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运用1H→13CCP/MASNMR、29SiMASNMR、IR、XRD和元素分析等表征方法,研究了以四丙基溴化铵(TPABr)为模板剂的合成体系中,Ti酯和模板剂用量以及不同碱源对TS-1分子筛的影响,考察了不同Ti含量固体样品催化丙烯环氧化反应.实验结果表明:随着凝胶中Ti酯用量的增加,制得的分子筛结构对称性由单斜晶系逐渐向正交晶系转变,其丙烯环氧化活性也相应增加.尽管凝胶中所加减源只调变凝胶碱度而不起模板剂作用,然而凝胶的强碱环境对骨架钛原子引入有利.当凝胶中TPABr/SiO2摩尔比值在0.05-0.25之间时,TPABr加入量的变化不影响TS-1分子筛中骨架钛含量.
Using 1H - 13CCP / MASNMR, 29SiMASNMR, IR, XRD and elemental analysis, the effects of different amounts of Ti ester and templating agent on the synthesis of tetrapropylammonium bromide (TPABr) TS-1 molecular sieve, the effect of solid samples with different Ti content on the epoxidation of propylene was investigated. The experimental results show that with the increase of the amount of Ti ester in the gel, the structure symmetry of the obtained molecular sieve gradually changes from monoclinic to orthorhombic and the epoxidation activity of propylene increases accordingly. Although the addition and subtraction of gels in the gel can not only modulate the basicity of the gel but can not serve as a template, the strong alkaline environment of the gel is advantageous for the introduction of the framework titanium atoms. When the molar ratio of TPABr / SiO2 in the gel is between 0.05 and 0.25, the amount of TPABr added does not affect the framework titanium content in TS-1 zeolite.