微通道反应器中环氧树脂单体AOO的合成工艺研究  

Synthesis of epoxy monomer AOO in microchannel reactor

作　　者：徐蒙 张跃[1,2,3] 刘涛 严生虎[1,2,3] 刘建武[2,3] 沈介发[2,3] 马晓明[2,3] 辜顺林[2,3] XU Meng;ZHANG Yue;LIU Tao;YAN Sheng-hu;LIU Jian-wu;SHEN Jie-fa;MA Xiao-ming;GU Shun-lin(School of Petrochemical Engineering,Changzhou University,Changzhou 213164,China;School of Pharmacy,Changzhou University,Changzhou 213164,China;Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry,Changzhou University,Changzhou 213164,China;Zhejiang Wanfeng Chemical Co.,Ltd.,Shaoxing 312073,China)

机构地区：[1]常州大学石油化工学院,江苏常州213164 [2]常州大学药学院,江苏常州213164 [3]常州大学石油和化工行业连续流技术工程实验室,江苏常州213164 [4]浙江万丰化工股份有限公司,浙江绍兴312073

出　　处：《现代化工》2022年第10期154-158,164,共6页Modern Chemical Industry

基　　金：工信部产业技术基础公共服务平台(2020-0107-3-1)。

摘　　要：以3-环己烯甲酸-3'-环己烯甲酯(A)为原料、H_(2)O_(2)为氧源、1,2-二氯乙烷为溶剂,在连续流微通道反应器中环氧化合成3,4-环氧环己基甲酸-3',4'-环氧环己基甲酯(AOO)。考察了A与其他物质添加量的比、反应温度、缓冲剂的用量、停留时间以及溶剂用量对AOO合成的影响并进行工艺优化。结果表明,当A与H_(2)O_(2)(质量分数为35%)的物质的量比为1∶3.0、A与乙酸酐的物质的量比为1∶3.0、A与乙酸钠的物质的量比为1∶0.5、A与1,2-二氯乙烷的体积比为1∶2.5、反应温度为55℃、停留时间为5 min时,测得A的转化率达到100%,AOO的收率可达97.7%,纯度达96.43%,环氧当量为130.21 g/mol。3,4-Epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate(AOO)is synthesized in a continuous flow microchannel reactor by using 3-cyclohexenyl 3-cyclohexene 1-carboxylate(A)as raw material,H_(2)O_(2) as oxygen source and 1,2-dichloroethane as solvent.The influences of the addition ratios between A and other substances,the dosages of buffer and solvent,reaction temperature and residence time on the synthesis of AOO are investigated,and the process is optimized.The results show that the conversion of A,the yield of AOO and the purity of AOO reach 100%,97.7%and 96.43%,respectively,and epoxy equivalent reaches 130.21 g·mol^(-1) when the molar ratio of A to H_(2)O_(2)(35%by mass)is 1∶3,the molar ratio of A to acetic anhydride is 1∶3,the molar ratio of A to sodium acetate is 1∶0.5,the volume ratio of A to 1,2-dichloroethane is 1∶2.5,reaction temperature is 55℃,and residence time is 5 min.

关 键 词：3-环己烯甲酸-3'-环己烯甲酯 环氧化反应 连续流工艺 微通道反应器 3 4-环氧环己基甲酸-3' 4'-环氧环己基甲酯 

分 类 号：TQ322.4[化学工程—合成树脂塑料工业]