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机构地区:[1]天津大学化工学院,天津300072
出 处:《天津大学学报》2006年第1期45-48,共4页Journal of Tianjin University(Science and Technology)
基 金:天津市自然科学基金资助项目(023802311).
摘 要:对碱性水介质中空气氧化对硝基甲苯邻磺酸(NTS)合成4,4’-二硝基二苯乙烯-2,2’-二磺酸(DNS)的工艺进行了改进.改进的工艺包括:NTS氧化反应液不进行中和而直接冷却结晶获得DNS产品,而过滤得到的碱性母液部分循环回用于DNS合成.采用高效液相色谱对NTS氧化过程和反应液降温冷却过程进行了跟踪.实验结果表明,冷却过程中DNS损失小于0.5%;碱性母液部分多次循环回用后,DNS产品收率稳定在87%以上,产品晶体纯度下降小于0.7%.从经济性和环境效益考虑,该工艺适于工业生产.An improved process of oxidation of 4-nitrotoluene-2-sulfonic acid (NTS) to 4, 4′-dinitrostilbene-2, 2′-disulfonic acid(DNS) in aqueous alkali medium was studied. The process included separating DNS crystal directly from the reaction-finished reactants by cooling instead of neutralizing, and then recycling the alkaline mother liquid to the next oxidation process. High efficiency liquid chromatography(HPLC) was employed to detect the content of NTS and DNS during cooling and oxidation courses. The experimental results show that the loss of DNS is less than 0.5% during the reactants cooling step, and the DNS yield is steady at 87% and the product purity decrease by less than 0.7% after the alkaline mother liquid having been recycled for many times. The improved process is appropriate to industrial production for its economic effectiveness and environmental benefit.
关 键 词:4 4′-二硝基二苯乙烯-2 2′-二磺酸合成 碱性母液 循环回用
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