TiO2@(AC/Fe3O4) (AC is activated carbon) was prepared by using AC and Fe3O4 as joint support. The morphological features, crystal structure, and magnetism of the final product were characterized. The results indicate that TiO2 particles formed on the surface of AC and Fe3O4; the sizes of TiO2 and Fe3O4 were 0.5 and 0.7 μm respectively, and that of AC fell within a wide range. The highly crystalline cubic structures of the TiO2 particles was in accord with the standard X-ray diffractometry spectrum of magnetite and anatase. The maximum saturation magnetization of TiO2@(AC/Fe3O4) was 75 emu g−1, which was enough to support magnetic recovery. The rate of methylene blue (MB) removal photocatalyzed by TiO2@(AC/Fe3O4) was higher by 50% than that achieved with AC/Fe3O4 photocatalysis, and similar to that achieved with TiO2@AC. The removal rate (kobs) decreased drastically from 1.77 × 10−2 to 9.36 × 10−3min−1 when the initial concentration of MB solution increased from 2.0 to 5.0 mg L−1. The kobs value increased from 9.41 × 10−3 to 1.34 × 10−2min−1 with increasing photocatalyst dosage from 0.2 to 1.0 g, then slightly decreased to 1.33 × 10−2min−1 at 2.0 g dosage.

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