Ilmenite type titanates have, very wide applications in 'various' fields. In this, paper, we report the synthesis of mesoporous NiTiO3 ilmenite nanorods via a sonochemical approach. The method is vety facile and effective allowing the preparation of NiTiO3 nanopartides with a high yield and uniform size distribution. The reaction intermediate and particularly the final product have been well characterized by various analytical tools (IR, XRD, Raman; TEM, BET, XPS). The final NiTiO3 nanopartides can be described as a hierarchical structure Composed of small nanopartides interconnected generating nanoporous rods. In comparison With anatase TiO2 nanopartides, the catalytic removal rate for the pollutant Tergitol (NP-9) by a process combined with zonation is two and half-fold higher in the presence of mesoporous NiTiO3 ilmenite nanorods.