Epoxide-assisted alumina aerogels by rapid supercritical extraction

Stephen J. Juhl; Nicholas J.H. Dunn; Mary K. Carroll; Ann M. Anderson; Bradford A. Bruno; José E. Madero; Michael S. Bono

doi:10.1016/j.jnoncrysol.2015.06.030

Epoxide-assisted alumina aerogels by rapid supercritical extraction

Stephen J. Juhl, Nicholas J.H. Dunn, Mary K. Carroll, Ann M. Anderson, Bradford A. Bruno, José E. Madero, Michael S. Bono

Research output: Contribution to journal › Article › peer-review

35 Scopus citations

Abstract

Aerogels offer a potential alternative to noble metals that could reduce both the cost and environmental impact associated with catalytic converter production. The environmental impact of the production of aerogel catalysts could be further reduced by using a rapid supercritical extraction (RSCE) technique, which reduces the time and solvent waste associated with aerogel preparation. Alumina aerogels, which have shown activity in catalyzing exhaust processing reactions, were prepared using an epoxide-assisted gelation technique with RSCE processing in a contained mold in a hydraulic hot press. Samples were characterized by FTIR, XRD, SEM, EDX, nitrogen adsorption porosimetry and pycnometry. Solvent characterization by GC-MS headspace analysis shows that excess propylene oxide and chloropropanol products of an irreversible epoxide ring-opening reaction are present in the alumina gel following gelation, but can be removed via solvent exchange. Alumina aerogels with surface areas as high as 790 m²/g and bulk densities as low as 0.05 g/mL were prepared. Preliminary characterization of these aerogels, utilizing a catalytic test bed and a simulated emission gas blend, demonstrates that they have moderate ability for removal of hydrocarbons, carbon monoxide and nitrogen oxide.

Original language	English (US)
Pages (from-to)	141-149
Number of pages	9
Journal	Journal of Non-Crystalline Solids
Volume	426
DOIs	https://doi.org/10.1016/j.jnoncrysol.2015.06.030
State	Published - Oct 15 2015
Externally published	Yes

Bibliographical note

Funding Information:
This material is based upon work supported by the National Science Foundation (NSF) under Grant Nos. CHE-0847901 and DMR-1206631 . The authors thank Michael E. Hagerman for helpful discussions, Justin E. Rodriguez for assistance with the catalytic test bed measurements, and the Union College Geology Department for use of the XRD instrument. SJJ and NJHD are grateful for summer funding from the Union College Summer Research Fellowship Program . Additional support of this project was provided through the Union College Faculty Research Fund , Student Research Grant and Presidential Green Grant programs. The SEM instrument was funded through grants from the National Science Foundation (NSF MRI 0619578 ) and New York State Assembly RESTORE-NY .

Publisher Copyright:
© 2015 Elsevier B.V. All rights reserved.

Keywords

Alumina aerogels
Catalytic aerogels
Rapid supercritical extraction

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10.1016/j.jnoncrysol.2015.06.030

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title = "Epoxide-assisted alumina aerogels by rapid supercritical extraction",

abstract = "Aerogels offer a potential alternative to noble metals that could reduce both the cost and environmental impact associated with catalytic converter production. The environmental impact of the production of aerogel catalysts could be further reduced by using a rapid supercritical extraction (RSCE) technique, which reduces the time and solvent waste associated with aerogel preparation. Alumina aerogels, which have shown activity in catalyzing exhaust processing reactions, were prepared using an epoxide-assisted gelation technique with RSCE processing in a contained mold in a hydraulic hot press. Samples were characterized by FTIR, XRD, SEM, EDX, nitrogen adsorption porosimetry and pycnometry. Solvent characterization by GC-MS headspace analysis shows that excess propylene oxide and chloropropanol products of an irreversible epoxide ring-opening reaction are present in the alumina gel following gelation, but can be removed via solvent exchange. Alumina aerogels with surface areas as high as 790 m2/g and bulk densities as low as 0.05 g/mL were prepared. Preliminary characterization of these aerogels, utilizing a catalytic test bed and a simulated emission gas blend, demonstrates that they have moderate ability for removal of hydrocarbons, carbon monoxide and nitrogen oxide.",

keywords = "Alumina aerogels, Catalytic aerogels, Rapid supercritical extraction",

author = "Juhl, {Stephen J.} and Dunn, {Nicholas J.H.} and Carroll, {Mary K.} and Anderson, {Ann M.} and Bruno, {Bradford A.} and Madero, {Jos{\'e} E.} and Bono, {Michael S.}",

note = "Funding Information: This material is based upon work supported by the National Science Foundation (NSF) under Grant Nos. CHE-0847901 and DMR-1206631 . The authors thank Michael E. Hagerman for helpful discussions, Justin E. Rodriguez for assistance with the catalytic test bed measurements, and the Union College Geology Department for use of the XRD instrument. SJJ and NJHD are grateful for summer funding from the Union College Summer Research Fellowship Program . Additional support of this project was provided through the Union College Faculty Research Fund , Student Research Grant and Presidential Green Grant programs. The SEM instrument was funded through grants from the National Science Foundation (NSF MRI 0619578 ) and New York State Assembly RESTORE-NY . Publisher Copyright: {\textcopyright} 2015 Elsevier B.V. All rights reserved.",

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doi = "10.1016/j.jnoncrysol.2015.06.030",

language = "English (US)",

volume = "426",

pages = "141--149",

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T1 - Epoxide-assisted alumina aerogels by rapid supercritical extraction

AU - Juhl, Stephen J.

AU - Dunn, Nicholas J.H.

AU - Carroll, Mary K.

AU - Anderson, Ann M.

AU - Bruno, Bradford A.

AU - Madero, José E.

AU - Bono, Michael S.

N1 - Funding Information: This material is based upon work supported by the National Science Foundation (NSF) under Grant Nos. CHE-0847901 and DMR-1206631 . The authors thank Michael E. Hagerman for helpful discussions, Justin E. Rodriguez for assistance with the catalytic test bed measurements, and the Union College Geology Department for use of the XRD instrument. SJJ and NJHD are grateful for summer funding from the Union College Summer Research Fellowship Program . Additional support of this project was provided through the Union College Faculty Research Fund , Student Research Grant and Presidential Green Grant programs. The SEM instrument was funded through grants from the National Science Foundation (NSF MRI 0619578 ) and New York State Assembly RESTORE-NY . Publisher Copyright: © 2015 Elsevier B.V. All rights reserved.

PY - 2015/10/15

Y1 - 2015/10/15

N2 - Aerogels offer a potential alternative to noble metals that could reduce both the cost and environmental impact associated with catalytic converter production. The environmental impact of the production of aerogel catalysts could be further reduced by using a rapid supercritical extraction (RSCE) technique, which reduces the time and solvent waste associated with aerogel preparation. Alumina aerogels, which have shown activity in catalyzing exhaust processing reactions, were prepared using an epoxide-assisted gelation technique with RSCE processing in a contained mold in a hydraulic hot press. Samples were characterized by FTIR, XRD, SEM, EDX, nitrogen adsorption porosimetry and pycnometry. Solvent characterization by GC-MS headspace analysis shows that excess propylene oxide and chloropropanol products of an irreversible epoxide ring-opening reaction are present in the alumina gel following gelation, but can be removed via solvent exchange. Alumina aerogels with surface areas as high as 790 m2/g and bulk densities as low as 0.05 g/mL were prepared. Preliminary characterization of these aerogels, utilizing a catalytic test bed and a simulated emission gas blend, demonstrates that they have moderate ability for removal of hydrocarbons, carbon monoxide and nitrogen oxide.

AB - Aerogels offer a potential alternative to noble metals that could reduce both the cost and environmental impact associated with catalytic converter production. The environmental impact of the production of aerogel catalysts could be further reduced by using a rapid supercritical extraction (RSCE) technique, which reduces the time and solvent waste associated with aerogel preparation. Alumina aerogels, which have shown activity in catalyzing exhaust processing reactions, were prepared using an epoxide-assisted gelation technique with RSCE processing in a contained mold in a hydraulic hot press. Samples were characterized by FTIR, XRD, SEM, EDX, nitrogen adsorption porosimetry and pycnometry. Solvent characterization by GC-MS headspace analysis shows that excess propylene oxide and chloropropanol products of an irreversible epoxide ring-opening reaction are present in the alumina gel following gelation, but can be removed via solvent exchange. Alumina aerogels with surface areas as high as 790 m2/g and bulk densities as low as 0.05 g/mL were prepared. Preliminary characterization of these aerogels, utilizing a catalytic test bed and a simulated emission gas blend, demonstrates that they have moderate ability for removal of hydrocarbons, carbon monoxide and nitrogen oxide.

KW - Alumina aerogels

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U2 - 10.1016/j.jnoncrysol.2015.06.030

DO - 10.1016/j.jnoncrysol.2015.06.030

M3 - Article

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SN - 0022-3093

VL - 426

SP - 141

EP - 149

JO - Journal of Non-Crystalline Solids

JF - Journal of Non-Crystalline Solids

ER -

Epoxide-assisted alumina aerogels by rapid supercritical extraction

Abstract

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Keywords

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