摘要
以磷钨杂多酸季铵盐为催化剂,双氧水(H2O2)为氧源,催化氧化双环戊二烯(DCPD)制备了二氧化双环戊二烯。考察了催化剂(种类及用量)、反应溶剂、双氧水浓度、反应温度及反应时间等条件对环氧化反应的影响。结果表明,适宜的反应条件为:以1,2二氯乙烷为溶剂,十八烷基三甲基溴化铵磷钨杂多酸盐为催化剂,n(Cat):n(DCPD):n(H2O2)=2.86:1000:2600,ωH2O2=50%的H2O2为氧源,反应温度60℃,反应时间15 h。在此条件下,反应物的转化率可达到99.99%,二氧化双环戊二烯的选择率达到97.47%。合成产物经色谱-质谱和1HNMR分析为目标产物二氧化双环戊二烯。
Dicyclopentadien diepoxide was synthesized by epoxidation of dicyelopentadiene with hydrogen peroxide in the presence of catalyst of quaternary ammonium heteropolyphosphato tungstates. Effects of catalyst dosage and type, solvent type, hydrogen peroxide solution concentration, reaction temperature and reaction time on epoxidation of dicydlopentadiend were investigated. The conversion of dieyclopentadiene and the selectivity to dicyclopendadiene diepoxide are 99, 99% and 97.47%, respectively at the optimal conditions：1 ,2- dichcloroethane as solvant, 50% （mass fraction） hydrogen peroxide as oxidant, octadecy trimethyl ammonium bromide heteropoly phosphato tungstate as catalyst, the mole ratio of catalyst, dicyclopentadiene and hydrogen peroxide 2.86 ： 1000 ： 2600, reaction temperature 60 ℃ and reaction time 15 h. Composition of the product and the content of dicyclopentadiene diepoxide were determined by means of GC - MS and 1HNMR .
出处
《西南科技大学学报》
CAS
2009年第4期29-35,共7页
Journal of Southwest University of Science and Technology
关键词
磷钨杂多酸季铵盐
二氧化双环戊二烯
环氧化反应
过氧化氢
Quaternary ammonium heteropoIy phosphato tungstate
Diclopentadiene dioxide
Epoxidation
Hydrogen peroxide
