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Carbon dioxide can act as a molecular stimulus for amine\u2010rich polymers such as PEIs, a property that has been exploited in CO\u2082\u2010mediated desalination. This process entails amine\u2010mediated CO\u2082 capture and the in situ formation of bicarbonate ions, which subsequently undergo ion exchange with chloride ions present in both model and real seawater. In this study, we prepared a series of alkylated PEIs with different chainlengths (C4\u2010C18) and degrees of alkylation (10\u201040% alkylation) via simple alkylation as previously reported. The obtained hydrophobic PEI, specifically PEI\u2010C16, was further investigated in terms of its crystalline structure using powder X\u2010ray diffraction, small\u2010angle X\u2010ray scattering, thermogravimetric analysis, and inelastic neutron scattering. Based on our analysis, we conclude that the subtle structural changes of hydrophobic poly(ethyleneimine)s were induced by acid\u2010mediated protonation and ion exchange, while the polymer maintained its integrity across multiple desalination cycles. These findings advocate for the employment of hydrophobic poly(ethyleneimine) in CO\u2082\u2010responsive processes and carbon capture applications.<\/jats:p>","DOI":"10.1002\/chem.202500764","type":"journal-article","created":{"date-parts":[[2025,5,8]],"date-time":"2025-05-08T04:53:44Z","timestamp":1746680024000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Comprehensive Analysis of Crystalline Hydrophobic Alkylated Poly(ethyleneimine)s"],"prefix":"10.1002","volume":"31","author":[{"given":"Anand Sharadha\u2010Ravi","family":"Ayyar","sequence":"first","affiliation":[{"name":"Department of Chemistry, Nano\u2010Science Center University of Copenhagen  Universitetsparken 5, Copenhagen \u00d8 Copenhagen 2100 Denmark"},{"name":"The Novo Nordisk Foundation CO<sub>2<\/sub> Research Center Aarhus University  Gustav Wieds Vej 10C Aarhus C 8000 Denmark"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1528-845X","authenticated-orcid":false,"given":"Rodrigo J. 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