对称N,N-二乙基丙烯酰胺的合成研究

以二乙胺和丙烯酸甲酯为原料,经双键保护、催化胺解、催化热裂解、减压精馏等过程制得N,N-二乙基丙烯酰胺(DEAA)。考察了反应温度、反应时间、原材料配比对反应结果的影响。实验表明,对于加成反应过程,催化剂用量10%,反应时间12 h,反应温度55℃,甲醇与丙烯酸甲酯的配比为2.5∶1,丙烯酸甲酯的转化率为95.1%,产品收率为93.9%;催化胺解过程:催化剂用量2%,反应时间4 h,反应温度100℃,二乙胺与甲氧基丙酸甲酯的配比为1.15∶1,甲氧基丙酸甲酯的转化率为96.9%,产品收率为92.9%;催化裂解过程,反应时间为3 h,溶剂用量为78%左右,N,N-二乙基丙烯酰胺的收率≥79%,产品总收率≥72%。

Research on the synthesis of N,N-diethylacrylamide

Methylacrylate and diethylamine were used as raw materials.After double bond protection,catalytic aminolysis reaction,catalytic pyrolysis and subsequent vacuum distillation,DEAA product was obtained successfully.In addition,the effect of temperature,reaction time,ratio of raw materials in synthesis process were investigated.It has been proved that for addition reaction catalyst amount was 10%,reaction time was 12 h,reaction temperature was 55 ℃,the molar ratio of methanol to methylacrylate was 2.5∶1,the percent conversion of methylacrylate was 95.1%,the yield was 93.9%;for catalytic aminolysis reaction catalyst amount was 2%,reaction time was 4 h,reaction temperature was 100 ℃,the molar ratio of diethylamine to methyl-4-aminobenzene sulfonylcarbamate was 1.15∶1,the percent conversion was 96.9%,the yield was 92.9%;for catalytic pyrolysis reaction time was 3 h,solvent was 78%,the yield of DEAA was over 93.9%,the total yield was over 72%.