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机构地区:[1]安徽理工大学化学工程学院,安徽淮南232000 [2]盐城工学院化学与生物工程学院,江苏盐城224051
出 处:《化学试剂》2015年第11期1039-1042,共4页Chemical Reagents
基 金:国家自然科学基金资助项目(31170543)
摘 要:以脱氢枞酸(DHA)与Na OH作用后生成的脱氢枞酸钠(DHA-Na)和环氧氯丙烷(ECH)为原料,经缩合反应制备标题化合物DHAGE。探讨了溶剂类型、催化剂类型、反应时间、反应温度及物料比对产物收率的影响,用FT-IR、GC-MS表征了产物结构,环氧值分析法测定产物中DHAGE的含量。实验结果表明,制备脱氢枞酸缩水甘油酯的适宜条件为:二甲苯作溶剂,四丁基溴化铵(TBAB)作催化剂,反应时间为4.0 h,反应温度为95℃,n(ECH)∶n(脱氢枞酸钠)=4.0∶1.0;在此条件下DHAGE的收率为83.1%。Dehydroabietic glycidyl ester( DHAGE) was prepared via condensation reaction with sodium dehydroabietate,which was the product of dehydroabietic acid reacted with sodium hydroxide,and epichlorohydrin( ECH) as basic materials. The effects of solvent,catalyst,reaction time,reaction temperature and mass ratio of reactants on the yield of DHAGE were investigated. The product was confirmed by FT-IR and GC-MS,and the content of DHAGE in the product was determined by measuring the epoxy value. Experimental results indicated the suitable condition for preparing the DHAGE was as following: xylene was utilized as solvent,tetrabutyl ammonium bromide( TBAB) was catalyst,reaction time was 4. 0 h,reaction temperature was 95 ℃ and that of ECH versus sodium dehydroabietate was 4. 0 ∶ 1. 0. Under this condition,the yield of DHAGE was 83. 1%.
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