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Uranium is a key element in the nuclear industry and also a global environmental contaminant with combined highly toxic and radioactive. Currently, the materials based on post-modification of amidoxime have been developed for uranium detection and adsorption. However, the affinity of amidoxime group for vanadium is stronger than that of uranium, which is the main challenge hindering the practical application of amidoxime-based adsorbents. Herein, we synthesized a fluorescent covalent organic framework (TFPPy-BDOH) through integrating biphenyl diamine and pyrene unit into the π-conjugated framework. TFPPy-BDOH has an excellent selectivity to uranium due to the synergistic effect of nitrogen atom in the imine bond and hydroxyl groups in conjugated framework. It can achieve ultra-fast fluorescence response time (2 s) and ultra-low detection limit (8.8 nM), which may be attributed to its intrinsic regular porous channel structures and excellent hydrophilicity. More excitingly, TFPPy-BDOH can chemically reduce soluble U (VI) to insoluble U (IV), and release the binding site to adsorb additional U (VI), achieving high adsorption capacity of 982.6 ± 49.1 mg g−1. Therefore, TFPPy-BDOH can overcome the challenges faced by current amidoxime-based adsorbents, making it as a potential adsorbent in practical applications. [Display omitted] • A fluorescent COF (TFPPy-BDOH) is synthesized by a one-step method. • TFPPy-BDOH has ultra-fast fluorescence response time for UO 2 2+. • TFPPy-BDOH can selectively chemically reduce soluble U(VI) to insoluble U(IV). • TFPPy-BDOH achieves high sensitivity and selectivity for detecting and capturing UO 2 2+ in harsh environments. [ABSTRACT FROM AUTHOR]

• Highly stable sp2 carbon-conjugated covalent organic framework (COF-PDAN-AO) was synthesized and characterization. • Acid and radiation resistant COF-PDAN-AO exhibits efficient adsorption of UO 2 2+ from radioactive wastewater. • COF-PDAN-AO possesses short adsorption equilibrium time and selectivity for uranium. • The emission of COF-PDAN-AO was selectively quenched upon adding UO 2 2+. Uranium is an important element in the nuclear industry while the discharge of radioactive wastewater can cause serious damages to the environment. In this work, an ultra-stable sp2 carbon-conjugated covalent organic framework (COF-PDAN-AO) is synthesized with amidoxime-substituted monomers for detection and efficient adsorption of uranium from radioactive wastewater. Abundant amidoxime groups laced on the open 1D channels of COF-PDAN-AO exhibit exceptional accessibility and the regular pores facilitate the mass transfer. Based on these features, COF-PDAN-AO achieves ultra-low detection limit of 6.5 nM, high uranium adsorption capacity (410 mg/g) and selective interaction with uranium. In addition, various spectroscopies verify COF-PDAN-AO possesses excellent radioresistance in acidic solution. Regeneration studies have shown that COF-PDAN-AO maintained good structural stability after seven cycles. These results indicate that our sp2 carbon conjugated COF can be potentially used for practical detection and adsorption of uranium from radioactive wastewater. This strategy can be extended to detection and extraction of other contaminants by designing the target ligand. [ABSTRACT FROM AUTHOR]