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[Display omitted] • Novel cationic electrospun nanofibers (NCE fibers) were designed and synthesized. • Specific anion traps with hydrophobic microenvironment were constructed. • NCE fibers exhibited fast kinetics and high uptake for ReO 4 −. • NCE fibers showed good removal depth and satisfying selectivity toward ReO 4 −. • The column adsorption was also conducted with the treatment capacity of 1540 BV. Developing cationic adsorbents for efficient radioactive pertechnetate (99TcO 4 −) removal from water is of great significance in both nuclear fuel management and nuclear-related environmental treatment fields. However, tremendous efforts should be taken to improve the comprehensive performance of the adsorbent materials. Herein, novel cationic electrospun nanofibers were synthesized via the blending electrospinning from the branched polyethylenimine based solution and the following quaternization reaction by benzyl bromide. Consequently, abundant specific anion traps with hydrophobic microenvironment were constructed on the fibers. The obtained fiber adsorbents were systematically investigated to remove perrhenate (ReO 4 −) ions (the nonradioactive surrogate for TcO 4 −), which exhibit satisfying adsorption performance in several aspects: high adsorption capacity (943 mg g−1), fast kinetics (30 min), good removal depth (distribution coefficient = 1.1 × 106 mL g−1), large dynamic column adsorption volume (1540 bed volume), and excellent ReO 4 − capture from solution with high ionic strength or acidity/alkalinity. The adsorption performance surpassed all macroscopic shapeable adsorbents and many powdery advanced porous materials, owing to their abundant adsorption sites, tailored anion traps and macroscopic fibrous structures. Overall, this work gives a useful insight into designing novel adsorbents for effective TcO 4 −/ReO 4 − capture. [ABSTRACT FROM AUTHOR]