有机溶剂中合成4,4＇-二氨基-1,1＇-联蒽醌-3,3＇-二磺酸

Synthesis of 4,4'-diamino-1,1'-dianthraquinone-3,3'-disulfonic acid in organic solvent systems

研究了在有机溶剂体系中催化溴氨酸进行Ullmann偶联反应合成4,4'-二氨基-1,1'-联蒽醌-3,3'-二磺酸(DAS)的工艺。有机溶剂可回收利用,大大减少了工业生产技术中含酸含盐废水的排放,并降低处理费用。考察了单一溶剂、不同组成和比例的混合溶剂对Ullmann偶联反应的影响,确定最优的溶剂体系为DMF:甲醇=1:2的混合溶剂;研究了最优溶剂体系下的反应时间、温度等因素的影响。对不同添加剂和铜粉粒径对反应的影响进行研究,阳离子交换树脂为最佳添加剂,23μm铜粉催化效果最优。所得DAS的含量最高为91.56%,收率最高为88.43%。

Organic solvent systems for synthesizing 4,4＇-diamino-1,1＇-dianthraquinone-3,3＇-disulfonic acid（DAS）by Ullmann coupled reaction were investigated. Organic solvent can be recycled to avoid significant emissions of acidic and salty wastewater produced in the industrial synthetic methods. The effects of different kinds of single solvents, mixed solvent with different composition and proportion were studied. The results showed that the mixed solvent system of DMF：methanol = 1：2 was the best. The experiments to find out the optimal factors such as reaction time, temperature were conducted. The influence of additives and different particle sizes of copper powder was researched.The results indicated that the cation exchange resin can improve the content and yield of DAS and can be easily separated from the reaction system. The copper powder（23 μm） was optimal with the best catalytic performance. The highest content and yield of DAS was 91.56% and 88.43%, respectively.