The catalytic properties of FeSO 4, nanocluster ferro-molybdenum polyoxometalate { Mo 72 Fe 30} and nanocluster molybdenum polyoxometalate { Mo 132} have been studied during the oxidation of phenol in ethanol-isobutanol solution with persulfate. To determine the oxidation products, phenol, ethanol and isobutanol of an acidic nature, sulfonic cation exchanger KU-2 (the grade of ion exchange resin established by the state standard of the Russian Federation GOST 20298-74) was added to the reaction mixture in each experiment to catalyze the esterification reaction of acid oxidation products with the initial alcohols. Acid esterification products were identified by the vapor-phase chromatography method with a mass spectroscopic detector. According to the conversion of phenol, ethanol and isobutanol, the catalytic properties of a homogeneous FeSO 4 catalyst (similar to Fenton's reagent) with heterogeneous catalysts (polyoxometalates) were compared. These data suggest the possibility of further searching for heterogeneous catalysts containing Fe and Mo in their composition during the destruction of phenol by peroxide compounds.