Novel TiO2/carbon nanocomposites were prepared through the pyrolysis of TiO2/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 TiO2/C samples were prepared based on different TiO2 nanoparticle sizes and TiO2/FA ratios. All of the samples were characterized using X-ray diffraction, infrared, and Raman spectroscopy. The results indicated effective FA polymerization onto the TiO2 (anatase) nanoparticles, polymer conversion to disordered carbon following the pyrolysis, and a simultaneous TiO2 anatase-rutile phase transition. The resulting TiO2/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 60 min) with several advantages over traditional TiO2-based photocatalysts. (C) 2011 Elsevier Inc. All rights reserved.