三相相转移催化法制备二氧化双环戊二烯

发布时间：2018-06-11 15:01

  本文选题：三相相转移催化 + 二氧化双环戊二烯　； 参考：《应用化学》2010年09期

【摘要】：以氯甲基化大孔聚苯乙烯-二乙烯基苯交联树脂(PS)接枝N-苄基-N,N-二甲基十二烷基季铵磷钨杂多酸盐为三相相转移催化剂,质量分数为50%的工业双氧水为氧化剂,制备了二氧化双环戊二烯(DCPDDO)。采用FTIR和1HNMR对产物进行表征。考察了溶剂和催化剂用量、物料摩尔比、反应温度和时间对环氧化反应的影响。采用正交试验法获得的最佳反应条件为(以0.05mol双环戊二烯(DCPD)计):1,2-二氯乙烷18mL,催化剂2.25g,n(DCPD)∶n(H2O2)=1∶2.75,反应温度60℃,反应时间12h。在此条件下,DCPDDO的收率可达89%以上,催化剂回收方便且重复使用7次未见活性明显降低。
[Abstract]:N-benzyl-N-dimethyl-dodecylammonium phosphotungstophosphate heteropoly salt grafted with chloromethylated macroporous polystyrene-divinylbenzene crosslinked resin (PSPS) was used as a three-phase transfer catalyst and commercial hydrogen peroxide with a mass fraction of 50% was used as oxidant. Dicyclopentadiene oxide (DCPDDOA) was prepared. The products were characterized by FTIR and 1H NMR. The effects of the amount of solvent and catalyst, the molar ratio of materials, reaction temperature and time on the epoxidation reaction were investigated. The optimum reaction conditions obtained by orthogonal test were as follows: (0.05mol dicyclopentadiene dichloroethane 18ml), catalyst 2.25g DCPD: n H _ 2O _ 2H _ 2O _ 2H _ 2O _ 2: 2.75, reaction temperature 60 鈩，

本文编号：2005696