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Using ZSM-5 as a model, samples with varied dealumination degrees were prepared by adjusting treatment time. Advanced solid-state nuclear magnetic resonance (NMR) techniques including 1H\u20131H double-quantum single-quantum (DQ-SQ), triple-quantum single-quantum (TQ-SQ), and hyperpolarized (HP) 129Xe NMR were employed to track the structural evolution of framework Al. These results reveal that alkaline treatment progressively removes framework Al, leading to a decrease in Br\u00f8nsted acid site (BAS) density. Extracted Al initially forms hydroxylated tetracoordinated Al\u2013OH (AlIV), not directly octahedral extra-framework species. HP 129Xe NMR reveals altered micropore environments from Al removal and redeposition. Alkaline treatment prolongs the methanol to olefin reaction lifetime to 70 h via synergistic mass transport and acidity effects. This work elucidates framework Al evolution during alkaline treatment, offering insights for precise zeolite modification and catalyst design.<\/jats:p>","DOI":"10.1021\/acs.jpclett.6c02364","type":"journal-article","created":{"date-parts":[[2026,8,21]],"date-time":"2026-08-21T20:14:03Z","timestamp":1787343243000},"page":"10293-10301","source":"Crossref","is-referenced-by-count":0,"title":["Unveiling the\nStructural Evolution and Deposition\nBehavior of Leached Al Species during Alkaline Treatment of ZSM-5\nZeolites"],"prefix":"10.1021","volume":"17","author":[{"given":"Huihui","family":"Chen","sequence":"first","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jing","family":"Niu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinzhi","family":"Ding","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6204-0022","authenticated-orcid":true,"given":"Caiyi","family":"Lou","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junjie","family":"Li","sequence":"additional","affiliation":[{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1518-3930","authenticated-orcid":true,"given":"Yuchun","family":"Zhi","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0412-1980","authenticated-orcid":true,"given":"Yingxu","family":"Wei","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7999-2940","authenticated-orcid":true,"given":"Zhongmin","family":"Liu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4722-8371","authenticated-orcid":true,"given":"Shutao","family":"Xu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"Dalian Institute of Chemical Physics, Chinese Academy of Sciences , , 457 Zhongshan Road , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]},{"name":"Liaoning Binhai Laboratory , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,20]]},"reference":[{"issue":"2","key":"2026090315413086500_cit1","doi-asserted-by":"publisher","first-page":"226","DOI":"10.1002\/anie.198802261","article-title":"Zeolites:\nCatalysts for Organic Syntheses","volume":"27","author":"Ho\u0308lderich","year":"1988","journal-title":"Angew. 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Dissolution of activated silicalite-1 and\nZSM-5 with different aluminum content","volume":"4","author":"C\u030ciz\u030cmek","year":"1997","journal-title":"Microporous\nmaterials"},{"issue":"4","key":"2026090315413086500_cit28","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202416564","article-title":"Unravelling\nthe Crucial of Spatial Al Distribution to Realize Precise Alkali-Treatment\nfor Target Acid-Catalyzed Reactions","volume":"64","author":"Li","year":"2025","journal-title":"Angew.\nChem., Int. Ed."},{"issue":"16","key":"2026090315413086500_cit29","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202523357","article-title":"Engineering Al-Pair-Enriched\nHierarchical\nZeolites via D-6R SBU-Directed Aluminum Reorganization During Desilication","volume":"65","author":"Yu","year":"2026","journal-title":"Angew. Chem., Int. 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