溴胺酸Ullmann缩合反应工艺  

Study on Ullmann Condensation Reaction of Bromamine Acid

作　　者：费学宁[1] 杨少斌[1] 刘丽娟[1] 石博杰[1] 张宝莲[1] 

机构地区：[1]天津城市建设学院材料科学与工程系,天津300384

出　　处：《应用化学》2007年第10期1136-1139,共4页Chinese Journal of Applied Chemistry

基　　金：教育部科学技术重点资助项目(205013)

摘　　要：采用强酸阳离子交换树脂-乙醇-铜粉催化体系代替传统工艺中硫酸-水-铜粉催化体系,对溴胺酸进行Ullmann缩合反应。考察了强酸离子交换树脂用量、有机溶剂种类及反应温度等因素对反应收率的影响。结果表明,在V(乙醇)∶V(水)=9∶1介质中,在溴胺酸、铜粉存在下,树脂用量为16g/L,在70℃下反应3h,溴胺酸缩合产物收率可达94.0%。反应中所使用的离子交换树脂、铜粉和乙醇均可回收再利用,强酸离子交换树脂重复使用5次后其催化活性仍未降低;乙醇回收率可达70%～80%,铜粉的回收率可达85%～90%。The catalytic system of sulfuric acid-water-copper used in Ullmann condensation reaction of bromamine acid was replaced with a strong acid ion exchange resin-ethanol-copper system. The effect of the ion exchange resin loading, the kind of solvent, and the reaction temperature on the yield of the condensation product was investigated. The results show that the yield of the condensation product could reach 94. 0% in ethanol-water（9：1 ） at 70 ℃ after 3 h. The strong acid ion exchange resin, copper powder and ethanol could be reused under the reaction conditions. The activity of the resin was not obviously reduced after reusing 5 times, and 70% - 80% ethanol and 85% -90% copper powder in the reaction can be recovered.

关 键 词：强酸型离子交换树脂 Ullmann缩合 氨基溴蒽醌磺酸钠 C.I颜料红177中间体 

分 类 号：O625[理学—有机化学]