{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,21]],"date-time":"2026-10-21T15:55:18Z","timestamp":1792598118571,"version":"4.5.0"},"reference-count":46,"publisher":"American Chemical Society (ACS)","license":[{"start":{"date-parts":[[2026,10,20]],"date-time":"2026-10-20T00:00:00Z","timestamp":1792454400000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-029"},{"start":{"date-parts":[[2026,10,20]],"date-time":"2026-10-20T00:00:00Z","timestamp":1792454400000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-037"},{"start":{"date-parts":[[2026,10,20]],"date-time":"2026-10-20T00:00:00Z","timestamp":1792454400000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-045"}],"funder":[{"DOI":"10.13039\/501100012226","name":"Fundamental Research Funds for the Central Universities","doi-asserted-by":"publisher","award":["lzujbky-2025-xczx02"],"award-info":[{"award-number":["lzujbky-2025-xczx02"]}],"id":[{"id":"10.13039\/501100012226","id-type":"DOI","asserted-by":"publisher"}]},{"name":"National Basic Research Program of China (973 Program)","award":["2023YFB4104501"],"award-info":[{"award-number":["2023YFB4104501"]}]},{"name":"Science and Technology Innovation Talent Project of Gansu Province","award":["24RCKA001"],"award-info":[{"award-number":["24RCKA001"]}]},{"name":"National Natural Science Foundation of China (NSFC)","award":["U24A20493"],"award-info":[{"award-number":["U24A20493"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":[],"abstract":"<jats:title>Abstract<\/jats:title>\n                  <jats:p>Employing CO2\/H2 as a sustainable methylating agent offers a transformative strategy for advancing conventional methylation processes, yet achieving controllable C\u2013C coupling with high efficiency remains a formidable challenge. Here, we report a novel tandem process that integrates CO2 hydrogenation with phenol methylation over a Zr-doped In2O3 solid-solution catalyst. The optimized In7Zr3Ox catalyst exhibits &amp;gt;95% selectivity toward ortho-methylation with tunable product distribution, ranging from 92% o-cresol at 16% conversion to 86% 2,6-xylenol at 97% conversion, while maintaining stable operation for 140 h. Mechanistic studies identify surface formaldehyde species (CH2O*) generated from CO2 hydrogenation as the active methylating intermediates that kinetically couple CO2 reduction to phenol methylation. This pathway exhibits a markedly lower apparent activation energy of 58.8 kJ mol\u20131 than the conventional methanol-mediated route of 116.3 kJ mol\u20131. Continuous consumption of CH2O* also shifts the CO2 hydrogenation equilibrium, imparting a thermodynamic driving effect absent in CO2 hydrogenation alone. These findings demonstrate the potential of CO2-based methylation for selective C\u2013C bond formation and expand opportunities for CO2 valorization.<\/jats:p>","DOI":"10.1021\/jacs.6c16522","type":"journal-article","created":{"date-parts":[[2026,10,20]],"date-time":"2026-10-20T14:57:17Z","timestamp":1792508237000},"source":"Crossref","is-referenced-by-count":0,"title":["Selective Methylation\nof Phenol with CO2\/H2 to\n                    <i>o<\/i>\n                    -Cresol\nand 2,6-Xylenol"],"prefix":"10.1021","author":[{"given":"Changxin","family":"He","sequence":"first","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiaxin","family":"Zhang","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junqi","family":"Tian","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jun","family":"Yuan","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongfang","family":"Yang","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruihui","family":"Zhang","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhihe","family":"Mao","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiaojing","family":"Wu","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jieyun","family":"Zhang","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jianian","family":"Cheng","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hao","family":"Wang","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengyuan","family":"Liu","sequence":"additional","affiliation":[{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230029"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9301-7850","authenticated-orcid":true,"given":"Can","family":"Li","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]},{"name":"Chinese Academy of Sciences, Dalian National Laboratory for Clean Energy , , , ,","place":["Dalian, Liaoning, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zelong","family":"Li","sequence":"additional","affiliation":[{"name":"Lanzhou University , , , ,","place":["Lanzhou, Gansu, China, 730000"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,10,20]]},"reference":[{"issue":"1","key":"2026102111101728600_cit1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-019-13638-9","article-title":"CO2 hydrogenation to high-value\nproducts via heterogeneous catalysis","volume":"10","author":"Ye","year":"2019","journal-title":"Nat. Commun."},{"issue":"9","key":"2026102111101728600_cit2","doi-asserted-by":"publisher","first-page":"2277","DOI":"10.1016\/j.chempr.2021.02.024","article-title":"Recent advances in carbon dioxide\nhydrogenation to produce olefins and aromatics","volume":"7","author":"Wang","year":"2021","journal-title":"Chem"},{"issue":"6737","key":"2026102111101728600_cit3","doi-asserted-by":"publisher","DOI":"10.1126\/science.adn9388","article-title":"Hydrogenation of CO2 for\nsustainable fuel and chemical production","volume":"387","author":"Ye","year":"2025","journal-title":"Science"},{"issue":"8","key":"2026102111101728600_cit4","doi-asserted-by":"publisher","first-page":"2215","DOI":"10.1002\/cctc.202000036","article-title":"Catalytic Methylation\nof Aromatic Hydrocarbons using CO2\/H2 over Re\/TiO2 and H-MOR Catalysts","volume":"12","author":"Ting","year":"2020","journal-title":"ChemCatChem"},{"issue":"34","key":"2026102111101728600_cit5","doi-asserted-by":"publisher","DOI":"10.1126\/sciadv.aba5433","article-title":"Selective methylation\nof toluene using CO2 and H2 to para-xylene","volume":"6","author":"Zuo","year":"2020","journal-title":"Sci. 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Catal.,\nA"},{"issue":"2","key":"2026102111101728600_cit12","doi-asserted-by":"publisher","first-page":"609","DOI":"10.1039\/D2NJ05267A","article-title":"Alkylation of benzene\nusing CO2 and H2 over ZnZrOx\/ZSM-5:\nthe effect of Y doping","volume":"47","author":"Bian","year":"2023","journal-title":"New J. Chem."},{"issue":"37","key":"2026102111101728600_cit13","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202309377","article-title":"Xylene Synthesis Through\nTandem CO2 Hydrogenation and Toluene Methylation Over a\nComposite ZnZrO Zeolite Catalyst","volume":"62","author":"Shang","year":"2023","journal-title":"Angew. Chem.,\nInt. Ed."},{"issue":"16","key":"2026102111101728600_cit14","doi-asserted-by":"publisher","first-page":"12016","DOI":"10.1021\/acscatal.4c02253","article-title":"Boosting Benzene Alkylation Conversion\nwith CO2\/H2 via a Triple Composite Catalyst","volume":"14","author":"Cao","year":"2024","journal-title":"ACS Catal."},{"issue":"3","key":"2026102111101728600_cit15","doi-asserted-by":"publisher","DOI":"10.1016\/j.jece.2025.116704","article-title":"Highly dispersed ZnZrOx supported on silicalite-1 boost\nsynergistic catalysis with HZSM-5 for benzene alkylation with CO2\/H2","volume":"13","author":"Liu","year":"2025","journal-title":"J. Environ. Chem. Eng."},{"issue":"1","key":"2026102111101728600_cit16","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-024-55640-w","article-title":"C\u2013C bond coupling with sp3 C\u2013H bond via\nactive intermediates from CO2 hydrogenation","volume":"16","author":"Ma","year":"2025","journal-title":"Nat. Commun."},{"issue":"1","key":"2026102111101728600_cit17","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-025-67695-4","article-title":"CO2 hydrogenation toward toluene methylation\nfor selective para-xylene synthesis","volume":"17","author":"Tian","year":"2026","journal-title":"Nat. Commun."},{"issue":"2","key":"2026102111101728600_cit18","doi-asserted-by":"publisher","first-page":"241","DOI":"10.1016\/0926-860X(94)85194-8","article-title":"Alkylation of phenol\nwith methanol over magnesium-aluminium\ncalcined hydrotalcites","volume":"119","author":"Velu","year":"1994","journal-title":"Appl. Catal., A"},{"issue":"1","key":"2026102111101728600_cit19","doi-asserted-by":"publisher","first-page":"141","DOI":"10.1016\/0926-860X(96)00133-0","article-title":"Selective C-alkylation of phenol with methanol over\ncatalysts derived from copper-aluminium hydrotalcite-like compounds","volume":"145","author":"Velu","year":"1996","journal-title":"Appl. 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Catal."},{"issue":"1","key":"2026102111101728600_cit23","doi-asserted-by":"publisher","first-page":"11","DOI":"10.1021\/acs.inorgchem.4c04101","article-title":"The Alkylation\nof Phenol with Methanol: The Influence of Acid\u2013Base Properties\nof X Zeolite on the Selectivity of para- and meta-Cresol","volume":"64","author":"Li","year":"2025","journal-title":"Inorg. Chem."},{"issue":"1","key":"2026102111101728600_cit24","doi-asserted-by":"publisher","first-page":"264","DOI":"10.1006\/jcat.1998.2159","article-title":"Ortho-Selective Methylation\nof Phenol\nCatalyzed by CeO2-MgO Prepared by Citrate Process","volume":"178","author":"Sato","year":"1998","journal-title":"J. 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A:Chem."},{"issue":"10","key":"2026102111101728600_cit27","doi-asserted-by":"publisher","first-page":"1057","DOI":"10.1002\/jctb.1060","article-title":"Ortho-selective vapour phase methylation\nof phenol over nanocrystalline ferrospinels of varying Zn2+\/Mn2+ ionic composition","volume":"79","author":"Reddy","year":"2004","journal-title":"J. Chem.\nTechnol. Biotechnol."},{"issue":"2","key":"2026102111101728600_cit28","doi-asserted-by":"publisher","first-page":"340","DOI":"10.1016\/j.jcat.2009.11.019","article-title":"Catalytic methylation\nof phenol on MgO \u2013 Surface chemistry and mechanism","volume":"269","author":"Cavani","year":"2010","journal-title":"J. Catal."},{"issue":"5","key":"2026102111101728600_cit29","doi-asserted-by":"publisher","first-page":"2205","DOI":"10.1021\/ie201063e","article-title":"Mg\u2013Zn\nand Mn\u2013Zn Ferrites Derived from Coil Core Materials as New\nPhenol Methylation Catalysts","volume":"51","author":"Klimkiewicz","year":"2012","journal-title":"Ind. Eng. Chem.\nRes."},{"key":"2026102111101728600_cit30","doi-asserted-by":"publisher","first-page":"373","DOI":"10.1016\/j.fuel.2016.05.120","article-title":"Microwave-dried \u03b1-Fe2O3 as a highly efficient catalyst for ortho-methylation of phenol with\nmethanol","volume":"182","author":"Huang","year":"2016","journal-title":"Fuel"},{"key":"2026102111101728600_cit31","doi-asserted-by":"publisher","first-page":"90","DOI":"10.1016\/j.catcom.2017.01.015","article-title":"Preparation of Fe2O3\ndoped SBA-15 for vapor phase ortho-position C-alkylation of phenol\nwith methanol","volume":"92","author":"Liu","year":"2017","journal-title":"Catal. Commun."},{"key":"2026102111101728600_cit32","doi-asserted-by":"publisher","first-page":"86","DOI":"10.1016\/j.apcata.2018.01.001","article-title":"Mg\/Ga mixed-oxide\ncatalysts\nfor phenol methylation: Outstanding performance in 2,4,6-trimethylphenol\nsynthesis with co-feeding of water","volume":"552","author":"Tabanelli","year":"2018","journal-title":"Appl. Catal.,\nA"},{"key":"2026102111101728600_cit33","doi-asserted-by":"publisher","DOI":"10.1016\/j.mcat.2021.111857","article-title":"(\u03b1-Fe2O3)1-x(V2O5)x catalysts\nwith enhanced acid-base property for the highly active and ortho-selective\nmethylation of phenol","volume":"515","author":"Liu","year":"2021","journal-title":"Mol. Catal."},{"issue":"2","key":"2026102111101728600_cit34","doi-asserted-by":"publisher","first-page":"423","DOI":"10.1016\/j.jcat.2007.07.033","article-title":"The transformations\ninvolving methanol in the acid- and base-catalyzed gas-phase methylation\nof phenol","volume":"251","author":"Ballarini","year":"2007","journal-title":"J. Catal."},{"issue":"2","key":"2026102111101728600_cit35","doi-asserted-by":"publisher","first-page":"278","DOI":"10.1016\/j.jcat.2006.07.014","article-title":"Selective ortho-methylation\nof phenol with methanol over copper manganese mixed-oxide spinel catalysts","volume":"243","author":"Reddy","year":"2006","journal-title":"J. Catal."},{"issue":"10","key":"2026102111101728600_cit36","doi-asserted-by":"publisher","DOI":"10.1126\/sciadv.1701290","article-title":"A highly selective and stable ZnO-ZrO2 solid solution\ncatalyst for CO2 hydrogenation\nto methanol","volume":"3","author":"Wang","year":"2017","journal-title":"Sci. Adv."},{"issue":"1","key":"2026102111101728600_cit37","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-023-38336-5","article-title":"Selective\nconversion of CO2 to isobutane-enriched C4 alkanes\nover InZrOx-Beta composite catalyst","volume":"14","author":"Wang","year":"2023","journal-title":"Nat. Commun."},{"issue":"15","key":"2026102111101728600_cit38","doi-asserted-by":"publisher","first-page":"5059","DOI":"10.1039\/D0GC01597K","article-title":"A highly\nactive Pt\/In2O3 catalyst for CO2 hydrogenation\nto methanol with enhanced stability","volume":"22","author":"Sun","year":"2020","journal-title":"Green Chem."},{"issue":"46","key":"2026102111101728600_cit39","doi-asserted-by":"publisher","first-page":"19523","DOI":"10.1021\/jacs.0c07195","article-title":"Strong Electronic\nOxide\u2013Support\nInteraction over In2O3\/ZrO2 for Highly\nSelective CO2 Hydrogenation to Methanol","volume":"142","author":"Yang","year":"2020","journal-title":"J. Am. Chem. Soc."},{"issue":"21","key":"2026102111101728600_cit40","doi-asserted-by":"publisher","first-page":"6261","DOI":"10.1002\/anie.201600943","article-title":"Indium Oxide\nas a Superior Catalyst\nfor Methanol Synthesis by CO2 Hydrogenation","volume":"55","author":"Martin","year":"2016","journal-title":"Angew. Chem., Int. Ed."},{"key":"2026102111101728600_cit41","doi-asserted-by":"publisher","DOI":"10.1016\/j.susc.2021.121894","article-title":"On the wrong\nassignment of the XPS O1s signal at 531\u2013532 eV attributed to\noxygen vacancies in photo- and electro-catalysts for water splitting\nand other materials applications","volume":"712","author":"Idriss","year":"2021","journal-title":"Surf. Sci."},{"issue":"38","key":"2026102111101728600_cit42","doi-asserted-by":"publisher","first-page":"17365","DOI":"10.1021\/jacs.2c01005","article-title":"Direct Detection of Reactive Gallium-Hydride\nSpecies on the Ga2O3 Surface via Solid-State\nNMR Spectroscopy","volume":"144","author":"Chen","year":"2022","journal-title":"J. Am. Chem. Soc."},{"issue":"3","key":"2026102111101728600_cit43","doi-asserted-by":"publisher","first-page":"721","DOI":"10.1016\/j.chempr.2023.01.004","article-title":"Synergistic interplay\nof dual active sites on spinel ZnAl2O4 for syngas\nconversion","volume":"9","author":"Han","year":"2023","journal-title":"Chem."},{"issue":"12","key":"2026102111101728600_cit44","doi-asserted-by":"publisher","first-page":"4873","DOI":"10.1002\/anie.201914953","article-title":"Formation and Fate of Formaldehyde\nin Methanol-to-Hydrocarbon Reaction:\nIn Situ Synchrotron Radiation Photoionization Mass Spectrometry Study","volume":"59","author":"Wen","year":"2020","journal-title":"Angew. Chem., Int. Ed."},{"issue":"2","key":"2026102111101728600_cit45","doi-asserted-by":"publisher","first-page":"215","DOI":"10.1016\/j.jcat.2008.03.012","article-title":"Mechanistic\nstudies of the role of formaldehyde in the gas-phase methylation of\nphenol","volume":"256","author":"Ballarini","year":"2008","journal-title":"J. Catal."},{"key":"2026102111101728600_cit46","doi-asserted-by":"publisher","first-page":"447","DOI":"10.1016\/j.jcat.2019.01.014","article-title":"A cascade\nmechanism for a simple\nreaction: The gas-phase methylation of phenol with methanol","volume":"370","author":"Tabanelli","year":"2019","journal-title":"J. Catal."}],"container-title":["Journal of the American\nChemical Society"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jacs.6c16522","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/doi\/10.1021\/jacs.6c16522\/68914804\/jacs.6c16522.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/doi\/10.1021\/jacs.6c16522\/68914804\/jacs.6c16522.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,10,21]],"date-time":"2026-10-21T15:23:58Z","timestamp":1792596238000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/jacsat\/article\/doi\/10.1021\/jacs.6c16522\/5454430\/Selective-Methylation-of-Phenol-with-CO2-H2-to-o"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,10,20]]},"references-count":46,"URL":"https:\/\/doi.org\/10.1021\/jacs.6c16522","relation":{},"ISSN":["0002-7863","1520-5126"],"issn-type":[{"value":"0002-7863","type":"print"},{"value":"1520-5126","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,10,20]]}}}