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A novel fly ash cenospheres (FACs)-supported CeO2 composite (CeO2/FACs) was successfully synthesized by the modi-fied pyrolysis process. The prepared composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and diffuse reflection spectra (DRS) techniques. XRD results indicated that the CeO2 film coated on cenospheres was a face-centered cubic structure. SEM images confirmed that the CeO2 film was relatively com-pact. XPS results showed that Ce was present as both Ce4+and Ce3+oxidation states in CeO2 film coated on FACs substrate. The bandgap of the composite was narrower compared with the pure CeO2. The as-prepared material exhibited good photocatalytic activ-ity for the decolorization of methylene blue (MB) under visible light irradiation, and the first-order reaction rate constant (k) of 0.0028 min–1 for CeO2/FACs composite was higher than 0.0015 min–1 of pure CeO2. The fact that they floated on water meant that CeO2/FACs composites were easily recovered from water by filtration after the reaction. The recycling test revealed that the compos-ites were quite stable during the MB photocatalytic decolorization. The CeO2/FACs catalyst was therefore promising for practical use in the degradation of pollutants or water cleanup.

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