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)=1.11,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.
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)
出处
《广州化工》
CAS
2021年第14期73-75,共3页
GuangZhou Chemical Industry
关键词
微通道
硝化
连续流
micro-channel
nitrificatio
continuous flow
