With increasing importance of the electroless nickel plating technology in many fields such as electronic and automobile industries, the treatment of the spent baths is becoming a serious problem. The spent baths are currently treated by the conventional precipitation method, and nickel in these baths is not recovered. We are developing a recycling process of nickel in the spent baths using solvent extraction (Fig. 1). Nickel in the spent baths is efficiently extracted by a hydroxyoxime reagent at a pH higher than 6 and is readily stripped with sulfuric acid. The impurity metal ions (iron and zinc) are selectively extracted with organophosphorous reagent before extracting nickel.