Plating industry is one of the largest polluting small scale industries and nickel plating is among the important surface finishing process in this industry. The waste generated during this operation contains toxic nickel. Nickel removal and recovery is of great interest from spent bath for environmental and economic reasons. Spent electroless nickel solution from a reed relay switch manufacturing industry situated in Chennai was taken for electrolytic recovery of nickel. Electrolytic experiment was carried out with mild steel and gold coated mild steel as cathode and the different parameters such as current density, time, mixing and pH of the solution were varied and recovery and current efficiency was studied. It was noticed that there was an increase in current efficiency up to 5 A/dm2 and after that it declines. There is no significant improvement with mixing but with modified cathode there was some improvement. Removal of nickel from the spent electroless nickel bath was 81.81% at 5 A/dm2 and pH 4.23. Under this condition, the content of nickel was reduced to 0.94 g/L from 5.16 g/L. with 62.97% current efficiency.