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Herein, we report an anaerobic photocatalytic strategy to directly upgrade CH4 and water into acetone (C3) over a RhPd alloy-engineered TiO2 catalyst without external CO or chemical oxidants. At 90 \u00b0C and 15 bar of CH4, this system delivers an acetone production rate of 873 \u03bcmol gcat\u20131 h\u20131 with an 85% liquid-phase selectivity, demonstrating maximized photon utilization alongside efficient H2 evolution. Mechanistic tracking reveals that hole-mediated H2O oxidation generates active hydroxyl radicals (\u2022OH) that primarily drive methane homolysis to sequentially yield adsorbed carbonyl (*CO) equivalents. Crucially, the electronically coupled RhPd co-catalyst acts as an efficient extraction hub to divert photogenerated electrons via a continuous hydrogen-evolution relief channel to optimize charge separation, while concurrently utilizing its enhanced adsorption affinity to pool these in situ formed *CO species and migrating methyl fragments for relay carbonylation toward exclusive C3 acetone synthesis. This orchestrated harmony establishes a mild, anaerobic strategy for methane conversion, offering a pristine paradigm for controlling complex multi-carbon coupling trajectories in solar-to-chemical conversions.<\/jats:p>","DOI":"10.1021\/jacs.6c14611","type":"journal-article","created":{"date-parts":[[2026,9,12]],"date-time":"2026-09-12T15:02:34Z","timestamp":1789225354000},"source":"Crossref","is-referenced-by-count":0,"title":["Direct Photocatalytic\nAnaerobic Conversion of Methane\nand Water to Acetone over RhPd Alloy-Modified TiO2"],"prefix":"10.1021","author":[{"given":"Zhiyong","family":"Guo","sequence":"first","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Heng","family":"Zhang","sequence":"additional","affiliation":[{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]},{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Anyi","family":"Chen","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiarong","family":"Li","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuxuan","family":"Duan","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiaoyun","family":"Jia","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuejiao","family":"Wu","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Adeel","family":"Mehmood","sequence":"additional","affiliation":[{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bing","family":"Wang","sequence":"additional","affiliation":[{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]},{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9130-5376","authenticated-orcid":true,"given":"Jiadong","family":"Xiao","sequence":"additional","affiliation":[{"name":"University of Chinese Academy of Sciences , , ,","place":["Beijing, China, 101408"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0764-2279","authenticated-orcid":true,"given":"Ye","family":"Wang","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7112-4700","authenticated-orcid":true,"given":"Kang","family":"Cheng","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,12]]},"reference":[{"issue":"13","key":"2026091211022808200_cit1","doi-asserted-by":"publisher","first-page":"8497","DOI":"10.1021\/acs.chemrev.6b00715","article-title":"Direct Conversion of Methane to Value-Added Chemicals\nover Heterogeneous Catalysts: Challenges and Prospects","volume":"117","author":"Schwach","year":"2017","journal-title":"Chem. 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