在低模板剂浓度和弱碱介质中合成催化材料Si-MCM-41、Sn-MCM-41, 并用XRD、N2物理吸附-脱附、FT-IR、ICP-AES和TEM等手段对催化材料进行了表征. 研究了合成方法对制备Sn掺杂MCM-41介孔分子筛的影响, 结果表明: 水热晶化法(DHT)合成的Sn-MCM-41, Sn物种主要进入分子筛的骨架中; 而模板离子交换法(TIE)合成的Sn-MCM-41, Sn物种主要位于分子筛的表面. Sn-MCM-41介孔分子筛催化环己酮Baeyer-Villiger氧化反应结果表明, n(H2O2):n(酮)＝3:1, 30g1,4-二氧六环为溶剂, H2O2为氧源, 70℃反应6 h, 环己酮的转化率可达40.02%, ε-己内酯的选择性为45.69%.
The molecular sieve catalysis material of Si-MCM-41, Sn-MCM-41 were preparaed under the condition of low template concentration in weak base and the samples were characterized by XRD, N2 adsorption-desorption, FT-IR, ICP-AES and TEM techniques. Effect of the synthesis methods on the Sn-containing MCM-41 were studied. The results showed that Sn species were mainly incorporated into the framework of MCM-41 molecular sieves prepared by direct hydrothermal synthesis method (DHT), while Sn species were mainly existed on the wall surface of Sn-MCM-41 molecular sieves prepared by template-ion exchange method (TIE). The catalytic properties of Sn containing MCM-41 molecular sieves in Baeyer-Villiger oxidation of cyclohexanone were investigated. Catalytic activity results show that under the reaction condition of n(H2O2):n(Cyclohexanone)＝3:1, 30 g dioxane, at 70℃ for 6 h, the conversion of cyclohexanone and the selectivity of ε-caprolactone reach 40.02% and 45.69%, respectively.
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