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/FeCl3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,[Bmim]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.