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Through molecule self-assembly and subsequent surface functionalization, novel uranium adsorbent AO−OB hierarchical self-assembled polyimide microspheres (AO-OBHSPIMs) were obtained by introducing the amidoxime groups into hierarchical self-assembled polyimide microspheres for the efficient and selective recovery of uranium from wastewater. The results of Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), X-ray diffraction (XRD), and nitrogen adsorption−desorption isotherm showed that AO-OBHSPIMs were a semicrystalline polymer material with self-supporting hierarchical structure and low pore volume, and they were equipped with abundant amidoxime groups. Given the recognized selectivity of amidoxime groups and their hierarchical structure, AO-OBHSPIMs exhibited excellent selectivity to uranyl ions. Moreover, AO-OBHSPIMs exhibited good stability and recyclability and remarkable removal percentage within lowconcentration solution (99.4%) and simulated uranium-containing wastewater (97.3%). AO-OBHSPIMs could be applied to fixedbed column adsorption due to their large particle size and self-supporting hierarchical structure that can facilitate water flow. The indepth discussion of the adsorption mechanism showed that the adsorption mainly depended on the combined action of electrostatic interactions and complexation, and the adsorption process was a spontaneous endothermic monolayer adsorption. In summary, AO-OBHSPIMs exhibited good application prospects in uranium-containing wastewater remediation.

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