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Preparation ofphotocatalytic regenerationable activated carbon (AC) is the key step for the practical application of in situ regeneration of exhausted AC. A novel photocatalytic regenerationable AC was prepared by sol-gel TiO2 in this work. The adsorption and regeneration performance of TiO2/AC were evaluated using phenol as model compound. Scanning electron microscope (SEM)and nitrogen (77 K) adsorption isotherm were used to determine the surface area, pore structure and the distribution of TiO2. The results showed that with the increase of TiO2 loading, adsorption capacity of TiO2/AC decreased and the regeneration efficiency increased. The photocatalytic regenerationable AC with suitable TiO2 loading (2 wt%) exhibited suitable adsorption capacity and regeneration efficiency. TiO2 located mainly in the entrance of macro-pore of carbon. The prepared TiO2/AC exhibited similar surface structure and pore structure with material carbon.