Effect of sodium ions in synthesis of titanium silicalite-1 on its catalytic performance for cyclohexanone ammoximation

Abstract

Titanium silicalite-1 (TS-1) has been hydrothermally synthesized with tetrapropylammonium hydroxide (TPAOH) as the template in the presence of various amounts of Na⁺, characterized by inductively coupled plasma, X-ray diffraction, scanning electron microscope, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and ultro-violet-visible spectroscopy and studied in cyclohexanone ammoximation. The characterization results show that with the increase of Na⁺ concentration in the synthesis, both the crystal sizes of TS-1and extra framework Ti increase but framework Ti decreases. The addition of Na⁺ below 3 mol-% of TPAOH in the synthesis does not influence the catalytic properties with above 98% conversion of cyclohexanone and 99.5% selectivity to cyclohexanone oxime. However, at the concentrations of Na⁺≥3 mol-% of TPAOH in the synthesis, the catalysts are deactivated faster with the increase of Na⁺ addition, which can be attributed to more high molecular weight byproducts deposited in the large TS-1 particles and the loss of the frame-work titanium. The results of this work are of great importance for the industry.

Keywords

titanium silicalite-1 / sodium ion / crystal size / extra framework Ti / cyclohexanone ammoximation

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Acknowledgments

This work has been supported by Natural Science Foundation of China (Grant No. 21276183) and Program of Introducing Talents of Discipline to Universities (No. B06006).

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2014 Higher Education Press and Springer-Verlag Berlin Heidelberg