Abstract:MoV0.31Te0.23Nb0.24 oxide catalysts for propane ammoxidation were synthesized by co-precipitation method under different calcination atmosphere conditions. The effects of calcination atmosphere on the physicochemical properties of the catalysts were investigated. The catalysts were characterized by X-ray diffraction (XRD), Raman Spectrum and X-ray photoelectron spectroscopy (XPS). The catalytic performance was evaluated using propane ammoxidation to acrylonitrile as a model reaction. The results showed that the obtained catalyst exhibits good performance on propane ammoxidation under an inert atmosphere of nitrogen in the calcination process. This was because, under the nitrogen atmosphere, the elements constituting the catalyst formed an appropriate distribution of the active phases of M1 and M2 in a reasonable valence state during the calcination process. That significantly enhanced the catalytic performance for propane ammoxidation: propane conversion was up to 58.7%, and acrylonitrile selectivity was up to 35.0%. Under air and oxygen atmosphere during the calcination, simple oxides were formed in a higher valence state, which was not in favor of the selective oxidation of propane to acrylonitrile.