双丙酮丙烯酰胺的合成及工艺优化

Synthesis of diacetone acrylamide and its process optimalization

以二丙酮醇和丙烯腈为原料 ,利用简便、温和的反应条件合成新型乙烯基功能单体 -双丙酮丙烯酰胺。通过四因素四水平的正交实验并结合条件实验 ,得到制备中间产物的最佳条件 :加料温度 2 0℃ ,二丙酮醇与丙烯腈的摩尔比 1∶1 2 ,反应时间 4h ,稀释用丙酮 2 0 0mL(相对于 1mol二丙酮醇 )。利用熔点法、IR、1H NMR对产品进行了鉴定。

Diacetone acrylamide(DAAm) was prepared by reacting acrylonitrile with diacetone alcohol in 98% sulfuric acid, obtaining an intermediate and then neutralizing the intermediate by ammonia. Through the orthogonal test results and conditional tests, a convenient process for synthesizing the intermediate and its optimum conditions were found. The optimum conditions are: the temperature of the material added is 20?℃, the mole ratio of diacetone alcohol to acrylonitrile 1.0∶1.2, the reaction time 4 hours and the amount of acetone added 200?mL/1?mol diacetone alcohol. The product was identifed by the method of melting point, IR and NMR.