分子筛固定床脱水合成N-(1-环己烯基)吗啉

STUDU ON SYNTHESIS OF N-(1-CYCLOHEXENYL)MORPHOINE BY ZEOLITE FIXED BED DEHYDRATION

以吗啉和环己酮为原料,采用分子筛固定床脱水,回流反应合成N-(1-环己烯基)吗啉。考察了催化剂、n(吗啉)∶n(环己酮)、对苯二酚、回流时间对实验结果的影响。实验结果表明,较佳的实验条件为:n(吗啉)∶n(环己酮)=4∶1、w(催化剂)=2.0%、w(对苯二酚)=0.1%、干燥剂为反应物质量的10%、回流反应2 h,产品收率可达95.0%以上,产品纯度98.7%。此工艺操作简便、产品收率高、分子筛固定床可连续循环使用、易于进行工业化生产。

N-(1-cyclohexenyl)morpholine was synthesized from morpholine and cyclohexanone by zeolite fixed bed dehydration and reflux reaction.The effects of catalyst,n(morpholine)∶n(cyclohexanone),desiccant hydroquinone and reflux time on the experimental results were studied.The experimental results showed that the optimal n(morpholine)∶n(cyclohexanone)was 4,catalyst dosage was 2.0%,hydroquinone dosage was 0.1%,desiccant dosage was 10%and reflux reaction time was 2 h.The yield of the product was over 95.0%,and the purity of the product was 98.7%.The process was easy to operate,high yield,continuous recycling of zeolite fixed bed and easy to industrialize.