In this work composites based on Activated Carbon (AC) and TiO2 were synthesized by sol-gel method (containing 10 and 20 of TiO2, w%) using glycerol as source of carbon. These materials were used as photocatalysts for the removal of phenol in seawater. The photocatalysts were characterized by: Adsorption-Desorption of N2, Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), Infrared Spectroscopy (FTIR), and X-Ray Photoelectronic Spectroscopy (XPS). The photocatalytic test were carried out under UV-C light (254 nm) and Visible light (320−700 nm). The AC-TiO2 composites showed a high surface area, in special AC which reported 1900 (m2. g−1). The TiO2 contained in the composites corresponds to the crystalline form of Anatase. The addition of TiO2 to AC sensitized the material. The AC-TiO2 composites are good photocatalyst for the removal of phenol in seawater, they were superior to the commercial TiO2 (in both situation: under UV and Visible light). The presence of salts of seawater did not affect the heterogeneous photocatalysis under UV light, significantly; moreover, it was benefic under Visible light. In the photocatalysis, the best AC-TiO2 composite removed up to 70 mg of phenol.gcat−1 under UV-C light, and 55 mg of phenol.gcat−1 under Visible light. According to our results, the AC-Ti composites showed promising properties for applications in the removal of organic compounds in seawater. The mechanism, photocatalyst reuse, the effect of scavenger and seawater salts are discussed.