羟乙基乙二胺的连续流制备工艺  

Continuous flow preparation process of hydroxyethyl ethylenediamine

作　　者：董凡 朱建民 董振鹏 陈慕华[1] 朱新宝[1] 付博[1] DONG Fan;ZHU Jianmin;DONG Zhenpeng;CHEN Muhua;ZHU Xinbao;FU Bo(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,Jiangsu,China;Jiangsu Oxiranchem Chemical Co.,Ltd.,Yangzhou 211400,Jiangsu,China)

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]江苏奥克化学有限公司,江苏扬州211400

出　　处：《精细化工》2024年第2期458-464,共7页Fine Chemicals

基　　金：国家重点研究计划项目(2022YFD2200802)。

摘　　要：以乙二胺和环氧乙烷为原料,在具有特殊微结构的连续流微反应器内发生乙氧基化反应合成羟乙基乙二胺。考察了原料物质的量比、乙二胺含水量、反应温度、停留时间对反应的影响。结果表明,在n(乙二胺)∶n(环氧乙烷)=3∶1、乙二胺含水量为0.96%(质量分数)、反应温度为80℃、停留时间为60 s的最佳工艺条件下,环氧乙烷转化率接近100%,羟乙基乙二胺的选择性为87.4%,二羟乙基乙二胺的选择性为9.2%。间歇釜式反应工艺在相同物料比和反应温度条件下,羟乙基乙二胺的选择性为83.5%,二羟乙基乙二胺的选择性为15.9%。连续流微反应器能有效提高羟乙基乙二胺的选择性,降低副反应的发生,同时大大缩短了反应时间,提高了反应效率。Hydroxyethyl ethylenediamine was synthesized from ethoxylation of ethylenediamine and ethylene oxide in a continuous flow microreactor with special microstructure.The effects of molar ratio of materials,water content of ethylenediamine,reaction temperature and residence time on the reaction were then analyzed.The results showed that under the optimal conditions of n(ethylenediamine)∶n(ethylene oxide)=3∶1,water content of ethylenediamine being 0.96%(mass fraction),reaction temperature of 80°C,and residence time of 60 s,the conversion of ethylene oxide was close to 100%,the selectivity of hydroxyethyl ethylenediamine was 87.4%and the selectivity of dihydroxyethyl ethylenediamine was 9.2%,while in the batch kettle reactor,the selectivity of hydroxyethyl ethylenediamine was 83.5%and the selectivity of dihydroxyethyl ethylenediamine was 15.9%with the same material ratio and reaction temperature.Therefore,the continuous flow microreactor could effectively improve the selectivity of hydroxyethyl ethylenediamine,reduce the occurrence of side reactions,greatly shorten the reaction time and boost the reaction efficiency.

关 键 词：环氧乙烷 乙氧基化反应 羟乙基乙二胺 连续流微反应器 精细化工中间体 

分 类 号：TQ226.3[化学工程—有机化工]