Crystal transformation method of aluminum hydride

A technology of aluminum trihydride and crystal transformation, which is applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of low conversion rate, long time consumption, etc., and achieves low cost, high crystal transformation efficiency, and crystal transformation conditions. mild effect

Active Publication Date: 2017-07-18
河南纳宇新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can gradually convert the β and γ crystal forms of aluminum hydride into α-type aluminum hydride, the conversion rate is low and it takes a long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for crystal transformation of aluminum hydride, comprising the following steps: taking polycrystalline aluminum hydride and adding it to a solvent under a dry inert gas atmosphere, the solvent is tetrahydrofuran, and the mass-volume ratio of polycrystalline aluminum hydride to the solvent is: 5g︰400mL, stirred for 20min, and suction filtered to remove insoluble impurities to obtain an aluminum hydride solution; then ultrasonically treated for 2 hours at an ultrasonic frequency of 130kHz; followed by rotary evaporation to obtain aluminum hydride granular crystals; aluminum hydride granular crystals Place it in air with a humidity of 30% RH for 3 hours, then add a solvent for secondary dissolution, filter, and rotary evaporate, and dry the product at a vacuum of 490mmHg and 70°C for 2 hours to obtain 4.2g of aluminum trihydride. The X-ray diffraction test was carried out on the aluminum hydride obtained by crystallization, and the result showed that the proportion...

Embodiment 2

[0024] A method for crystal transformation of aluminum hydride, comprising the following steps: taking polycrystalline aluminum hydride and adding it to a solvent under a dry inert gas atmosphere, the solvent is ether, and the mass-volume ratio of polycrystalline aluminum hydride to the solvent is: 10g︰200mL, stirred for 30min, removed insoluble impurities by suction filtration, and obtained aluminum trihydride solution; then carried out ultrasonic treatment for 4 hours, and the ultrasonic frequency was 50kHz; followed by rotary evaporation to obtain aluminum trihydride granular crystals; Place it in air with a humidity of 50% RH for 1 hour, then add a solvent for secondary dissolution, filter, and rotary evaporate, and dry the product at a vacuum of 320mmHg and 50°C for 5 hours to obtain 8.6g of aluminum trihydride. The X-ray diffraction test was carried out on the aluminum hydride obtained by crystallization, and the result showed that the proportion of α-aluminum hydride in ...

Embodiment 3

[0026] A method for crystal transformation of aluminum hydride, comprising the following steps: taking polycrystalline aluminum hydride and adding it to a solvent under a dry inert gas atmosphere, the solvent is tetrahydrofuran, and the mass-volume ratio of polycrystalline aluminum hydride to the solvent is: 8g︰300mL, stirred for 25min, removed insoluble impurities by suction filtration, and obtained aluminum trihydride solution; then carried out ultrasonic treatment for 3 hours, and the ultrasonic frequency was 100kHz; then carried out rotary evaporation to obtain aluminum trihydride granular crystals; Place it in air with a humidity of 40% RH for 2 hours, then add a solvent for secondary dissolution, filter, and rotary evaporate, and dry the product at a vacuum of 395mmHg and 60°C for 3.5 hours to obtain 7.1g of aluminum trihydride. The X-ray diffraction test was carried out on the aluminum hydride obtained by crystallization, and the result showed that the proportion of α-al...

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PUM

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Abstract

The invention discloses a crystal transformation method of aluminum hydride. The crystal transformation method of the aluminum hydride comprises the following steps: adding the aluminum hydride into a solvent under the atmosphere of dry nitrogen, stirring, performing suction filtration and removing insoluble impurities to obtain an aluminum hydride solution; performing ultrasonic treatment; performing rotary evaporation to obtain aluminum hydride solid granules; putting the aluminum hydride solid granules into the air, dissolving, filtering, performing rotary evaporation and vacuum-drying the product. According to the crystal transformation method of the aluminum hydride, the aluminum hydride, which exists in beta and gamma crystal forms, in the aluminum hydride is converted into alpha-aluminum hydride with higher stability, and the impurity aluminum and the rest aluminum hydride which exist in an unstable crystal form are removed from the aluminum hydride. The crystal transformation method provided by the invention is high in crystal transformation efficiency, mild in crystal transformation condition and easy to operate and control. The purity of the alpha-aluminum hydride obtained after crystal transformation can reach above 99 percent, and the alpha-aluminum hydride can exist stably in the air atmosphere.

Description

technical field [0001] The invention relates to a method for crystal transformation of aluminum hydride, and specifically belongs to the technical field of energetic material preparation. Background technique [0002] Aluminum hydride (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%, and has a relatively high hydrogen storage capacity. Using aluminum hydride instead of fuel aluminum powder in traditional solid propellants, the solid propellant can generate more heat and gas, and can significantly increase the specific impulse value of the solid propellant. It has important military application value. [0003] Aluminum hydride is heterogeneous. 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
CPCC01B6/06C01P2006/80
Inventor 任明安李守良
Owner 河南纳宇新材料有限公司
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