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Entrainer for Batch Distillation of Acetic Acid –Water System 871

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Entrainer for Batch Distillation of Acetic Acid –Water System 871 Journal of Scientific & Industrial Research Vol. 68, October GADEKAR 2009, pp. et al:871-875 ENTRAINER FOR BATCH DISTILLATION OF ACETIC ACID –WATER SYSTEM 871 Entrainer for batch distillation of acetic acid –water system S V Gadekar1, R V Naik2 and S N Kaul3* 1Department of Chemical Engineering, Bharati Vidyapeeth University College of Engineering, Pune, India 2National Chemical Laboratory, Pune, India 3National Environmental Engineering Research Institute, Nagpur, India Received 19 February 2008; revised 24 June 2009; accepted 21 July 2009 Acetic acid–water system (AW) poses a challenge in reactive distillation, acetic acid purity and loss of acetic acid in aqueous solutions. Feasible separation of AW has been studied using entrainers but acetic acid loss in lean phase cannot be avoided. This study presents feasible region to operate column with toluene and benzene as entrainer for AW. Liquid -liquid equilibrium data and nature of tie line for ethyl acetate are given priority. Keywords: Acetic acid, Batch distillation, Benzene, Entrainer, Toluene Introduction feasible separation have been reported8. Simulations have Under batch distillation, to reduce further recovery been done to find out suitable entrainer for AW9-11. of pure components, products are highly dependent on This study presents toluene, benzene and ethyl acetate initial mixture compositions. Use of batch rectifier and as an entrainer for AW to reduce amount of acetic acid stripper for heteroazeotropic systems has gained loss in aqueous phase of distillate using Residue Curve popularity1. Hillman2 studied many process alternatives Map (RCM). to achieve successful batch distillation operations. Distillation of heterogeneous mixture, which require Experimental decanter for handling liquid –liquid phase split, differs Residue Curve Map (RCM) from ideal systems. Vapor condenses and condensate RCM12 is a geometrical tool to find feasible separation, collects in decanter as entrainer rich phase and entrainer column sequencing and optimum parameters for distillation lean phase. Options are reported3-7 for sending entrainer operations. RCM are ternary diagrams displaying traces rich phase to column. Application of entrainer has of liquid compositions remaining in a single batch still as a smoothened process of complex heterogeneous systems. result of vaporization over a period of time. These liquid Efficiency of azeotropic batch distillation depends largely traces are known as residue curves. According to RCM upon choice of suitable entrainer for the system. technique13, any ternary diagram is divided into nodes Acetic acid-water (AW) system was studied with (stable and unstable), saddles and distillation regions. A certain entrainer on lab scale in batch mode of operation stable node is highest boiling vertex in a distillation region. and showed: a) decrease in loss of acetic acid from All residue curves in a distillation region point towards a aqueous layer of distillate; and b) reduced reaction time stable node. An unstable node is generally lowest boiling to complete equilibrium controlled reaction with high vertex in any distillation region, where all residue curves conversion for a particular configuration of batch will originate from an unstable vertex. A saddle point, an distillation assembly. Parameters (role of reflux, mode intermediate point in a distillation region, has neither residue of operation, entrainer inventory, and feed position) for curves coming or going through it. Residue curve runs from unstable node to stable node via a saddle point. *Author for correspondence Tel: 91-020-3027 3670; Fax: 91-020-25442770 Distillation boundary is a hazy line joining a stable node to E-mail: [email protected] azeotrope present in system or formed by joining two 872 J SCI IND RES VOL 68 OCTOBER 2009 Table 1— LLE data for AWT system13 (experimental tie lines in mole% at 40°C) S No Left phase Right phase Water Acetic acid Water Acetic acid 1 95.371 4.574 0.507 1.369 2 90.923 8.959 0.753 3.465 3 88.869 10.982 0.997 4..863 4 85.859 13.959 1.232 7.687 5 82.310 17.468 1.469 8.816 6 79.243 20.466 1.687 12.722 7 72.854 26.519 2.129 16.675 8 62.796 35.572 2.775 21.091 9 58.320 39.517 4.066 24.126 azeotropes in the system. It divides ternary plot into distillation regions. Fig. 1—Nature of residue curve for acetic acid-water-toluene system System was studied properly by vapor liquid equilibrium data for AW using toluene and benzene as entrainer. Tie line was compared for AW with toluene, benzene and ethyl acetate. Results and Discussion 1. Acetic Acid –Water –Toluene (AWT) System Liquid-liquid equilibrium (LLE) data (Table 1) for AWT was referred from DECHEMA14. In AWT, acetic acid is highest boiling vertex (BP 118°C) and becomes stable node (Fig. 1). There is presence of minimum boiling azeotropes between water and toluene at 84.4°C (Azeo 1) and acetic acid and toluene at 104.5°C (Azeo 2). Due to presence of azeotropes, entire ternary diagram is divided into three distillation regions (A, B and C). One of the distillation boundaries is formed Fig. 2—Triangular diagram showing selected VLE along with between acetic acid and Azeo 1 and other between Azeo bimodal curve 1 and Azeo 2 (Table 2). In Region A, acetic acid is stable node, and water-saddle point and Azeo 1 is unstable node. In Region B, acetic acid is stable node, and Azeo 2-saddle point and Azeo 1 is unstable node. In Region C, toluene is stable node, and Azeo 2-saddle point and Azeo 1 is unstable node. Under vapor-liquid equilibrium (VLE) data, there is no much difference in region A between liquid and vapor composition, suggesting that for feed in region A, time required will be more (Fig. 2). In region C, stable node is toluene, so nature of distillate will be richer in toluene, which is undesired (Fig. 1). Distillation in region B was found to be more superior to be operated. There were significant jumps between liquid and vapor compositions for points in region B, indicating that with minimum time Fig. 3—Feasible reason to operate column (acetic acid-water- and stages one can get desired output. Intensity of jump toluene system) GADEKAR et al: ENTRAINER FOR BATCH DISTILLATION OF ACETIC ACID –WATER SYSTEM 873 Table 2— Experimental VLE data for AWT ternary system Point number Liquid temp. Liquid composition Vapor composition °C Mole% Mole% Water Acetic acid Water Acetic acid Region C 1 101.5 2.6 35.35 7.88 35.88 2 101 2.9 25.97 2.55 19.622 3 100 9.11 35.40 9.4 34.2 4 102.5 2.157 39.289 8.88 35.47 5 102 5.3 41.5 9.75 36.27 6 103 7.14 32.55 5.911 13.67 7 104 0.214 13.3 1.7 30.50 8 105 5.911 13.67 6.904 28.848 Region B 9 98 5.59 53.47 2.3 17.36 10 90.5 24.5 54.71 55.82 8.3 11 92.5 11.39 56.23 68 30.22 Region A 12 103.5 24.05 72.26 51.5 43 13 101.5 40.80 48.42 64.27 34.31 14 102 42.80 47.628 62 36.9 15 92 41.27 52.45 62.19 35.72 16 94 34.5 62.29 53.28 34.09 17 100 63.02 36.77 76.5 22.35 18 101 46.6 50.70 83.51 15.90 19 100 62.34 37.36 72.19 27.39 for some points is such that it shows only 0-10% loss of Table 3— Experimental LLE data for AWB system acetic acid in aqueous phase. (experimental tie line in mole%) Points 9 and 10 (Fig. 3) shows significant jumps with S No. Left phase Right phase distillate composition below 8% tie line. Region B would Water Acetic acid Water Acetic acid be most favorable region for column operation since distillate collected in this region has shown some 1 95.000 4.500 1.025 2.943 magnificent jumps, indicating efficient separation without 2 76.400 22.800 2.933 10.780 3 57.270 39.353 6.192 23.482 much loss of acetic acid in aqueous solution. According 4 41.500 47.500 10.000 30.000 to nature of VLE data in this region and conceptual 5 30.500 49.000 16.000 40.000 methodology, feed position in shaded portion of region B would lead to negligible loss in acetic acid (0-2%) and may lead to less time in product separation. stable node, Azeo 2- saddle point and Azeo 1 is unstable node. In Region C, benzene is stable node, Azeo 2- saddle 2. Acetic Acid –Water –Benzene (AWB) System point and Azeo 1 is unstable node. One of the distillation LLE data for AWB system is given in Table 3. VLE boundaries is present between acetic acid and Azeo 1 data for some points are given in Table 4. In AWB and other distillation boundary is between Azeo 1 and system, acetic acid is highest boiling vertex and forms a Azeo 2. It is quite similar to AWT system. Nature of stable node. There is presence of azeotrope between residue curves in region A is showing still path to be benzene and water at 70.5°C (Azeo 1) and acetic acid increasing and become richer in acetic acid (stable node). and benzene at 80°C (Azeo 2). Due to presence of It is similar nature of residue curves in region B. Entire azeotropes, entire ternary diagram is divided into three residue curves are approaching stable node acetic acid.
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