摘要
应用离子交换膜法通过自行设计的电解槽由邻氯苯胺电解合成制备2,2′-二氯氢化偶氮苯。讨论了电解反应温度、电流密度等因素对电解还原反应的影响。结果表明在电流密度5A/dm2,温度80℃时反应条件最佳,产率为95%。采用液相色谱跟踪产物含量变化,对照阴极电势描述整个反应过程;使用电化学工作站的循环伏安法研究反应历程,揭示了2,2′-二氯偶氮苯向2,2′-二氯氢化偶氮苯的转化是该电解反应的控制步骤,并讨论了反应前期和后期副产物的主要来源。
2,2＇-Dichlorohydrazobenzene was electrolytic synthesized from o-chloroaniline by ion-exchange membrane method with self-designed electrolyzer.The effects of electrolysis reaction temperature and current density on electrolytic reduction reaction were discussed.The results showed that the best reaction conditions were current density 5A/dm2 and temperature 80℃,the yield was 95%.The content changes of product were tracked by liquid chromatography and the whole reaction course was described based on the cathode potential.The reaction mechanism was studied by cyclic voltammetry of electrochemical workstation and revealed that the transformation from 2,2＇-dichloroazobenzene to 2,2＇-dichlorohydrazobenzene was the control step of the electrolysis reaction.The main sources of byproducts formed in the pre-and post-reaction were also studied.
出处
《染料与染色》
CAS
2010年第4期37-41,共5页
Dyestuffs and Coloration
