树脂固化剂N-乙酰乙酰基吗啉的合成研究

Synthesis of N-acetoacetyl Morpholine as a Resin Hardener

以双乙烯酮、吗啉为原料,在溶剂和阻聚剂的作用下合成了N-乙酰乙酰基吗啉。考察了反应时间、温度、阻聚剂种类及用量、原料配比等对产品收率的影响。结果表明,优化工艺条件为:以2,2,6,6-四甲基-4-羟基哌啶氮氧自由基为阻聚剂,苯为溶剂,n(双乙烯酮):n(吗啉):n(苯):n(2,2,6,6-四甲基-4-羟基哌啶氮氧自由基)为1:1.15:2.88:0.017,反应温度90~95℃,反应时间9 h,此条件下产品收率达93.93%。

N-acetoacetyl morpholine was synthesized from diketene and morpholine respectively as a solvent and a polymerization inhibitor.We studied the effects of the reaction time,temperature,the polymerization inhibitor amount,and the molar ratio between diketene and morpholine to benzene on the product yield.The results showed that under the optimized reaction conditions as follows:4-hydroxy-2,2,6,6-tetramethylpiperidine nitroxide radical used as a polymerization inhibitor,benzene as a solvent,n(diketene):n(morpholine):n(benzene):n(4-hydroxy-2,2,6,6-tetramethylpiperidine nitroxide radical)was 1:1.15:2.88:0.017,reaction temperature 90-95 C,and reaction time 9 hours,the yield of product will reach 93.93%.