Production of Butyl Levulinate by Butanolysis of Furfuryl Alcohol using WO3-ZrO2 as a solid acid catalyst

Rao, Thuppati Upender and Maity, Sunil Kumar (2019) Production of Butyl Levulinate by Butanolysis of Furfuryl Alcohol using WO3-ZrO2 as a solid acid catalyst. Masters thesis, Indian institute of technology Hyderabad.

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Abstract

The gradual depletion of fossil fuels and the continuous deterioration of the environment by greenhouse gases draws the world’s attention to look for carbon-neutral renewable energy resources such as biomass. The transportation fuels are the second largest sector, which is consuming nearly 28% of the world's energy. The biomass-derived alkyl levulinates can be considered as the attractive fuel additives because of their unique physicochemical properties. The present work is thus entitled to the production of butyl levulinate by the butanolysis of furfuryl alcohol in the presence of WO3-ZrO2 as a solid acid catalyst. In this work, WO3-ZrO2 catalysts were prepared by the evaporation-induced self-assembly (EISA) method (one pot synthesis). The prepared catalysts were characterized by BET, FTIR analysis, pyridine probed FTIR, and Raman spectra. The butanolysis of furfuryl alcohol was carried out in a high-pressure batch reactor in the presence of WO3-ZrO2 catalyst. The liquid sample products were quantified using gas chromatography equipped with a flame ionization detector (GC-FID) and identified using gas chromatography equipped with mass spectroscopy (GC-MS). The calcination temperature highly impacts the textural properties and performance of the WO3- ZrO2 catalysts. In this work, WO3-ZrO2 catalyst was calcined at different temperatures ranging from 873 K to 1123 K. The activity of the catalyst was boosted with the increase in calcination temperature. The calcination temperature also enhanced the dispersion of W-atoms on the surface of ZrO2 support. The optimum calcination temperature for WO3-ZrO2 catalyst was observed to be 1073 K. However, the wt% of butyl levulinate was decreased with increase in calcination temperature due to the formation of intermediate product 2-butoxy methyl furan (2- BMF) was more. The WO3 loading also impacts the activity of the catalyst. With increasing WO3 loading, the specific surface area of the catalysts was increased due to the formation of W⎯O⎯Zr bond. The pure ZrO2 (at 1073 K calcination temperature) was found to be inactive for butanolysis reaction. The 2.5WZr1073 catalyst showed very less activity due to the less dispersion of W-atoms over the ZrO2 surface and more exposed bare ZrO2 surface. The activity of the catalysts was increased till 10 wt% WO3 and then decreased at higher loading. It might be due to the formation of WO3 clusters at higher loading. The optimum WO3 loading was found to be 10 wt% for WO3-ZrO2 catalyst. However, the wt% butyl levulinate has not affected much by WO3 loading. The conversion of furfuryl alcohol was increased with the increase in the reaction temperature. The wt% of butyl levulinate was also increased with increase in reaction temperature.

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