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作 者:陈敏[1] 张燕[1] 袁新华[2] 张春燕[1] 刘华[1] 戴起勋[2]
机构地区:[1]江苏大学化学化工学院,江苏镇江212013 [2]江苏大学材料科学与工程学院,江苏镇江212013
出 处:《江苏大学学报(自然科学版)》2007年第2期131-134,共4页Journal of Jiangsu University:Natural Science Edition
基 金:国家自然科学基金资助项目(20207003);江苏大学高级人才科研启动基金资助项目(6810000019)
摘 要:为合成新型功能高分子中间体,分别研究了在AlCl3,FeCl3,ZnCl2等无机盐和[Bmim]Cl/FeC l3离子液体催化作用下,苊在温和条件常温常压下的偶联反应.经GC/MS分析发现生成了3,3′联苊.用GC法考察了不同反应条件对3,3′联苊产率的影响,得到了各催化剂作用的优化反应条件.结果表明,上述几种催化剂中,[Bm im]Cl/FeCl3离子液体对苊的偶联反应催化效果最好,在该催化剂作用的优化反应条件下,3,3′联苊产率为48.71%,选择性78.56%,且[Bmim]Cl/FeCl3离子液体对环境无污染,并可循环使用.通过重结晶、层析等方法得到了功能高分子中间体3,3′联苊纯品,并用GC/MS,FTIR和1H NMR等分析测试手段鉴定了其结构.To obtain new functional aromatic polymer intermediates, the coupling reaction of acenaphthene catalyzed by inorganic salts, such as AlCl3, FeCl3, ZnCl2 and ionic liquid( [ Bmim] Cl / FeCl3 ) , was investigated at room temperature and ambient atmosphere. The 3,3'- biacenaphthene was determined by GC/MS analysis and the effects of various reaction conditions were studied by GC analysis. The results showed that [ Bmim] Cl / FeCl3 was the optimum catalyst, and under the optimum synthesis condition, the yield of 3,3'- biacenaphthene is 48.7% and selectivity is 78.56%. Furthermore, [ Bmim ] Cl / FeCl3 is environmentally benign, and can be reused at least 6 times without loss of any activity. 3,3'- biacenaphthenys, which may be used as an intermediate of function aromatic polymer materials, was prepared by recrystalling and chromatography the reaction mixture. The structure of 3,3'- biacenaphthene was identified by GC, GC/MS, FTIR and ^1H NMR analyses.
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