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A serial of Co3O4 catalysts were prepared through a facile method of calcining of ZIF-67 at different temperatures. Physicochemical properties of the samples were characterized by the powder X-ray diffraction (XRD), thermogravimetric analysis-differential thermal analysis(TGA-DTA), scanning electron microscopy(SEM), the Brunauer-Emmett-Teller(BET) equation, H2 temperature-programmed reduction (H2-TPR) and The X-ray photoelectron spectroscopy (XPS) techniques, and their catalytic performance were investigated for the oxidation of toluene. The structural characterization certified that the calcination temperature has an important effect to catalytic activities. With the increase of the calcination temperature, the BET surface area reduces, pore size increases and the ratio of Co3+/Co2+ and Oads/Olatt firstly increase then decrease. The results showed that the conversion of toluene on the Co3O4-400 catalyst could reach 100 % when the reaction temperature was 240 oC. The Co3O4-400 catalyst presented better performance and excellent resistance to H2O, which are very important to Industrial application.