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硫酸钙晶须催化合成一缩二乙二醇双甲基丙烯酸酯
Synthesis of Glycol Ether Dimethacrylic Acid Ester Catalyzed by Calcium Sulfate Whisker
【摘要】 以一缩二乙二醇和甲基丙烯酸甲酯为主要原料,酯交换合成一缩二乙二醇双甲基丙烯酸酯。硫酸钙晶须对合成一缩二乙二醇双甲基丙烯酸酯具有高效催化作用,而半水和无水硫酸钙均没有催化活性。考察了甲基丙烯酸甲酯与一缩二乙二醇物质的量比、催化剂用量、阻聚剂用量等因素对收率的影响,得出了最佳反应条件:n(甲基丙烯酸甲酯)∶n(一缩二乙二醇)=3.5∶1,反应温度为回流温度,催化剂硫酸钙晶须、阻聚剂氮氧自由基加入量分别为一缩二乙二醇质量的3%、0.1%。在此条件下合成的一缩二乙二醇双甲基丙烯酸酯的收率大于96.3%,纯度达97%。
【Abstract】 Transesterification synthesis of glycol ether dimethacrylic acid ester is obtained by the reaction of diethylene glycol with methacrylic acid.Calcium sulfate whisker is an efficient catalyst for the reaction,while anhydrite and calcium sulfate hydrate have no catalytic activity.The effects of the ratio of methacrylic acid to glycol ether,amount of catalyst and amount of inhibitor on the yield are investigated.The optimized conditions is screened as follows:n(methacrylic acid)∶n(glycol ether)=3.5∶1,the reaction temperature are circumfluence temperature,the amount of catalyst calcium sulfate whisker and inhibitor nitroxyl oxides of free radical is 3%,0.1%.Yield of glycol ether dimethacrylic acid ester can reach above 90% and its purity is 97%,respectively.
【Key words】 calcium sulfate whisker; transesterification; glycol ether dimethacrylic acid ester; catalysis;
- 【文献出处】 材料导报 ,Materials Review , 编辑部邮箱 ,2009年10期
- 【分类号】TQ225.24
- 【被引频次】14
- 【下载频次】272