In order to more easily separate TiO 2 photocatalyst from the treated wastewater, TiO 2 film was immobilized on the surface of activated carbon fibers (ACFs) by employing two kinds of coating procedures, dip-coating, and hydrothermal treatment. The effects of coating procedures on microstructure of TiO 2 -coated ACFs (TiO 2 /ACFs), such as morphology, porous property, crystal structure, and light absorption characteristics were investigated in detail. The adhesion property between TiO 2 film and ACFs was evaluated by ultrasonic vibration, and the photocatalytic activity of TiO 2 /ACFs was tested by the photocatalytic decoloration of methylene blue solution. The results show that hydrothermal treatment presented many advantages to obtain high-performance TiO 2 /ACFs photocatalyst in comparison with dip-coating. Hydrothermal treatment could improve the binding property between TiO 2 films and ACFs, which endowed the as-obtained TiO 2 /ACFs photocatalyst with improved reusable performance, and TiO 2 /ACFs synthesized by hydrothermal treatment presented higher photocatalytic activity.