微波促进甘脲合成的工艺研究  

Study on Promoting the Synthesis of Glycoluril by Microwave Technology

作　　者：郑志花[1] 王建龙[1] 李永祥[1] 王艳红[1] 

机构地区：[1]中北大学化工与环境学院,山西太原030051

出　　处：《中北大学学报（自然科学版）》2015年第2期202-207,共6页Journal of North University of China(Natural Science Edition)

基　　金：中北大学研究生科技基金项目(20131034)

摘　　要：研究了常压下微波加热促进尿素与乙二醛缩合成甘脲的反应,考察了在盐酸为催化剂时,原料配比、反应温度、反应时间、反应pH值对甘脲得率的影响.实验结果表明,微波对此反应有很好的促进作用,不仅使产品得率提高,而且可以大大缩短反应时间.获得的较佳工艺条件为:脲与乙二醛的物质的量之比为2.1∶1,pH=1,在82℃下,反应14min,经稀碱液洗涤,蒸馏水洗涤至中性,乙醇洗涤,制得甘脲,平均得率为88.4%.同时用红外光谱、核磁共振氢谱及元素分析等对产物进行了表征,表明结构正确;高效液相色谱分析其纯度为98.5%.Glycoluril was synthesized by microwave heating under atmospheric pressure with glyoxal and urea.The influence of various factors on the yield of glycoluril was investigated,in the presence of HCl, such as raw material ratio,reaction temperature,reaction time and pH.The experimental results show that through microwave heating the product yield is improved and the reaction time is shortened.The better process conditions are as follows：the ratio of urea and glyoxal 2.1∶1,pH=1,under 82 ℃,re-action time 14 min,dilute NaOH washing,washing with distilled water to pH=7,washing with etha-nol,and the average glycoluril yield is 88.4% .The structure of production was characterized by FTIR, 1 H NMR,elemental analysis and so on,and analysis results show that the structure of production is correct.The purity of production is 98.5% by HPLC.

关 键 词：甘脲 尿素 乙二醛 缩合反应 微波加热 

分 类 号：TQ225.52[化学工程—有机化工] TQ226.36