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Removal of radioactive technetium‐99 (99TcO4−) from water by effective adsorbents is highly desired but remains a challenge. The currently used resin adsorbents possess several obstacles, such as slow adsorption kinetics and low adsorption capacity. To address these issues, herein a type of fibrous adsorbent with porosity and hyper‐branched quaternary ammonium groups, namely porous cationic electrospun fibers (PCE fibers), is successfully prepared. PCE fibers can remove 97% of 99TcO4− within 1 min and the equilibrium time of 99% removal is 20 min. The predicted maximum adsorption capacity toward the surrogate ReO4− can reach 826 mg g−1, which is higher than the state of art anion‐exchange resins and most of the other reported adsorbents. Furthermore, PCE fibers have good selectivity for ReO4− in the presence of competitive anions, and can retain ReO4− uptake under extreme conditions including high acid–base and gamma irradiation. Importantly, PCE fibrous adsorptive membrane is employed for dynamic ReO4− removal from simulated Hanford LAW stream with a processing capacity of 600 kg simulated stream per kilogram PCE fibers. The excellent performance highlights the advantages of PCE fibers over traditional resins in technetium removal. [ABSTRACT FROM AUTHOR]

Highly efficient removal of bilirubin from blood by hemoperfusion for liver failure therapy remains a challenge in the clinical field due to the low adsorption capacity and slow adsorption kinetics of currently used bilirubin adsorbents (e.g., activated carbon and ion‐exchange resin). Recently, porous aromatic frameworks (PAFs) with high surface areas, tunable structures, and remarkable stability provide numerous possibilities to obtain satisfying adsorbents. Here, a cationic PAF with more mesopores, named iPAF‐6, is successfully constructed via a de novo synthetic strategy for bilirubin removal. The prepared iPAF‐6 exhibits a record‐high adsorption capacity of 1249 mg g−1 and can adsorb bilirubin from 150 mg L−1 to normal concentration in just 5 min. Moreover, iPAF‐6 shows a removal efficiency of 96% toward bilirubin in the presence of 50 g L−1 bovine serum albumin. It is demonstrated that positively charged aromatic frameworks and large pore size make a significant contribution to its excellent adsorption ability. More notably, iPAF‐6/polyethersulfone composite fibers or beads are fabricated for practical hemoperfusion adsorption, which also show better removal performance than commercial adsorbents. This work can offer a new possibility for designing PAF‐based bilirubin adsorbents with an appealing application prospect. [ABSTRACT FROM AUTHOR]