The invention relates to a heterogeneous Fe-Ce fenton-like catalyst and a preparation method and use thereof, belonging to the technical fields of catalyst preparation and application. The preparation method comprises the following steps: (1) preparing a mixed solution of ferric nitrate, cerium nitrate and oxalic acid; (2) repeatedly dipping granular activated alumina into the mixed solution obtained in the step (1), filtering, washing and drying; (3) putting the material obtained in the step (2) into a muffle furnace for calcining to obtain the heterogeneous Fe-Ce fenton-like catalyst. A fenton-like reaction system formed by the heterogeneous Fe-Ce fenton-like catalyst and hydrogen peroxide can be used for carrying out catalytic degradation on high-concentration p-nitrophenol waste water efficiently under UV-irradiation; the heterogeneous Fe-Ce fenton-like catalyst has the advantages of being low in synthesis temperature, simple in preparation technology, lower in cost, large in specific surface area, narrow in pore size distribution, high in catalytic activity, wide in pH application scope, etc.