Improved process for preparing alpha-aluminum hydride

A technology of aluminum trihydride and lithium aluminum hydride, applied in metal hydrides, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of complicated preparation of AlH3, complicated separation and purification of reaction products, unstable hydrogen release performance, etc. The reaction conditions are easy to control, the safety is satisfied, and the price is low.

Active Publication Date: 2017-07-18
河南纳宇新材料有限公司
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  • Summary
  • 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
[0003] The traditional synthesis method converts lithium aluminum hydride and other alkal

Method used

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  • Improved process for preparing alpha-aluminum hydride

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Embodiment 1

[0020] Embodiment 1 An improved process for preparing α-aluminum hydride, comprising the following steps:

[0021] (1) Refining with anhydrous ether, specifically: take 40g of sodium metal and cut it into thin slices and place it in a reaction vessel filled with 10L of industrial ether, reflux at 30°C for 50min, and then collect the distilled fraction at 36-42°C and seal it spare.

[0022] (2) Refining toluene, specifically: take 40g of sodium and cut it into thin slices and place it in a reactor containing 10L of industrial toluene, reflux at 120°C for 60min, then collect the distilled fractions at 108-128°C, seal and reserve .

[0023] (3) Lithium aluminum hydride refining, specifically: take 8000g of lithium aluminum hydride and add it to a 200L glass reactor, add 100L of refined anhydrous diethyl ether at the same time, stir, then add 30L of refined toluene, continue stirring evenly, and let stand for 12h , then filtered under reduced pressure, and the filtrate was disti...

Embodiment 2

[0027] Embodiment 2 An improved process for preparing α-aluminum hydride, comprising the following steps:

[0028] (1) Refining of anhydrous ether, specifically: take 80g of sodium metal and cut it into thin slices and place it in a reaction vessel filled with 10L of industrial ether, reflux at 50°C for 20min, and then collect the distilled fraction at 36-42°C and seal it spare.

[0029] (2) Toluene refining, specifically: take 80g of sodium and cut it into thin slices and place it in a reactor filled with 10L of industrial toluene, reflux at 140°C for 30min, then collect the distilled fractions at 108-128°C, seal and reserve .

[0030] (3) Lithium aluminum hydride refining, specifically: take 10,000g of lithium aluminum hydride and add it to a 200L glass reactor, add 80L of refined anhydrous ether at the same time, stir, then add 50L of refined toluene, continue stirring evenly, and let it stand for 24 hours , then filtered under reduced pressure, and the filtrate was disti...

Embodiment 3

[0034] Embodiment 3 An improved process for preparing α-aluminum hydride, comprising the following steps:

[0035] (1) Refining with anhydrous ether, specifically: take 60g of sodium metal and cut it into thin slices and place it in a reaction vessel filled with 10L of industrial ether, reflux at 40°C for 35min, and then collect the distilled fractions at 36-42°C and seal them spare.

[0036] (2) Toluene refining, specifically: take 60g of sodium and cut it into thin slices and place it in a reactor filled with 10L of industrial toluene, reflux at 130°C for 45min, then collect the distilled fractions at 108-128°C, seal and reserve .

[0037] (3) Lithium aluminum hydride refining, specifically: take 9000g of lithium aluminum hydride and add it to a 200L glass reactor, add 90L of refined anhydrous ether at the same time, stir, then add 40L of refined toluene, continue stirring evenly, and let stand for 18h , then filtered under reduced pressure, and the filtrate was distilled ...

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Abstract

The invention discloses an improved process for preparing alpha-aluminum hydride. The improved process comprises the following steps: (1) refining absolute ether; (2) refining methylbenzene; (3) refining lithium aluminum hydride; (4) preparing a mixed solution of anhydrous AlCl3 and diethyl ether; (5) preparing a mixed solution of LiAlH4 and anhydrous AlCl3; and (6) preparing the alpha-aluminum hydride. The invention provides the improved process for preparing the alpha-aluminum hydride, graphene is used to activate a reaction solution in the process, the production is safe and reliable, the yield is high, the purity of the obtained alpha-aluminum hydride is high, and the distribution of the particle size of a product is even. A preparation method is low in reaction temperature, shorter in reaction time, low in energy consumption, low in equipment requirement, simple in operations and easy in control of the reaction conditions, and is favorable for industrial production. According to the alpha-aluminum hydride prepared with the method, the product purity is more than or equal to 99%, the particle size range is 5-20 microns, the direct cost is less than or equal to 4000 yuan per kilogram.

Description

technical field [0001] The invention relates to an improved process for preparing α-aluminum hydride, and specifically belongs to the interdisciplinary field of inorganic material preparation and energetic material technology. Background technique [0002] From the point of view of the effect of increasing energy, adding high-energy additives to explosives can increase energy much more than other methods. At present, the most widely used method is to add metal Al powder with high calorific value to explosives. As we all know, weapons seek to increase the high energy of explosives, so AlH 3 , B, BeH 2 The addition of high-energy substances instead of aluminum powder has gradually attracted the attention of researchers and put a lot of energy into research. Since AlH 3 Due to its high hydrogen content, high heat of combustion, and non-toxic properties, it can be used in the field of high-energy fuels. Thermochemical calculations show that with AlH 3 Replacing aluminum ca...

Claims

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Application Information

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IPC IPC(8): C01B6/06
Inventor 任明安李守
Owner 河南纳宇新材料有限公司
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