High-purity Bi2O3 was prepared using extraction-preparation stripping method from BiCl3 leach solution. Parameters such as oxalic acid concentration, phase ration, aging duration, feeding duration, were examined for their effect on the stripped rate of Bi and the morphologies of precipitates. The precipitate was characterized by XRD, SEM, DSC-TGA and FT-IR. Bi2O3 was characterized by elements analysis, particle size analysis and SEM. Bi2O3 product of 680 nm was obtained using 15 g/L oxalic acid, 1/1 phase ration, 0 min aging duration, 0 min feeding duration and calcinating at 600 ℃ for 2 hours.