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A kind of synthesis technique of α-aluminum hydride

A technology of aluminum hydride and synthesis process, which is applied in the direction of metal hydride, inorganic chemistry, chemical instruments and methods, etc., which can solve the problems of energy consumption, low single-batch output, and large energy consumption in the synthesis process, so as to reduce equipment cost and energy consumption level, increase single batch output, and reduce the effect of energy consumption level

Active Publication Date: 2021-02-09
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since AlH 3 Ether complexes have limited solubility in ether, resulting in a low single-batch yield of the compound. At the same time, the solvent ether must be distilled off during the deetherification process, which consumes a lot of energy and leads to high energy consumption in the synthesis process.
Literature (Preparation, characterization and decomposition ofγ-andα-alane AlH 3 , AIAA 2011-5583) reported that the prepared AlH 3 The ether in the ether complex solution is evaporated to dryness under reduced pressure, and the obtained solid-state aluminum trihydride ether complex is subjected to solid-phase deetherification in a vacuum oven or toluene after grinding. In this method, special ether distillation is required. Recovery device and decompression vacuum device, while solid AlH 3 The solid powder of ether complex needs to be ground, and it is easy to catch fire during the process, which leads to a high safety risk of this method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 45 grams of lithium aluminum hydride in 0.38 L of anhydrous ether, and dissolve 48 grams of AlCl 3 Dissolve in 0.15L of anhydrous ether, under nitrogen protection, mix aluminum trichloride ether solution and lithium aluminum hydride ether solution at -10°C for 30 minutes, stop the reaction and filter to remove the by-product lithium chloride, at 30 rpm Under the condition of agitation per minute, the filtrate was heated to 15°C as the aluminum trihydride diethyl ether complex slurry, and the stirring was stopped after 20 minutes. The slurry was transferred to 0.19L of toluene at 82°C for deetherization. After distilling out the distilled ether in the condenser, the reaction system was lowered to room temperature, filtered, washed with distilled water and ethanol, and dried to obtain 30.6 g Alpha-aluminum hydride products.

Embodiment 2

[0025] Dissolve 49 grams of lithium aluminum hydride in 0.65 L of anhydrous ether, and dissolve 48 grams of AlCl 3 Dissolve in 0.18L of anhydrous ether, under nitrogen protection, mix aluminum trichloride ethyl ether solution and lithium aluminum hydride ether solution for 40 minutes at -8°C, stop the reaction and filter to remove the by-product lithium chloride, at 50 rpm Under the stirring condition of 1 / min, the filtrate was heated to 10° C. as the aluminum trihydride diethyl ether complex slurry, and the stirring was stopped after 30 minutes. After standing still, 0.57 L of diethyl ether solvent in the upper layer was transferred. Transfer the remaining aluminum trihydride etherate slurry to 0.19L of toluene at 84°C for deetherization. After the condenser has no condensed ether distilled off, the reaction system is lowered to room temperature, filtered, and then After washing with distilled water and ethanol, 31.6 grams of α-aluminum hydride product was obtained after dryi...

Embodiment 3

[0027] Dissolve 52 grams of lithium aluminum hydride in 0.82 L of anhydrous ether, and dissolve 48 grams of AlCl 3 Dissolve in 0.2L of anhydrous ether, under nitrogen protection, mix aluminum trichloride ether solution and lithium aluminum hydride ether solution for 45 minutes at -5°C, stop the reaction and filter to remove the by-product lithium chloride, at 80 rpm Under the stirring condition of 1 / min, the filtrate was heated to 20° C. as the aluminum trihydride diethyl ether complex slurry, and the stirring was stopped after 40 minutes. After standing still, 0.87 L of diethyl ether solvent in the upper layer was transferred. Transfer the remaining aluminum trihydride diethyl ether complex slurry to 0.25L toluene at 86°C for deetherization. After the condenser has no condensed diethyl ether distilled off, the reaction system is lowered to room temperature, filtered, and then After washing with distilled water and ethanol, 31.4 grams of α-aluminum trihydride product was obtai...

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Abstract

The invention belongs to the technical field of hydrogen storage materials, and particularly relates to an alpha-aluminum trihydride synthesis technology. According to the aluminum trihydride preparation method, a diethyl ether solvent adopted in synthesis can be directly recycled not through a distillation process, and the raw material cost of the alpha-aluminum trihydride is lowered. The recycled diethyl ether solvent can be directly recycled not through a distillation process, and the energy consumption level of the alpha-aluminum trihydride ether removal crystallization reaction process islowered.

Description

technical field [0001] The invention belongs to the technical field of hydrogen storage materials, and in particular relates to a synthesis process of α-aluminum trihydride. Background technique [0002] α-aluminum hydride (α-AlH 3 ), is a binary covalent hydride with a hydrogen storage volume of 0.148kg H 2 / L (more than twice the density of liquid hydrogen), the mass hydrogen storage reaches 10.08%, has a high hydrogen storage capacity, and can be used in propellants, explosives, reducing agents, hydrogen fuel cells, atomic layer deposition technology, etc. Aluminum hydride is heterogeneous, and there are seven different crystal forms of unsolvated aluminum hydride, namely α-AlH 3 , β-AlH 3 , γ-AlH 3 , δ-AlH 3 , ε-AlH 3 , θ-AlH 3 , α'-AlH 3 , where aluminum hydride is α-AlH 3 , β-AlH 3 and γ-AlH 3 There are mainly three crystal forms. Among the seven crystal forms, α-AlH 3 It has the most stable structure and can exist stably in the air. Current availability o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B6/06
CPCC01B6/06
Inventor 邱贤平朱朝阳庞爱民郭翔张思陈克海杜利孙忠祥余凯伦王洋杨亦婷
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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