第 52 卷第 3 期 Vol. 52 No. 3 2022 年 6 月 Jun 2022

所属栏目：农药及中间体 微通道反应器在唑草酮硝化反应中的应用

李金平，丁小兵 （江苏苏化集团技术中心，江苏 苏州 215007）

摘　要：应用微通道反应器对唑草酮中间体连续硝化工艺进行研究，包括反应器的选型、空速比、硝酸与底物1-（4-氯-2-氟苯基）-3-甲基-4-二氟甲基-1H-1，2，4-三唑啉-5-酮的配比、硫酸的浓度与套用、反应温度梯度控制等工艺条件的优化。结果表明，使用特种合金微反应器，在n（底物）∶n（硝酸）∶n（85%硫酸）=1.0∶1.1∶6.6、空速比为60 h-1、一级反应器控温（35±2） ℃、二级反应器控温（45±2） ℃条件下，底物硝化转化率≥99%，产品收率≥95%，并实现了工艺连续化。相对于釜式间歇反应，具有收率高、反应通量大、更安全高效的特点。

关键词：微通道反应器；唑草酮；硝化反应；空速比

中图分类号：TQ457　　文献标识码：A　　文章编号：1009-9212（2022）03-0016-04

Application of Microchannel Reactor in the Nitration Reaction of Carfentrazone-ethyl Intermediate

LI Jin-ping, DING Xiao-bing (Jiangsu Chemical Group Technology Center, Suzhou 215007, China)

Abstract：A process for continuous nitration of Carfentrazone-ethyl intermediate using microchannel reactors was systematically studied. Factors including type of microchannel reactors, space velocity ratio, molar ratio of nitric acid and substrates [1-(4-chloro-2-fluorophenyl)-3-methyl-4-(difluoromethyl)-1H-1,2,4-triazol-5-one], concentration and recycle of sulfuric acid, reaction temperature gradient control and other process were evaluated; The optimal condition were as followings: n(substrate)∶n(nitric acid)∶n(85% sulfuric acid)=1.0∶1.1∶6.6; the space velocity ratio was 60ｈ-1 using microreactors (special alloy); the control temperature of the first reactor was of (35±2) ℃; and the　temperature of the second reactor was of (45±2) ℃; Under optimal conditions, the nitration conversion rate of the substrate was ≥99%; a total yield was of ≥95%. Compared with the batch reaction, it has the advantages including higher yield, higher reaction throughput, safer and faster.

Key words：microchannel reactor; Carfentrazone-ethyl; nitration reaction; space velocity ratio

作者简介：李金平（1968－），男，江西新余人，高级工程师，研究方向：农药、有机合成、微反应器化学应用研究（E-mail：ljp@jsgc.com）。

收稿日期：2021-12-10