Experimental studies of a continuous catalytic distillation column from startup to steady state for the production of methyl acetate

Mallaiah Mekala

doi:10.1515/ijcre-2023-0127

Article

Experimental studies of a continuous catalytic distillation column from startup to steady state for the production of methyl acetate

Mallaiah Mekala

Published/Copyright: December 22, 2023

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From the journal International Journal of Chemical Reactor Engineering Volume 22 Issue 2

Abstract

Esterification of acetic acid with methanol to produce methyl acetate and water has been studied in a continuous packed bed catalytic reactive distillation. The key challenge is the startup method of the experiments fora continuous reactive distillation as well as reactive zone height selection. In the present study, the effect of various operating conditions on the methyl acetate composition (mole fraction) is studied. Indion 180 ion-exchange resin solid catalyst is used in the reactive zone. The catalyst is immobilized by using a novel equivalent Katapak-S in the reactive section. Experiments were performed under different operating conditions to find the high purity methyl acetate product in the distillation. The experiments were performed for various conditions like total feed flow rate, reboiler temperature, reflux ratio, methanol to acetic acid mole ratio and catalyst loading with the time. The experiments were carried out till the system reaches to the steady state under different conditions. The maximum methyl acetate concentration is obtained at 80 °C reboiler temperature, 2.01 reflux ratio, 16.3 g/min flow rate, 60 g catalyst loading and 1 mol ratio of methanol to acetic acid. The highest purity of methyl acetate obtained under optimal condition is 95 % by mole.

Keywords: esterification; resin catalyst; reactive distillation; mole ratio

Corresponding author: Mallaiah Mekala, Department of Chemical Engineering, Chaitanya Bharathi Institute of Technology, Hyderabad 500075, India, E-mail: mmyadav2001@gmail.com

Research ethics: Not applicable.
Author contributions: The author has accepted responsibility for the entire content ofthis manuscript and approved its submission.
Competing interests: The author state no conflict of interest.
Research funding: No funding for present work.
Data availability: Not applicable.

References

[1] V. H. Agreda and L. R. Partin, “Reactive distillation process for the production of methyl acetate,” U.S. Patent 4435595.o. 1984, Available at: https://patents.google.com/patent/US4435595A/en.Search in Google Scholar

[2] R. Taylor and R. Krishna, “Modeling reactive distillation,” Chem. Eng. Sci., vol. 55, pp. 5183–5229, 2000, https://doi.org/10.1016/S0009-2509(00)00120-2.Search in Google Scholar

[3] E. Altmana, P. Kreis, T. van Gerven, G. D. Stefanidis, A. Stankiewicz, and A. Gorak, “Pilot plant synthesis of n-propyl propionate via reactive distillation with decanter separator for reactant recovery. Experimental model validation and simulation studies,” Chem. Eng. Proc., vol. 49, pp. 965–972, 2010, https://doi.org/10.1016/j.cep.2010.04.008.Search in Google Scholar

[4] M. Kloker, E. Y. A. KenigGorak, A. P. Markusse, and G. P. KwantMoritz, “Investigation of different column configurations for the ethyl acetate synthesis via reactive distillation,” Chem. Eng. Proc., vol. 43, pp. 791–801, 2004, https://doi.org/10.1016/S0255-2701(03)00084-9.Search in Google Scholar

[5] R. Baur, A. P. Higler, R. Taylor, and R. Krishna, “Comparison of equilibrium stage and nonequilibrium stage models for reactive distillation,” Chem. Eng. J., vol. 76, pp. 33–47, 2000, https://doi.org/10.1016/S1385-8947(99)00114-X.Search in Google Scholar

[6] L. U. Kreul, A. Gorak, C. Dittrich, and P. I. Barton, “Dynamic catalytic distillation: advanced simulation and experimental validation,” Comput. Chem. Eng., vol. 22, pp. S371–S378, 1998, https://doi.org/10.1016/S0098-1354(98)00077-5.Search in Google Scholar

[7] T. E. Corrigan and W. R. Ferris, “A development study of methanol acetic acid esterification,” Can. J. Chem. Eng., vol. 47, pp. 334–335, 1969, https://doi.org/10.1002/cjce.5450470404.Search in Google Scholar

[8] V. H. Agreda, L. R. Partin, and W. H. Heiss, “High purity methyl acetate via reactive distillation,” Chem. Eng. Prog., vol. 86, pp. 40–46, 1990.Search in Google Scholar

[9] B. Bessling, J. Loning, A. Ohligschlager, G. Schembecker, and K. Sundmacher, “Investigation on the synthesis of methyl acetate in a heterogeneous reactive distillation process,” Chem. Eng. Technol., vol. 21, pp. 393–400, 1998, https://doi.org/10.1002/(SICI)1521-4125(199805)21:5<393::AID-CEAT393>3.0.CO;2-9.10.1002/(SICI)1521-4125(199805)21:5<393::AID-CEAT393>3.0.CO;2-9Search in Google Scholar

[10] T. Popken, S. Steinigeweg, and J. Gmehling, “Synthesis and hydrolysis of methyl acetate by reactive distillation using structured catalytic packings: studies and simulation,” Ind. Eng. Chem. Res., vol. 40, pp. 1566–1574, 2001, https://doi.org/10.1021/ie0007419.Search in Google Scholar

[11] Z. Xu, A. Afacan, and K. T. Chuang, “Removal of acetic acid from water by catalytic distillation Part 1: experimental studies,” Can. J. Chem. Eng., vol. 77, pp. 676–681, 1999, https://doi.org/10.1002/cjce.5450770408.Search in Google Scholar

[12] A. Gorak and A. Hoffmann, “Catalytic distillation in structured packings: methyl acetate synthesis,” AIChE J., vol. 47, pp. 1067–1076, 2001, https://doi.org/10.1002/aic.690470513.Search in Google Scholar

[13] K. Sandesh, P. E. Jagadeeshbabu, S. Math, and M. B. Saidutta, “Reactive distillation using an ion exchange catalyst: experimental and simulation studies for the production of methyl acetate,” Ind. Eng. Chem. Res., vol. 52, pp. 6984–6990, 2013, https://doi.org/10.1021/ie3029174.Search in Google Scholar

[14] P. Suess and L. Spiegel, “Hold-up of mellapak structured packings,” Chem. Eng. Proc., vol. 31, pp. 119–124, 1992, https://doi.org/10.1016/0255-2701(92)85005-M.Search in Google Scholar

[15] K. H. Johnson, “Catalytic distillation structure,” US Patent 5189001, 1993. Available at: https://patents.google.com/patent/CA2078908A1/en.Search in Google Scholar

[16] Z. Olujic, A. F. Seibert, and J. R. Fair, “Influence of corrugation geometry on the performance of structured packings: an experimental study,” Chem. Eng. Proc., vol. 39, pp. 335–342, 2000, https://doi.org/10.1016/s0255-2701(99)00095-1.Search in Google Scholar

[17] L. Gotze, O. Bailer, P. Moritz, and C von Scala, “Reactive distillation with KATAPAK,” Catal. Today., vol. 69, pp. 201–208, 2001, https://doi.org/10.1016/S0920-5861(01)00370-4.Search in Google Scholar

[18] M. Mekala, S. K. Thamida, and V. R. Goli, “Pore diffusion model to predict the kinetics of heterogeneous catalytic esterification of acetic acid and methanol,” Chem. Eng. Sci., vol. 104, pp. 565–573, 2013, https://doi.org/10.1016/j.ces.2013.09.039.Search in Google Scholar

[19] M. Mekala and V. R. Goli, “Comparative kinetics of esterification of methanol-acetic acid in the presence of liquid and solid catalysts,” Asia-Pacific J. Chem. Eng., vol. 9, pp. 791–799, 2014, https://doi.org/10.1002/apj.1798.Search in Google Scholar

[20] M. Mekala, “Experimental and simulation studies of a continuous reactive distillation for an esterification process,” Int. J. Chem. React. Eng., vol. 20, pp. 1193–1207, 2022, https://doi.org/10.1515/ijcre-2021-0268.Search in Google Scholar

Received: 2023-06-24

Accepted: 2023-11-27

Published Online: 2023-12-22

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Articles in the same Issue

https://doi.org/10.1515/ijcre-2023-0127

Keywords for this article

esterification; resin catalyst; reactive distillation; mole ratio