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。
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
m-toluidine
diazotization
hydrolysis
m-cresol
