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  Unraveling Direct Formation of Hierarchical Zeolite Beta by Dynamic Light Scattering, Small Angle X-ray Scattering, and Liquid and Solid State NMR: Insights at the Supramolecular Level

Castro, M., Losch, P., Park, W., Haouas, M., Taulelle, F., Loerbroks, C., et al. (2018). Unraveling Direct Formation of Hierarchical Zeolite Beta by Dynamic Light Scattering, Small Angle X-ray Scattering, and Liquid and Solid State NMR: Insights at the Supramolecular Level. Chemistry of Materials, 30(8), 2676-2686. doi:10.1021/acs.chemmater.8b00109.

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 Creators:
Castro, Maria1, Author              
Losch, Pit1, Author              
Park, Woojin2, Author
Haouas, Mohamed3, Author
Taulelle, Francis4, Author
Loerbroks, Claudia5, Author              
Brabants, Gert4, Author
Breynaert, Eric4, Author
Kirschhock, Christine4, Author
Ryoo, Ryong2, Author
Schmidt, Wolfgang1, Author              
Affiliations:
1Research Group Schmidt, Max-Planck-Institut für Kohlenforschung, Max Planck Society, ou_1445618              
2CNCR, Institute for Basic Science, Daejeon 34141, Republic of Korea, ou_persistent22              
3Institut Lavoisier de Versailles, UVSQ, CNRS, 78000 Versailles, France, ou_persistent22              
4Center for Surface Chemistry and Catalysis, KU Leuven, Leuven 3000, Belgium, ou_persistent22              
5Research Department Thiel, Max-Planck-Institut für Kohlenforschung, Max Planck Society, ou_1445590              

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 Abstract: A case study on the understanding of the formation of hierarchical Beta zeolites using gemini-type piperidine based multiammonium surfactant (N6-diphe) is reported. Complementary techniques were used to investigate N6-diphe’s structure-directing effect at the molecular level. Combining characterization of the resulting zeolite materials with the toolboxes herein developed for studying clear solutions and dense gels discloses self-assembly processes that govern the growth (and growth inhibition) of nano-Beta zeolite crystals. In clear solution, small-angle X-ray scattering and liquid-state NMR provide insights about the formation of nanoparticles and their degree of order. 14N and 1H-DOSY NMR probe the dynamics and mobility of soluble species. In a dense gel, on the other side, 27Al- and 29Si-(MAS) NMR elucidate the varying local connectivity between initial nano-objects and the final solid products. It has been found that cylindrical micelles control the transformation of solubilized silica and alumina during the formation of zeolite nuclei and guide their crystal growth to nano-Beta rods with bimodal mesoporosity. The predominant smaller mesopores (6 to 8 nm) originate from the template’s hydrophobic alkyl chains, while larger mesopores (10 to 30 nm) are supposed to result from a spinodal decomposition-type segregation of phases consisting of as-formed hydrophobic zeolite rods and an aqueous solution.

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Language(s): eng - English
 Dates: 2018-01-102018-03-122018-04-24
 Publication Status: Published in print
 Pages: 11
 Publishing info: -
 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1021/acs.chemmater.8b00109
 Degree: -

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Title: Chemistry of Materials
  Abbreviation : Chem. Mater.
Source Genre: Journal
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Publ. Info: Washington, D.C. : American Chemical Society
Pages: - Volume / Issue: 30 (8) Sequence Number: - Start / End Page: 2676 - 2686 Identifier: ISSN: 0897-4756
CoNE: https://pure.mpg.de/cone/journals/resource/954925561571