三相相转移催化法制备二氧化双环戊二烯  

Preparation of Dicyclopentadiene Dioxide via a Tri-Phase Phase Transfer Catalysis

作　　者：王永珊[1] 章亚东[1] 王振兴[1] 

机构地区：[1]郑州大学化工与能源学院,郑州450001

出　　处：《应用化学》2010年第9期1021-1025,共5页Chinese Journal of Applied Chemistry

基　　金：河南省高校科技创新人才计划(2010HASTIT037)

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。Preparation of dicyclopentadiene dioxide （ DCPDDO） by the epoxidation of dicyclopentadiene （ DCPD） with 50% industrial hydrogen peroxide as oxidant and the macroporous crosslinked polystyrene resin （ PS） grafted N-benzyl-N,N-dimethyl-N-dodecyl quaternary ammonium phosphor tungsten heterpoly acid salts as tri-phase phase transfer catalyst was reported.The product was characterized by FTIR and 1↑H NMR.Effects of the volume of solvent,the amount of catalyst,the molar ratio of reactants,reaction temperature and reaction time on the reaction were studied.The optimal reaction conditions obtained by means of orthogonal test were （ based on 0.05 mol DCPD） ：dichloroethane 18 mL,catalyst 2.25 g,n（DCPD）∶n（ H2O2）=1∶2.75, reaction temperature 60 ℃,reaction time 12 h.Under these conditions,the yield of DCPDDO can reach 89% .The catalyst can be easily recycled and no significant decrease in terms of catalytic activity could be observed after seven recycles.

关 键 词：三相相转移催化 二氧化双环戊二烯 双环戊二烯 环氧化 双氧水 

分 类 号：O624.1[理学—有机化学]