Hybrid TiO2/microcrystalline cellulose (MC) nanophotocatalyst was prepared in situ by a facile and simple synthesis utilizing benign precursors such as MC and TiCl4. The as-prepared nanocomposite was characterized by XRD, XPS, BET surface area analyzer, UV-vis DRS and TGA. Surface morphology was assessed by the means of SEM and HR-TEM. Statistics-based factorial design (FD) was adopted to investigate the effect of precursors concentrations and therefore to optimize the nanocomposite synthesis through catalytic adsorption of methylene blue (MB) from aqueous solutions. The results indicated that TiO2/MC nanocomposites were photocatalytically active in diminishing 40-90% of MB in 4 h. (C) 2011 Elsevier Ltd. All rights reserved.