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The effective capture of iodine with high volatility and poisonousness is significant for reprocessing the spent nuclear fuel. In this article, we report a hierarchically porous poly(ionic liquid)‐organic cage composite membrane (PIL@CC3) possessing a gradient content distribution of CC3 cage crystals throughout the membrane to capture iodine vapor. The introduction of microporous CC3 can significantly enhance the uptake capacity of iodine up to 980 mg g−1, which is superior to that of a pristine PIL membrane carrying large meso‐ and macropores (99 mg g−1), and CC3 crystalline powder (662 mg g−1). Such enhanced performance benefits from the micro‐meso‐macroporous structure of the PIL@CC3 membrane in which the large meso‐ and macropores facilitate the mass transfer of iodine molecules from the external environment into the surface of the CC3 crystal, followed by diffusion of iodine molecules from the CC3 surface into the interior and exterior pores of the CC3 crystal. In addition, the asymmetric distribution of CC3 crystals across the PIL@CC3 membrane also displays its advantage in intercepting trace iodine, revealing its great potential for practical application. This study provides an idea for constructing hierarchically porous membrane composites for the removal of toxic vapors. [ABSTRACT FROM AUTHOR]

Imparting mesopores to organic cages of an intrinsic microporous nature to build up hierarchically porous cage soft materials is a grand challenge and will reshape the property and application scope of traditional organic cage molecules. Herein, we discovered how to engineer mesopores into microporous organic cages via their host–guest interactions with long chain ionic surfactants. Equally important, the ionic head of surfactants equips the supramolecularly assembled porous structures with charge‐selective uptake and release function in solution. Interestingly, such hierarchically porous organic cage can serve as a nanoreactor once trapping enzymes within the cavity, which show 5‐fold enhanced activity of enzymatic catalysis when compared with the free enzymes. [ABSTRACT FROM AUTHOR]