Synthesis of biomass derived levulinate esters on novel sulfated Zr/KIL-2 composite catalysts

Popova, Margarita and Szegedi, Ágnes and Lazarova, H. and Ristić, Alenka and Kalvachev, Yuri (2016) Synthesis of biomass derived levulinate esters on novel sulfated Zr/KIL-2 composite catalysts. MICROPOROUS and Mesoporous Materials, 235. pp. 50-58. ISSN 1387-1811

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Abstract

Zirconia nanomaterials were prepared by impregnation of KIL-2 type silica with 4, 8, 15 and 25 wt% of ZrO2, and were modified by sulfate groups in order to vary the type, strength and density of the active sites. The samples were characterized by X-ray powder diffraction (XRD), EDX analysis, N-2 physisorption, SEM, TEM, UV Vis spectroscopy, XPS, and thermogravimetric analysis (TGA). The acidic properties were investigated by FT-IR spectroscopy of adsorbed pyridine. The catalytic properties of ZrKIL-2 catalysts and their sulfated varieties were studied in levulinic acid (LA) esterification with ethanol or n-butanol. The sulfated materials showed significantly higher activity compared to the non-sulfated ones due to their stronger Bronsted and Lewis acid sites. It was found that the silica supported sulfated samples show different activity depending on the applied alcohol. With increasing ZrO2 content up to 15 wt% increasing catalytic activity and selectivity was observed to produce levulinate esters. A further increase of the amount of zirconia leads to a decrease in catalytic activity because of the significant decrease of ZrO2 dispersion and the structure deterioration of the catalyst. For the first time insight was provided into the relation between sulfates group leaching and zirconia dispersion. (C) 2016 Elsevier Inc. All rights reserved.

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