微通道连续流工艺在甲磺草胺中间体硝化反应中的应用  

Application of microchannel continuous process in the nitration of sulfentrazone intermediate

作　　者：纪璐 李书龙 安亭旺 郭帅 魏微 王珂 范娜 刘东[1] JI Lu;LI Shulong;AN Tingwang;GUO Shuai;WEI Wei;WANG Ke;FAN Na;LIU Dong(Shenyang Research Institute of Chemical Industry Co.,Ltd.,Shenyang 110021,China)

机构地区：[1]沈阳化工研究院有限公司,沈阳110021

出　　处：《农药》2025年第2期94-100,共7页Agrochemicals

摘　　要：[目的]利用微通道反应器研究甲磺草胺中间体2-(2,4-二氯苯基)-4-二氟甲基-5-甲基-2,4-二氢-3H-1,2,4-三唑-3-酮(TZL)的硝化反应工艺。[方法]用二氯乙烷溶解原料TZL,与混酸在微反应器内进行连续硝化反应得到硝化产品。[结果]在n(TZL)∶n(硝酸)∶n(108%硫酸)为1∶1.04∶8,进料温度为35℃,反应器温度为75℃的条件下,原料转化率达到100%,产品收率≥96%,与间歇工艺相比,反应时间由2 h降低至57 s。[结论]该工艺具有反应时间短、收率高、安全性和经济效益好等优势,可以实现工业化生产。[Aims]The objective is to use microchannel reactors to study the nitration reaction process of sulfentrazone intermediate 2-(2,4-dichlorophenyl)-4-(difluoromethyl)-5-methyl-2,4-dihydro-3H-1,2,4-triazol-3-one(TZL).[Methods]The raw material was dissolved by dichloroethane and the product was obtained by continuous nitration reaction with mixed acid in microreactor.[Results]Under the conditions of n(TZL)∶n(nitric acid)∶n(108%sulfuric acid)=1∶1.04∶8,feed temperature of 35℃,and reactor temperature of 75℃,the conversion rate of TZL reached 100%,and the product yield was≥96%.Compared with the batch process,the reaction time was reduced from 2 h to 57 s.[Conclusions]This process has the advantages of short reaction time,high yield,high safety and economic benefits,and can achieve industrial production.

关 键 词：甲磺草胺中间体 微通道反应器 硝化反应 

分 类 号：TQ457[化学工程—农药化工]