Diacetyl (2,3-butanedione) synthesis from methyl ethyl ketone over oxidation zeolites using O-2 as oxidant was studied. Various zeolites with Fe, V and Ti as active sites were employed. VS-1,Ti-NCL, Ti-MCM-41 and FeBEA type materials were synthesized and characterized by BET, FTIR, XRD, pyridine adsorption and template desorption. The detailed study of the effect of reaction temperature, the effect of concentration of oxygen and the addition of water was realized. The most active catalyst was zeolites with V as oxidation center.