分散蓝WF-PTS的合成工艺研究

Research on Synthesis of Disperse Blue WF-PTS

本文介绍了以2,4-二硝基-6-溴苯胺与3-(N,N-二烯丙基)氨基-4-甲氧基乙酰苯胺为原料合成分散蓝WF-PTS的工艺,并用高分辨率质谱对其结构进行了表征。通过对反应温度、氰化亚铜用量、溶剂用量、析出条件等进行单因素实验分析,确定了最佳反应条件:中间体染料∶氰化锌=1∶0.5,氰化亚铜用量为中间体染料投料量的1.1%,溶剂为DMF,用量为80 m L(中间体染料投料量为0.1 mol时),升温到100℃反应2 h,自然降温至60℃时滴加100 m L甲醇,加完后再自然降温至室温,搅拌30 min,过滤,用清水洗涤,得到染料粗品。得到的粗品染料再进行除毒处理后,便得到分散蓝WF-PTS滤饼。得到的产品HPLC在97%左右,收率在88%以上。经性能测试,产品具有优异的耐水洗牢度和耐升华牢度。

Disperse Blue WF-PTS was synthesized from 2,4-dinitro-6-bromoaniline and 3- （ N, N-diallyl） amino-4-methoxy-N-aeetylani- line, and its structure was characterized by HR-MS. Based on the single factor experiments such as reaction temperature, dosage of cu- prous cyanide, dosage of solvent, and precipitation conditions, the optimum reaction condition was confirmed： intermediate dye： zinc cyanide = 1 ： 0. 5, cuprous cyanide with amount of 1.1% intermediate dye in weight, solvent DMF 80 mL （in case of 0. 1 mol interme- diate dye） ; reacting at 100~C for 2 h, natural cooling to 60~C and dropping methanol 100mL, after natural cooling to room temperature, stirring for 30 min and filtering, washing with water to get crude dye; Disperse Blue WF-PTS filter cake was obtained by harmlessness treatment of the crude dye. The content （HPLC） of product was about 97%, the yield was above 88%. The product presented excellent washing fastness and sublimation fastness by the performance test.