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• A highly efficient adsorbent was prepared and used for the treatment of uranium wastewater. • MXene/PAO hydrogel beads exhibit outstanding adsorption capacity under different conditions. • MXene/PAO hydrogel beads have excellent practicality coupling through columns. • Adsorption mechanism under F− conditions is the coordination of MXene and amidoxime to uranium complexes. The treatment of radioactive wastewater is crucial to ensure the safe and rapid development of nuclear energy. However, efficient disposal of uranium wastewater containing high concentrations of fluoride ions (F−) generated during uranium enrichment and conversion poses a formidable and pressing challenge. In this study, we successfully synthesized MXene/PAO hydrogel beads (MPH beads) by self-assembling two-dimensional Ti 3 C 2 T x MXene nanosheets with amidoxime through ionic cross-linking. MPH beads exhibited exceptional uranium adsorption capacity (625 mg/g), remarkable adsorption selectivity, and good reusability. Notably, MPH beads demonstrated a maximum uranium adsorption capacity of 400 mg/g in an aqueous solution containing 8000 ppm F−. Furthermore, MPH beads showed favorable F− resistance and were able to remove>95% of U(Ⅵ) even after being immersed in an extreme environment for 15 days. Additionally, MPH beads achieved a high U(Ⅵ) recovery of 98.2% from real environment water samples using dynamic column experiments, showcasing their excellent application performance. The efficient U(Ⅵ) adsorption and anti-fluoride effect were mainly attributed to the combined complexation between the C(NH 2) = N-OH, C-Ti-OH groups and U(Ⅵ), as demonstrated by experiments, characterization, and DFT calculations. Our study highlights the significant potential of MPH beads in the treatment of uranium from radioactive wastewater, especially wastewater with high concentrations of F−. [ABSTRACT FROM AUTHOR]