阳离子蓝X-BL绿色合成方法研究  

Study on the green synthesis method of cationic blue X-BL

作　　者：霍二福 刘晨义 王延花 程伟琴 王攀峰 王柏楠 HUO Er-fu;LIU Chen-yi;WANG Yan-hua;CHENG Wei-qin;WANG Pan-feng;WANG Bo-nan(Henan Chemical Iudustry Research Institute Co.,Ltd.,Zhengzhou 450052,China;Pingdingshan Mingyuan Chemical Co.,Ltd.,Pingdingshan 467000,China;Fine Chemical Intermediate Engineering Technology Research Center of Henan Province,Zhengzhou 450052,China)

机构地区：[1]河南省化工研究所有限责任公司,河南郑州450052 [2]平顶山市铭源化工有限公司,河南平顶山467002 [3]河南省精细化工中间体工程技术研究中心,河南郑州450052

出　　处：《化学研究与应用》2023年第3期720-726,共7页Chemical Research and Application

基　　金：河南省科学院重大科研项目聚焦项目(210108004)资助;河南省科学院杰出青年人才培养项目(200408004)资助。

摘　　要：针对合成2-氨基-1,3,4-噻二唑产生高盐、高化学需氧量(Chemical Oxygen Demand,简称COD)废水问题,采用逆向合成法,将现用合成阳离子蓝X-BL的重氮组分和偶合组分互换:以4-(N,N-二甲氨基)氯化重氮苯为重氮组分、2-(N,N-二异丙氨基)-1,3,4-噻二唑为偶合组分合成阳离子蓝X-BL。此法减少了制备2-氨基-1,3,4-噻二唑的原料氨基硫脲的消耗量,从源头上减少高污染、高毒原料水合肼和硫氰酸铵的使用量。本文还探索采用加压的方法合成了2-(N,N-二异丙基)氨基-1,3,4-噻二唑,具有合成条件简单、绿色环保、产品纯度高、收率高等优点。实验表明,回收的反应溶剂不需要处理即可循环使用7次,高盐、高COD的废水量减少80%。In view of the problem of high salt and high COD wastewater generated from the synthesis of 2-amino-1,3,4-thiadiazole,the diazo component and coupling component of the currently used synthetic cationic blue X-BL were exchanged by reverse synthesis,4-(N,N-dimethylamino)diazobenzene chloride was used as diazo component,2-(N,N-diisopropylamino)-1,3,4-thiadiazole was used as coupling component to synthesize cation dye X-BL,which could reduce the consumption of thiosemicarbazide,hydrazine hydrate and ammonium thiocyanate.2-(N,N-Diisopropyl)amino-1,3,4-thiadiazole was synthesized under pressure,which had the advantages of simple synthesis conditions,environmental protection,high purity and yield.After many comparative experiments,it was found that the mother liquor in the reaction process can be recycled for 7 times without treatment,and the waste water with high salt and COD can be reduced by 80%.

关 键 词：2-(N N-二异丙基)氨基-1 3 4-噻二唑 阳离子蓝染料X-BL 合成新方法 

分 类 号：O625.6[理学—有机化学]