对硝基甲苯邻磺酸合成新工艺  

A Novel Process for Synthesizing p-Nitrotoluene-o-sulfonic Acid

作　　者：秦丽红[1] 张凤宝[1] 张国亮[1] 覃志忠[1] 

机构地区：[1]天津大学化工学院,天津300072

出　　处：《染料与染色》2006年第2期31-33,43,共4页Dyestuffs and Coloration

摘　　要：以对硝基甲苯为原料,50%发烟硫酸作为磺化剂,废硫酸作为稀释剂制备对硝基甲苯邻磺酸。反应经磺化、保温达终点后,冷却,结晶和过滤,部分滤液作为稀释剂循环使用于制备过程中,该工艺对硝基甲苯邻磺酸收率可达98.9%以上。与采用20%发烟硫酸磺化相比,此过程的50%废硫酸生成量减少了75%左右。对反应温度、时间、原料配比及废酸回用量等影响反应的因素进行了研究,确定了适宜的反应条件90℃时磺化反应60min,110℃时保温60min,n(pNT)∶n(SO3)=1.0∶1.1、m(回用废酸)∶m(50%发烟硫酸)=1∶1。p - Nitrotoluene - o - sulfonic acid, a key intermediate for whitening agents, was prepared from p - nitrotoluene via sulfonation by using 50% oleum as sulfonation agent and waste sulfuric acid as diluted agent, as well as heat transfer medium. After the reactive mass was crystallized and filtrated, a certain amount of filtrate was reused in the sulfonation and the residue was hydrolysed to obtain the NTS dissolved. The yield of NTS could reach to 98.9% while the amount of 50% waste sulfuric acid aqueous solution could be reduced 75% approximately, with the comparison of the conventional procedure using 20% oleum as the sulfonation agent. The dependence of temperatures, time, ratio of raw materials and the amount of waste sulfuric acid added on the yield was investigated, and the proposed optimum conditions were to conduct the sulfonation 60min at 90℃, to maintain the sulfonation mixture 60min at 110℃, p - Nitrotoluene： SO3 = 1.0 ： 1.1, and the amount of waste sulfuric acid reused ： 50% oleum = 1 ： 1.

关 键 词：对硝基甲苯 对硝基甲苯邻磺酸 磺化 废硫酸 50%发烟硫酸 

分 类 号：TQ247[化学工程—有机化工]