化工学报2017,Vol.68Issue(1):146-153,8.DOI:10.11949/j.issn.0438-1157.20161009
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
摘要
Abstract
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(23μm) was optimal with the best catalytic performance. The highest content and yield of DAS was 91.56%and 88.43%, respectively.关键词
溴氨酸/溶剂/Ullmann偶联反应/合成/催化/阳离子交换树脂/铜粉Key words
bromamine acid/solvent/Ullmann coupled reaction/synthesis/catalysis/cation exchange resin/copper powder分类
化学化工引用本文复制引用
张天永,朱少迪,李彬,刘茜,海莉,张光辉,张夏,吕东军..有机溶剂中合成4,4'-二氨基-1,1'-联蒽醌-3,3'-二磺酸[J].化工学报,2017,68(1):146-153,8.基金项目
国家自然科学基金项目(21276187);天津市自然科学基金项目(16JCYBJC20800);天津市科技创新平台计划项目(14TXGCCX00017)。 ()