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Here, we report hydroxyl\u2010functionalized three\u2010dimensional covalent organic framework (COF) membranes that regulate proton\u2010coupled electron transfer within ordered nanochannels. Phenolic hydroxyl groups are precisely embedded in the membrane pores as internal proton reservoirs, while the continuous COF framework provides pathways for photogenerated electron transport. By tuning hydroxyl density, the dihydroxylated COF\u20102OH membrane establishes an optimal proton\u2010management microenvironment, promoting O\n                    <jats:sub>2<\/jats:sub>\n                    adsorption, charge separation, superoxide\/*OOH intermediate formation, and dynamic proton recycling. Under one\u2010sun irradiation in pure water and ambient air, COF\u20102OH achieves an H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rate of 21.79\u00a0mmol g\n                    <jats:sup>\u2013<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    h\n                    <jats:sup>\u2013<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    without sacrificial agents or cocatalysts, greatly outperforming the corresponding powder catalyst. Mechanistic experiments and simulations reveal that membrane confinement and hydroxyl\u2010mediated proton buffering jointly synchronize proton and electron fluxes during continuous photocatalysis. The free\u2010standing membrane can also be integrated into a tubular Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \u2010supported reactor for in situ H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    \u2010driven photo\u2010Fenton degradation of organic pollutants. This work establishes proton\u2010managing COF membranes as programmable reaction interfaces for efficient solar H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production and integrated water treatment.\n                  <\/jats:p>","DOI":"10.1002\/adma.73980","type":"journal-article","created":{"date-parts":[[2026,7,9]],"date-time":"2026-07-09T07:23:06Z","timestamp":1783581786000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Membrane\u2010Confined Proton Management Orchestrates Proton\u2010Electron Transfer for Efficient Photocatalytic Hydrogen Peroxide Synthesis"],"prefix":"10.1002","volume":"38","author":[{"given":"Zhiwei","family":"Xing","sequence":"first","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education Zhejiang University  Hangzhou 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University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiangju","family":"Meng","sequence":"additional","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education Zhejiang University  Hangzhou China"},{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1897-7069","authenticated-orcid":false,"given":"Shengqian","family":"Ma","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of North Texas  Denton Texas USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1698-8741","authenticated-orcid":false,"given":"Qi","family":"Sun","sequence":"additional","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education Zhejiang University  Hangzhou 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