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 by chlorobenzene and H2SO4 solution. The electrochemcial 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. Influence of some key factors (such as cathode material, volume fraction of cosolvent, current density, temperature and H2SO4 concentration) on this reaction was investigated. Under the optimized condition, the yield of 2,6-dichloro-4-aminophenol reached by 94.8%. The yield could still be maintained at about 95% after the catholyte was continuously recycled eight times, indicating the catholyte can be reused multiple times without activity loss.