UDC 544.65 A method is developed for separating nickel-copper alloy by electrolysis of crushed nickel matte in sulfuric acid solution to obtain a cathode precipitate, an electrolyte solution saturated with nickel, and sulfur-sulfide sludge. A distinctive feature of this work is use of a bulk anode formed by crushed matte particles with a size of 0.5-5 mm. Nickel matte is formed by nickel phase Ni 3 S 2 and precipitates of Ni-Ni 3 S 2 eutectic 10-40 μm in size. Nickel metal also occurs at particle boundaries in the form of localized inclusions. The possibility of conducting anodic dissolution of crushed nickel matte in the form of a bulk anode and cathodic reduction of compact nickel-copper deposit in one electrolysis bath is confirmed by experiment. It is found that dissolution of metallized phase occurs most intensively from a particle surface. Electrolysis regimes are determined. With a sulfuric acid concentration in the electrolyte of 10 g/dm 3 , a bath voltage of 2.2-2.5 V, and an anode current density of 25 A/m 2 , anodic current efficiency of 87% is achieved. As a result of electrolysis of nickel matte with the parameters selected a compact nickel-copper deposit with a nickel content of more than 90% may be obtained on the cathode.