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作 者:王志萍[1] 于世涛[1] 刘福胜[1] 解从霞[1]
出 处:《精细化工》2004年第6期425-428,455,共5页Fine Chemicals
基 金:国家自然科学基金资助项目(No.30070608);山东省优秀中青年科学家科研奖励基金资助项目(No.2001-51)~~
摘 要:制备了Zr/Mo MCM 41中孔分子筛,采用XRD、FTIR、BET、ESR和NH3 TPD对其结构进行了表征。结果表明,Zr/Mo MCM 41中孔分子筛具有较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非五价钼的氧化物形式存在。将Zr/Mo MCM 41用于催化2 甲氧基萘与乙酸酐的傅 克酰基化反应,得到较佳工艺条件为:n(Si)∶n(Mo)=1∶0 06,催化剂1 2g,2 甲氧基萘0 025mol,n(2 甲氧基萘)∶n(乙酸酐)=1∶6,反应温度130℃,反应时间24h。2 甲氧基萘的转化率达93 8%,1 乙酰基 2 甲氧基萘的选择性达94 9%。A mesoporous molecular sieve Zr/Mo-MCM-41 with Si/Mo molar ratio 1∶0.06 was prepared.Its structure was characterized by XRD,FTIR,BET,ESR and NH_3-TPD.The results show that the obtained Zr/Mo-MCM-41 has good long-range order and crystallinity,but Mo atom lies on the surface rather than in the frame of Zr/Mo-MCM-41 in the form of oxides other than Mo^(5+).Acetylation of 2-methoxynaphthalene was studied by using Zr/Mo-MCM-41 as catalyst.Influences of reaction conditions such as molar ratios of Si/Mo,amount of catalyst,molar ratios of reactants,reaction temperature and reaction time were examined in detail.The optimum conditions were n(Si)∶n(Mo)=1∶0.06,amount of catalyst 1.2 g,amount of 2-methoxynaphthalene 0.025 mol,n(2-methoxynaphthalene)∶n(acetic anhydride)=1∶6,reaction temperature 130 ℃ and reaction time 24 h.The conversion of 2-methoxynaphthalene was 93.8% and the selectivity to 1-acetyl-2-methoxynaphthalene was 94.9%.
关 键 词:FRIEDEL-CRAFTS反应 乙酰化反应 中孔分子筛 2-甲氧基萘
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