Abstract.The Fe-Co-Ce composite catalysts were prepared by co-precipitation method, and the effect of calcination temperature and calcination time on the performances of the Fe-Co-Ce composite catalysts were investigated. The results indicated that the optimum calcination temperature and calcination time of the Fe-Co-Ce composite catalysts were 450 °C and 7 h, respectively. Using the catalysts which prepared under the optimum calcination conditions catalytic wet oxidation of methyl orange simulated wastewater, after 90 min, the COD, COD removal rate, absorbance, decolorization rate and pH of the methyl orange simulated wastewater were 737.7, 70.5%, 0.348, 95.3%, and 5.31, respectively. According to the analyses of the SEM, FTIR, and TG-DTA curves, the components of the catalysts which prepared under the optimum calcination conditions distributed evenly, and the chemical compositions of the catalysts including C-O, -OH, and H-O-H, showing a good thermal stability.