离子液体催化1-羟基甲基丙烯酸环己烷酯的合成  

Catalytic synthesis of 1-hydroxy cyclohexane methacrylate by ionic liquid

作　　者：姚治国 孙屹婷 邓倩 马颖超 李继新[1] 王海玥[1] YAO Zhi-guo;SUN Yi-ting;DENG Qian;MA Ying-chao;LI Ji-xin;WANG Hai-yue(School of Petrochemical Engineering,Shenyang University of Technology,Liaoning 111003,China)

机构地区：[1]沈阳工业大学石油化工学院,辽宁辽阳111003

出　　处：《应用化工》2021年第S02期196-200,共5页Applied Chemical Industry

摘　　要：以1-乙基咪唑与溴代正丁烷合成离子液体[Beim]Br并对该离子液体的结构进行表征。以环氧环己烷(CHO),甲基丙烯酸(MAA)为原料,对苯二酚为阻聚剂,用离子液体[Beim]Br、三乙基苄基氯化铵(TEBAC)、苄基三甲基氯化铵(DMBAC)、四丁基氯化铵(TBAC)四种不同催化剂采用直接酯化的方法合成1-羟基甲基丙烯酸环己烷酯。并对该合成酯结构进行表征。以反应转化率和颜色光泽为指标,通过正交实验探究了反应时间、反应温度、催化剂用量、反应物摩尔比对于产物收率的影响,从而确定了催化作用下1-羟基甲基丙烯酸环己烷酯制备的最佳工艺条件为:反应时间4 h,反应温度85℃,催化剂用量0.3%,反应物摩尔比1.1。通过对比,发现离子液体[Beim]Br在MAA和CHO的反应过程中催化效果更好,收率最高为97.4%,呈浅黄透明液体。Ionic liquid[Beim]Br was synthesized with 1-ethylimidazole and n-butane bromide,and its the structure of the ionic liquid was characterized.Take epoxy cyclohexane(CHO),methacrylic acid(MAA) as raw materials,hydroquinone as polymerization inhibitor,use ionic liquid[Beim]Br,triethylbenzylammonium chloride(TEBAC),benzyl four different catalysts,trimethylammonium chloride(DMBAC) and tetrabutylammonium chloride(TBAC),were used to synthesize 1-hydroxy methacrylate cyclohexane ester by direct esterification,the structure of the synthetic ester was characterized.Taking the reaction conversion rate and color gloss as indicators,the effects of reaction time,reaction temperature,catalyst dosage,and reactant molar ratio on the product yield were explored through orthogonal experiments,so as to determine the effect of 1-hydroxymethacrylic acid cyclohexane under catalysis.The optimal process conditions for the preparation of alkyl esters are:reaction time 4h,reaction temperature 85 ℃,catalyst dosage 0.3%,reactant molar ratio 1.1.By comparison,it is found that the ionic liquid[Beim]Br has a better catalytic effect in the reaction process of MAA and CHO,and the highest yield is 97.4%,it is light yellow transparent liquid.

关 键 词：1-羟基甲基丙烯酸环己烷酯 三乙基苄基氯化胺 酯化反应 对苯二酚 离子液体 

分 类 号：O624.32[理学—有机化学]