Aldol condensation of cyclohexanone and furfural in fixed-bed reactor

Abstract

Aldol condensation reaction is usually catalysed using homogeneous catalysts. However, the heterogeneous catalysis offers interesting advantages and the possibility of cleaner biofuels production. Nowadays, one of the most used kinds of heterogeneous catalysts are hydrotalcites, which belong to a group of layered double hydroxides. This paper describes the aldol condensation of cyclohexanone (CH) and furfural (F) using Mg/Al mixed oxides and rehydrated mixed oxides in order to compare the catalyst activity after calcination and rehydration, as well as the possibility of its regeneration. The catalysts were synthesized by calcination and subsequent rehydration of the laboratory-prepared and commercial hydrotalcites, with Mg:Al molar ratio of 3:1. Their structural and chemical properties were determined by several analytical methods (inductively coupled plasma analysis (ICP), X-ray diffraction (XRD), diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), specific surface area (BET), thermogravimetric analysis (TGA), temperature programmed desorption (TPD)). F-CH aldol condensation was performed in a continuous fixed-bed reactor at 80◦C, CH:F = 5:1, WHSV 2 h−1. The rehydrated laboratory-prepared catalysts showed a 100% furfural conversion for more than 55 h, in contrast to the calcined ones (only 24 h). The yield of condensation products FCH and F2CH was up to 68% and 10%, respectively. Obtained results suggest that Mg/Al mixed oxides-based heterogeneous catalyst is suitable for use in the aldol condensation reaction of furfural and cyclohexanone in a fixed-bed reactor, which is an interesting alternative way to obtain biofuels from renewable sources.