{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,23]],"date-time":"2026-10-23T19:46:09Z","timestamp":1792784769663,"version":"4.5.0"},"reference-count":48,"publisher":"American Chemical Society (ACS)","issue":"36","license":[{"start":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T00:00:00Z","timestamp":1788393600000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-029"},{"start":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T00:00:00Z","timestamp":1788393600000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-037"},{"start":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T00:00:00Z","timestamp":1788393600000},"content-version":"stm-asf","delay-in-days":0,"URL":"https:\/\/doi.org\/10.15223\/policy-045"}],"funder":[{"name":"National Basic Research Program of China (973 Program)","award":["2016YFB0301603"],"award-info":[{"award-number":["2016YFB0301603"]}]},{"name":"National Natural Science Foundation of China (NSFC)","award":["21802136"],"award-info":[{"award-number":["21802136"]}],"id":[{"id":"https:\/\/ror.org\/01h0zpd94","id-type":"ROR","asserted-by":"crossref"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":[],"published-print":{"date-parts":[[2026,9,16]]},"abstract":"<jats:title>Abstract<\/jats:title>\n                  <jats:p>For decades, the consensus has been that the pore dimensions of microporous titanosilicate catalysts are too small to accommodate bulky reactants, which are critical to the fine chemicals and pharmaceutical industries. This limitation has confined catalyst design to tuning pore size based on the assumption that transport and reactivity are governed mainly by framework geometry. Here, we show that solvent-free operation can instead enhance reactivity in a system where it would normally be hampered: bulky-molecule epoxidation over microporous zeolites. In cyclohexene epoxidation over conventional titanium silicalite-1, solvent-free conditions yield 88.8% conversion with &amp;gt;89% epoxide selectivity, whereas conversion remains below 6.9% in methanol. We attribute this contrast to the solvent-gated accessibility of confined Ti sites. Solvent molecules occupying the microporous environment block bulky substrates from reaching the internal reactive space, while vacant or weakly occupied voids allow transient access and productive epoxidation. This trend extends to larger cyclic olefins and titanium-containing porous catalysts. By eliminating solvents and boosting efficiency, our solvent-free method proves that tailoring the confined environment is as important as the framework structure to unlock reactivity in porous catalysts.<\/jats:p>","DOI":"10.1021\/jacs.6c12516","type":"journal-article","created":{"date-parts":[[2026,9,4]],"date-time":"2026-09-04T04:24:28Z","timestamp":1788495868000},"page":"39112-39120","source":"Crossref","is-referenced-by-count":0,"title":["Solvent-Free Catalysis\nUnlocks Bulky-Molecule Oxidation\nwithin Titanosilicate Micropores"],"prefix":"10.1021","volume":"148","author":[{"given":"Xun","family":"Wu","sequence":"first","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences, Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7143-2658","authenticated-orcid":true,"given":"Mingbin","family":"Gao","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fangxiu","family":"Ye","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences, Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liping","family":"Yang","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Danhua","family":"Yuan","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shiji","family":"Li","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhexiong","family":"Zheng","sequence":"additional","affiliation":[{"name":"Xiamen University , , ,","place":["Xiamen, China, 361005"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuhan","family":"Song","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences, Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7775-4183","authenticated-orcid":true,"given":"Jingfeng","family":"Han","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4722-8371","authenticated-orcid":true,"given":"Shutao","family":"Xu","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiacheng","family":"Xing","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5165-5803","authenticated-orcid":true,"given":"Yunpeng","family":"Xu","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7999-2940","authenticated-orcid":true,"given":"Zhongmin","family":"Liu","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,3]]},"reference":[{"key":"2026091609123213900_cit1","doi-asserted-by":"publisher","first-page":"159","DOI":"10.1038\/378159a0","article-title":"Heterogeneous catalysts obtained\nby grafting metallocene complexes onto mesoporous silica","volume":"378","author":"Maschmeyer","year":"1995","journal-title":"Nature"},{"key":"2026091609123213900_cit2","doi-asserted-by":"publisher","first-page":"71","DOI":"10.1080\/01614940.2017.1389111","article-title":"Catalytic\nperformance of advanced titanosilicate selective oxidation catalysts\u2013a\nreview","volume":"60","author":"Pr\u030cech","year":"2018","journal-title":"Catal. Rev."},{"key":"2026091609123213900_cit3","doi-asserted-by":"publisher","first-page":"48","DOI":"10.1038\/s41929-025-01465-9","article-title":"Titanium mordenite-confined\nlow-loaded Pd for efficient oxime production with H2 and O2","volume":"9","author":"Wan","year":"2026","journal-title":"Nat. Catal."},{"key":"2026091609123213900_cit4","doi-asserted-by":"publisher","first-page":"283","DOI":"10.1126\/science.ade1771","article-title":"A 3D extra-large-pore zeolite enabled by 1D-to-3D topotactic\ncondensation of a chain silicate","volume":"379","author":"Li","year":"2023","journal-title":"Science"},{"key":"2026091609123213900_cit5","doi-asserted-by":"publisher","first-page":"99","DOI":"10.1038\/s41586-024-07194-6","article-title":"Interchain-expanded\nextra-large-pore zeolites","volume":"628","author":"Gao","year":"2024","journal-title":"Nature"},{"key":"2026091609123213900_cit6","doi-asserted-by":"publisher","first-page":"83","DOI":"10.1126\/science.aec4882","article-title":"A 36-ring zeolite with\nintrinsic cylindrical mesopores","volume":"392","author":"Sun","year":"2026","journal-title":"Science"},{"key":"2026091609123213900_cit7","volume-title":"Concepts of modern catalysis and kinetics","author":"Chorkendorff","year":"2017"},{"key":"2026091609123213900_cit8","doi-asserted-by":"publisher","first-page":"385","DOI":"10.1038\/nature01980","article-title":"A combustion-free methodology for\nsynthesizing zeolites and zeolite-like materials","volume":"425","author":"Lee","year":"2003","journal-title":"Nature"},{"key":"2026091609123213900_cit9","doi-asserted-by":"publisher","first-page":"aaa8075","DOI":"10.1126\/science.aaa8075","article-title":"Function-led design\nof new porous materials","volume":"348","author":"Slater","year":"2015","journal-title":"Science"},{"key":"2026091609123213900_cit10","doi-asserted-by":"publisher","first-page":"517","DOI":"10.1021\/acs.accounts.6b00510","article-title":"Heterogeneous catalysis: a central science for a sustainable future","volume":"50","author":"Friend","year":"2017","journal-title":"Acc. 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Soc."},{"issue":"33","key":"2026091609123213900_cit14","doi-asserted-by":"publisher","DOI":"10.1002\/ejic.202300483","article-title":"An Overview\nof Heterogeneous Transition Metal-Based Catalysts for Cyclohexene\nEpoxidation Reaction","volume":"26","author":"Dong","year":"2023","journal-title":"Eur. J. Inorg. Chem."},{"key":"2026091609123213900_cit15","doi-asserted-by":"publisher","first-page":"321","DOI":"10.1038\/368321a0","article-title":"Titanium-containing\nmesoporous molecular sieves for catalytic oxidation of aromatic compounds","volume":"368","author":"Tanev","year":"1994","journal-title":"Nature"},{"key":"2026091609123213900_cit16","doi-asserted-by":"publisher","first-page":"137546","DOI":"10.1016\/j.fuel.2025.137546","article-title":"Efficient construction of active TiO6 species in TS-1 zeolite via\ntreatment with amines and ammonium salts for enhanced cyclohexene\nepoxidation","volume":"407","author":"Wang","year":"2026","journal-title":"Fuel"},{"key":"2026091609123213900_cit17","doi-asserted-by":"publisher","first-page":"112035","DOI":"10.1016\/j.micromeso.2022.112035","article-title":"Charge transformation of framework titanium (IV) into\ntitanium (III) in vanadium-titanium doped MFI zeolite for enhanced\nalkene epoxidation","volume":"341","author":"Lv","year":"2022","journal-title":"Microporous Mesoporous Mater."},{"key":"2026091609123213900_cit18","doi-asserted-by":"publisher","first-page":"901","DOI":"10.1021\/cs2002143","article-title":"MFI titanosilicate nanosheets with\nsingle-unit-cell thickness as an oxidation catalyst using peroxides","volume":"1","author":"Na","year":"2011","journal-title":"ACS Catal."},{"key":"2026091609123213900_cit19","doi-asserted-by":"publisher","first-page":"10868","DOI":"10.1039\/D2SC02679A","article-title":"Switching between classical\/nonclassical\ncrystallization pathways of TS-1 zeolite: implication on titanium\ndistribution and catalysis","volume":"13","author":"Bai","year":"2022","journal-title":"Chem. Sci."},{"key":"2026091609123213900_cit20","doi-asserted-by":"publisher","first-page":"770","DOI":"10.1007\/s10562-022-04005-3","article-title":"Engineering Dandelion-Like\nHollow TS-1@ SiO2: Structural Design and Oxidation Application","volume":"153","author":"Wang","year":"2023","journal-title":"Catal. Lett."},{"key":"2026091609123213900_cit21","doi-asserted-by":"publisher","first-page":"605","DOI":"10.3390\/gels11080605","article-title":"Anatase-Free Nanosized Hierarchical Titanosilicate\nTS-1 Synthesis via Nitric Acid-Catalyzed Gel Preparation","volume":"11","author":"Bikbaeva","year":"2025","journal-title":"Gels"},{"key":"2026091609123213900_cit22","doi-asserted-by":"publisher","first-page":"512","DOI":"10.1021\/acs.iecr.7b03719","article-title":"Mesoporous\/Microporous\nTitanium Silicalite with Controllable Pore Diameter for Cyclohexene\nEpoxidation","volume":"57","author":"Zuo","year":"2018","journal-title":"Ind. Eng. Chem. Res."},{"key":"2026091609123213900_cit23","doi-asserted-by":"publisher","first-page":"7892","DOI":"10.1021\/acs.iecr.9b00467","article-title":"Enhanced activity of\nhierarchical TS-1 synthesized via tuning porosity and titanium coordination","volume":"58","author":"Guo","year":"2019","journal-title":"Ind. Eng. Chem. Res."},{"key":"2026091609123213900_cit24","doi-asserted-by":"publisher","first-page":"2650","DOI":"10.1021\/acscatal.0c05144","article-title":"Extra-large pore titanosilicate synthesized via reversible\n3D\u20132D\u20133D structural transformation as highly active\ncatalyst for cycloalkene epoxidation","volume":"11","author":"Jiao","year":"2021","journal-title":"ACS Catal."},{"key":"2026091609123213900_cit25","doi-asserted-by":"publisher","first-page":"115748","DOI":"10.1016\/j.jcat.2024.115748","article-title":"Ti-Beta zeotypes with\nopen Ti (OSi) 3OH sites for the efficient epoxidation of cyclohexene\nwith H2O2","volume":"439","author":"Xu","year":"2024","journal-title":"J. Catal."},{"key":"2026091609123213900_cit26","doi-asserted-by":"publisher","first-page":"1857","DOI":"10.1039\/C9CY00071B","article-title":"Ultrafast synthesis of nanosized Ti-Beta as an efficient oxidation\ncatalyst via a structural reconstruction method","volume":"9","author":"Wang","year":"2019","journal-title":"Catal. Sci. Technol."},{"key":"2026091609123213900_cit27","doi-asserted-by":"publisher","first-page":"246","DOI":"10.1016\/j.cattod.2021.10.010","article-title":"Ti-PMO materials as selective catalysts\nfor the epoxidation of cyclohexene and vernonia oil","volume":"390","author":"Awoke","year":"2022","journal-title":"Catal. Today"},{"key":"2026091609123213900_cit28","doi-asserted-by":"publisher","first-page":"75","DOI":"10.1016\/j.jcat.2009.01.013","article-title":"Direct room-temperature synthesis of methyl-functionalized\nTi-MCM-41 nanoparticles and their catalytic performance in epoxidation","volume":"263","author":"Lin","year":"2009","journal-title":"J. Catal."},{"key":"2026091609123213900_cit29","doi-asserted-by":"publisher","first-page":"11","DOI":"10.1016\/j.apcata.2017.10.017","article-title":"Pore size-tunable titanosilicates post-synthesized\nfrom germanosilicate by structural reorganization and H2TiF6-assisted\nisomorphous substitution","volume":"550","author":"Liu","year":"2018","journal-title":"Appl. Catal., A"},{"key":"2026091609123213900_cit30","doi-asserted-by":"publisher","first-page":"111437","DOI":"10.1016\/j.micromeso.2021.111437","article-title":"Expanded titanosilicate\nMWW-related materials synthesized from a boron-containing precursor\nas an efficient catalyst for cyclohexene oxidation","volume":"327","author":"Tang","year":"2021","journal-title":"Microporous Mesoporous Mater."},{"key":"2026091609123213900_cit31","doi-asserted-by":"publisher","first-page":"110645","DOI":"10.1016\/j.micromeso.2020.110645","article-title":"Atom-planting synthesis of MCM-36 catalyst to investigate\nthe influence of pore structure and titanium coordination state on\nepoxidation activity","volume":"310","author":"Wang","year":"2021","journal-title":"Microporous Mesoporous\nMater."},{"key":"2026091609123213900_cit32","doi-asserted-by":"publisher","first-page":"260","DOI":"10.1007\/s10562-022-03954-z","article-title":"Effect of surface polarity\nof titanium-loaded ERB-1 catalyst on epoxidation and ammoximation","volume":"153","author":"Xu","year":"2023","journal-title":"Catal. Lett."},{"key":"2026091609123213900_cit33","doi-asserted-by":"publisher","first-page":"44","DOI":"10.1016\/j.micromeso.2012.06.035","article-title":"Direct synthesis of a titanosilicate\nmolecular sieve containing large and medium pores in its structure","volume":"164","author":"Moliner","year":"2012","journal-title":"Microporous Mesoporous Mater."},{"key":"2026091609123213900_cit34","doi-asserted-by":"publisher","first-page":"113319","DOI":"10.1016\/j.micromeso.2024.113319","article-title":"One-step synthesis\nof hierarchical Ti-MCM-41\/MFI composites for cyclohexene epoxidation\nreactions","volume":"380","author":"Lv","year":"2024","journal-title":"Microporous Mesoporous Mater."},{"key":"2026091609123213900_cit35","doi-asserted-by":"publisher","first-page":"362","DOI":"10.1126\/science.1120560","article-title":"Solvent-free oxidation\nof primary alcohols to aldehydes using Au-Pd\/TiO2 catalysts","volume":"311","author":"Enache","year":"2006","journal-title":"Science"},{"key":"2026091609123213900_cit36","doi-asserted-by":"publisher","first-page":"832","DOI":"10.1038\/39843","article-title":"Solvent-assisted proton transfer\nin catalysis by zeolite solid acids","volume":"389","author":"Haw","year":"1997","journal-title":"Nature"},{"issue":"1","key":"2026091609123213900_cit37","doi-asserted-by":"publisher","first-page":"1060","DOI":"10.1038\/s41467-020-14860-6","article-title":"Understanding solvent effects on adsorption and protonation\nin porous catalysts","volume":"11","author":"Gould","year":"2020","journal-title":"Nat. Commun."},{"key":"2026091609123213900_cit38","doi-asserted-by":"publisher","first-page":"11301","DOI":"10.1021\/jacs.4c18771","article-title":"Hydroformylation over Zeolite Catalysts with Solvophobic\nMicropores","volume":"147","author":"Wu","year":"2025","journal-title":"J. Am. Chem. Soc."},{"key":"2026091609123213900_cit39","doi-asserted-by":"publisher","first-page":"1068","DOI":"10.1126\/science.aao0092","article-title":"Control of zeolite framework\nflexibility and pore topology for separation of ethane and ethylene","volume":"358","author":"Bereciartua","year":"2017","journal-title":"Science"},{"key":"2026091609123213900_cit40","doi-asserted-by":"publisher","first-page":"491","DOI":"10.1126\/science.abn7667","article-title":"In situ imaging of the sorption-induced subcell topological flexibility\nof a rigid zeolite framework","volume":"376","author":"Xiong","year":"2022","journal-title":"Science"},{"issue":"12","key":"2026091609123213900_cit41","doi-asserted-by":"publisher","first-page":"962","DOI":"10.1038\/nmat1784","article-title":"The flexibility window in zeolites","volume":"5","author":"Sartbaeva","year":"2006","journal-title":"Nat. Mater."},{"issue":"1","key":"2026091609123213900_cit42","doi-asserted-by":"publisher","first-page":"269","DOI":"10.1016\/j.micromeso.2007.02.041","article-title":"Catalytical studies on trimethylsilylated\nTi-MCM-41 and Ti-MCM-48 materials","volume":"104","author":"Igarashi","year":"2007","journal-title":"Microporous\nMesoporous Mater."},{"issue":"3","key":"2026091609123213900_cit43","doi-asserted-by":"publisher","first-page":"318","DOI":"10.1039\/B300244F","article-title":"Green and selective epoxidation of alkenes catalysed\nby new TiO 2 \u2212SiO 2 SBA mesoporous solids","volume":"5","author":"Chiker","year":"2003","journal-title":"Green Chem."},{"issue":"2","key":"2026091609123213900_cit44","doi-asserted-by":"publisher","first-page":"513","DOI":"10.1016\/j.jcat.2004.11.024","article-title":"Optimisation of olefin\nepoxidation catalysts with the application of high-throughput and\ngenetic algorithms assisted by artificial neural networks (softcomputing\ntechniques)","volume":"229","author":"Corma","year":"2005","journal-title":"J. Catal."},{"key":"2026091609123213900_cit45","doi-asserted-by":"publisher","first-page":"76","DOI":"10.1016\/j.micromeso.2017.01.035","article-title":"Synthesis and modification of titanium containing wrinkled mesoporous\nsilica for cyclohexene epoxidation","volume":"243","author":"Wang","year":"2017","journal-title":"Microporous\nMesoporous Mater."},{"key":"2026091609123213900_cit46","doi-asserted-by":"publisher","first-page":"257","DOI":"10.1023\/A:1016614218678","article-title":"The role of the solvent in TS-1 chemistry:\nactive or passive? An early study revisited","volume":"15","author":"Clerici","year":"2001","journal-title":"Top. Catal."},{"key":"2026091609123213900_cit47","doi-asserted-by":"publisher","first-page":"936","DOI":"10.1016\/j.catcom.2006.04.008","article-title":"Is 1-hexene epoxidation in TS-1 diffusion limited in different solvents?","volume":"7","author":"Ramachandran","year":"2006","journal-title":"Catal. Commun."},{"key":"2026091609123213900_cit48","doi-asserted-by":"publisher","first-page":"79","DOI":"10.1023\/A:1019079328642","article-title":"Effects of hydrophobicity on the\nepoxidation of cyclohexene by tert-butyl hydroperoxide on TiO2\u2013SiO2\nmixed oxides","volume":"59","author":"Figueras","year":"1999","journal-title":"Catal. Lett."}],"container-title":["Journal of\nthe American Chemical Society"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jacs.6c12516","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/148\/36\/39112\/68332793\/jacs.6c12516.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/148\/36\/39112\/68332793\/jacs.6c12516.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,9,16]],"date-time":"2026-09-16T13:49:41Z","timestamp":1789566581000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/jacsat\/article\/148\/36\/39112\/5416595\/Solvent-Free-Catalysis-Unlocks-Bulky-Molecule"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,9,3]]},"references-count":48,"journal-issue":{"issue":"36","published-online":{"date-parts":[[2026,9,3]]},"published-print":{"date-parts":[[2026,9,16]]}},"URL":"https:\/\/doi.org\/10.1021\/jacs.6c12516","relation":{},"ISSN":["0002-7863","1520-5126"],"issn-type":[{"value":"0002-7863","type":"print"},{"value":"1520-5126","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,9,3]]}}}