In this work, we report the synthesis and characterization of new amorphous graphene-like TiO 2 / chitosan carbon microspheres and its performance as photocatalyst. Four different carbon chitosan microspheres materials were obtained based on the distinctive procedure to incorporate TiO 2 and TiOSO 4 to chitosan structure by pyrolysis at 600 °C. Detailed characterizations were carried out using many different techniques, as thermogravimetric analysis/differential scanning calorimetry (TGA/DSC), scanning electron miscroscopy/energy dispersive X-ray spectroscopy (SEM/EDS), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), N 2 adsorption-desorption, and the obtained materials show an amorphous and a graphene-like structure, which improve the photocatalytic activity. The synthesized materials promoted a fast degradation of three micropollutants under UV-A radiation and, in all cases the degradation rate was approximately 98% at 30 min of reaction, being superior to the P-25 TiO 2 efficiency. Due to the amorphous graphene-like structure, all the materials present low adsorption capacity, the high photocatalytic efficiency can be attributed to the material structure that promotes the effective charge separation which reduces the recombination electron/hole, enhancing the photocatalytic efficiency.