Novel solid-state synthesis of halide free alane

The traditional aluminum hydride (alane, AlH3) synthesis involves reacting AlCl3 and LiAlH4 in diethyl ether, resulting in the formation of the alane etherate adduct, AlH3·h[(C2H5)2O]. The desired crystallized, stable a-AlH3 can only be obtained by either extensive vacuum distillation and heating of...

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Main Authors: Knight, D., Dinh, L., Paskevicius, M., Buckley, Craig, Zidan, R.
Format: Conference Paper
Published: AMER CHEMICAL SOC 2012
Online Access:http://hdl.handle.net/20.500.11937/36124
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author Knight, D.
Dinh, L.
Paskevicius, M.
Buckley, Craig
Zidan, R.
author_facet Knight, D.
Dinh, L.
Paskevicius, M.
Buckley, Craig
Zidan, R.
author_sort Knight, D.
building Curtin Institutional Repository
collection Online Access
description The traditional aluminum hydride (alane, AlH3) synthesis involves reacting AlCl3 and LiAlH4 in diethyl ether, resulting in the formation of the alane etherate adduct, AlH3·h[(C2H5)2O]. The desired crystallized, stable a-AlH3 can only be obtained by either extensive vacuum distillation and heating of the etherate or by a crystallization process involving a large, heated bath of a benzene/toluene solution. These processes tend to be costly due to the several hours of vacuum pumping and/or heating required as well as dangerously using large amounts of flamable, toxic solvents. It is demonstrated here that a-AlH3 can be obtained by simply mixing AlCl3 and LiAlH4 in the solid state and slowly heating to 75° C. The a-AlH3 product can be washed with minimal solvents to remove the LiCl bi-product, leading to zero formation of any alane adducted materials. Although simple mixing and heating the reactants can provide a 40% yield of alane, the application of moderate pressure while heating increases this yield to over 60 % of cvrystalline a-AlH3.
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institution Curtin University Malaysia
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spelling curtin-20.500.11937-361242018-12-14T00:52:35Z Novel solid-state synthesis of halide free alane Knight, D. Dinh, L. Paskevicius, M. Buckley, Craig Zidan, R. The traditional aluminum hydride (alane, AlH3) synthesis involves reacting AlCl3 and LiAlH4 in diethyl ether, resulting in the formation of the alane etherate adduct, AlH3·h[(C2H5)2O]. The desired crystallized, stable a-AlH3 can only be obtained by either extensive vacuum distillation and heating of the etherate or by a crystallization process involving a large, heated bath of a benzene/toluene solution. These processes tend to be costly due to the several hours of vacuum pumping and/or heating required as well as dangerously using large amounts of flamable, toxic solvents. It is demonstrated here that a-AlH3 can be obtained by simply mixing AlCl3 and LiAlH4 in the solid state and slowly heating to 75° C. The a-AlH3 product can be washed with minimal solvents to remove the LiCl bi-product, leading to zero formation of any alane adducted materials. Although simple mixing and heating the reactants can provide a 40% yield of alane, the application of moderate pressure while heating increases this yield to over 60 % of cvrystalline a-AlH3. 2012 Conference Paper http://hdl.handle.net/20.500.11937/36124 AMER CHEMICAL SOC restricted
spellingShingle Knight, D.
Dinh, L.
Paskevicius, M.
Buckley, Craig
Zidan, R.
Novel solid-state synthesis of halide free alane
title Novel solid-state synthesis of halide free alane
title_full Novel solid-state synthesis of halide free alane
title_fullStr Novel solid-state synthesis of halide free alane
title_full_unstemmed Novel solid-state synthesis of halide free alane
title_short Novel solid-state synthesis of halide free alane
title_sort novel solid-state synthesis of halide free alane
url http://hdl.handle.net/20.500.11937/36124