Sheng Yingxia, Xiao Qianjin, Hu Hui, Zhang Tianya, Guan Guofeng
College of Safety Science and Engineering, Nanjing Tech University, Nanjing 211816, China.
Jiangsu TaiJieZhiBang Testing Technology Co., Ltd., Nantong 226009, China.
Molecules. 2025 Jul 11;30(14):2939. doi: 10.3390/molecules30142939.
This paper introduces the nitration process of obtaining the synthetic intermediate 1-(2-chloro-4-fluoro-5-nitrobenzene)-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1)-one of pyraclostrobin using raw materials fluorobenzotriazolone, fuming nitric acid, fuming sulfuric acid, and toluene. The exothermic characteristics of the nitration, quenching, extraction, and alkali washing in the nitration reaction were studied, and the thermal decomposition risk of the raw materials and the secondary decomposition risk of the products in the nitration process were evaluated. The results showed that the thermal decomposition risk of the four raw materials was level 1. The acceptable level of runaway reaction in the nitration process was evaluated to be level 2, the acceptable level of runaway reaction in the quenching was level 3, the acceptable level of runaway reaction in the extraction and the alkali washing was level 1, the process hazard level of the nitration reaction and the quenching was evaluated to be level 5, and the process hazard level of the extraction and the alkali washing was level 1. Based on the comprehensive assessment results, targeted risk mitigation and control strategies are proposed to ensure process safety.
本文介绍了以氟苯并三唑酮、发烟硝酸、发烟硫酸和甲苯为原料，制备吡唑醚菌酯的合成中间体1-(2-氯-4-氟-5-硝基苯)-4-二氟甲基-4,5-二氢-3-甲基-1,2,4-三唑-5(1)-酮的硝化过程。研究了硝化反应中硝化、淬灭、萃取和碱洗的放热特性，评估了硝化过程中原料的热分解风险和产物的二次分解风险。结果表明，四种原料的热分解风险为1级。硝化过程中失控反应的可接受水平评估为2级，淬灭过程中失控反应的可接受水平为3级，萃取和碱洗过程中失控反应的可接受水平为1级，硝化反应和淬灭的过程危险等级评估为5级，萃取和碱洗的过程危险等级为1级。基于综合评估结果，提出了针对性的风险缓解和控制策略，以确保过程安全。
