以3-环己烯甲酸-3'-环己烯甲酯(A)为原料、H₂O₂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H₂O₂(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,H₂O₂ 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 H₂O₂ (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.

徐蒙(1994-),女,硕士研究生,研究方向为连续流化工工艺开发,19085216440@smail.cczu.edu.cn