Zr/Mo-MCM-41中孔分子筛催化2-甲氧基萘乙酰化反应

Acetylation of 2-Methoxynaphthalene on Mesoporous Molecular Sieve Zr/Mo-MCM-41

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%.