Controllable wet synthesis of multicomponent copper-based catalysts for Rochow reaction†
Abstract
This work aims to provide a facile, low-cost and scalable method for the preparation of multicomponent Cu–Cu2O–CuO catalysts, which are of high interest to the organosilane industry. A series of submicrometer-sized and Cu-based catalysts containing CuO, Cu2O and Cu, or some combination of them, were synthesized by a simple low-temperature wet chemical method using CuSO4·5H2O as the precursor and N2H4·H2O as a reducing agent. The samples were characterized by X-ray diffraction, thermogravimetric analysis, temperature-programmed reduction, X-ray photoelectron spectroscopy, transmission electron microscopy, and scanning electron microscopy techniques. It was observed that the composition of the samples could be tailored by varying the amount of reducing agent at a given reaction temperature and time. These catalysts were then tested in the Rochow reaction, using silicon powder and methyl chloride (MeCl) as reactants to produce dimethyldichlorosilane (M2), which is the most important organosilane monomer in the industry. Compared with bare CuO and Cu particles, the ternary CuO–Cu2O–Cu catalyst displayed much improved M2 selectivity and Si conversion, which can be attributed to the smaller copper particle size and the synergistic effect among the different components in the CuO–Cu2O–Cu catalyst. This catalyst preparation method is expected to yield efficient and low-cost copper catalysts for the organosilane industry.