The reduction/reoxidation mechanism of a multicomponent molybdate catalyst for propylene ammoxidation was studied by using X-ray powder diffraction (XRD), Laser Raman spectroscopy (LRS) and thermogravimetric analysis methods. XRD and LRS results of the catalysts with various reduced degrees show that catalyst reduction happens in the order: (2)->(3)->(4)->(5), and the lattice oxygen migration range is extended from iron molybdates to cobalt/nickel molybdate. The thermogravimetric analysis results show that the reoxidation of the catalyst is attributed to the replenishment of the bulk lattice oxygen in the lower temperature which is respectively combined with Bi, Fe and Mo. and the replenishment of the surface lattice oxygen in the higher temperature. The favorable reoxidation temperature is found to be around 440 degrees C. (C) 2009 Elsevier B.V. All rights reserved.