Abstract: The aim of this work is to synthesize economical and environment-friendly functional nanofiber materials with high adsorption capacity and high selectivity for U(Ⅵ). First, the amidoxime-based polyacrylonitrile nanofibers(AO-PAN) and carboxyl/amidoxime-based polyacrylonitrile nanofibers(AC-PAN) are prepared by electrospinning and characterized by different means. Then the effects of pH, ionic strength, contact time, initial concentration of U(Ⅵ), temperature and coexisting ions on the adsorption of U(Ⅵ) on synthetic materials are investigated in detail, and the reusability of AO-PAN and AC-PAN is also studied. The experimental results show that the adsorption of U(Ⅵ) on AO-PAN and AC-PAN is significantly affected by pH, but the effect of ionic strength is weak; the adsorption of U(Ⅵ) on AC-PAN can reach equilibrium within 30 minutes, and its maximum adsorption capacity is 3.33 mmol/g, which is about 8 times that of AO-PAN. The increasing temperature is beneficial to the adsorption of U(Ⅵ) on synthetic materials, which indicates that the adsorption process is an endothermic reaction; AO-PAN and AC-PAN perform well in the adsorption selectivity for U(Ⅵ), and the adsorption rate of U(Ⅵ) still exceeds 99% after reuse for 3 times. Therefore, AO-PAN and AC-PAN have good application prospect in the treatment of uranium-containing wastewater.