Novel methods for synthesizing halide-free alane without the formation of adducts

Many of the current synthesis methods for aluminium hydride (alane—AlH3) involve reacting AlCl3 and LiAlH4 in solvents. The reaction requires the formation of an alane adduct such as AlH3•[(C2H5)2O] prior to obtaining crystallized stable a-AlH3. This process requires several hours of pumping in a va...

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Main Authors: Dinh, L., Knight, D., Paskevicius, Mark, Buckley, Craig, Zidan, R.
Format: Journal Article
Published: Springer 2012
Online Access:http://hdl.handle.net/20.500.11937/26742
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author Dinh, L.
Knight, D.
Paskevicius, Mark
Buckley, Craig
Zidan, R.
author_facet Dinh, L.
Knight, D.
Paskevicius, Mark
Buckley, Craig
Zidan, R.
author_sort Dinh, L.
building Curtin Institutional Repository
collection Online Access
description Many of the current synthesis methods for aluminium hydride (alane—AlH3) involve reacting AlCl3 and LiAlH4 in solvents. The reaction requires the formation of an alane adduct such as AlH3•[(C2H5)2O] prior to obtaining crystallized stable a-AlH3. This process requires several hours of pumping in a vacuum system to remove the ether and convert the alane etherate into stable a-alane. This crystallization process is both costly and hazardous because a large amount of highly flammable material (e.g. ether) is removed by vacuum pumps over several hours. Conversely, the work presented herein describes novel methods to synthesize adduct-free alane. It is demonstrated here that AlH3 can form by mixing AlCl3 and LiAlH4 in the solid state and heating to 75°C; only a-AlH3 was obtained. The a-AlH3 product can be washed with minimal solvents leading to zero formation of alane adducts. In addition, the unwanted LiCl by-product is also removed during the solvent wash, resulting in halide-free a-alane. Although simply mixing and heating the reactants led to a 40% yield of alane, having the reactants compacted and mechanically pressed while heating increases the yield to 60% crystalline a-AlH3.
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spelling curtin-20.500.11937-267422017-09-13T15:51:39Z Novel methods for synthesizing halide-free alane without the formation of adducts Dinh, L. Knight, D. Paskevicius, Mark Buckley, Craig Zidan, R. Many of the current synthesis methods for aluminium hydride (alane—AlH3) involve reacting AlCl3 and LiAlH4 in solvents. The reaction requires the formation of an alane adduct such as AlH3•[(C2H5)2O] prior to obtaining crystallized stable a-AlH3. This process requires several hours of pumping in a vacuum system to remove the ether and convert the alane etherate into stable a-alane. This crystallization process is both costly and hazardous because a large amount of highly flammable material (e.g. ether) is removed by vacuum pumps over several hours. Conversely, the work presented herein describes novel methods to synthesize adduct-free alane. It is demonstrated here that AlH3 can form by mixing AlCl3 and LiAlH4 in the solid state and heating to 75°C; only a-AlH3 was obtained. The a-AlH3 product can be washed with minimal solvents leading to zero formation of alane adducts. In addition, the unwanted LiCl by-product is also removed during the solvent wash, resulting in halide-free a-alane. Although simply mixing and heating the reactants led to a 40% yield of alane, having the reactants compacted and mechanically pressed while heating increases the yield to 60% crystalline a-AlH3. 2012 Journal Article http://hdl.handle.net/20.500.11937/26742 10.1007/s00339-012-6791-z Springer restricted
spellingShingle Dinh, L.
Knight, D.
Paskevicius, Mark
Buckley, Craig
Zidan, R.
Novel methods for synthesizing halide-free alane without the formation of adducts
title Novel methods for synthesizing halide-free alane without the formation of adducts
title_full Novel methods for synthesizing halide-free alane without the formation of adducts
title_fullStr Novel methods for synthesizing halide-free alane without the formation of adducts
title_full_unstemmed Novel methods for synthesizing halide-free alane without the formation of adducts
title_short Novel methods for synthesizing halide-free alane without the formation of adducts
title_sort novel methods for synthesizing halide-free alane without the formation of adducts
url http://hdl.handle.net/20.500.11937/26742