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Method for preparing α-aluminum hydride by mixed catalysis of lithium aluminum hydride and lithium borohydride

A technology of lithium aluminum hydride and lithium borohydride, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of high cost, slow outgassing, decomposition, and inability to meet the requirements, and achieves low production cost and easy production. Operation, high stability effect

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

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Problems solved by technology

But AlH 3 There are also many problems in practical application: AlH 3 The preparation is more complicated and the cost is higher; there is still instability in hydrogen desorption performance at low temperature; due to AlH 3 It is a substance composed of two strongly reducing atoms, even the most stable α-AlH 3 , there are still phenomena such as slow degassing and decomposition, which cannot meet the requirements of practical applications
In response to this problem, Yang Yulin and others 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 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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  • Method for preparing α-aluminum hydride by mixed catalysis of lithium aluminum hydride and lithium borohydride

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Embodiment 1

[0027] Embodiment 1 The method for preparing α-aluminum hydride with lithium aluminum hydride and lithium borohydride mixed catalysis comprises the following steps:

[0028] (1) Preparation of mixed catalyst solution: take LiAlH by weight 4 and LiBH 4 , placed in a reaction flask, added refined anhydrous diethyl ether, and fully stirred for 10 minutes to obtain a mixed catalyst solution for subsequent use;

[0029] (2) Synthesis of α-aluminum trihydride: Take 2000mL of refined toluene and place it in a 10L reaction vessel, and then pass nitrogen gas into the reaction vessel. After repeating twice, add 300mL of the mixture obtained in step (1) through vacuum filtration. Catalyst solution, under reflux state, stir and heat up, begin to distill out the diethyl ether in the catalyst, at this moment slowly add dropwise 350mLLiAlH 4 and anhydrous AlCl 3 Mix the solution, control the dropping rate at 10ml / min, after the dropwise addition is completed, raise the temperature to 85°C...

Embodiment 2

[0033] Embodiment 2 The method for preparing α-aluminum trihydride with lithium aluminum hydride and lithium borohydride mixed catalysis, comprises the following steps:

[0034] (1) Preparation of mixed catalyst solution: take LiAlH by weight 4 and LiBH 4 , placed in a reaction flask, added refined anhydrous diethyl ether, and fully stirred for 50 minutes to obtain a mixed catalyst solution for subsequent use;

[0035] (2) Synthesis of α-aluminum trihydride: take 3000mL of refined toluene and place it in a 10L reaction vessel, and pass nitrogen gas into the reaction vessel. After repeating 4 times, add 200mL of the mixture obtained in step (1) through vacuum filtration. Catalyst solution, under reflux state, stir and heat up, begin to distill out the diethyl ether in the catalyst, at this moment slowly add dropwise 500mLLiAlH 4 and anhydrous AlCl 3 Mix the solution, control the rate of addition to 20ml / min, after the dropwise addition is completed, heat up to 95°C and reflu...

Embodiment 3

[0040] Embodiment 3 The method for preparing α-aluminum trihydride with lithium aluminum hydride and lithium borohydride mixed catalysis, comprises the following steps:

[0041] (1) Preparation of mixed catalyst solution: take LiAlH by weight 4 and LiBH 4 , placed in a reaction flask, added refined anhydrous diethyl ether, and fully stirred for 30 minutes to obtain a mixed catalyst solution for subsequent use;

[0042] (2) Synthesis of α-aluminum trihydride: Take 2500mL of refined toluene and place it in a 10L reaction vessel, and then pass nitrogen gas into the reaction vessel. After repeating 3 times, add 250mL of the mixture obtained in step (1) through vacuum filtration. Catalyst solution, under reflux state, stir and heat up, begin to distill out the diethyl ether in the catalyst, at this moment slowly add dropwise 450mLLiAlH 4 and anhydrous AlCl 3 Mix the solution, control the dropping rate at 15ml / min, after the dropwise addition is completed, raise the temperature t...

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Abstract

The invention discloses a method for preparing alpha-aluminum trihydride by carrying out mixed catalysis of lithium aluminum hydride and lithium borohydride. The method comprises the following steps: (1) preparing mixed catalyst solutions; (2) synthesizing alpha-aluminum trihydride; (3) refining and drying a product. The method for preparing alpha-aluminum trihydride by carrying out the mixed catalysis of lithium aluminum hydride and lithium borohydride provided by the invention can be carried out at a relatively low reaction temperature under constant pressure; the method is simple in processes, easy to operate, simple in device, and can be applied to industrial production. The method disclosed by the invention is economical and high-efficient, and is low in production cost; a crystal form of the obtained alpha-aluminum trihydride is single, the purity of the product is so high to be up to 99.8%, and the product is high in stability and easy to store; moreover, the chemical stability performance of the product is beneficial for being applied to energetic materials, propellants, fuel cells and the like.

Description

technical field [0001] The invention relates to a method for preparing α-aluminum hydride by mixed catalysis of lithium aluminum hydride and lithium borohydride, and specifically belongs to the technical field of metal hydride preparation. Background technique [0002] At present, all countries in the world are working on the synthesis of high-energy-density materials, but this part of the work is quite complicated and arduous. Germany first synthesized RDX in 1899, and Octokin (HMX) until 1941. It was only discovered and separated, and HMX has been used as the highest energy explosive for the armed forces to this day. Considering the current reality, it is difficult to make breakthroughs in the near future to synthesize compounds with better performance than HMX and achieve marketization. Therefore, for a considerable period of time in the future, HMX will still be the explosive with the highest energy for the armed forces, and a considerable part of ground suppression wea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B6/06
CPCC01B6/06C01P2002/72C01P2006/80
Inventor 刘吉平韩佳任明安王栋李守良李树磊苏岩
Owner 河南纳宇新材料有限公司
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