Poly(cyclotriphosphazene-co-4,4′-diaminodiphenyl ether) crosslinked microspheres with active amino groups on the surface were prepared by one-step precipitation polymerization method. The as-prepared material were characterized by means of FTIR, XPS, XRD, EDS and SEM. The effects of pH, time of contact, dosage, initial concentration and temperature on the adsorption of uranium(VI) by the crosslinked microspheres were studied, and the adsorption mechanism was elucidated. Under the optimized adsorption conditions, the adsorption removal efficien...