The Catalytic Wet Oxidation (CWO) method was investigated to treat phenol cleaning wastewater from chemical container which is difficult dispose with traditional biological methods. In this paper, high-efficiency catalysts were prepared, two methods were used to prepare the catalyst: impregnating, sol-gel. Effects of metal salts concentration, calcination temperature and calcination time on each catalysts performance were explored and optimal catalyst preparation condition was optimized. The results show that the optimum sol-gel condition: Cu / Mn / Ce ratio of 2:2:2, the calcination temperature is 700 °C, calcination time is 5h.; the optimum impregnating condition: Cu / Mn / Ce ratio of 2:2:2, impregnated carrier (AC) of 0.9g/L mixture, the calcination temperature is 300 °C, calcination time is 4h; the sol-gel catalyst has longer service life, the samples prepared by impregnating technique were more active than the samples prepared by sol-gel technique at given reaction conditions.