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A new synthetic method was designed to prepare poly (trimesoyl chloride-co-polyethyleneimine) (PEI-TMC). Characterization of PEI-TMC was investigated by FTIR, SEM, EDS, XPS, TGA, and BET. TGA test revealed that the PEI-TMC had excellent thermal stability. The BET specific surface area (4.74 ​m2 ​g−1) and pore diameter of about 9.44 ​nm indicated that PEI-TMC possessed a mesoporous structure. The adsorption behavior of U(VI) on the PEI-TMC was investigated. The thermodynamic analysis showed that the process of PEI-TMC adsorption of U(VI) was endothermic and spontaneous, and the adsorption efficiency was better at higher temperatures. The U(VI) sorption on PEI-TMC was conformed to the Langmuir adsorption isotherm and pseudo-second-order kinetic models. The adsorption mechanism of U(VI) with PEI-TMC was systematically elucidated by XPS and FTIR. Under the best condition, the maximum adsorption capacity of PEI-TMC could reach 212.8 ​mg ​g−1 ​by calculating the Langmuir isothermal model. It indicated that PEI-TMC was a potential adsorbent for the treatment of U(VI)-containing wastewater. Diagram of PEI synthesis and its adsorption mechanism for U(VI). Image 1 • A new and facile method is used to prepare PEI-TMC. • The application field of PEI-TMC was expanded for the separation of U(VI). • Excellent adsorption performance was demonstrated. [ABSTRACT FROM AUTHOR]