Synthesis of Mesoporous Titanium Silicalite-1 with High Stability in Cyclohexanone Ammoximation  

作　　者：王亚权 叶家鑫 王书海 林永杰 王守桂 刘伟 

机构地区：[1]Key Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University

出　　处：《Transactions of Tianjin University》2016年第3期254-260,共7页天津大学学报（英文版）

基　　金：Supported by the National Natural Science Foundation of China(No.21276183)

摘　　要：Mesoporous titanium silicalite-1(TS-1)was hydrothermally synthesized with the addition of triethanolamine(TEA)in the conventional process, and used in the cyclohexanone ammoximation in a continuous slurry reactor. The as-prepared TS-1 was characterized with X-ray diffraction(XRD), scanning electron microcopy(SEM), N_2 adsorption-desorption, Fourier transform infrared(FT-IR)spectroscopy, UV-Visible(UV-Vis)diffuse reflectance spectra and UV Raman spectroscopy. The results indicated that the addition of TEA resulted in the formation of mesopores and the slight increase of framework titanium in TS-1. TS-1 synthesized with the addition of TEA exhibited a higher stability in the cyclohexanone ammoximation than that without the addition of TEA, attributing to the increase of mesopore volumes and the slight increase of the framework titanium in TS-1. However, when the addition of TEA was up to TEA/SiO_2 ratio of 0.24, the crystallinity and framework titanium of TS-1 decreased markedly, and the average crystal sizes of TS-1 increased, with the catalyst stability becoming poor.Mesoporous titanium silicalite-1 （TS-1）was hydrothermally synthesized with the addition of triethanolamine （TEA） in the conventional process, and used in the cyclohexanone ammoximation in a continuous slurry reactor. The as-prepared TS-1 was characterized with X-ray diffraction（XRD）, scanning electron microcopy（SEM）, N2 adsorption-desorption, Fourier transform infrared （FT-IR）spectroscopy, UV-Visible （UV-Vis） diffuse reflectance spectra and UV Raman spectroscopy. The results indicated that the addition of TEA resulted in the formation of mesopores and the slight increase of framework titanium in TS- 1. TS- 1 synthesized with the addition of TEA exhibited a higher stability in the cyclohexanone ammoximation than that without the addition of TEA, attributing to the increase of mesopore volumes and the slight increase of the framework titanium in TS- 1. However, when the addition of TEA was up to TEA/SiO2 ratio of 0.24, the crystallinity and framework titanium of TS-1 decreased markedly, and the average crystal sizes of TS-1 increased, with the catalyst stability becoming poor.

关 键 词：TS-1 TRIETHANOLAMINE cyclohexanone ammoximation MESOPORE STABILITY 

分 类 号：O621.251[理学—有机化学]