摘要
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.
出处
《化工科技》
CAS
2015年第5期48-51,共4页
Science & Technology in Chemical Industry
关键词
丙酮
丙烯腈
双丙酮丙烯酰胺
合成
Acetone
Acrylonitrile
Diacetone acrylamide
Synthesis