Synthesis method of alpha-aluminum trihydride

A synthesis method, aluminum hydride technology, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve problems such as difficult purification, moisture sensitivity, etc., achieve easy control of reaction, convenient operation, and reduce equipment requirements Effect

Active Publication Date: 2020-11-27
HUBEI INST OF AEROSPACE CHEMOTECH
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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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  • Synthesis method of alpha-aluminum trihydride
  • Synthesis method of alpha-aluminum trihydride

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[0017] The present invention provides a kind of synthetic method of α-aluminum trihydride, comprises the following steps:

[0018] Step 1: Add bis(bromomethyl)benzene to an anhydrous ether solution of lithium aluminum hydride, and react under an inert atmosphere, and obtain an ether complex of aluminum trihydride after the reaction is completed.

[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( 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 (that is, the ratio of the amount of substances) to bis(bromomethyl)benzene is 2.1-3.0:1.

[0022] In a preferred embodiment, the reaction is carried out at 5-30°C for a reaction time of 2-24 hours, with stirring during the reaction; preferably, the...

Embodiment 1

[0030] 9.5 g LiAlH 4 (0.25mol) was dissolved in 1L of anhydrous ether, protected by nitrogen, added 26.4 grams of 1,2-bis(bromomethyl)benzene (0.1mol), stirred and reacted at 15°C for 2 hours, and transferred the reaction solution to 82°C Carry out ether removal and crystallization in 0.7L of toluene. After no diethyl ether is distilled out in the condenser, the reaction system is lowered to room temperature, filtered, and then washed with ethanol. After drying at normal pressure at 50°C, 4.32 grams of α-AlH are obtained. 3 product. α-AlH 3 The SEM electron microscope picture 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, protected by nitrogen, added 39.6 grams of 1,3-bis(bromomethyl)benzene (0.15mol), stirred and reacted at 20°C for 4 hours, and transferred the reaction solution to 83°C Carry out ether removal and crystallization in 2L of toluene. After no diethyl ether is distilled out in the condenser, the reaction system is cooled 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 synthesis method of alpha-aluminum trihydride, which comprises the following steps of: step 1, adding bis (bromomethyl) benzene into an anhydrous ether solution of lithium aluminum hydride, and reacting in an inert atmosphere to obtain an aluminum trihydride ether complex after the reaction is finished; and step 2, conveying the aluminum trihydride diethyl ether complex into toluene, carrying out deetherification precipitation, filtering, washing a filter cake, and drying the filter cake to obtain alpha-aluminum trihydride. According to the synthesis method, the used raw material bis (bromomethyl) benzene is easy to purify, the problems that the raw materials contain impurities such as FeCl3, are difficult to purify, are sensitive to moisture in air and the like are solved, a byproduct LiBr generated in the synthesis process is dissolved in a solvent diethyl ether, and an intermediate AlH3. N [(C2H5) 2O] solution in the synthesis process can be directly subjected to ether removal and crystal transformation in high-temperature toluene without filtration to generate alpha-AlH3, so that the equipment requirement and the process operation difficulty are reduced, and the obtained product is high in yield and good in quality.

Description

technical field [0001] The invention belongs to the technical field of synthesizing energetic materials, in particular to a method for synthesizing α-aluminum trihydride. Background technique [0002] Solid rocket motor is the power system of various advanced strategic and tactical missiles. Solid propellant technology is the core technology and supporting technology of solid rocket motor. Research institutions and scholars from all over the world have been committed to the development and use of new high-energy fuels. At least seven crystal forms of α, α′, β, γ, δ, ε, and ξ have been found at this stage, among which α-aluminum hydride (α-AlH 3 ) has a relative molecular mass of 30.0 and a density of 1.48g cm -3 , because α-AlH 3 With high hydrogen content, small molecular weight of combustion products, and relatively high thermal decomposition temperature, it is regarded as an ideal high-energy fuel for a new generation of solid propellants in the field of energetic mate...

Claims

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Application Information

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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 CHEMOTECH
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