Dye wastewater flocculation using TiCl4 and FeSO4 coagulants was studied for organic removal and precipitation efficiency. Moreover, TiCl4 was assessed in a pilot-scale flocculation process to investigate organic removal and solution pH effect. A large amount of TiO2 was produced from sludge of Ti-salt flocculation in dye wastewater. This flocculation process simultaneously reduces a large amount of sludge produced from wastewater. The TiO2 nanoparticle was characterized in terms of physical and chemical properties. Results showed that 77.6% of organic matter was removed from dye wastewater when using FeSO4 as coagulant, while TiCl4 degraded 75.9% of organic matter. On the other hand, floc precipitation efficiency was better for TiCl4 if compared with FeSO4. The optimum concentration of TiCl4 for pilot-scale flocculation was found to be equal to 2.1 g/L. DWT (Dye wastewater titania) size was 15-20 nm, mainly doped with carbon atoms and exhibited a dominant anatase structure. DWT was similar to P-25 in decomposing acetaldehyde under UV-irradiation and complete photocatalytic degradation was achieved after 140 min.