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羟乙基乙二胺的连续流制备工艺

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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.
Continuous flow preparation process of hydroxyethyl ethylenediamine
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 ℃,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.

ethylene oxideethoxylation reactionhydroxyethyl ethylenediaminecontinuous flow microreactorfine chemical intermediates

董凡、朱建民、董振鹏、陈慕华、朱新宝、付博

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南京林业大学 化学工程学院,江苏 南京 210037

江苏奥克化学有限公司,江苏 扬州 211400

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

国家重点研究计划项目

2022YFD2200802

2024

精细化工
大连化工研究院设计院 中国化工学会精细化工专业委员会 辽宁省化工研究院

精细化工

CSTPCD北大核心
影响因子:0.557
ISSN:1003-5214
年,卷(期):2024.41(2)
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