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磷钨杂多酸季铵盐催化合成二氧化双环戊二烯
引用本文:李学超,;吴学明,;唐安斌. 磷钨杂多酸季铵盐催化合成二氧化双环戊二烯[J]. 四川建材学院学报, 2009, 0(4): 29-35
作者姓名:李学超,  吴学明,  唐安斌
作者单位:[1]西南科技大学材料科学与工程学院,四川绵阳621010; [2]四川东材科技集团股份有限公司国家绝缘材料工程技术研究中心,四川绵阳621000
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15h。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%。合成产物经色谱一质谱和。HNMR分析为目标产物二氧化双环戊二烯。

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

Epoxidation of Diclopentadiene Catalyzed by Quaternary Ammonium Heteropolyphosphatotungstates
Affiliation:LI Xue-chao, WU Xue-ming , TANG An-bin ( 1. School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, Sichuan, China; 2. The State Technology Center of Insulating Material, Siehuan Dongfang Insulating Material Co. , Ltd. , Mianyang 621000, Siehuan, China)
Abstract: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 .
Keywords:Quaternary ammonium heteropoIy phosphato tungstate  Diclopentadiene dioxide  Epoxidation  Hydrogen peroxide
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