{sup 1}H and {sup 23}Na MAS NMR spectroscopy of cationic species in CO{sub 2} selective alkaline earth metal porous silicoaluminophosphates prepared via liquid and solid state ion exchange

Journal Article · Sun Jul 15 04:00:00 EDT 2012 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2012.03.005· OSTI ID:22012172

Arevalo-Hidalgo, Ana G ^[1]; Dugar, Sneha; Fu, Riqiang ^[2]

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1. Department of Chemical Engineering, University of Puerto Rico-Mayagueez Campus, Mayagueez, PR 00681-9000 (Puerto Rico)
2. National High Magnetic Field Laboratory, Florida State University, Tallahassee, FL 32310 (United States)

The location of extraframework cations in Sr{sup 2+} and Ba{sup 2+} ion-exchanged SAPO-34 was estimated by means of {sup 1}H and {sup 23}Na MAS NMR spectroscopy and spectral deconvolution. Incorporation of the alkaline earth metal cations onto the SAPO framework was achieved via liquid state ion exchange, coupled partial detemplation/solid-state ion exchange, and combination of both techniques. MAS NMR revealed that the level of ion exchange was limited by the presence of protons and sodium cations near hexagonal prisms (site SI), which are relatively difficult to exchange with the alkaline earth metal due to steric and charge repulsion criteria. In addition, the presence of ammonium cations in the supercages facilitated the exchange of otherwise tenacious hydrogen as corroborated by unit cell compositional data as well as enhanced CO{sub 2} adsorption at low partial pressures. The extraframework ammonium species were produced from partial detemplation of the structure-directing agent employed for the SAPO-34 synthesis, tetraethylammonium. - Graphical abstract: MAS NMR was used to elucidate the position the cationic species in alkaline earth metal exchanged silicoaluminophosphates. These species played a significant role during the ion exchange process and, therefore, the materials ultimate CO{sub 2} adsorption performance. Highlights: Black-Right-Pointing-Pointer Location of extraframework Sr{sup 2+} or Ba{sup 2+} cations was estimated by means of {sup 1}H and {sup 23}Na MAS NMR. Black-Right-Pointing-Pointer Level of Sr{sup 2+} or Ba{sup 2+} ion exchange was limited by the presence of protons and sodium cations. Black-Right-Pointing-Pointer Presence of ammonium cations in the supercages facilitated the exchange. Black-Right-Pointing-Pointer Sr{sup 2+} and Ba{sup 2+} ion exchanged SAPOs are outstanding CO{sub 2} adsorbents.

• OSTI ID: 22012172
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. . 191; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ADSORBENTS
ADSORPTION
ALKALINE EARTH METALS
BARIUM IONS
CARBON DIOXIDE
CATIONS
LIQUIDS
NUCLEAR MAGNETIC RESONANCE
PARTIAL PRESSURE
POROUS MATERIALS
PRISMS
SOLIDS
SPECTROSCOPY
STRONTIUM IONS
SYNTHESIS