Spectroscopic Investigation of the Mechanisms Responsible for the Superior Stability of Hybrid Class 1/Class 2 CO2 Sorbents: A New Class 4 Category

Wilfong, Walter Christopher; Kail, Brian W.; Jones, Christopher W.; Pacheco, Carlos; Gray, McMahan L.

doi:10.1021/acsami.6b02062

Title: Spectroscopic Investigation of the Mechanisms Responsible for the Superior Stability of Hybrid Class 1/Class 2 CO₂ Sorbents: A New Class 4 Category

Journal Article · Wed May 04 00:00:00 EDT 2016 · ACS Applied Materials and Interfaces

DOI:https://doi.org/10.1021/acsami.6b02062· OSTI ID:1433612

Wilfong, Walter Christopher ^[1]; Kail, Brian W. ^[2]; Jones, Christopher W. ^[3]; Pacheco, Carlos ^[4]; Gray, McMahan L. ^[5]

National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
AECOM, Oak Ridge, TN (United States)
Georgia Inst. of Technology, Atlanta, GA (United States). School of Chemical and Biomolecular Engineering
Pennsylvania State Univ., University Park, PA (United States). Dept. of Chemistry
National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)

Hybrid Class 1/Class 2 supported amine CO₂ sorbents demonstrate superior performance under practical steam conditions, yet their amine immobilization and stabilization mechanisms are unclear. Uncovering the interactions responsible for the sorbents’ robust features is critical for further improvements and can facilitate practical applications. We employ solid state ²⁹Si CP-MAS and 2-D FSLG ¹H–¹³C CP HETCOR NMR spectroscopies to probe the overall molecular interactions of aminosilane/silica, polyamine [poly(ethylenimine), PEI]/silica, and hybrid aminosilane/PEI/silica sorbents. A unique, sequential impregnation sorbent preparation method is executed in a diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) setup to decouple amine binding mechanisms at the amine–silica interface from those within bulk amine layers. These mechanisms are correlated with each sorbents’ resistance to accelerated liquid H₂O and TGA steam treatments (H₂O stability) and to oxidative degradation (thermal stability). High percentages of CO₂ capture retained (PCR) and organic content retained (OCR) values after H₂O testing of N-(3-(trimethoxysilyl)propyl)ethylenediamine (TMPED)/PEI and (3-aminopropyl)trimethoxysilane (APTMS)/PEI hybrid sorbents are associated with a synergistic stabilizing effect of the amine species observed during oxidative degradation (thermal gravimetric analysis-differential scanning calorimetry, TGA-DSC). Solid state NMR spectroscopy reveals that the synergistic effect of the TMPED/PEI mixture is manifested by the formation of hydrogen-bonded PEI–NH₂···NH₂–TMPED and PEI–NH₂···HO–Si/O–Si–O (TMPED, T²) linkages within the sorbent. DRIFTS further determines that PEI enhances the grafting of TMPED to silica and that PEI is dispersed among a stable network of polymerized TMPED in the bulk, utilizing H-bonded linkages. These findings provide the scientific basis for establishing a Class 4 category for aminosilane/polyamine/silica hybrid sorbents.

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Research Organization:: Oak Ridge Inst. for Science and Education (ORISE), Oak Ridge, TN (United States); National Energy Technology Laboratory (NETL), Pittsburgh, PA, Morgantown, WV (United States)

Sponsoring Organization:: USDOE Office of Fossil Energy (FE); AECOM, Oak Ridge, TN (United States); National Science Foundation (NSF)

Grant/Contract Number:: CBET-1403239; DE-FE0004000

OSTI ID:: 1433612

Journal Information:: ACS Applied Materials and Interfaces, Vol. 8, Issue 20; ISSN 1944-8244

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 39 works

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Title: Spectroscopic Investigation of the Mechanisms Responsible for the Superior Stability of Hybrid Class 1/Class 2 CO2 Sorbents: A New Class 4 Category

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Title: Spectroscopic Investigation of the Mechanisms Responsible for the Superior Stability of Hybrid Class 1/Class 2 CO₂ Sorbents: A New Class 4 Category