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Herein, three novel spongy-like chitosan-based covalent organic framework (CS-COF) aerogels (Captors 1\u20133) were synthesized for the selective adsorption of Cd2+ ions. Captors 1\u20133 were fabricated via a Schiff base reaction between CS and three aldehyde (\u2212CHO)-containing cross-linkers (terephthalaldehyde, [1,1\u2032-biphenyl]-4,4\u2032-dicarbaldehyde, and 2,3-dihydroxyterephthalaldehyde), yielding ultralight monolithic aerogels (5.0\u201320.3 mg\/cm3) with ordered 2D crystalline frameworks, uniform micropore distributions (1.37\u20131.60 nm), and abundant multifunctional active sites (\u2212HC\u2550N\u2013, \u2212NH2, \u2212OH). Such features synergistically enable fast Cd2+ ion transfer and strong Cd2+-binding events. Findings showed that Captors 1\u20133 had high adsorption capacities (725.1\u2013771.5 mg\/g) and removed over 95% of Cd2+ within 10 s at pH 8.0. The Langmuir and pseudo-second-order models confirmed that the adsorption process is primarily driven by chemisorption. Computational modeling, XPS, and elemental mapping revealed that Cd2+ adsorption proceeds via covalent and noncovalent interactions. Selectivity over competing cations at pH 8 arises principally from speciation. Cd2+ remains fully cationic while several competitors hydrolyze to species of reduced charge. Geometric matching between the imine-rich chelating pocket and the Cd2+\u2019s octahedral coordination preference reinforces this effect. Captors 1\u20133 retained &amp;gt;90% removal efficiency after five regeneration cycles and achieved &amp;gt;90% Cd2+ removal from real water matrices, confirming structural robustness and practical applicability. This work establishes a rational, scalable, and eco-friendly CS-COF aerogel platform with broad potential for environmental remediation applications.<\/jats:p>","DOI":"10.1021\/jacs.6c11066","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:16:00Z","timestamp":1785849360000},"page":"33865-33883","source":"Crossref","is-referenced-by-count":1,"title":["Schiff Base-Derived\nMicroporous Covalent Organic Framework\nAerogels as Chemo-Captors for Exceptional Rapid, High-Capacity, and\nSelective Cadmium Ion Adsorption"],"prefix":"10.1021","volume":"148","author":[{"given":"Hassanien","family":"Gomaa","sequence":"first","affiliation":[{"name":"Nankai University , , ,","place":["Tianjin, China, 300071"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wei-Liang","family":"Jin","sequence":"additional","affiliation":[{"name":"Nankai University , , ,","place":["Tianjin, China, 300071"]},{"name":"Tianjin University , , ,","place":["Tianjin, China, 300072"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rui","family":"Wang","sequence":"additional","affiliation":[{"name":"Nankai University , , ,","place":["Tianjin, China, 300071"]},{"name":"Tianjin University , , ,","place":["Tianjin, China, 300072"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hong-Xin","family":"Jiang","sequence":"additional","affiliation":[{"name":"Ministry of Agriculture and Rural Affairs , , ,","place":["Tianjin, China, 300191"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5411-9216","authenticated-orcid":true,"given":"An-Na","family":"Tang","sequence":"additional","affiliation":[{"name":"Nankai University , , ,","place":["Tianjin, China, 300071"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6396-1592","authenticated-orcid":true,"given":"Li-Na","family":"Zhu","sequence":"additional","affiliation":[{"name":"Tianjin University , , ,","place":["Tianjin, China, 300072"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9216-8040","authenticated-orcid":true,"given":"De-Ming","family":"Kong","sequence":"additional","affiliation":[{"name":"Nankai University , , ,","place":["Tianjin, China, 300071"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,29]]},"reference":[{"key":"2026081210095135300_cit1","doi-asserted-by":"publisher","DOI":"10.1016\/j.psep.2025.106965","article-title":"Tailored\nGlutamine Modified Nanozeolite-Y\/Xanthan Gum Composite Based on Rice\nStraw for Enhanced Adsorption of Cadmium Ions from Aqueous Media","volume":"196","author":"Obaid","year":"2025","journal-title":"Process Saf. 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