摘要
以氯苯/硫酸水溶液为电解液,在三维铜网阴极上电解2,6-二氯-4-硝基苯酚制备2,6-二氯-4-氨基苯酚。在铜微电极上用循环伏安法对其电化学行为进行研究,表明2,6-二氯-4-硝基苯酚的电还原反应是一个受扩散控制的不可逆反应。对电极材料、助溶剂的体积分数、电流密度、温度和硫酸浓度进行了单因素考察,得到最佳实验条件为:以铜网为阴极、助溶剂氯苯的体积分数为10%、电流密度为800 A/m2、温度为40℃、支持电解质硫酸浓度为2 mol/L。在该条件下,2,6-二氯-4-氨基苯酚的产率为94.8%。阴极电解液连续循环使用8次后,产率仍维持在95%左右。表明阴极电解液没有活性损失,可以被重复利用。
2,6-dichloro-4-aminophenol was prepared by the electroreduction of 2,6-dichloro-4-nitrophenol on a three-dimensional copper mesh cathode in the electrolyte composed of chlorobenzene and H2SO4 solution.The electrochemical behaviour was studied on Cu microelectrode by cyclic voltammetry,which indicated that electrochemical reduction of 2,6-dichloro-4-nitrophenol was an irreversible reaction controlled by diffusion.The influence of some key factors（such as cathode material,volume fraction of cosolvent,current density,temperature and H2SO4concentration） on the reaction was investigated.Under the optimized conditions（copper mesh cathode,chlorobenzene volume fraction of 10%,current density of 800 A/m2,temperature of 40 ℃,H2SO4 concentration of 2 mol/L）,the yield of 2,6-dichloro-4-aminophenol reached94.8%.The yield could still be maintained at about 95% after the catholyte was continuously recycled eight times,indicating that the catholyte can be reused multiple times without activity loss.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2015年第4期447-450,456,共5页
Fine Chemicals
