Multinuclear MAS NMR Monitoring of the Effect of Silicate Speciation on the Mechanism of Zeolite BEA Formation: Toward Engineering of Crystal Size and Morphology

Ivanova, I.I.; Andriako, E.P.; Kostyukov, I.A.; Zasukhin, D.S.; Fedosov, D.A.; Zarubin, D.N.

Статья опубликована в высокорейтинговом журнале

Информация о цитировании статьи получена из Scopus
Статья опубликована в журнале из списка Web of Science и/или Scopus
Дата последнего поиска статьи во внешних источниках: 20 февраля 2024 г.

Авторы: Ivanova Irina I., Andriako Egor P., Kostyukov Ilya A., Zasukhin Dmitry S., Fedosov Daniil A., Zarubin Dmitry N.
Журнал: Crystal Growth and Design
Том: 23
Номер: 8
Год издания: 2023
Издательство: American Chemical Society
Местоположение издательства: United States
Первая страница: 5677
Последняя страница: 5689
DOI: 10.1021/acs.cgd.3c00336
Аннотация: Time-resolved in situ 13C, 27Al, and 29Si MAS NMR and ex situ XRD, X-ray fluorescence, and TG studies have been applied for the elucidation of the mechanisms of hydrothermal synthesis of zeolite BEA from a clear solution and a dense hydrogel. Isotopic labeling with 29Si and 13C isotopes has been used to follow the fate of siliceous species and structure-directing agent ((13CH3-CH3)4NOH)). The results point to different mechanistic pathways depending on silicate speciation in the initial reaction mixture: (i) an aggregation/nucleation process for the reaction mixture prepared from a colloidal silica source and (ii) solution-mediated crystallization for the reaction mixture prepared from a dense silica hydrogel. The products obtained have been characterized using a set of physicochemical methods including XRD, X-ray fluorescence analysis, TEM, low-temperature nitrogen adsorption–desorption, and NH3-TPD. The results demonstrate that the crystallization mechanism affects the crystal size and morphology: the aggregation/nucleation process leads to very tiny crystals with a size of 5–15 nm, whereas solution-mediated crystallization results in dense polycrystals with a size of 300–700 nm with the core enriched with Al. The evaluation of the catalysts in liquid-phase alkylation of benzene with propylene points to the higher activity of zeolite BEA obtained from a colloidal silica source.
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Multinuclear MAS NMR Monitoring of the Effect of Silicate Speciation on the Mechanism of Zeolite BEA Formation: Toward Engineering of Crystal Size and Morphologyстатья Исследовательская статья

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