We present a facile synthesis of highly dispersed Ce and Fe metal oxide nanoparticles (NPs) with the size distribution of about 1–2 nm on reduced graphene oxide (RGO). The obtained Ce-Fe/RGO hybrid material is structurally characterized by TEM, XRD, XPS, Raman, BET, and H2-TPR. The results show that the addition of Fe promotes the formation of high surface area Ce-Fe/RGO hybrid material due to the inhibition of different species on crystal growth. The enhanced adsorption properties mainly come from the monolayer dispersion and the reduced particle size of NPs on the graphene. The driving force for the adsorption is the electrostatic action between adsorbent materials with positive electricity and CR with negative electricity, and the NPs and RGO together interact with the Congo red (CR) in the adsorption process. The Ce-Fe/RGO hybrid material exhibits a high adsorption capacity of 179.5 mg g−1 for the CR in water, suggesting their potential use in water treatment.