Liru Wu, Yifu Liu, Hanghang Dong, Yuzhe Liu, Fu Wang, Xifan Wu, Yongsheng Xiang, Yanjun Cui, Yuan Sun, Zhenbin Chen
ABSTRACT This work fabricated a star thermosensitive block copolymer‐modified intelligent ion‐imprinted polymer Pd(IV)‐EDTA‐S‐TIIP via an imprinting strategy integrated with thermoresponsive macromolecules. Characterizations analyzed its microstructure, morphology, and pore structure, while systematic tests evaluated its adsorption capacity, desorption efficiency, kinetic and isotherm behavior, reusability, and practical separation performance, alongside the selective enrichment mechanism of Pd(IV) in multi‐component solutions. The material displayed specific recognition toward Pd(IV) with a saturated adsorption capacity of 0.11 mmol/g, and the single‐cycle desorption ratio reached 80.2% in binary eluent. Adsorption followed pseudo‐first‐order kinetics and a monolayer Langmuir isotherm. For spent catalyst leachate containing platinum group metals, one adsorption–desorption cycle lifted Pd purity from 12.16% to 28.16% and total PGM content from 41.35% to 65.05%. After seven recycling tests, 89.4% of the initial desorption efficiency was retained, which proved outstanding reusability. Compared with the reported linear Pd(II)‐EDTA‐T‐IIP, the star‐structured adsorbent delivered a 29.4% higher maximum adsorption capacity and superior cyclic stability, which verified the unique superiority of star topology for designing stimuli‐responsive imprinted separation materials.