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Here, we report a scalable \u201cliving nanosheet\u201d strategy for synthesizing covalent organic framework (COF) membranes with robust laminar structures. COF nanosheets and residual monomers are collectively cast onto smooth substrates, followed by heating in an enclosed environment. The slow shear\u2010flows make COF nanosheets accurately aligned into laminar structures while avoiding possible distortion. The COF nanosheets are still \u201cliving\u201d, so that they can continue to react with remaining monomers upon heating, further healing the intercrystalline defects and stabilizing the laminar membranes. This strategy allows upscalable preparation of membranes with a large area of up to 600 cm\n                    <jats:sup>2<\/jats:sup>\n                    . The resulting COF membranes exhibit ultrahigh permeability (1.1\u00a0\u00d7\u00a010\n                    <jats:sup>4<\/jats:sup>\n                    \u00a0L m\n                    <jats:sup>\u22122<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    bar\n                    <jats:sup>\u22121<\/jats:sup>\n                    nm for methanol) and a sharp molecular weight cutoff (360\u00a0Da), outperforming state\u2010of\u2010the\u2010art OSN membranes. Notably, it achieves a sharp and durable separation process of photosensitizers (e.g., 98.3% rejection of TMPyP4 tosylate) and\u00a0&gt;92% solvent recovery. This work establishes a versatile approach for scalable synthesis of COF membranes, enabling energy\u2010efficient molecular separations in pharmaceutical and chemical industries.\n                  <\/jats:p>","DOI":"10.1002\/anie.202518250","type":"journal-article","created":{"date-parts":[[2025,11,3]],"date-time":"2025-11-03T08:17:37Z","timestamp":1762157857000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["\u201cLiving Nanosheets\u201d of Covalent Organic Frameworks Aligned into Laminar Membranes for Sharp and Durable Molecular Separations"],"prefix":"10.1002","volume":"64","author":[{"given":"Zhe","family":"Zhang","sequence":"first","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu, and School of Environmental Science and Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Youxin","family":"Gong","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu and College of Chemical Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming","family":"Liu","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu and College of Chemical Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng","family":"Chen","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu and College of Chemical Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Congcong","family":"Yin","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu, and School of Energy and Environment Southeast University Nanjing Jiangsu 210096 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mingjie","family":"Wei","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu and College of Chemical Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8653-514X","authenticated-orcid":false,"given":"Yong","family":"Wang","sequence":"additional","affiliation":[{"name":"Key Lab of Functional Polymers for Sustainability of Jiangsu and College of Chemical Engineering Nanjing Tech University Nanjing Jiangsu 211816 P. R. 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