q3 Q1
15 DWC/TCLR-EG R2 R3 Q2 Q1 Q2 R3 R2 Q1
16
17 DWC/TCVR-EG R2 R3 Q2 Q1 R3 Q2 R2 Q1
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 30
1
2
3 Table 8. Optimum closed loops and energy consumption, CO2 emissions, toxicity and
4 cost of solvent used for all analyzed sequences.
5
6 Total Emissions Solvent
7
8
Control Reboiler duty CO2 Toxicity Cost
9 IAE Ethanol IAE Water [kW] [tons/hour] Category* [Dollar/kg]
10 SSVR-GL 0.008570903a 4.90910E-04a 5118.425 23.93034 0 0.825
11 a b
SSVR-EG 0.014097702 8.48955E-05 4907.893 67.71364 5 2
12 CVR-GL 0.008675855a 2.79768E-03a 4902.925 24.11146 0 0.825
13
14 CVR-EG 0.010519718a 1.59011E-02a 5005.800 25.01390 5 2
15 CLR-EG 0.010172300a 5.06862E-02a 4837.323 26.06645 5 2
a b
16 DWC/TCVR-EG 0.010521612 9.63112E-03 5018.671 28.14349 5 2
17 DWC/TCLR-EG 0.011971880a 1.21791E-02a 4934.136 27.81083 5 2
18
19 a
20 Loop LV
b
21 Loop RGA
22 * TAGGED UNDER THE GLOBAL SYSTEM HARMONIZED (Decree 307/2009).
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60 31

Dynamic Behavior of Alternative Separation Processes For Ethanol Dehydration by Extractive Distillation

Uploaded by

Copyright:

Available Formats

You might also like

Dynamic Behavior of Alternative Separation Processes For Ethanol Dehydration by Extractive Distillation

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Dynamic Behavior of Alternative Separation Processes For Ethanol Dehydration by Extractive Distillation

Uploaded by

Copyright:

Available Formats

Subscriber access provided by Mississippi State University Libraries

Industrial & Engineering Chemistry Research is published by the American Chemical

You might also like