The present work describes the preparations of active carbon (AC) - titania composites with different AC/TiO2 ratio, their characterization using XRD, BET and SEM and evaluation of adsorption capacity and photocatalytic activity in aqueous solution using azo-dye Acid Orange 7 (AO7). Composite materials based on AC/TiO2 were prepared from commercial active carbon (1737 m(2) g(-1)) and TiO2 (P25, 45 m(2) g(-1)) materials by the mixing method. The studied parameters were the ratio of AC/TiO2, hydrothermal treatment and milling of as-prepared composites. The composites show increased BET surface area proportional to the content of AC in the material. The disappearance of AO7 is due to the combination of two processes, e.g. adsorption and photocatalytic oxidation which take place in parallel. Thus the overall removal of AO7 has been corrected on adsorption (measured in dark) to obtain the rate of AO7 disappearance due to photocatalytic oxidation (PO). The optimum ratio of AC/TiO2 was found to be 0.23 where PO rate is only slightly lower than that for P25 and overall AO7 removal is twice higher than for P25 itself. The less intensive (low-frequency) milling of the composite results in the decrease of carbon particle size, increase in AO7 adsorption and decline in the PO of AO7. More intensive milling (high-frequency) results in the decrease of the anatase content, appearance of the small amount of brookite and almost negligible PO rate of AO7. Irradiation of low-frequency milled AC/TiO2 composite in aqueous suspensions resulted in the generation of a comparable concentration of hydroxyl radical spin-adduct ((DMPO)-D-center dot-OH) as non-milled composite, high-frequency milled composite revealed substantially lower (DMPO)-D-center dot-OH concentration which can be explained by the increased concentration of carbon-centered radicals in AC acting as scavengers of photogenerated electrons.