双丙酮丙烯酰胺的合成研究

以丙酮、丙烯腈为原料,在98%浓硫酸催化作用下合成一种环状中间体,利用结晶提取中间体,再中和开环制得双丙酮丙烯酰胺(DAAM)。研究反应条件对中间体收率的影响,结果表明,合成中间体的适宜条件为:n(丙酮)∶n(丙烯腈)∶n(98%浓硫酸)=2.3∶1.0∶2.5、反应温度50℃、反应时间4 h。根据晶体生长理论确定影响结晶的主要因素,并研究了这些因素对中间体的收率及纯度的影响,确定提取中间体的工艺条件为:结晶稀释剂用量(相对0.5 mol丙烯腈)250mL、结晶温度为0℃。在适宜的合成工艺条件下,制得中间体相对丙烯腈的收率为58.8%,DAAM产物纯度为98.7%,熔点为56.1~56.7℃,相对丙烯腈的收率为50.4%,采用红外光谱、气相色谱及熔点测定方法对产物进行了分析表征。

Study on Synthesis of Diacetone Acrylamide

Diacetone acrylamide(DAAM) was prepared with acetone and acrylonitrile as raw materials and 98% sulfuric acid as catalyst.An intermediate was formed,and then was withdrawn through crystallization and neutralized.The effects of reaction conditions on the yield of intermediate were studied.The results indicated that the optimal synthesis conditions of the intermediate are as follows,n(acetone)∶n(acrylonitrile)∶n(98% sulfuric acid)=2.3∶1.0∶2.5,reaction temperature 50℃,reaction time 4 h.The optimal withdrawing conditions obtained in consideration of the crystallization theory are as follows:the amount of acetone for dilution(based on 0.5 mol acrylonitrile),250 mL;and the crystallization temperature,0℃.The yield of the intermediate was 58.8% based on acrylonitrile.DAMM was obtained with purity of 98.7% and melting point of 56.1～56.7℃.The yield of DAAM was 50.4% based on acrylonitrile.The product was identified and analyzed by IR,GC and mp.