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苯并三唑制备中重氮偶合工艺的优化

Diazo coupling process optimization in preparation of benzontriazole
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摘要 以邻硝基苯胺和浓硫酸制成重氮液,再与对甲基苯酚偶合成苯并三唑中间体。研究了重氮化过程中浓硫酸用量和亚硝酸钠溶液含量的影响,及偶合过程中温度、pH和搅拌方式对产品质量的影响。结果表明,浓硫酸用量8 mL,亚硝酸钠溶液的质量分数为7%,偶合温度5℃左右,p H控制在8~10,电子恒速搅拌器的搅拌方式,产品的收率最高可达97.6%、质量分数在95.7%左右,达到了工业生产最优水平。 Diazo compound was made by reacting with o-nitroaniline and concentrated sulfuric acid,then coupled with methyl phenol to synthesis benzotriazole.The amount of concentrated sulfuric acid,sodium nitrite solution content was studied during diazo process.Reaction temperature,p H stirring style also have been explored.The results showed optimal conditions as following:vitriol dosage 8 m L,mass fraction of sodium nitrite solution is 7%,coupling temperature is 5℃,p H is about 8~10,electronic constant rate agitating.The product yield could reach 97.6%,and mass fraction of product is about 95.7%in the intermixture which achieve the optimal level of industrial production.
作者 李建光 郑朝红 张军华 禄婷 吴越超 王玉林 吕亮 LI Jianguang;ZHENG Chaohong;ZHANG Junhua;LU Ting;WU Chaoyue;WANG Yulin;LÜLiang(College of Chemical and Material Engineering,Quzhou University;Lianlongkerun new materials Limited Corporation,Quzhou,Zhejiang 324200)
出处 《化工生产与技术》 CAS 2021年第1期12-15,42,I0003,共6页 Chemical Production and Technology
基金 衢州市科技计划项目(2017G05)。
关键词 紫外线吸收剂 苯并三唑 重氮化 偶合反应 ultraviolet absorber benzotriazole diazotization coupling reation
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