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Inspired by phospholipid bilayers, we developed a bilayer self\u2010assembly strategy for 2D covalent polymer synthesis with tailored functionalized surface. Ionic amphiphilic styrene monomers employ intramolecular face\u2010to\u2010face stacking, inducing a folded monomer conformation that achieves a critical packing parameter near unity. This drives 2D nanosheet formation in basic aqueous solution. Concurrent electrostatic repulsion enabled spontaneous exfoliation. In situ radical polymerization within preorganized framework, accelerated by nanoconfinement effect, converted supramolecular assemblies into covalent bilayer polymers with 95% monomer conversion. Incorporating sulfonic acid\u2010functionalized 2D polymers (0.66\u00a0wt%) into Nafion D2020 membrane enhanced mechanical strength and proton conductivity at room temperature. Fuel cell testing (70\u00b0C, 100% RH) demonstrated increased open\u2010circuit voltage (1.00\u00a0V vs. 0.96\u00a0V), suppressed hydrogen permeation, elevated peak power density (678.9\u00a0vs. 454.6 mW\u00b7cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    ), and reduced ohmic resistance (25.2\u00a0vs. 55.1\u00a0m\u03a9).\n                  <\/jats:p>","DOI":"10.1002\/anie.202525878","type":"journal-article","created":{"date-parts":[[2026,2,9]],"date-time":"2026-02-09T07:35:37Z","timestamp":1770622537000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Supramolecular Nanoconfinement\u2010Accelerated Synthesis of Two\u2010Dimensional Styrenic Polymers Boosting Proton Conductivity in Nafion\u2010doped Membranes"],"prefix":"10.1002","volume":"65","author":[{"given":"Chenyu","family":"Wang","sequence":"first","affiliation":[{"name":"Institute of Physics Science and Information Technology Anhui University  Hefei Anhui China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Qibao","family":"Dong","sequence":"additional","affiliation":[{"name":"Hunan TiFul New Material Co., Ltd. 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