合成四甲氧甲基甘脲工艺条件的研究

Process Conditions for Synthesizing Tetramethoxy methyl glycoluril

四甲氧甲基甘脲是一种新型粉末涂料的交联剂。通过碱催化把甘脲和多聚甲醛缩合成四羟甲基甘脲中间体,然后再与过量的甲醇在酸性条件下合成四甲氧甲基甘脲。研究了反应物摩尔比、pH值、反应时间和温度,以及滴加速度等各因素对四羟甲基甘脲中间体和四甲氧甲基甘脲收率的影响,并通过正交实验得到最佳工艺条件。产物采用红外色谱仪(FT-IR)进行了表征;使用了高效液相色谱仪和紫外色谱仪检测了产品的纯度和产率。据上述红外、液相色谱分析可知,本方法合成的四甲氧甲基甘脲产率高,能达到80%(质量分数),纯度也高达到92%。

Tetramethoxymethyl glycoluril is crosslinking agent of powder coating. It was synthesized under acidic conditions from from excessive methanol and tetrahydroxymethyl glycoluril intermediate. The intermediate was synthesized from glycoluril and paraformaldehyde by base-catalyzed condensation. Optimum conditions and process parameters were obtained by investigating the effects of molar ratio, pH, reaction time and temperature, and the dropping rate of solution on the yields of tetrahydroxymethyl glycoluril and tetramethoxymethyl glycoluril. The products were characterized by Infrared chromatography, UV spectroscopy and high performance liquid chromatography.