An investigation on the recovery of nickel from spent electroless plating solutions has been performed using the electrowinning method. For this aim, nickel in spent electroless plating solutions was separated as nickel hydroxide through the addition of caustic soda. Nickel hydroxide was completely dissolved with sulfuric acid and an electrolysis was performed for electrowinning of nickel from nickel solutions. As a result, it was found that more than 99% of nickel in spent electroless plating solutions could be precipitated as nickel hydroxide above pH 10 with the addition of caustic soda. As far as the current efficiency in electrowinning of nickel was concerned, it was decreased with increase in the current density.