A novel method to prepare high-purity vanadium pentoxide (V2O5) was proposed, and V2O5 with a purity of above 99.95 wt%, in which the concentration of Fe was at 0.0060%, the concentration of Al was at 0.0040%, and Si, K, Na, and other impurities were under the determination limit, was obtained. In this method, anhydrous aluminum chloride (AlCl3) was adopted, which replaced toxic and corrosive Cl-2 in the traditional chlorination method. Moreover, the reaction temperature was relatively low at 160 degrees C compared to Cl-2 chlorination method.