为研究1,4-二氯-2-(1,1,2,3,3,3-六氟丙氧基)-5-硝基苯(虱螨脲中间体)的连续硝化合成工艺技术路线、反应器结构型式、反应温度和停留时间等参数.以m(浓硫酸)∶m(浓硝酸)为3∶1组成的混酸为硝化剂,采用循环管式反应器结构型式,研究反应与熟化工艺串联技术路线,考察25、30、35和40℃4种反应温度与40 ℃熟化温度下的组合工艺的硝化反应效率,并计算总停留时间.研究表明,连续硝化合成工艺转化率明显高于间歇硝化工艺的转化率,反应控制温度由间歇20～25℃提升至35 ℃,反应时间由间歇工艺15 h降低至4 h,产品产量和质量亦较为稳定,同时连续硝化反应工艺利于快速移走反应热,确保反应安全.
In order to study the continuous nitration synthesis process,reactor structure type,reaction temperature,and residence time of 1,4-dichloro-2-(1,1,2,3,3,3-hexafluoropropoxy)-5-nitrobenzene(an intermediate of Lufenuron),a mixed acid composed of concentrated sulfuric acid and nitric acid with a mass ratio of 3∶1 was used as a nitrating agent.A circulating tubular reactor was adopted to study the integrated technology route of reaction and maturation processes.The nitration reaction efficiency was examined at four reaction temperatures of 25 ℃,30 ℃,35 ℃,and 40 ℃ with a maturation temperature at 40 ℃,and the total residence time was calculated.The results showed that the conversion rate of the continuous nitration synthesis process was significantly higher than that of the intermittent nitration process.The controlled reaction temperature increased from the intermittent range of 20 ℃-25 ℃ to 35 ℃,and the reaction time was reduced from 15 hours in the intermittent process to 4 hours.The product yield and quality were also more stable.Additionally,the continuous nitration reaction process was conducive to a quick removal of reaction heat,ensuring reaction safety.
李双涛;魏东旭;黄益平;夏燕喃;黄晶晶;周明杰;何伟;刘辉;沈文彬
中建安装集团有限公司,江苏 南京 210046天津大学化工学院,天津 300072天津如有科技有限公司,天津 300192南京工业大学生物与制药工程学院,江苏 南京 211800河南金鹏化工有限公司,河南开封 475003
化学工程
循环管式反应器;1,4-二氯-2-(1,1,2,3,3,3-六氟丙氧基)-5-硝基苯;间歇硝化工艺;连续硝化工艺
circulating tube reactor;1,4-dichloro-2-(1,1,2,3,3,3-hexafluoropropyl)-5-nitrobenzene;intermittent nitrification process;continuous nitrification process
《南京工业大学学报（自然科学版）》 2024 (003)
272-280 / 9
国家自然科学基金面上项目(22178168);江苏省重点研发计划(BE2022791);中国建筑集团有限公司2021年科技研发计划(CSCEC-2021-Z-51)
10.3969/j.issn.1671-7627.2024.03.004
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