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Selective Hydrogenation of Bio-refined Succinic Acid to 1,4-Butanediol Using Palladium-Alumina Bi-functional Catalyst: Effects of Calcination Temperature, Pressure, and Reaction Time

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Abstract

A series of 5% Palladium-Alumina (5% Pd-Al) catalysts are examined for hydrogenation of succinic acid to produce 1,4-Butanediol. 5% of Pd-Al catalysts are prepared by a single-step sol–gel method. The catalysts are calcined for six hours at various temperatures for stabilization of mechanical properties and to bring changes in pore size distribution and surface area. The same is followed by the reduction of the catalyst using hydrogen gas for 12 h at a total pressure of 30 bar. The catalysts are characterized by XRD, TGA, BET, FESEM, and FT-IR for structural, thermal stability, and textural properties of the Pd-Al bi-functional catalysts. High-pressure hydrogenation reactions are carried out in a 600 ml batch reactor at 250 °C and fewer than 60 bar total pressure with a total reaction time of 4 h. Statistical modeling of the overall process is done with a Box-Behnken Design using Response surface methodology by Design Expert 9.0 software. These correlate yield and various operating process parameters like calcination temperature, hydrogenation reaction pressure, and time. It is shown that the porous surface area, crystal size and temperature stability of the Pd-Al bi-functional catalyst could be controlled by changing the calcination temperature of the Alumina support. Palladium showed various forms after being deposited on the γ-Al2O3 surface, due to metal interaction with the support and higher oxygen affinity. The support and catalyst calcination temperatures and the action of the reaction mixture are important factors accounting for this variety.

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Acknowledgements

The authors thank UGC, India for RGNF fellowship provided to Mr. P. K. Baidya, the first author and contingency. The involvement of TCG Lifesciences, Bose Institute, and School of Material Science & Nanotechnology, Jadavpur University are acknowledged for providing with high-pressure hydrogenation apparatus, GCMS based analysis and physical characterization [FESEM and XRD] of catalyst samples respectively.

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Authors and Affiliations

  1. Department of Chemical Engineering, Jadavpur University, Kolkata, 700032, India

    Pabitra Kumar Baidya, Niwesh Ojha & Ujjaini Sarkar

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  1. Pabitra Kumar Baidya
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  2. Niwesh Ojha
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  3. Ujjaini Sarkar
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Contributions

PKB: He has prepared the catalysts and prepared the biorefined succinic acid, which has served as the raw material for high pressure hydrogenation, manage the high pressure hydrogenation setup for the experiments. He has also carried out the statistical analysis using Response Surface Methodology (RSM). US: Prof Sarkar has conceptualized a biorefinery with Crotalaria juncea as the feedstock, for the first time in India. She has helped in the completeness of this piece of research in terms of design of experiments, supplementing new ideas throughout and analysis of the data. The manuscript has been corrected by her based on the comments from the reviewers. NO: He has carried out the specific physical as well as chemical characterization of the catalysts. Further, he has carried out the experiments on high pressure hydrogenation. He has worked on additional characterization protocols suggested by the esteemed reviewers.

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Correspondence to Ujjaini Sarkar.

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Baidya, P.K., Ojha, N. & Sarkar, U. Selective Hydrogenation of Bio-refined Succinic Acid to 1,4-Butanediol Using Palladium-Alumina Bi-functional Catalyst: Effects of Calcination Temperature, Pressure, and Reaction Time. Catal Lett 153, 3454–3465 (2023). https://doi.org/10.1007/s10562-022-04240-8

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