第 39 卷第 3 期Vol. 39 No. 3
2009 年 6 月Jun 2009

所属栏目:农药及中间体

2-氯-6-三氯甲基吡啶的制备研究
陈朝辉,胡晓珊 (湖南国发精细化工科技有限公司,湖南 岳阳 414013)
摘 要:采用等质量混合的三乙醇胺与过氧化苯甲酰作为催化剂,在管式反应器中2-甲基吡啶盐酸盐(MPCH)与氯气反应合成了2-氯-6-三氯甲基吡啶(NP),研究了催化剂用量、反应原料、原料配比、加料速率和反应温度对氯化产物中NP含量及制备过程收率的影响。优化反应条件为:采用MPCH作原料,m(催化剂) ∶ m(2-甲基吡啶)=0.01 ∶ 1,n(Cl2) ∶ n(MPCH)=6 ∶ 1,反应温度为180~190℃,MPCH和氯气的较佳进料速率分别为15 g/h和49.4 g/h,此时氯化产物中NP的含量可达78.5%,制备过程收率达93.4%。氯化反应NP选择性高,工艺简单,易于实现工业化。
关键词:2-氯-6-三氯甲基吡啶;氯气;2-甲基吡啶;氯化;管式反应器
中图分类号:TQ253.21  文献标识码:A  文章编号:1009-9212(2009)03- 0021-04
A Study on the Preparation of 2-Chloro-6-(trichloromethyl)pyridine
CHEN Zhao-hui,HU Xiao-shan (Hunan Guofa Fine Chemicals and Technology Co.,Ltd.,Yueyang 414013,China)
Abstract:2-Chloro-6-(trichloromethyl)pyridine(NP) was prepared by chlorination of 2-methylpyridine hydrochloride(MPCH)with Cl2 in a gas-liquid countercurrent tubular reactor. A mixture of triethanolamine and benzoylperoxide with identical concentration was used as catalyst. The optimum reaction conditions were as follows: m(Catalyst) ∶ m(MP)= 0.01 ∶ 1, n(Cl2) ∶ n(MPCH)= 6 ∶ 1, reaction temperature 180~190℃, feed rates of MPCH 15 g/h and of Cl2 49.4 g/h. Under optimal conditions, the content of NP in chlorination products and the yield of NP reached 78.5% and 93.4%, respectively.
Key words:2-chloro-6-(trichloromethyl)pyridine;chlorine;2-methylpyridine;chlorination;tubular reactor
作者简介:陈朝辉(1968-),男,湖南临湘人,工程师,从事农药及精细化工中间体合成及生产研究。(E-mail:czh19680520@qq.com)
收稿日期: 2008-05-0