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Time‐Resolved In Situ MAS NMR Monitoring of the Nucleation and Growth of Zeolite BEA Catalysts under Hydrothermal Conditions
Author(s) -
Ivanova Irina I.,
Kolyagin Yury G.,
Kasyanov Ivan A.,
Yakimov Alexander V.,
Bok Tatiana O.,
Zarubin Dmitry N.
Publication year - 2017
Publication title -
angewandte chemie
Language(s) - English
Resource type - Journals
eISSN - 1521-3757
pISSN - 0044-8249
DOI - 10.1002/ange.201709039
Subject(s) - hydrothermal circulation , zeolite , nucleation , hydrothermal synthesis , mesoporous material , in situ , catalysis , chemistry , solid state nuclear magnetic resonance , chemical engineering , materials science , organic chemistry , nuclear magnetic resonance , physics , engineering
Time‐resolved 13 C, 23 Na, 27 Al, and 29 Si MAS NMR has been applied in situ for monitoring the hydrothermal synthesis of zeolite BEA. Isotopic labelling with 29 Si and 13 C isotopes has been used to follow the fate of siliceous species and structure directing agent (( 13 CH 3 −CH 2 ) 4 NOH). Two mechanistic pathways, namely solution‐mediated and solid–solid hydrogel rearrangement have been distinguished for two synthesis procedures studied. The mechanisms of structure‐directing behavior of TEA + cations in two reaction pathways have been elucidated. The results show that multinuclear MAS NMR can serve as a superior tool for monitoring hydrothermal synthesis of various solids including zeolites, zeotypes, mesoporous materials, metal–organic frameworks and so on and for the design of novel outstanding materials for different applications.