羟乙基乙二胺的连续流制备工艺研究

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、停留时间等对反应的影响。确定了最佳工艺条件为：n(乙二胺) : n(环氧乙烷) = 3:1、乙二胺含水量控制在5%（质量分数）以内、反应温度为80 ℃、停留时间为60 s。在此条件下，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%，与之相比，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。

Study on continuous flow preparation process of hydroxyethyl ethylenediamine

Hydroxyethyl ethylenediamine(AEEA) was synthesized from ethylenediamine(EDA) and ethylene oxide(EO) by ethoxylation in a continuous flow microreactor with special microstructure. The effects of material ratio, water content of ethylenediamine, reaction temperature and residence time on the reaction were investigated. The optimal process conditions were determined: n(EDA): n(EO) = 3:1, the water content of ethylenediamine should be controlled within 5% (mass fraction), reaction temperature was 80 °C, and residence time was 60 s. Under these conditions, the conversion of EO is close to 100%, the selectivity of AEEA was 87.4% and the selectivity of dihydroxyethyl ethylenediamine was 9.2%. In the batch kettle reactor, the selectivity of AEEA is 83.5% and the selectivity of dihydroxyethyl ethylenediamine is 15.9% under the same material ratio and reaction temperature. Compared with that, the continuous flow microreactor can effectively improve the selectivity of AEEA, reduce the occurrence of side reactions, greatly shorten the reaction time and improve the reaction efficiency.