高效杀虫剂原料2,6-二氟苯胺合成工艺的研究  

Study on Synthesis Technology of 2,6-difluoroaniline Material for High Efficient Insecticide

作　　者：熊国兰[1] 蒋柏泉[2] 赖晓波 

机构地区：[1]新余高等专科学校,江西新余338031 [2]南昌大学环境科学与工程学院,江西南昌330031 [3]江西省化学工业研究所,江西南昌330029

出　　处：《安徽农业科学》2008年第23期9848-9849,共2页Journal of Anhui Agricultural Sciences

摘　　要：[目的]优化2，6-二氯苯甲腈法合成2，6-二氟苯胺的最佳工艺。[方法]采用2，6二氯苯甲腈法合成2，6二氟苯胺，通过单因素试验，研究各工艺参数对氟代反应、水解反应和霍夫曼重排反应产率的影响。[结果]氟代反应的最佳工艺条件为：DCBN／KF为1.0：2，8，反应前期温度170～180℃，时间2h；反应后期温度230～240℃，时间4h，该条件下，反应产率为88％～90％。水解反应的最佳工艺条件为：硫酸浓度85％，反应温度70℃，反应时间4h，该条件下，水解产率为98．4％。霍夫曼重排反应的最佳工艺条件为：反应温度60～70℃，反应时间2h，溴用量16．5～17．0g。[结论]在最佳工艺条件下，2，6-二氯苯甲腈法合成2，6-二氟苯胺的产率达68.5％，且易于实现工业化。[ Objective ] The aim was to optimize the best technology of synthesis of 2, 6 -difluoroaniline with 2, 6 -Dichloro -cyanobenzene method. [ Method ] The 2, 6-difluoroaniline was synthesized by using 2, 6-Dichloro-cyanobenzene, the effect of each process parameter on the yields for reaction of fluoridation, hydrolysis, and Hofmann rearrangement was studied through single factor test, [ Result] The optimal process conditions of fluoridation reaction were： DCBN/KF was 1.0：2.8 ,temperature 170 - 180 ℃ in the early stage for 2 h, temperature 230 -240℃in the later stage for 4h, and reaction yield was 88% - 90% under these conditions. The best process conditions of hydrolysis reaction were ： the sulfuric acid concn, of 85% , reaction temperature 70 ℃, reaction time 4h, and the hydrolysis yield was 98.4% under these conditions. The optimal process conditions of Hofmann rearrangement reaction were： reaction temperature 60 -70 ℃ , reaction time 2h, bromine dosage 16.5 - 17.0 g. [ Conclusion] Under the best process conditions, the yield for 2, 6-difluoroaniline synthesized by 2, 6-Dichloro-cyano- benzene was up to 68.5% ,which was easy to realize industrialization.

关 键 词：2 6-二氟苯胺 2 6-二氯苯甲腈 合成工艺 

分 类 号：S482.3[农业科学—农药学]