This work intends to evaluate photocatalytic properties of Peruíbe 's Black Mud, in the phenol degradation process by heterogeneous-photocatalysis. The Black Mud was tested as a catalyst in this process, pure and also doped with commercial TiO2. Three conditions were tested: in the dark, in the presence of UV-C radiation (UV-C, 254 nm), and in the presence of H2O2 plus UV-C light (UV-C, 254 nm; Fotofenton). The catalysts were characterized by XRD, EDX and Fourier FTIR. The reaction was monitored by UV-Vis Spectroscopy. The tests indicate that Black Mud presents photocatalytic properties for degradation of phenol in aqueous medium; this property is improved by the doping of TiO2 in low concentrations (10%w/w).