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The nanocomposites were obtained from commercial multi-walled carbon nanotubes (MWCNTs) and with titanium tetra propoxide as TiO 2 precursor, and heat treated at 400 C and 500 C to form crystalline phases of TiO 2 . The nanocomposites were investigated for their photocatalytic activity, employing them as catalysts in the degradation of organic methyl orange dye in an aqueous solution under UV radiation. The results were associated with the characteristics of the nanocomposite structure, using techniques such as x-ray diffraction, transmission electron microscopy, and Raman spectroscopy. Optical characterization was obtained by photoluminescence spectroscopy and diffuse reflectance spectroscopy. The highest photocatalytic efficiency was observed in the TiO 2 -MWCNT nanocomposites obtained in an acid medium and heat treated at 500 C. These results could be associated with the lower transition energy and level of defects in the TiO 2 of these nanocomposites when compared to the other samples.