Revealing long- and short-range structural modifications within phosphorus-treated HZSM-5 zeolites by atom probe tomography, nuclear magnetic resonance and powder X-ray diffraction

Danisi, Rosa Micaela; Schmidt, Joel E.; Lucini Paioni, Alessandra; Houben, Klaartje; Poplawsky, Jonathan D.; Baldus, Marc; Weckhuysen, Bert M.; Vogt, Eelco T.  C.

doi:10.1039/c8cp03828g

Revealing long- and short-range structural modifications within phosphorus-treated HZSM-5 zeolites by atom probe tomography, nuclear magnetic resonance and powder X-ray diffraction

Journal Article · Thu Aug 23 00:00:00 EDT 2018 · Physical Chemistry Chemical Physics. PCCP

DOI:https://doi.org/10.1039/c8cp03828g· OSTI ID:1482432

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Utrecht University (The Netherlands). Inorganic Chemistry and Catalysis
Utrecht University (The Netherlands). NMR Spectroscopy, Bijvoet Center for Biomolecular Research
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science (CNMS)
Utrecht University (The Netherlands). Inorganic Chemistry and Catalysis; Albemarle Catalyst Company BV, Amsterdam (The Netherlands)

In this study, the average and the local structure of phosphorus-treated HZSM-5 zeolites were investigated by means of atom probe tomography, powder X-ray diffraction (at ambient and cryogenic temperatures) and ¹H, ²⁹Si, ²⁷Al, and ³¹P magic angle spinning (MAS) solid state nuclear magnetic resonance (NMR) spectroscopy. Phosphatation to yield a product with P/Al ≤ 1 followed by thermal treatment leads to breaking of the Si–OH–Al bridging groups, and subsequent partial dealumination of the zeolite framework, as shown by the contraction of the orthorhombic unit-cell volume and by the loss of tetrahedral framework Al, as observed in the ²⁷Al Multiple Quantum (MQ) MAS NMR spectrum. Most of the framework Al is present in an electronic environment distorted by the presence of phosphorus and appears not to be involved in classic Si–OH–Al Brønsted acid sites. The ³¹P MAS NMR signals indicate that phosphorus interacts with the zeolitic framework to locally form silico-aluminophosphate (SAPO) domains and the presence of a new kind of acidic site was confirmed by the resonance at ~8.6 ppm in the ¹H MAS NMR spectra, attributed to P–OH groups. Increasing the phosphorus loading (P/Al >> 1) promotes further dealumination of the framework and cross-dehydroxylation between P–OH and Si–OH species, leading to the formation of a crystalline silicon orthophosphate phase. With decreasing Al content, the monoclinic HZSM-5 structure becomes preferred, especially at 85 K where the strain relaxation is higher. Nevertheless, the presence of a higher amount of silicophosphate impurities hinders the low-temperature strain release of the framework, indicating that some of these species are localized in the zeolite pores and contribute to the strain build up.

View Accepted Manuscript (DOE)

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1482432

Journal Information:: Physical Chemistry Chemical Physics. PCCP, Journal Name: Physical Chemistry Chemical Physics. PCCP Journal Issue: 44 Vol. 20; ISSN 1463-9076; ISSN PPCPFQ

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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