离子液中制备颜料红177的方法

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

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：2.0g DAS，10g [BSMIm]OTF，反应温度150℃，反应时间5h，[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%。

Abstract:

The synthesis of the 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, reaction temperature on the yield of PR177 were studied. The acidity of ionic liquids satisfied the acidity requirement of desulfonation of the 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 2.0g and 10g separately, the reaction temperature was 150℃, the reaction time was 5h, the number of recycle of ionic liquids after dichloromethane extraction was 6, the average yield of PR177 was 92.3%.