In the article research results of formation capability of active surface Co–Mn/Al2O3/Al-frame catalysts for liquid phase oxidations xylenes in conditions of heat treatment of samples in an electromagnetic field of microwave – range are submitted. It has been determined that more intensive absorption of microwave radiation energy and it’s transformation in heat at stage of formation oxides of active metals takes place in case g-Al2O3/Al samples tnat impregnated with a mix of nitrates of cobalt and manganese thane their individual salts. And spontaneous temperature rise samples from 400 till 727 K obtains at formation of the manganese cobaltite phase. The received results are suggested that generation of active Co–Mn/Al2O3/Al catalysts surface for liquid-phase oxidation in SHF thermal treatment is reasonable for practical realization and it has more good differ from traditional thermal actions through synthesis time saving