五羟乙基二乙烯三胺合成工艺优化研究

Study on Optimized Synthesis Process of N,N,N,N,N′-Pentakis(2-hydroxyethyl)-1,4,7-triazaheptane

以二乙烯三胺与2-氯乙醇为主要原料合成五羟乙基二乙烯三胺,采用单因素试验和正交实验对原料配比及工艺条件进行优化,最佳配比为:二乙烯三胺与2-氯乙醇的摩尔比为1∶6.5;最佳工艺条件为:反应温度85℃,反应时间5 h,收率达到了98.76%,并用羟值测定、胺值测定、FT-IR、1H-NMR及ES-MS等方法对产物进行结构表征.

N,N,N,N,N′-Pentakis(2-hydroxyethyl)-1,4,7-triazaheptane was synthesized by diethylenetriamine and2-chloroethanol as the main raw materials.Single-factor experiments and orthogonal experiments were used to optimize the ratio of raw materials and process conditions.The optimum molar ratio of diethylenetriamine and2-chloroethanol was1:6.5,and the optimum process conditions were as follows:reaction temperature was85℃and reaction time was5h.Under the optimal reaction conditions,the yields can reach98.76%.The structure of final product was characterized by determining hydroxyl value and amine value,FT-IR,1H-NMR and ES-MS.