Preparation of titania compounds by double-reductive hydrochloric acid leaching of ilmenite concentrate is reported. A rod-shaped nanostructure titania compound was obtained via centrifugation of leach liquors as a by-product. The liquors of leaching experiments were subjected to zetasizer test. The suspended particles in leach liquors were investigated using SEM and TEM analysis. The results revealed that the rod-shaped particles were smaller than 100 nm in width. The XRD analysis verified the formation of rutile and pseudorutile phases as main phases. Regarding to the XRF analysis, The TiO2 content of ilmenite increased from 33% in ilmenite concentrate to about 80% in the products containing some constituents such as Fe2O3, SiO2 and Al2O3. (C) 2013 Elsevier B.V. All rights reserved.