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Herein, we developed a photocatalysis\u2013ion\u2010exchange coupling strategy for closed\u2010loop removal and recycling of radioactive metal in nuclear wastewater based on a novel bifunctional K\u2010SnS\/TiO\n                    <jats:sub>2<\/jats:sub>\n                    heterojunction. The photocatalytic reduction with in situ ion\u2010exchange converted mobile\n                    <jats:sup>99<\/jats:sup>\n                    TcO\n                    <jats:sub>4<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    into immobilized\n                    <jats:sup>99<\/jats:sup>\n                    Tc\n                    <jats:sup>3+<\/jats:sup>\n                    . HCOOH\u2010assisted photocatalysis by generating \u00b7CO\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    radicals on TiO\n                    <jats:sub>2<\/jats:sub>\n                    , thus driving rapid\n                    <jats:sup>99<\/jats:sup>\n                    TcO\n                    <jats:sub>4<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    reduction. Simultaneously, layered K\u2010SnS captured\n                    <jats:sup>99<\/jats:sup>\n                    Tc\n                    <jats:sup>3+<\/jats:sup>\n                    via in situ ion\u2010exchange with the K\n                    <jats:sup>+<\/jats:sup>\n                    in the framework, thereby forming stable coordination environments that inhibited the re\u2010oxidation of\n                    <jats:sup>99<\/jats:sup>\n                    Tc\n                    <jats:sup>3+<\/jats:sup>\n                    to soluble\n                    <jats:sup>99<\/jats:sup>\n                    TcO\n                    <jats:sub>4<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    . Finally, the\n                    <jats:sup>99<\/jats:sup>\n                    Tc\n                    <jats:sup>3+<\/jats:sup>\n                    could be recycled by reverse ion\u2010exchange in concentrated KCl solution. This coupled electron\u2013ion transfer established a dynamic interfacial mechanism that linked redox transformation with structural confinement. The system achieves efficient\n                    <jats:sup>99<\/jats:sup>\n                    Tc removal across diverse aqueous chemistries, including high ionic strength conditions, and enables complete recovery through reverse ion\u2010exchange. Our results provide a generalizable route for integrating the transformation, immobilization, and recovery of redox\u2010active contaminants, thereby advancing sustainable nuclear wastewater management.\n                  <\/jats:p>","DOI":"10.1002\/anie.9417552","type":"journal-article","created":{"date-parts":[[2026,8,6]],"date-time":"2026-08-06T11:16:09Z","timestamp":1786014969000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Recycling\n                    <sup>99<\/sup>\n                    Tc From Nuclear Wastewater by Coupling Photocatalysis and In Situ Ion\u2010Exchange on Bifunctional K\u2010SnS\/TiO\n                    <sub>2<\/sub>\n                    Heterojunction"],"prefix":"10.1002","volume":"65","author":[{"given":"Xiaoming","family":"Deng","sequence":"first","affiliation":[{"name":"School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 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