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Here, we deploy five metal\u2013organic frameworks with graded pore apertures to elucidate pore-size effects on HMF adsorption. Integrated kinetic, thermodynamic, and dynamic breakthrough studies reveal a volcano-type trend governed by a dual trade-off between steric accessibility and spatial confinement. MIL-53(Al)-TDC, with an optimally matched 8.1 \u00c5 pore balancing rapid intracrystalline diffusion with strong host\u2013guest affinity, synergizes \u03c0\u2013\u03c0 stacking and hydrophobic microenvironments to deliver an HMF capacity of 579.58 mg\u00b7g\u20131 and mass transfer coefficient of 22.36 L\u00b7g\u20131\u00b7h\u20131. Breakthrough experiments demonstrate its potential for continuous purification of simulated hydrolysate. A technoeconomic assessment confirms 33\u201350% lower equipment investment and 47\u201351% lower annualized cost vs conventional distillation. This work establishes a predictive framework coupling pore commensurability with interfacial interactions, guiding rational design of adsorbents for biorefinery separations.<\/jats:p>","DOI":"10.1021\/acsami.6c13523","type":"journal-article","created":{"date-parts":[[2026,9,25]],"date-time":"2026-09-25T01:02:26Z","timestamp":1790298146000},"page":"54224-54240","source":"Crossref","is-referenced-by-count":0,"title":["Volcano-Type Pore-Size Dependence of HMF Adsorption in Aluminum-Based Metal\u2013Organic Frameworks: A Transport\u2013Affinity Tradeoff for Sugar Purification"],"prefix":"10.1021","volume":"18","author":[{"given":"Fei","family":"Xiao","sequence":"first","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5802-9944","authenticated-orcid":true,"given":"Xingjie","family":"Wang","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hao","family":"Zhao","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rui","family":"Li","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jianlin","family":"Wang","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7699-4484","authenticated-orcid":true,"given":"Libo","family":"Li","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, China, 510640"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7837-8252","authenticated-orcid":true,"given":"Junli","family":"Ren","sequence":"additional","affiliation":[{"name":"South China University of Technology , , ,","place":["Guangzhou, PR China, 510641"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,24]]},"reference":[{"key":"2026100708065220800_cit1","doi-asserted-by":"publisher","first-page":"743","DOI":"10.1016\/j.rser.2017.05.063","article-title":"Ethanol from biomass: a comparative overview","volume":"80","author":"Manochio","year":"2017","journal-title":"Renew. 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