Chinese Journal of Catalysis ›› 2012, Vol. 33 ›› Issue (5): 898-904.DOI: 10.3724/SP.J.1088.2012.11201

• Research papers • Previous Articles    

Preparation and Characterization of Sn-β Zeolites by a Two-Step Postsynthesis Method and Their Catalytic Performance for Baeyer-Villiger Oxidation of Cyclohexanone

KANG Zihua, LIU Hai’ou, ZHANG Xiongfu*   

  1. State Key Laboratory of Fine Chemicals, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, Liaoning, China
  • Received:2011-12-02 Revised:2012-03-06 Online:2012-05-09 Published:2012-05-09

Abstract: A Sn-β zeolite was prepared by a two-step postsynthesis method. The procedure consists of first creating vacant T-sites with associated silanol groups by dealumination of Al-β zeolite with nitric acid and then impregnating the resulting Si-β zeolite with an aqueous solution of SnCl4·5H2O, followed by calcination at varying temperatures. The effects of the amount of vacant T-sites, SiO2/Al2O3 ratio of Al-β zeolite and calcination temperature on the formation of the Sn-β zeolites and their catalytic performances for Baeyer-Villiger oxidation of cyclohexanone were investigated. The structure of the catalysts was characterized by X-ray diffraction, infrared spectroscopy, UV-Vis spectrophotometry, scanning electron microscopy, X-ray fluorescence spectrometry and inductively coupled plasma atomic emission spectrometry. The results show that, the Sn-β zeolite has been synthesized using a two-step postsynthesis method, and the Sn4+ ions are incorporated in the framework of the zeolite in a tetrahedral environment. The synthesized Sn-β zeolite shows impressive catalytic performance in Baeyer-Villiger oxidation of cyclohexanone using hydrogen peroxide as an oxidant.

Key words: tin, heteroatom zeolite β, cyclohexanone, Baeyer-Villiger oxidation, ε-caprolactone