It has been shown that aliphatic and aromatic disulphides are oxidized by hydrogen peroxide in the presence of sodium tungstate and molybdate and an interphase catalyst to the corresponding thiolsulphonates and disulphones. The structure of the oxidation products depends on the interphase catalyst used: in the presence of triethylbenzylammoniumbromide, thiosulphonates are formed, while in the presence of cetyltrimethylammoniumbromide, disulphones are formed. The main reason for this difference is the solubility in the organic phase of the intermediate peroxy complex formed by the reaction of hydrogen peroxide with the metal compound in the presence of phosphoric acid. The rate of the reaction and the yields of oxidation products depend on the temperature, the solvent used and the ratio of the reactants.