Novel TiO 2 /carbon nanocomposites were prepared through the pyrolysis of TiO 2 /poly(furfuryl alcohol) hybrid materials, which were obtained by the sol–gel method, starting from titanium tetraisopropoxide (TTIP) and furfuryl alcohol (FA) precursors. Six different TiO 2 /C samples were prepared based on different TiO 2 nanoparticle sizes and TiO 2 /FA ratios. All of the samples were characterized using X-ray diffraction, infrared, and Raman spectroscopy. The results indicated effective FA polymerization onto the TiO 2 (anatase) nanoparticles, polymer conversion to disordered carbon following the pyrolysis, and a simultaneous TiO 2 anatase–rutile phase transition. The resulting TiO 2 /carbon composites were used as photocatalysts in the advanced oxidative process (AOP) for the degradation of reactive organic dyes in aqueous solution. The results indicate excellent photocatalytic performance (degradation of 99% of the dye after 60min) with several advantages over traditional TiO 2 -based photocatalysts.