采用高温漫反射红外光谱考察了钛硅分子筛TS-1的稳定性,发现960cm^-1吸收峰在673K时没有变化,表明所表征的骨架钛具有一定的高温稳定性,而表征分子筛骨架振动的两个吸收峰在673K下向低波数位移了约13cm^-1。探讨了H2O2吸附对TS-1分子筛骨架钛的影响,发现960cm^-1处的吸收峰在吸附H2O2后强度减弱,并且向高波数位移了11cm^-1;抽真空或加热,吸收峰又复原,表明骨架钛可能存在Ti=O结构,H2O2与分子筛中的Ti=O作用,使相应的960cm^-1叫吸收峰向高波数位移。原位漫反射红外光谱考察了TS-1催化苯乙烯氧化反应,谱图分析表明,苯甲醛是主要产物,TS-1催化氧化的关键是H2O2吸附在TS-1的骨架钛上形成活性中心。
The Stability of framework of titanium silicalite-1 (TS-1) was investigated by high temperature diffuse reflectance FT- IR spectroscopy (DRIFTS), and the results showed that the 960 cm^-1 peak belonging to Ti-framework was stabilized at 673 K, but the two peaks belonging to framework shifted to lower frequencies by about 13 cm^-1 at 673 K. The effect on the framework after H2O2 adsorption was discussed. The results showed that the 960 cm^-1 peak lowered and shifted to high frequencies by about 11 cm^-1 , but it recovered with vacuum or heating up. It was suggested that the 960 cm^-1 peak characterizes Ti=O , and this explained why the 960 cm^-1 peak shifted to high frequencies well. TS-1 catalytic oxidization of styrene was investigated by in situ DRIFTS. The reaction process was detected and phenyl aldehyde was the main product. Based on in situ analysis, it was proposed that H2O2 was adsorbed on Ti in framework of TS-1 to form active center.