Structure I methane hydrate confined in C8-grafted SBA-15: A highly efficient storage system enabling ultrafast methane loading and unloading

Confinement of water and methane in mesopores of hydrophobized SBA-15 is demonstrated to promote methane hydrate formation. In comparison to as-synthesized SBA-15, hydrophobization by C8 grafting accelerates the kinetics of methane storage in and delivery from the hydrate. C8 grafting density was de...

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Vydané v:Applied energy Ročník 353; s. 122120
Hlavní autori: Beckwée, Emile Jules, Houlleberghs, Maarten, Ciocarlan, Radu-George, Chandran, C. Vinod, Radhakrishnan, Sambhu, Hanssens, Lucas, Cool, Pegie, Martens, Johan, Breynaert, Eric, Baron, Gino V., Denayer, Joeri F.M.
Médium: Journal Article
Jazyk:English
Vydavateľské údaje: Elsevier Ltd 01.01.2024
Predmet:
Clathrate hydrate
crystallization
desorption
energy
Ice
Kinetics
methane
Methane hydrate
NMR
nuclear magnetic resonance spectroscopy
porosity
SBA-15
species
spectral analysis
surface area
X-ray diffraction
Methane hydrate
NMR
Ice
Clathrate hydrate
Kinetics
SBA-15
ISSN:0306-2619, 1872-9118
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Abstract Confinement of water and methane in mesopores of hydrophobized SBA-15 is demonstrated to promote methane hydrate formation. In comparison to as-synthesized SBA-15, hydrophobization by C8 grafting accelerates the kinetics of methane storage in and delivery from the hydrate. C8 grafting density was determined at 0.5 groups nm−2 based on TGA and quantitative NMR spectroscopy. Multinuclear 1H-1H DQSQ and 1H-1H RFDR NMR provided spectroscopic evidence for the occurrence of C8 chains inside the mesopores of SBA-15, by showcasing close spatial proximity between the grafted C8 chains and pore-intruded water species. X-ray diffraction demonstrates formation of Structure I hydrate on SBA-15 C8. At 7.0 MPa and 248 K, the water-to-hydrate conversion on hydrophobized SBA-15 C8 reaches 96% as compared to only 71% on a pristine SBA-15 sample with comparable pore size, pore volume and surface area. The clathrate loading amounted to 14.8 g/g. 2D correlation NMR spectroscopy (1H-13C CP-HETCOR, 1H-1H RFDR) reveals hydrate formation occurs within pores of SBA-15 C8 as well as in interparticle volumes. Following the initial crystallization of SBA-15 C8-supported methane hydrate taking several hours, a pressure swing process at 248 K allows to desorb and re-adsorb methane from the structure within minutes and without thawing the frozen water structure. Fast loading and unloading of methane was achieved in 19 subsequent cycles without losses in kinetics. The ability to harvest the gas and regenerate the structure without the need to re-freeze the water represents a 50% energy gain with respect to melting and subsequently recrystallizing the hydrate at 298 K and 248 K, respectively. After methane desorption, a small amount of residual methane hydrate in combination with an amorphous yet locally ordered ice phase is observed using 13C and 2H NMR spectroscopy. This effect offers an explanation for the enhanced hydrate formation kinetics in adsorption-desorption cycles. These findings open new perspectives for clathrate hydrate-based methane storage. [Display omitted] •Hydrophobization of SBA-15 accelerates methane enclathration.•2D NMR reveals hydrate present within pores of SBA-15 C8.•Methane loading times were reduced from 207 min to 8 min by pressure cycling.•Amorphous yet ordered ice is observed between storage cycles by 13C and 2H NMR.•Pressure-induced crystallization-dissociation of hydrate saves up to 50% energy.
AbstractList Confinement of water and methane in mesopores of hydrophobized SBA-15 is demonstrated to promote methane hydrate formation. In comparison to as-synthesized SBA-15, hydrophobization by C8 grafting accelerates the kinetics of methane storage in and delivery from the hydrate. C8 grafting density was determined at 0.5 groups nm−2 based on TGA and quantitative NMR spectroscopy. Multinuclear 1H-1H DQSQ and 1H-1H RFDR NMR provided spectroscopic evidence for the occurrence of C8 chains inside the mesopores of SBA-15, by showcasing close spatial proximity between the grafted C8 chains and pore-intruded water species. X-ray diffraction demonstrates formation of Structure I hydrate on SBA-15 C8. At 7.0 MPa and 248 K, the water-to-hydrate conversion on hydrophobized SBA-15 C8 reaches 96% as compared to only 71% on a pristine SBA-15 sample with comparable pore size, pore volume and surface area. The clathrate loading amounted to 14.8 g/g. 2D correlation NMR spectroscopy (1H-13C CP-HETCOR, 1H-1H RFDR) reveals hydrate formation occurs within pores of SBA-15 C8 as well as in interparticle volumes. Following the initial crystallization of SBA-15 C8-supported methane hydrate taking several hours, a pressure swing process at 248 K allows to desorb and re-adsorb methane from the structure within minutes and without thawing the frozen water structure. Fast loading and unloading of methane was achieved in 19 subsequent cycles without losses in kinetics. The ability to harvest the gas and regenerate the structure without the need to re-freeze the water represents a 50% energy gain with respect to melting and subsequently recrystallizing the hydrate at 298 K and 248 K, respectively. After methane desorption, a small amount of residual methane hydrate in combination with an amorphous yet locally ordered ice phase is observed using 13C and 2H NMR spectroscopy. This effect offers an explanation for the enhanced hydrate formation kinetics in adsorption-desorption cycles. These findings open new perspectives for clathrate hydrate-based methane storage. [Display omitted] •Hydrophobization of SBA-15 accelerates methane enclathration.•2D NMR reveals hydrate present within pores of SBA-15 C8.•Methane loading times were reduced from 207 min to 8 min by pressure cycling.•Amorphous yet ordered ice is observed between storage cycles by 13C and 2H NMR.•Pressure-induced crystallization-dissociation of hydrate saves up to 50% energy.
Confinement of water and methane in mesopores of hydrophobized SBA-15 is demonstrated to promote methane hydrate formation. In comparison to as-synthesized SBA-15, hydrophobization by C₈ grafting accelerates the kinetics of methane storage in and delivery from the hydrate. C₈ grafting density was determined at 0.5 groups nm⁻² based on TGA and quantitative NMR spectroscopy. Multinuclear ¹H-¹H DQSQ and ¹H-¹H RFDR NMR provided spectroscopic evidence for the occurrence of C₈ chains inside the mesopores of SBA-15, by showcasing close spatial proximity between the grafted C₈ chains and pore-intruded water species. X-ray diffraction demonstrates formation of Structure I hydrate on SBA-15 C₈. At 7.0 MPa and 248 K, the water-to-hydrate conversion on hydrophobized SBA-15 C₈ reaches 96% as compared to only 71% on a pristine SBA-15 sample with comparable pore size, pore volume and surface area. The clathrate loading amounted to 14.8 g/g. 2D correlation NMR spectroscopy (¹H-¹³C CP-HETCOR, ¹H-¹H RFDR) reveals hydrate formation occurs within pores of SBA-15 C₈ as well as in interparticle volumes. Following the initial crystallization of SBA-15 C₈-supported methane hydrate taking several hours, a pressure swing process at 248 K allows to desorb and re-adsorb methane from the structure within minutes and without thawing the frozen water structure. Fast loading and unloading of methane was achieved in 19 subsequent cycles without losses in kinetics. The ability to harvest the gas and regenerate the structure without the need to re-freeze the water represents a 50% energy gain with respect to melting and subsequently recrystallizing the hydrate at 298 K and 248 K, respectively. After methane desorption, a small amount of residual methane hydrate in combination with an amorphous yet locally ordered ice phase is observed using ¹³C and ²H NMR spectroscopy. This effect offers an explanation for the enhanced hydrate formation kinetics in adsorption-desorption cycles. These findings open new perspectives for clathrate hydrate-based methane storage.
ArticleNumber 122120
Author Cool, Pegie
Beckwée, Emile Jules
Hanssens, Lucas
Ciocarlan, Radu-George
Breynaert, Eric
Radhakrishnan, Sambhu
Baron, Gino V.
Chandran, C. Vinod
Martens, Johan
Denayer, Joeri F.M.
Houlleberghs, Maarten
Author_xml – sequence: 1
  givenname: Emile Jules
  surname: Beckwée
  fullname: Beckwée, Emile Jules
  organization: Department of Chemical Engineering, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussel, Belgium
– sequence: 2
  givenname: Maarten
  surname: Houlleberghs
  fullname: Houlleberghs, Maarten
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 3
  givenname: Radu-George
  surname: Ciocarlan
  fullname: Ciocarlan, Radu-George
  organization: Laboratory of Adsorption and Catalysis, Department of Chemistry, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk, Belgium
– sequence: 4
  givenname: C. Vinod
  surname: Chandran
  fullname: Chandran, C. Vinod
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 5
  givenname: Sambhu
  surname: Radhakrishnan
  fullname: Radhakrishnan, Sambhu
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 6
  givenname: Lucas
  surname: Hanssens
  fullname: Hanssens, Lucas
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 7
  givenname: Pegie
  surname: Cool
  fullname: Cool, Pegie
  organization: Laboratory of Adsorption and Catalysis, Department of Chemistry, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk, Belgium
– sequence: 8
  givenname: Johan
  surname: Martens
  fullname: Martens, Johan
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 9
  givenname: Eric
  surname: Breynaert
  fullname: Breynaert, Eric
  organization: Centre for Surface Chemistry and Catalysis, NMRCoRe - NMR - XRAY - EM Platform for Convergence Research, Department of Microbial and Molecular Systems (M2S), KU Leuven, Celestijnenlaan 200F, 3001 Leuven, Belgium
– sequence: 10
  givenname: Gino V.
  surname: Baron
  fullname: Baron, Gino V.
  organization: Department of Chemical Engineering, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussel, Belgium
– sequence: 11
  givenname: Joeri F.M.
  surname: Denayer
  fullname: Denayer, Joeri F.M.
  email: joeri.denayer@vub.be
  organization: Department of Chemical Engineering, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussel, Belgium
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Keywords Methane hydrate
NMR
Ice
Clathrate hydrate
Kinetics
SBA-15
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Snippet Confinement of water and methane in mesopores of hydrophobized SBA-15 is demonstrated to promote methane hydrate formation. In comparison to as-synthesized...
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StartPage 122120
SubjectTerms Clathrate hydrate
crystallization
desorption
energy
Ice
Kinetics
methane
Methane hydrate
NMR
nuclear magnetic resonance spectroscopy
porosity
SBA-15
species
spectral analysis
surface area
X-ray diffraction
Title Structure I methane hydrate confined in C8-grafted SBA-15: A highly efficient storage system enabling ultrafast methane loading and unloading
URI https://dx.doi.org/10.1016/j.apenergy.2023.122120
https://www.proquest.com/docview/3040444776
Volume 353
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