In this report, a serie of the pillared interlayered clays by polyoxocation of mixed metals (Bent-Al-Fe (9/1), Bent-Al-Cu (9/1) and Bent-Al-(Fe+Cu) (9/1), (9/1 is the molar ratio of Al and other sulstituted metal(s) ) was prepared by intercalation of corespondant polyoxocations in the bentonite Dilinh sheets and then calcinated at temperature of 450°C for 4h. The structural and textural properties of obtained products were characterized by physical methods: XRD, IR, DTG-DTA, SEM, TEM and BET. The results obtained results showed that the pillared interlayered bentonite was successful synthesized. The catalyticaI activity of obtained solids was evaluated by the total oxidation of the phenol in aqueous solution with H2O2 in different conditions. The results experimental showed that these catalysts represent a high activity in the phenol conversion into CO2 and H2O.