A kind of process method for preparing α-aluminum trihydride with sodium borohydride catalysis

A technology for the preparation of aluminum hydride and catalysis, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc. Complicated operation process, slow outgassing, decomposition and other problems, to achieve the effect of easy control of reaction conditions, reduction of operation process and easy operation

Active Publication Date: 2019-10-25
河南纳宇新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] H 3 There are also some problems in practical aspects: AlH 3 At this stage, the preparation process is considered to be more complicated and the cost is higher; there is still instability in hydrogen desorption under low temperature conditions; due to AlH 3 It is a substance composed of two strongly reducing atoms, even if α-AlH 3 There are still phenomena such as slow degassing and decomposition, which are difficult to meet the needs of applications
In response to this problem, Yang Yulin and others have proposed to use diisobutyl aluminum hydride and LiBH 4 Controlled Preparation of α-AlH as Catalyst 3 , a higher yield of α-AlH can be obtained 3 , but the price of diisobutyl alumina used in this method is relatively high, which increases the production cost. At the same time, the post-synthesis treatment process of this method is cumbersome, requiring operations such as ether washing, dilute hydrochloric acid washing, deionized water washing, and vacuum drying. It is difficult to carry out large-scale industrial production

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  • A kind of process method for preparing α-aluminum trihydride with sodium borohydride catalysis

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Embodiment 1

[0023] A process for preparing α-aluminum hydride with sodium borohydride catalysis, comprising the following steps:

[0024] (1) The preparation of catalyst solution is specifically: in the glove box, weigh 0.8NaBH 4 and 0.5LiAlH 4 , first LiAlH 4 Dissolve in 200mL of refined anhydrous ether, then LiAlH 4 The mixed solution of diethyl ether was added to NaBH by vacuum filtration. 4 , stirred until dissolved to obtain a catalyst solution.

[0025](2) The preparation of α-aluminum trihydride is as follows: take 2000mL of refined toluene and place it in a reaction vessel, pass nitrogen gas to remove the air in the reactor, repeat this operation twice, and filter under reduced pressure Add 200mL of the catalyst solution obtained in step (1), stir and raise the temperature to 80°C under reflux, then start distillation, control the temperature at 80°C, and slowly add 350mL of LiAlH 4 and anhydrous AlCl 3 After the mixed solution was added dropwise, the temperature was raised ...

Embodiment 2

[0029] A process for preparing α-aluminum hydride with sodium borohydride catalysis, comprising the following steps:

[0030] (1) The preparation of catalyst solution is specifically: in the glove box, take 1.5gNaBH respectively 4 and 1.5gLiAlH 4 , first LiAlH 4 Dissolve in 300mL of refined anhydrous ether, then LiAlH 4 The mixed solution of diethyl ether was added to NaBH by vacuum filtration. 4 , stirred until dissolved to obtain a catalyst solution.

[0031] (2) The preparation of α-aluminum trihydride is as follows: take 4000mL of refined toluene and place it in a reaction vessel, pass through nitrogen to remove the air in the reactor, repeat this operation 4 times, and filter it under reduced pressure Add 400mL of the catalyst solution obtained in step (1), under reflux, stir and heat up to 95°C, then start distillation, the temperature is controlled at 97°C, and slowly add 550mL of LiAlH 4 and anhydrous AlCl 3 Mix the solution, after the dropwise addition, raise th...

Embodiment 3

[0035] A process for preparing α-aluminum hydride with sodium borohydride catalysis, comprising the following steps:

[0036] (1) The preparation of catalyst solution is specifically: in the glove box, take 1.2gNaBH respectively 4 and 1.0gLiAlH 4 , first LiAlH 4 Dissolve in 250mL of refined anhydrous ether, then LiAlH 4 The mixed solution of diethyl ether was added to NaBH by vacuum filtration. 4 , stirred until dissolved to obtain a catalyst solution.

[0037] (2) The preparation of α-aluminum trihydride is as follows: take 3000mL of refined toluene and place it in a reaction vessel, pass nitrogen gas to remove the air in the reactor, repeat this operation 3 times, and filter under reduced pressure Add 300mL of the catalyst solution obtained in step (1), under reflux, stir and heat up to 90°C, then start distillation, the temperature is controlled at 92°C, and slowly add 450mL of LiAlH 4 and anhydrous AlCl 3 Mix the solution, after the dropwise addition, raise the tempe...

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Abstract

The invention discloses a process method for preparing alpha-aluminum hydride by sodium borohydride catalysis. The method comprises a step (1) of preparing a catalyst solution; a step (2) of preparation of alpha-aluminum hydride; and a step (3) of product aftertreatment. The process method for preparing alpha-aluminum hydride by sodium borohydride catalysis can be implemented at a low temperature and normal pressure, and is suitable for industrial production. The obtained alpha-aluminum hydride is single in crystal form, the single-batch conversion rate is 86.5% or above, the purity reaches 98%, the thermal stability is high, and the alpha-aluminum hydride is favorable for being applied to fields of energetic materials, propellants and fuel cells and the like.

Description

technical field [0001] The invention relates to a process method for preparing α-aluminum trihydride by catalyzing sodium borohydride, and specifically belongs to the technical field of metal hydride preparation. Background technique [0002] The application of hydrogen energy in the aerospace industry has a long history, and the use effect is unique and remarkable. From the development and research at the end of World War II, to the trial and later use of the space shuttle in the 1950s, the mature experience in the application of rocket engine fuel in the 1960s, to the use in space shuttles, future orbital aircraft, and intercontinental military and civil aircraft in recent years. Widely used, it fully demonstrates its vitality and powerful vitality. Hydrogen is at the top of the periodic table of elements. It has the smallest mass and is a colorless and odorless gas at room temperature. Hydrogen reserves are very abundant on the earth, with high calorific value, good comb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B6/06C01B6/21B01J21/02B01J23/04
CPCB01J21/02B01J23/04C01B6/06C01B6/21C01P2002/72C01P2006/80
Inventor 任明安李守良
Owner 河南纳宇新材料有限公司
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