双丙酮丙烯酰胺的合成

Synthesis of diacetone acrylamide

M以丙酮和丙烯腈为原料,浓硫酸为催化剂,合成双丙酮丙烯酰胺（DAAM）,确定较优条件为反应时间5h,反应温度55℃,n（丙酮）∶n（丙烯腈）∶n（浓硫酸）=2.4∶1∶2.4,阻聚剂的用量为丙酮质量的0.5%。对分离精制过程中的碱液洗涤过程进行了优化,确定较佳条件为碱液质量分数20%,碱液用量30mL,碱洗时间60min。在上述条件下反应得到的产品的收率约为65%,产品质量分数达99.3%,熔点54-56℃。采用FT-IR与1 HNMR对产物结构进行了表征。

Diacetone acrylamide（DAAM）was synthesized with acetone and acrylonitrile as raw materials and concentrated sulfuric acid as catalyst.The obtained optimum reaction conditions were：reaction time 5h,reaction temperature 55℃,n（acetone）：n（acrylonitrile）∶n（sulfuric acid）=2.4∶1∶2.4,the quantity of inhibitor was equal to 0.5%acetone.The alkaline washing procedure of separation and purification process were optimized.The obtained optimum conditions were：the mass fraction of sodium hydroxide 20%,the amount of lye20 mL,caustic washing time 60 min.Under above conditions,the yield and purity of the product were about65%and 99.3%,respectively.The melting point of DAAM was 54~56℃.The structure of the product was characterized by FT-IR and1 HNMR.