Regeneration and Purification of Xenon from Exhaled Anesthetic Gas via Molecular Sieving in Ultra‐Microporous Materials

Abstract Recovering xenon (Xe) from exhaled anesthetic gas mixtures is vital to mitigate dependence on energy‐intensive processes for Xe production and to expand its clinical use, yet it remains challenging. Here, the highly efficient regeneration of Xe, N 2, and O 2 from exhaled anesthetic gases is demonstrated, with recovery rates exceeding 99%, followed by the isolation of high‐purity Xe (>99.9%) from the recovered Xe/O 2 /N 2 mixture using two isostructural ultra‐microporous materials. Their distinct separation functionalities, namely molecular sieving for CO 2 removal and strong preferential recognition of Xe over O 2 /N 2 , stem from the precisely tuned pore apertures and densely distributed carboxyl groups acting as robust binding centers. Breakthrough experiments validate their excellent Xe recovery performance under dynamic conditions, and demonstrate that the strong molecular sieving capability is well preserved even in humid environments. Single‐crystal X‐ray diffraction and in situ Fourier transform infrared spectroscopy analyses are performed, unveiling the separation mechanisms at the molecular level.