Acetalization of glycerol with acetone over various metal-modified SBA-15 catalysts

Abstract

Several catalysts containing metals such as Al, Zr, Ti and Nb were incorporated in SBA-15 with Si/M ratio = 20 using the hydrothermal process. These catalysts were evaluated for their reactivity during acid-catalyzed condensation of glycerol with acetone to yield a mixture of branched compounds, namely (2,2-dimethyl- {[}1,3] dioxane-4-yl)-methanol (solketal) and 2,2-dimethyl- {[}1,3] dioxane-5-ol, which are being used as fuel additives. The synthesised catalyst samples were characterized by ICP-AES analysis, N-2 adsorption-desorption measurements, X-ray diffraction, FT-IR, SEM-EDX, UV-visible diffuse reflectance spectroscopy, TPD of ammonia and ex situ pyridine-adsorbed FT-IR spectroscopy. The various characterization results confirm that metal oxides were incorporated in the pore wall of the SBA-15 matrices. The results of NH3-TPD and ex situ adsorbed pyridine FT-IR analyses showed that the acidity of the samples increased after incorporation of metal into the pure SBA-15 samples. Among various metals incorporated into the SBA-15, the Nb-SBA-15 (Si/Nb = 20) showed higher catalytic activity toward the acetalization of glycerol in liquid phase compared to that of other samples investigated. Under the optimal reaction conditions, the Nb-SBA-15 (Si/Nb = 20) exhibited 95\% glycerol conversion with 100\% solketal selectivity. The catalyst reusability studies indicated that the Nb-SBA-15 sample is regenerable and highly stable in the acetalization of glycerol.