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以三甲基氯硅烷和六甲基二硅氮烷为硅烷化试剂,分别采用气相和液相硅烷化法对HMS分子筛进行表面改性制备疏水性HMS分子筛。考察了改性方法、硅烷试剂与分子筛摩尔比、反应温度和时间对硅烷化效果的影响,研究了改性前后HMS的骨架特征、微观结构和疏水性、水热稳定性。结果表明:气相硅烷化法较液相法优势明显,硅烷化程度和效率均较高;在双硅烷化试剂、反应温度90℃、硅烷试剂与分子筛摩尔之比0.8、反应时间8 h等条件下,改性前后HMS的静态水吸附量分别为45.46%和1.38%,疏水性得到明显提高。HMS经硅烷化改性后保持介孔骨架结构和蠕虫状孔道,同时水热稳定性得到有效改善,800℃水蒸气处理6 h后介孔结构仍然存在。
Using trimethylchlorosilane and hexamethyldisilazane as silylating reagents, HMS molecular sieves were modified by gas phase and liquid phase silanization to prepare hydrophobic HMS molecular sieves. The effects of modification method, molar ratio of silane reagent to molecular sieve, reaction temperature and time on silanization were investigated. The skeleton, microstructure, hydrophobicity and hydrothermal stability of HMS before and after modification were investigated. The results showed that the gas-phase silanization method has obvious advantages over the liquid-phase method and the degree of silanization and the efficiency are high. Under the condition of the reaction temperature of 90 ℃, molar ratio of silane reagent to molecular sieve of 0.8, reaction time of 8 h , The static water adsorption capacity of HMS before and after modification were 45.46% and 1.38% respectively, and the hydrophobicity was obviously improved. Mesoporous structure and worm-like pores were retained by HMS after silanization, meanwhile the hydrothermal stability of HMS was effectively improved. The mesoporous structure still exists after 6 h steam treatment at 800 ℃.