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作 者:于世涛[1] 李露[1] 刘福胜[1] 解从霞[1]
出 处:《催化学报》2003年第6期428-432,共5页
基 金:国家自然科学基金资助项目 ( 3 0 0 70 60 8) ;山东省优秀中青年科学家科研奖励基金资助项目 ( 2 0 0 0 5 1)
摘 要:制备了Mo MCM 4 1中孔分子筛 ,并将BO3 -3 引入到分子筛中制得BO3 -3 /Mo MCM 4 1催化剂 .采用XRD ,FT IR ,ESR ,BET和NH3 TPD对分子筛催化剂的结构及酸强度进行了表征 .结果表明 ,Mo MCM 4 1和BO3 -3 /Mo MCM 4 1具有中孔分子筛的特征 ,有良好的长程有序性和结晶度 ;但Mo并未进入分子筛骨架内部而是在分子筛表面以MoO2 的形式存在 ;BO3 -3 附着于Mo MCM 4 1分子筛上形成强酸中心 .将BO3 -3 /Mo MCM 4 1用于催化 2 甲氧基萘乙酰化反应 ,考察了催化剂用量、Si/Mo比及BO3 -3 的引入方式对该反应性能的影响 ,发现BO3 -3 /Mo MCM 4 1对 2MCM 41 molecular sieve possesses a hexagonal arrangement of uniform size, one dimensional mesopores whose diameters can be systematically varied from 2 to 8 nm, and surface area more than 700 m 2/g, therefore, it should be a potential catalyst instead of AlCl 3 and H 2SO 4 for Friedel Crafts acylation involving larger molecules of reactants. However, MCM 41 has poorer acidity and low catalytic activity for Friedel Crafts acylation. Therefore, enhancing the acidity of MCM 41 is the key to its application as catalysts for Friedel Crafts acylation. The Mo MCM 41 molecular sieve was synthesized by hydrothermal system and BO 3- 3/Mo MCM 41 catalyst was prepared by impregnating Mo MCM 41 with H 3BO 3 solution or by grinding Mo MCM 41 with solid H 3BO 3. The Mo MCM 41 and BO 3- 3/Mo MCM 41 were characterized by XRD, FT IR, ESR, BET and NH 3 TPD. The results show that the molecular sieve and the catalyst obtained possess the characteristics of mesopores, better long range order and crystallinity, Mo atom lies on the surface of Mo MCM 41 in a form rather than Mo 5+ , and BO 3- 3 is combined with the framework of the molecular sieve so that its acidity is improved. BO 3- 3/Mo MCM 41 was used as a catalyst in acetylation of 2 methoxynaphthalene (2 CH 3O C 10 H 7) with CH 3COCl. The acetylation of 2 CH 3O C 10 H 7 dominantly occurs at the kinetically controlled 1 position. The effects of preparation conditions and amount of BO 3- 3/Mo MCM 41 on the reaction were examined. Under the optimum conditions, 2 CH 3O C 10 H 7 conversion can reach 97% and 1 CH 3CO 2 CH 3O C 10 H 6 selectivity is more than 98%.
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