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乙二醇基双环戊二烯基醚合成工艺研究
Process for the Synthesis of Ethylene Glycol Dicyclopentadiene Ether
【摘要】 用双环戊二烯(DCPD)和乙二醇(EG)为主要原料,在对甲基苯磺酸催化作用下进行亲电加成反应制备乙二醇基双环戊二烯基醚。采用正交试验法确定的反应条件为:n(DCPD)∶n(EG)=1∶1,对甲基苯磺酸、对苯二酚加入量分别为DCPD质量的3%、0.4%,反应温度120℃,反应时间6 h。在此条件下乙二醇基双环戊二烯基醚产率大于77%;确定粗产品精馏条件:釜温约138℃,馏程范围80~84℃、真空度-0.096 MPa.在上述条件下全收集产品,产品纯度大于99.0%。
【Abstract】 The synthesis of ethylene glycol dicyclopentadiene ether based on the electrophilic addtion reaction of dicyclopentadiene(DCPD) and ethylene glycol(EG) with toluene-p-sulfonic acid as catalyst was investigated.The optimal conditions were got by a series of orthogonal experiments as follows:the ratio of DCPD to EG was 1,the amounts of toluene-p-sulfonic acid and hydroquinone were as 3% and 0.4% as the mass of DCPD respectively,the reaction temperature was 120℃,the reaction time was 6h,under these conditions the yeild of ethylene glycol dicyclopentadiene ether was up to 77%.The process of distillation for the reaction products was carried out under the conditions as follows:the kettle temperature was about 138℃,the distillation range was 80℃~84℃,the degree of vacuum was-0.096 MPa.The purity of products collected was above 99.0%.
【Key words】 Dicyclopentadiene; toluene-p-sulfonic acid; hydroquinone; ethylene glycol dicyclopentadiene ether;
- 【文献出处】 化学与黏合 ,Chemistry and Adhesion , 编辑部邮箱 ,2006年04期
- 【分类号】TQ233
- 【被引频次】2
- 【下载频次】185