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以邻甲苯胺、硫酸、亚硝酸钠为原料,采用重氮化-偶合反应方法制备邻氨基偶氮甲苯。分别考察了硫酸浓度、亚硝酸钠浓度、以及亚硝酸钠与邻甲苯胺的量比等因素对邻氨基偶氮甲苯收率的影响,同时考察了采用一定量回收邻甲苯胺对邻氨基偶氮甲苯收率的影响。结果表明:浓度为36%硫酸溶液、36%亚硝酸钠溶液以及亚硝酸钠与邻甲苯胺的量比为1.1∶1条件下,邻氨基偶氮甲苯的收率达到87%的最高值,纯度为95%;在偶合反应中添加30%～50%的回收邻甲苯胺,产物收率在77%左右。
With o-toluidine, sulfuric acid, sodium nitrite as raw materials, the use of diazotization - coupling reaction of o-amino-azo toluene. The effects of sulfuric acid concentration, sodium nitrite concentration and the amount ratio of sodium nitrite to o-toluidine on the yield of o-amino-azo toluene were investigated respectively. The effects of o-toluidine on the yield of o- Effect of toluene yield. The results showed that the yield of ortho-azo-toluene reached the highest value of 87% at a concentration of 36% sulfuric acid solution, 36% sodium nitrite solution and the ratio of sodium nitrite to o-toluidine was 1.1:1. The purity Was 95%. In the coupling reaction, the recovery of o-toluidine was 30% ~ 50%. The yield of the product was about 77%.