离子液中制备颜料红177的方法  

Synthesis of C. I. Pigment Red 177 in Ionic Liquids

作　　者：张天永[1] 李威[1] 李彬[1,2] 姜爽[1] 吕东军 费学宁[4] 

机构地区：[1]天津大学化工学院天津市应用催化科学与工程重点实验室天津化学化工协同创新中心,天津300072 [2]大连理工大学精细化工国家重点实验室,辽宁大连116024 [3]山东宇虹新颜料股份有限公司,山东德州253000 [4]天津城建大学,天津300384

出　　处：《精细化工》2014年第9期1132-1135,1139,共5页Fine Chemicals

基　　金：国家自然科学基金(21103121;21276187);教育部高等学校博士学科点专项科研基金(20110032120011);天津市应用基础与前沿技术研究计划(13JCQNJC05800);精细化工国家重点实验室开放基金(KF1101)~~

摘　　要：用离子液体([BSMIm]HSO4、[BSMIm]OTF)代替硫酸进行4,4'-二氨基-1,1'-二蒽醌-3,3'-二磺酸钠(简称DAS)脱磺酸基反应制备颜料红177,考察了离子液体的酸度、离子液体的加入量、反应时间、反应温度及离子液体的循环套用对颜料红177收率的影响。离子液体的酸度可以满足DAS脱磺酸基的酸度要求,且离子液体循环套用方便,并且减少工业废水的排放,是一种环境友好的合成工艺。较适宜的工艺条件为:2.0 g DAS,10 g[BSMIm]OTF,反应温度150℃,反应时间5 h,[BSMIm]OTF经二氯甲烷萃取提纯后可至少循环利用6次,颜料红177平均收率为92.3%。The synthesis of C. I. Pigment Red 177（ PR177） was developed by the desulfonation of 4,4＇-diamino-1,1＇-dianthraquinonyl-3,3＇-disulfonic acids（ DAS） in ionic liquids（ [BSMIm]HSO4,[BSMIm]OTF） instead of H2SO4. The influences of the acidity,dosage and recycle of ionic liquids,reaction time,and reaction temperature on the yield of PR177 were studied. The acidity of ionic liquids satisfied the acidity requirement of desulfonation of DAS. The recycle of ionic liquids was convenient,and it reduced the discharge of wastewater. The synthesis technology was environmentally friendly. The optimal reaction conditions were as follows： The dosage of DAS and [BSMIm]OTF were 2. 0 g and 10 g separately,the reaction temperature was 150 ℃,the reaction time was 5 h. Under such conditions,the recycle of ionic liquids after extraction and purification with dichloromethane was at least 6 times,and the average yield of PR177 was 92. 3%.

关 键 词：离子液体 脱磺酸基反应 颜料红177 废水减排 特种染料与颜料 

分 类 号：TQ426.94[化学工程] TQ622.1