Porous nanocrystalline carbon and nitrogen (CN)-doped TiO2 photocatalyst was prepared using carbon tetrachloride and polyaniline as precursors. The obtained powders were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, and gravimetric analysis. The purpose of this work was to explore the state and location of nitrogen and carbon atoms introduced inside the TiO2 lattice and to study the exploitation of the photocatalytic activity of the CN-doped TiO2 for application in phenol degradation under UV illumination. After 30 min from the illumination onset, 64% and 57% of the phenol were degraded when the CN-doped TiO2 and TiO2 catalysts were used respectively.