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Herein, we report an exogenous reagent\u2010free dual\u2010substrate cooperative strategy. Without adding external chemicals (e.g., methanol, sulfite), the target pollutant phenol is directly used as an endogenous electron donor to drive the reduction of Cr(VI) and its own degradation over a thermally exfoliated graphitic carbon nitride (CN\u2010T) catalyst. Phenol fulfills two critical roles in this system: (i) it is oxidized and degraded by photogenerated holes (h\n                    <jats:sup>+<\/jats:sup>\n                    ), and (ii) it transfers electrons to CN\u2010T, enhancing Cr(VI) reduction by photogenerated electrons (e\n                    <jats:sup>\u2212<\/jats:sup>\n                    ). Kinetic studies, DFT calculations, and EPR spectroscopy reveal that phenol adsorbs on CN\u2010T via \u03c0\u2010\u03c0 stacking and hydrogen bonding, facilitating electron transfer from its HOMO to the CN\u2010T LUMO. This process suppresses e\n                    <jats:sup>\u2212<\/jats:sup>\n                    \u2010h\n                    <jats:sup>+<\/jats:sup>\n                    recombination and promotes Cr(VI) reduction. In the coexisting system, CN\u2010T achieved 76.4% Cr(VI) reduction and 99.8% phenol degradation, with a 6.4\u2010fold higher Cr(VI) reduction rate constant than in the single pollutant system. Substituted phenols (4\u2010methylphenol, 4\u2010chlorophenol, p\u2010nitrophenol) strongly correlate with electronic descriptors (Hammett constant, E\n                    <jats:sub>HOMO<\/jats:sub>\n                    ), establishing a robust quantitative structure\u2010activity relationship (QSAR) for predictive synergistic co\u2010removal. This work advances photocatalytic redox coupling and provides a \u201cwaste\u2010to\u2010waste\u201d strategy for sustainable complex wastewater.\n                  <\/jats:p>","DOI":"10.1002\/advs.75763","type":"journal-article","created":{"date-parts":[[2026,6,1]],"date-time":"2026-06-01T15:35:40Z","timestamp":1780328140000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Dual\u2010Substrate Synergistic Photocatalysis: Exogenous Reagent\u2010Free Co\u2010Removal of Phenol and Cr(VI) via Electron\u2010Donor\u2010Mediated Redox Coupling over Modified Carbon Nitride"],"prefix":"10.1002","volume":"13","author":[{"given":"Xiaoman","family":"Zhang","sequence":"first","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shuqi","family":"Wan","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cuiwei","family":"Du","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qilu","family":"Li","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chongfei","family":"Yu","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shuying","family":"Dong","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xianfa","family":"Su","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chun","family":"Hu","sequence":"additional","affiliation":[{"name":"School of Environment Key Laboratory for Yellow River and Huai River Water Environmental and Pollution Control Henan Normal University Ministry of Education Henan Key Laboratory for Environmental Pollution Control  Xinxiang Henan P. R. China"},{"name":"Institute of Environmental Research at Greater Bay Key Laboratory for Water Quality and Conservation of the Pearl River Delta Ministry of Education Guangzhou University  Guangzhou P. R. 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