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Method for preparing alpha-AlH3 under control of diisobutylaluminum hydride crystal transformation assistant

A technology of diisobutylaluminum hydride and crystal additives, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problem of low yield of α-AlH3

Active Publication Date: 2015-08-19
HARBIN INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the existing α-AlH 3 α-AlH obtained by the preparation method 3 The technical problem of low yield, the present invention provides a kind of diisobutyl aluminum hydride crystal transformation auxiliary agent to control the preparation of α-AlH 3 Methods

Method used

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  • Method for preparing alpha-AlH3 under control of diisobutylaluminum hydride crystal transformation assistant
  • Method for preparing alpha-AlH3 under control of diisobutylaluminum hydride crystal transformation assistant

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specific Embodiment approach 1

[0019] Specific implementation mode 1: This implementation mode provides a controlled preparation of α-AlH with a diisobutyl aluminum hydride crystal transformation aid 3 The method, the following steps are carried out under anaerobic conditions, the specific steps are as follows:

[0020] (1) AlH 3 Etherate and diisobutylaluminum hydride are dissolved in anhydrous toluene, where each gram of AlH 3 The amount of etherate anhydrous toluene is 70ml, the volume percentage of diisobutylaluminum hydride in anhydrous toluene is 0.5%, and then stirred at 94°C for 2h until the reaction is completed and allowed to stand at room temperature;

[0021] (2) The white reaction product was obtained by filtration, washed three times with diethyl ether, two times with dilute hydrochloric acid (0.5wt.%), and three times with deionized water, and then dried in vacuum at 60°C for 8 hours at a vacuum degree of 10 Pa. The product was obtained as a white powder. After X-ray diffraction (XRD) and ...

specific Embodiment approach 2

[0023] Embodiment 2: This embodiment is different from Embodiment 1 in that the solvent for crystallization is changed from toluene to benzene.

specific Embodiment approach 3

[0024] Specific implementation mode 3: This implementation mode provides a controlled preparation of α-AlH with a diisobutyl aluminum hydride crystal transformation aid 3 The method, the following steps are carried out under anaerobic conditions, the specific steps are as follows:

[0025] (1) AlH 3 Etherate and diisobutylaluminum hydride are dissolved in anhydrous toluene, where each gram of AlH 3 The amount of etherate anhydrous toluene is 65ml, the volume percentage of diisobutylaluminum hydride in anhydrous toluene is 0.1%, and then stirred at 92°C for 3h until the reaction is completed and allowed to stand at room temperature;

[0026] (2) The white reaction product was obtained by filtration, washed three times with diethyl ether, two times with dilute hydrochloric acid (1wt.%), and three times with deionized water, and then vacuum-dried at 80°C for 6 hours at a vacuum degree of 15 Pa to obtain White powder product. After X-ray diffraction (XRD) and scanning electron ...

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Abstract

The invention discloses a method for preparing alpha-AlH3 under the control of a diisobutylaluminum hydride crystal transformation assistant. The method comprises the following steps: 1, dissolving AlH3 etherate and diisobutylaluminum hydride in anhydrous toluene or benzene, stirring at 92-94DEG C for 2-3h until a reaction ends, and standing until room temperature; and 2, filtering to obtain a white reaction product, washing by using ether 2-4 times, washing by using dilute hydrochloric acid 1-2 times, washing by using deionized water 2-3 times, and carrying out vacuum drying at 40-90DEG C for 5-8h under a degree of vacuum of 5-20Pa to obtain a white powder product. The method allows the above raw material to react under the action of the diisobutylaluminum hydride crystal transformation assistant in order to generate high yield alpha-AlH3, and realizes no side reactions.

Description

technical field [0001] The present invention relates to a kind of control AlH 3 A preparation method for crystal transformation, specifically related to the controlled preparation of α-AlH by a diisobutyl aluminum hydride crystal transformation aid 3 Methods. Background technique [0002] The pursuit of higher energy is always an important development direction of solid propellant research. At present, the research on the energy enhancement of solid propellants mainly focuses on the following three aspects: (1) replace the conventional oxidant ammonium perchlorate with high energy density oxidant; Energy-containing groups such as nitrogen groups increase the energy of the solid propellant binder system; (3) use AlH 3 High-energy fuels such as metal hydrides can replace the current conventional metal fuel aluminum powder. Comparing comprehensively, the third method will increase the range of energy far greater than the first two. H 3 Not only is the energy content high,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
Inventor 杨玉林王金强安禹建范瑞清朱朝阳
Owner HARBIN INST OF TECH
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