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重氮化-水解法合成间甲酚的工艺研究

Study on Process of Synthesizing m-Cresol by Diazotization and Hydrolysis of m-Toluidine

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【作者】 梁荣宁叶庆国

【Author】 LIANG Rong-ning,YE Qing-guo(College of chemical engineering,Qingdao University of Science & Technology,Qingdao 266042,Shandong,China)

【机构】 青岛科技大学化工学院青岛科技大学化工学院 山东青岛266042山东青岛266042

【摘要】 间甲酚是一种重要的精细化工中间体,以间甲苯胺为原料,采用重氮化-水解法制备高纯度间甲酚,通过正交实验和单因素实验对重氮化反应工艺条件进行了优化。实验结果表明该反应的最佳反应条件为:硫酸与间甲苯胺的摩尔比为2.8:1,硫酸溶液浓度为35wt%,采用顺式加料法滴加27wt%的亚硝酸钠溶液,加料时间为40min。在最佳条件下重复实验,间甲酚收率可达85.2%,纯度99.5%。采用GS-MS对其结构和含量进行了表征。

【Abstract】 The m-cresol is an important intermediate of synthesizing many fine chemical products.The diazotization and hydrolysis process was used to synthesize high-purity m-cresol using m-toluidine as the main material.The reaction conditions were optimized by orthogonal design and single factor design.It indicated that the optimal conditions as follows:n(sulphuric acid)∶n(m-toluidine)=2.8∶1,the concentration of sulphuric acid solution 35wt%,ordinal method in adding 27wt% NaNO2 solution,the adding time 40min.The yield of m-cresol could reach 85.2% under those optimized conditions and the purity was 99.5%.The configuration and contents were characterized by GS-MS.

【关键词】 间甲苯胺重氮化水解间甲酚
【Key words】 m-toluidinediazotizationhydrolysism-cresol
  • 【文献出处】 化工中间体 ,Chemical Intermediates , 编辑部邮箱 ,2008年03期
  • 【分类号】TQ243.1
  • 【被引频次】8
  • 【下载频次】662
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