摘要
以对硝基甲苯为原料经还原、磺化两步反应合成4B酸。通过正交试验确定最佳工艺条件为磺化温度175C,硫酸与对甲苯胺的摩尔比为1.1:1,活性炭用量3 g,分出反应生成的水。在优化条件下,磺化收率达到93.7%,4B酸的总收率达到83.3%,产品纯度为98%。产品经元素分析、高效液相色谱分析证实了它的结构和纯度。
Abstract
4B acid was synthesized with p -Nitrotoluene as raw materials by reduction and sulfonation. The optimum reaction conditions were sulfofication temperature 175 C, mol ratio of sulfuric acid to ptoluidine 1.1: 1, the amount of active carbon 3 g, the water produced in the reaction process need to be separated. Under the optimum conditions, the yield of sulfofication was 93.7%, The total yield and purity of 4B acid can reach 83.3%, 98.0% respectively. The constitution and purity were confirmed by element analysis and HPLC detection.