Cited by 115Zeolite Catalysis and SynthesisChemical Synthesis and CharacterizationMetal-Organic Frameworks: Synthesis and Applications

Studies on the Role of Fluoride Ion vs Reaction Concentration in Zeolite Synthesis

Zones, Stacey I., Darton, Richard J., Morris, Russell, Hwang, Son-Jong·2005·The Journal of Physical Chemistry B

Abstract

This work is an experimental response to an intriguing paper recently published by Catlow and co-workers, which looked at the computational feasibility of fluorine location in three different all-silica zeotypes (Attfield, M. P.; Catlow, C. R. A.; Sokol, A. A. Chem. Mater. 2001, 13, 4708). The materials were chosen as representative of three unique host locations. Our present work examined the synthesis of zeotypes AST, IFR, and MTT using organo-cations with a strong preference for crystallizing these structures. We studied the effect of reaction time and the H(2)O/SiO(2) reactant ratio. The latter is probably the most important function in these zeolite crystallizations that use HF. As reaction conditions became more dilute, AST gave way to SGT and IFR to MTW as host structures, while the MTT synthesis was invariant. Our reactions were studied in terms of product yield vs time, product organo-cation content, fluorine content, and the representative (29)Si and (19)F NMR spectra for certain samples. A single crystal study was carried out for a sample of MTT. Our results showed that, consistent with other recent studies, low H(2)O/SiO(2) reactant ratios lead to more open framework host structures (i.e., IFR vs MTW), and there is typically a higher uptake of organo-cation and fluorine. The structure may well contain a higher population of 4-rings within the silicate substructure. While MTT that contains no 4-rings was chosen as the best possible candidate to achieve an ion-pair for the organo-cation and fluoride anion within the silicate host, both NMR and single crystal work confirm that fluoride is bonded to a 5-coordinate silica center within the lattice.

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Crossref · 10.1021/jp0402434

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  • The H2O/SiO2 ratio affects which kind of frameworks will be obtainable based on the density of the final material and the size of the crystals, especially in high silica gels in fluoride media.

    “The H2O/SiO2 ratio is important as well, especially in high silica gels in fluoride media, as it affects which kind of frameworks will be obtainable based on the density of the final material and the size of the crystals.113,117,118”

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Authors
Zones, S. I., Darton, R. J., Morris, R., & Hwang, S.-J.
Affiliations
California Institute of Technology (US)
Venue
The Journal of Physical Chemistry B
Published
2004-12-07
Volume
109
Issue
1
Pages
652-661
ISSN
  • 1520-5207 (ISSN-L)
  • 1520-6106
OpenAlex
W2023832328
Cited by
115
References
28
Citations by year
2026: 3 · 2025: 4 · 2024: 2 · 2023: 5 · 2022: 4 · 2021: 4 · 2020: 5 · 2019: 5 · 2018: 6 · 2017: 2 · 2016: 7 · 2015: 6 · 2014: 2 · 2013: 4 · 2012: 3
FWCI
5.28
Type
journal article
Language
en
Open access
closed
Locations
  • The Journal of Physical Chemistry B (publishedVersion)
  • PubMed (publishedVersion)
Topics
  • Physical Sciences › Chemistry › Inorganic Chemistry › Zeolite Catalysis and Synthesis
  • Physical Sciences › Environmental Science › Waste Management and Disposal › Chemical Synthesis and Characterization
  • Physical Sciences › Chemistry › Inorganic Chemistry › Metal-Organic Frameworks: Synthesis and Applications
Keywords
zeolite synthesis, fluoride, all-silica zeolites, reaction time (chemistry), ion pairs, single crystal structure, 29Si NMR, 19F NMR

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