微波辐射加热法合成乙亚胺

Synthesis of ethylenediamine tetraacetylimide by microwave

[目的]探讨微波辐射加热法合成乙亚胺的优越性。[方法]通过调整原料比例、微波功率和反应时间,确定最佳反应条件。然后,以传统方法合成乙亚胺,并将其结果与微波合成的结果相比较。[结果]微波辐射加热合成产物、传统方法合成产物、及标准品进行红外鉴定,确定它们为同一物质。在420 W的功率下,以甲酰胺∶乙二胺四乙酸(EDTA)=10.5∶1的比例反应12.5 min有最高产率,为75.6%。传统方法合成乙亚胺的产率为69.3%。相对于传统方法将反应时间缩短至原来的3.8%,并节约了46%的甲酰胺。[结论]微波合成乙亚胺相对于传统合成方法产率有所提高,并且大大缩短了反应时间,提高了原料甲酰胺的利用率。

[Objective] To research the superiorities of synthesizing ethylenediamine tetraacetylimide by microwave.[Method] The optimal condition for synthesis was determined by changing the proportion of the raw materials,the power of the microwave and the time of reaction.Ethylenediamine tetraacetylimide were also synthesized by traditional way.The superiorities of microwave method were concluded by comparing results of these two methods.Finally,products were identified by comparing the infragraph of standard.[Results] The highest yield（75.6%） was obtained while the proportion of formamide and EDTA was 10.5∶1,the power of microwave was 420 W and the reaction time was 12.5 min.It was higher than the yield of traditional method（69.3%）.Synthesizing ethylenediamine tetraacetylimide by using microwave just needed 3.8% of the time of original method,as well as saved 46% of formamide.Products made by this two ways and standard were checked by infragraph to ensure they were identical.[Conclusion] Synthesizing ethylenediamine tetraacetylimide by using microwave not only shorten the reaction time but also increase the yield of it and the utilization ratio of formamide compared to the traditional method.