This study examines the treatment of Naphthol-Blue-Black (NBB) dye and real textile wastewater through sonophotocatalytic technique. Fe, TiO2 and Fe-TiO2 were synthesized and characterized by SEM, XRD and DRS which revealed its high purity, good doping, nanosize and higher light absorption capacity. The effect of pH, gas content (Ar, O-2, air and N-2), H2O2 concentration and catalyst loading were examined. The maximum color removal was observed for initial pH 11, argon gas bubble, 44.1 mmol/L H2O2,3 g/L Fe, 4 g/L TiO2 and 2.2 g/L Fe-TiO2. However, 96% was achieved by sonophotocatalytic process for 2.2 g/L 1:7 Fe:TiO2. Similar methodology for real textile wastewater with Fe-TiO2 (1:7) could remove 91% of TOC. (C) 2015 Elsevier B.V. All rights reserved.