Abstract: Rutile titania (TiO₂) was successfully prepared via hydrolysis of TiCl₄ in the presence of AlCl₃. The powders were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and Brunauer−Emmett−Teller (BET) surface area analysis. In the present system, AlCl₃ functions as a nucleating agent and induces the formation of rutile TiO₂. The influences of HCl and isopropanol concentrations on the purity and morphology of the rutile TiO₂ were investigated. The purity of the rutile TiO₂ increased with increasing concentration of HCl. Evenly dispersed rutile TiO₂ particles with a spherical morphology were obtained when the HCl and isopropanol concentrations were 0.5 and 1 mol·L^−l, respectively. Furthermore, the prepared TiO₂ powders were used in adsorption tests of the heavy metal pollutant Cr(VI). Rutile TiO₂ sample S-9 demonstrated greater adsorption performance and a removal efficiency that was greater than 99.95% after 60 min of adsorption when the Cr(VI) concentration was 200 mg·L^−l. The maximum adsorption capacity on rutile TiO₂ was 28.9 mg·g⁻¹. This work provides an easy path to prepare a high-performance rutile TiO₂ adsorbent with potential applications in water pollution treatment.