二乙胺羟基化合成二乙基羟胺

以改性的TS-1分子筛为催化剂,研究了二乙胺与过氧化氢羟基化的工艺路线。考察了原料配比、反应时间、反应温度等因素对反应的影响,特别是溶剂对反应的重要性。实验表明,反应的最佳条件为:H2O2与二乙胺的物质的量比为1.0~1.1,反应温度75~80℃,反应时间70 min,催化剂浓度4%,叔丁醇-水作为混合溶剂,叔丁醇与水的体积比为2~2.5;H2O2有效转化率88.2%,二乙基羟胺的选择性达到80.1%。

Experimental Study on Synthesis of Diethyl Hydroxylamine from Diethylamine

Diethylamine hydroxylation with hydrogen peroxide on modified TS-1 molecular sieve has been investigated.The study is focused on these factors including diethylamine/H2O2 molar ratio,the reaction time and temperature etc.The effect of reaction medium and solvent is very important.Finally,the process of diethylamine hydroxylation is proposed.The suitable conditions of etherification reaction are found as follows： the molar ratio of diethylamine to H2O2 is 1.0~1.1,the reaction temperature is 75℃～80℃,the reaction time is 70 min,the conversion of H2O2 is over 98%,the yield of diethylamine is 80.1%.