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A kind of synthetic method of α-aluminum hydride

A synthesis method, the technology of aluminum trihydride, applied in chemical instruments and methods, metal hydride, inorganic chemistry, etc., can solve the problems of moisture sensitivity and difficult purification, and achieve the effects of convenient operation, easy control of reaction and high yield

Active Publication Date: 2022-05-24
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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Problems solved by technology

[0004] In order to overcome the deficiencies in the prior art, the present inventor has carried out intensive research and provided a synthetic method of α-aluminum trihydride, the raw material bis(bromomethyl)benzene used in the synthetic method is easy to purify, and overcomes the problem that the raw material contains FeCl 3 other impurities and difficult to purify, sensitive to moisture in the air, etc., the by-product LiBr produced in the synthesis process is dissolved in the solvent ether, and the intermediate AlH in the synthesis process 3 n[(C 2 h 5 ) 2 O] solution can be deether-transformed directly in high-temperature toluene without filtration to generate α-AlH 3 , thus completing the present invention

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  • A kind of synthetic method of α-aluminum hydride
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preparation example Construction

[0017] The invention provides a kind of synthetic method of alpha-aluminum trihydride, comprising the following steps:

[0018] In step 1, bis(bromomethyl)benzene is added to anhydrous diethyl ether solution of lithium aluminum hydride, and the reaction is carried out under an inert atmosphere. After the reaction is completed, an aluminum trihydride diethyl ether complex is obtained.

[0019] In a preferred embodiment, the bis(bromomethyl)benzene is selected from 1,2-bis(bromomethyl)benzene, 1,3-bis(bromomethyl)benzene or 1,4-bis(bromomethyl)benzene Any one or more of bromomethyl)benzene.

[0020] In a preferred embodiment, LiAlH 4 The ratio of the amount of the substance to the volume of anhydrous ether is 1mol: 1.4L~4.8L.

[0021] In a preferred embodiment, LiAlH 4 The molar ratio with bis(bromomethyl)benzene (ie, the ratio of the amount of substances) is 2.1 to 3.0:1.

[0022] In a preferred embodiment, the reaction is carried out at 5-30 °C, and the reaction time is 2-...

Embodiment 1

[0030] Put 9.5 g of LiAlH 4 (0.25mol) was dissolved in 1L of anhydrous ether, nitrogen protection was introduced, 26.4g of 1,2-bis(bromomethyl)benzene (0.1mol) was added, and the reaction was stirred at 15°C for 2 hours, and the reaction solution was transferred to 82°C Carry out deetherification and crystallisation in 0.7L toluene, and when no diethyl ether is distilled from the condenser, the reaction system is lowered to room temperature, filtered, washed with ethanol, and dried at normal pressure at 50 °C to obtain 4.32 g of α-AlH 3 product. α-AlH 3 The SEM electron microscope image is as figure 1 As shown, the X-ray diffraction pattern is as figure 2 shown.

Embodiment 2

[0032] 15.2 g LiAlH 4 (0.4mol) was dissolved in 1L of anhydrous ether, nitrogen protection was introduced, 39.6 g of 1,3-bis(bromomethyl)benzene (0.15mol) was added, and the reaction was stirred at 20 °C for 4 hours, and the reaction solution was transferred to 83 °C. Carry out deetherification and crystallization in 2L of toluene. After the condenser does not have diethyl ether distilled, the reaction system is lowered to room temperature, filtered, and then washed with diethyl ether. After drying at normal pressure at 40 °C, 7.29 grams of α-AlH are obtained. 3 product.

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Abstract

The invention provides a synthetic method of α-aluminum trihydride, comprising: step 1, adding bis(bromomethyl)benzene into anhydrous ether solution of lithium aluminum hydride, reacting under an inert atmosphere, and obtaining three Aluminum hydride diethyl ether complex; step 2, transporting the aluminum trihydride diethyl ether complex to toluene for deether precipitation, filtering, washing the filter cake, and drying to obtain α-aluminum trihydride. Synthetic method of the present invention uses raw material two (bromomethyl) benzene easy purification, overcomes that raw material contains FeCl 3 other impurities and difficult to purify, sensitive to moisture in the air, etc., the by-product LiBr produced in the synthesis process is dissolved in the solvent ether, and the intermediate AlH in the synthesis process 3 n[(C 2 h 5 ) 2 O] solution can be deetherified directly in high temperature toluene without filtration to generate α‑AlH 3 , reducing the equipment requirements and process operation difficulty, and the obtained products have high yield and good quality.

Description

technical field [0001] The invention belongs to the technical field of synthesis of energetic materials, in particular to a synthesis method of α-aluminum trihydride. Background technique [0002] The solid rocket motor is the power system of various advanced strategic and tactical missiles. The solid propellant technology is the core technology and supporting technology of the solid rocket motor. It is of great significance to improve the missile delivery capability and miniaturization capability. Research institutions and scholars around the world have been committed to the development and use of new high-energy fuels. At present, there are at least seven crystal forms of α, α′, β, γ, δ, ε, and ξ of aluminum trihydride, among which α-aluminum hydride (α-AlH 3 ) with a relative molecular mass of 30.0 and a density of 1.48 g cm -3 , because α-AlH 3 With high hydrogen content, small molecular weight of combustion products, and relatively high thermal decomposition temperat...

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王洋王小波吴翼余凯伦陈克海
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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