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−1, 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−1 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.