The aim of this study was to evaluate and compare the adsorption and photocatalytic activity of activated carbon-based photocatalysts. Titanium dioxide (TiO2) and zinc oxide (ZnO) were chosen as semiconductors to prepare composites with activated carbon by the wet impregnation method. Activated carbon was prepared using as starting material onion leaves (Allium fistulosum) and as activating agent phosphoric acid (H3PO4). Photooxidation and batch adsorption of phenol was studied to compare the efficiency of the materials prepared. The results showed that the composite AC–TiO2 has a greater photocatalytic activity and a better adsorption capacity compared to AC–ZnO composite.