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Co-Mn-Al hydrotalcite type solids were synthesized as precursors of catalysts for the total oxidation of toluene in air. For the as-prepared solids, XRD measurements indicate the coexistence of hydrotalcite and MnCO 3 phases. When calcination is performed at 500°C, different mixed oxides are found as a function of Co:Mn molar ratio and preparation method, and very high specific surface areas were obtained for the Co-Mn solids. The comparison of catalytic activities in the presence of calcined hydrotalcites with those in the presence of calcined hydroxides evidences the superiority of the first oxides due to their higher reducibility. Co-Mn-Al nano-oxides synthesized using hydrotalcite type solids as precursors, are very promising candidates for the substitution of noble metal based solids.