Waste treatment was studied in the electroless nickel plating line. “COD constituents” in the waste solution such as hypophosphite, phosphite, and organic compounds were oxidized completely by hypochlorite in the presence of a small amount of Cu+/Cu2+ redox catalyst in the form of the chloro complex. Phosphates and sulfates are precipitated by adding calcium salt. The filtrate is mixed with caustic soda to precipitate metal hydroxide, mostly nickel hydroxide. The reaction is simple and fast, and the process is relatively cheap compared to conventional procedures.