连续流微反应技术在2,4-二氯氟苯的硝化中的应用  

Application of Continuous Flow Microreaction Technology in Nitration of 2,4-dichlorofluorobenzene

作　　者：舒鑫琳 徐登铅 顾海宁 SHU Xin-lin;XU Deng-qian;GU Hai-ning(Hangzhou Xinbenli Pharmaceutical Co.,Ltd.,Zhejiang Hangzhou 311100,China)

机构地区：[1]杭州新本立医药有限公司,浙江杭州311100

出　　处：《广州化工》2021年第14期73-75,共3页GuangZhou Chemical Industry

摘　　要：在微通道反应器中,由2,4-二氯氟苯、硫酸和硝酸连续硝化合成2,4-二氯-5-氟硝基苯。先后考察硝酸摩尔比、反应温度、停留时间等因素的影响,优化了工艺条件。结果表明,当n(硝酸):n(2,4-二氯氟苯)=1.1:1、反应温度110℃、停留时间75 s时,2,4-二氯氟苯转化率达到100%,收率达到95.3%。与传统间歇釜式工艺相比,微通道工艺提高了2,4-二氯-5-氟硝基苯的收率和选择性,大大缩短了反应时间,减少了原料消耗,实现全连续,提高了生产安全性。In a micro-channel reactor,2,4-dichloro-5-fluoronitrobenzene was synthesized by continuous nitration of 2,4-dichlorofluorobenzene,sulfuric acid and nitric acid.The effects of the molar ratio of nitric acid,reaction temperature and residence time were investigated,and the process conditions were optimized.The results showed that when n(nitric acid)􀏑n(2,4-dichlorofluorobenzene)=1.1􀏑1,reaction temperature was 110℃and residence time was 75s,the conversion of 2,4-dichlorofluorobenzene reached 100%and the yield reached 95.3%.Compared with the traditional batch reactor process,the micro-channel process improved the yield and selectivity of 2,4-dichloro-5-fluoronitrobenzene,greatly shortened the reaction time,reduced the consumption of raw materials,realized full continuous production,and improved the production safety.

关 键 词：微通道 硝化 连续流 

分 类 号：TQ246[化学工程—有机化工]