甲基丙烯酸双环戊二烯基一氧一乙基酯的合成  

Synthesis of Methacrylic Acid Dicyclopentadiene-Oxygen-Ethyl Ester

作　　者：于洪艳[1] 王兴利[1] 梁红玉[1] 张连红[1] 

机构地区：[1]辽宁石油化工大学石油化工学院,辽宁抚顺113001

出　　处：《石油化工》2007年第1期63-66,共4页Petrochemical Technology

基　　金：国家高技术研究发展计划项目(2005AA001510)

摘　　要：以双环戊二烯、乙二醇、甲基丙烯酸为原料,采用两步合成法,首先合成中间产物乙二醇基双环戊烯基醚,再以二丁基氧化锡为催化剂、环己烷和甲苯的混合物为带水剂、对苯二酚和对羟基苯甲醚的混合物为阻聚剂,甲基丙烯酸与乙二醇基双环戊烯基醚反应合成甲基丙烯酸双环戊二烯基一氧一乙基酯。酯化反应的优化条件为:n(甲基丙烯酸)∶n(乙二醇基双环戊烯基醚)=1.1、二丁基氧化锡用量(质量分数,以乙二醇基双环戊烯基醚质量为基准,下同)3.0%、对苯二酚用量0.5%、对羟基苯甲醚用量0.1%、环己烷用量20.0%、甲苯用量30.0%、反应温度98℃。在此条件下合成的甲基丙烯酸双环戊二烯基一氧一乙基酯的酯化率大于90%,纯度达92.12%。Synthesis of methacrylic acid dicyclopentadiene-oxygen-ethyl ester from methacrylic acid （MAA）, dicyclopentadiene and ethylene glycol was investigated. Ethylene glycol dicyclopentadiene ether as intermediate was firstly prepared. The in .termediate successively reacted with MAA in esterification with dibutyl tin oxide as catalyst ,toluene and cyclohexane as water entraining agents, and hydroquinone and p-hydroxyanisole as inhibitors. Under optimal reaction conditions： n （ MAA ） ： n （ ethylene glycol dicyclopentadiene ether） 1.1, mass fraction of dibutyl tin oxide 3.0%, mass fraction of hydroquinone 0.5%, mass fraction of p-hydroxyanisole 0.1%, mass fraction of toluene 20.0%, mass fraction of cyclohexane 30.0% （ all based on ethylene glycol dicyclopentadiene ether） and reaction temperature 98℃, esterification rate of methacrylic acid dicyclopentadiene-oxygen-ethyl ester can reach above 90% and its purity is 92.12% ,respectively.

关 键 词：双环戊二烯 乙二醇 甲基丙烯酸 甲基丙烯酸双环戊二烯基-氧-乙基酯 酯化反应 二丁基氧化锡 催化剂 

分 类 号：TQ223.2[化学工程—有机化工]