摘要
通过强酸催化乙腈闭环制备2,4,6-三甲基-1,3,5-三嗪,经试验优化得到以三氟甲磺酸和乙腈摩尔比为3:1,在120℃下反应12h条件下产品收率可达78.0%,通过H^(1)NMR与熔点对所得产品进行表征,表征结果证明所得产品即为2,4,6-三甲基-1,3,5-三嗪,通过GC分析产品含量高达98.7%。此工艺与传统制备工艺中首先使用氯化氢气体、乙腈、乙醇制备出乙酰亚胺乙酯盐酸盐,再经碳酸钾中和后用冰醋酸闭环的三步反应相比,具有工艺过程短、不使用氯化氢气体、操作安全等优势。
In this paper,2,4,6-trimethyl-1,3,5-triazine was prepared by strong acid-catalyzed ring-closure of acetonitrile,the product yield can reach 78.0%when the molar ratio of trifluoromethane sulfonic acid and acetonitrile was 3:1 and the reaction condition was 120℃for 12 hours.The product obtained was characterized by H^(1)NMR and melting point.The characterization results showed that the product was 2,4,6-trimethyl-1,3,5-triazine,and the content of the product was as high as 98.7%by GC analysis.Compared with the traditional preparation process,three-step reaction,which first uses hydrogen chloride gas,acetonitrile and ethanol to prepare acetylimine ethyl ester hydrochloride,and then neutralizes it with K_(2)CO_(3)and uses glacial acetic acid for closed-loop,this process has the advantages of short process,no use of hydrogen chloride gas,safe operation and so on.
作者
李德锦
郑付伟
陈海涛
段显英
王龙
韩福娇
张慧青
LI De-jin;ZHENG Fu-wei;CHEN Hai-tao;DUAN Xian-ying;WANG Long;HAN Fu-jiao;ZHANG Hui-qing(Institute of Chemistry Co.,Ltd.,Henan Academy of Sciences,Zhengzhou 450002,Henan,China)
出处
《合成材料老化与应用》
2022年第5期41-43,共3页
Synthetic Materials Aging and Application
基金
河南省科学院基本科研业务费(No:220603060)
作者简介
李德锦,助理工程师,主要从事精细化学品技术研究。
