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为合成功能高分子中间体9-苯甲酰蒽,考察了以杂多酸型催化剂磷钨酸铝(AlPW12O40)催化蒽和苯甲酰氯的Friedel-Crafts酰基化反应,提纯得到w(9-苯甲酰蒽)=96.3,用GC/MS、FTIR和1HNMR等确认了其结构;考察了各反应条件对9-苯甲酰蒽产率和选择性的影响,得到9-苯甲酰蒽的优化合成条件为:反应温度90℃,反应时间5h,n(蒽):n(苯甲酰氯)=1.0:1.5,w(催化剂)=4.5,溶剂为环己烷。在上述条件下,9-苯甲酰蒽的产率和选择性分别可达47.4和91.8。证明AlPWO对目标产物选择性高、无环境污染,可以回收利用。
In order to synthesize the functional polymer 9-benzoyl anthracene, the Friedel-Crafts acylation of anthracene and benzoyl chloride catalyzed by the heteropolyacid type catalyst AlPW12O40 was investigated and purified to give w (9-benzene Formic acid anthracene) = 96.3, confirmed its structure by GC / MS, FTIR and 1HNMR, etc .; investigated the reaction conditions on the yield and selectivity of 9-benzoylanthrene anthracene anthracene anthracene optimization The synthesis conditions were: reaction temperature 90 ℃, reaction time 5h, n (benzoyl chloride) = 1.0: 1.5, w (catalyst) = 4.5 and cyclohexane as solvent. Under the above conditions, the yield and selectivity of 9-benzanthracene are up to 47.4 and 91.8, respectively. Prove AlPWO high selectivity of the target product, no environmental pollution, can be recycled.