CMPO is safely, reliably and rapidly decomposed under mild conditions. A CMPO-containing substance is emulsified in an electrolyte comprising an oxidation promoter (silver ion) by an emulsifier in an emulsifying tank, this electrolyte comprising the CMPO-containing substance is supplied to an anode chamber, and an electrolytic oxidation reaction is performed by passing an electric current. By emulsifying the CMPO-containing substance, the surface area of CMPO in contact with electrolyte is increased, and electrolytic decomposition is thereby promoted. As sufficient CMPO decomposition is not obtained by passing the emulsion only once through an electrolysis tank 1, a batch oxidation method is employed wherein an anolyte is recirculated by a recirculating pump 3a through the anode chamber, a constant temperature bath 7a and an emulsifying tank 6, so that electrolysis is performed with the CMPO-containing substance permanently emulsified in the electrolyte. To maintain a catholyte in a cathode chamber at the same temperature as the anolyte, the catholyte is recirculated by a recirculating pump 3b between the cathode chamber and a constant temperature bath 7b. The current supplied to an anode 4 and cathode 5 in the electrolysis tank 1 is controlled by a rectifier 8.