基于微通道技术合成邻氟苯酚  

Synthesis of ortho-fluorophenol based on microchannel technology

作　　者：严泽华 何星帅 刘听说 阮浩华 尹凯 YAN Zehua;HE Xingshuai;LIU Tingshuo;RUAN Haohua;YIN kai(Zhejiang Jitai New Materials Co.,Ltd.,Shaoxing 312369,Zhejiang,China;Zhejiang Nanjiao Chemistry Co.,Ltd.,Shaoxing 312369,Zhejiang,China)

机构地区：[1]浙江吉泰新材料股份有限公司,浙江绍兴312369 [2]浙江南郊化学有限公司,浙江绍兴312369

出　　处：《世界农药》2023年第6期34-38,共5页World Pesticide

摘　　要：邻氟苯酚是一种重要的医药和农产化学品的中间体,用于合成杀菌剂、除草剂,也可合成染料液晶、塑料及橡胶的添加剂等。主要以邻氟苯胺为原料,经微通道重氮,水解反应得到邻氟苯酚。系统研究了重氮反应温度、反应停留时间、硫酸用量、亚硝酸钠用量、催化剂、水解温度、水解酸浓度等因素对反应工艺的影响。重氮优化工艺为:硫酸与邻氟苯胺当量为6∶1,亚硝酸钠与邻氟苯胺当量为1.1∶1,重氮反应温度60℃,重氮停留时间32.7 s (持液体积27 m L);水解优化工艺为:水解温度185℃,催化剂硫酸铜用量为原料重量的10%,水解酸浓度40%最佳,最后邻氟苯酚收率可以达到90%。Ortho-fluoro phenol is an important intermediate for pharmaceuticals and agrochemicals,used in the synthesis of fungicides,herbicides,dyes,liquid crystals,plastics,rubber additives,among others.This article primarily discusses the synthesis of ortho-fluoro catechol from ortho-fluoro aniline through microchannel diazotization and hydrolysis reaction.The experiment systematically investigated the effects of diazotization reaction temperature,reaction time,sulfuric acid and sodium nitrite consumption,catalysts,as well as hydrolysis temperature and concentration on the reaction process.The optimum process for diazotization was found to be:sulfuric acid to ortho-fluoroaniline equivalent ratio of 6:1,sodium nitrite to ortho-fluoroaniline equivalent ratio of 1.1:1,diazotization reaction temperature of 60°C,and diazotization reaction time of 32.7 seconds(with a liquid holding capacity of 27 mL).The optimized hydrolysis process was found to be:hydrolysis temperature of 185°C,copper sulfate catalyst consumption of 10%of the raw material weight,and hydrolysis acid concentration of 40%.Finally,the yield of ortho-fluoro phenol can reach up to 90%.

关 键 词：中间体 邻氟苯酚 微通道 重氮 水解 

分 类 号：TQ450[化学工程—农药化工]