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Synthesis method of amino metal compounds

A technology of amino compound and synthesis method, which is applied in safe, reliable, and low-cost preparation. The synthesis of metal amino compound provides a field of simple operation, which can solve the problems of impossible high batch output, complicated operation, excessive ammonia, etc., and achieve improvement Solid phase reaction interface, simple process, and the effect of improving reactivity

Inactive Publication Date: 2014-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the reaction kettle is used for pressure in the general preparation process, the volume of the kettle body is not easy to be designed too large, so the batch output cannot be high
In addition, due to the need to use high ammonia pressure to promote the reaction, there is a serious excess of ammonia, which makes it necessary to recover the remaining liquid ammonia after the synthesis, which is more complicated in operation

Method used

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  • Synthesis method of amino metal compounds
  • Synthesis method of amino metal compounds
  • Synthesis method of amino metal compounds

Examples

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Embodiment 1

[0017] Magnesium Amide is the preparation of Mg(NH 2 ) 2 - An important raw material for LiH high-performance hydrogen storage materials, but there is no commercial product for this raw material. The present invention adopts 200 milliliter stainless steel ball mill tank, built-in stainless steel ball with diameter of 15 mm, gas switch valve is arranged on the tank cover, can lead into quantitative gas and seal in it. Accurately weigh 12 grams (0.5 moles) of magnesium particles with a particle size of about 2 mm or magnesium flakes with a length of about 5 mm in an argon glove box (the mass ratio of balls for ball milling is 1:100), and place them in a ball mill jar Inside and sealed. Finally, 8.5 grams (0.5 moles) of pure ammonia gas is introduced into the tank through the valve on the cover of the ball mill tank, and the pressure in the tank is about 8 atm (the ammonia gas is liquefied in the tank). After closing the valve, place the ball mill jar on a planetary ball mill ...

Embodiment 2

[0021]Considering the economical practicability of hydrogen storage materials, the metal in the Amide-hydride system is best to use cheap alkaline earth metals. Recently, the research on hydrogen storage systems containing calcium amide has gradually increased, which has led to an increase in the demand for calcium amide. However, this compound is also not No commercial product exists. The calcium amide can be prepared by adopting a synthetic method similar to the magnesium amide. The specific method is as follows: Accurately weigh 20 grams of blocky calcium metal in an argon glove box (the mass ratio of ball milling to balls is 1:150), and place it in a ball milling tank. Since the calcium metal used here is in the form of a large block, a small amount of ammonia gas (about 2 grams) can be introduced to adsorb the calcium block before ball milling, and the preliminary pulverization effect can be achieved through the penetration and diffusion of the gas and its interaction wit...

Embodiment 3

[0024] The optimization of the amide-hydride hydrogen storage system is inseparable from the modulation of the metal cations in it, because this can realize the modulation of the strength of the metal-nitrogen bond. Multi-metal components should be one of the development directions of the amide-hydride system in the future. First, it is necessary to realize the synthesis scale-up of polynary metal amides. Binary LiAl(NH 2 ) 4 The traditional synthesis of LiAl alloy is achieved by pre-firing LiAl alloy, which is subsequently heated with liquid ammonia under high temperature and high pressure. This method consumes a lot of energy, has a low safety factor and requires high alloying. The present invention directly adopts LiAlH 4 Composite hydride ammoniation method, similar to calcium amide synthesis process, synthesizes high-quality LiAl(NH 2 ) 4 Amino compounds. The specific method is: accurately weigh the powdered LiAlH in an argon glove box 4 19 grams (0.5 mol) of solid...

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Abstract

The invention discloses a synthesis method of amino metal compounds. Series of metal unitary or binary amino compounds are successfully synthesized by using a mechanical ball milling method in a ball-milling atmosphere controlled manner through combination of a subsequent method of roasting crystallization controlled under a low-pressure atmosphere. Compared with the traditional high-temperature and high-pressure roasting method, the synthesis method disclosed by the invention is simple and safe to operate, high in yield and low in cost, thereby providing the foundation for the compounds applied to hydrogen storage systems.

Description

technical field [0001] The invention relates to the preparation technology of metal amido compounds, in particular to provide a simple, safe, reliable and low-cost preparation method for synthesizing metal amido compounds. Background technique [0002] In recent years, the worldwide energy crisis and environmental degradation have prompted people to establish a more efficient and recyclable new energy system. Hydrogen has become an important component of the future energy system due to its abundant reserves, high combustion calorific value and non-polluting. The utilization of hydrogen energy needs to mainly solve several key technologies such as hydrogen preparation, storage, and transportation, among which hydrogen storage technology is a relatively weak link. Especially at present, the automobile industry is facing transformation. In the process of developing new energy vehicles, such as hydrogen fuel cell vehicles and hydrogen internal combustion engine vehicles, the pr...

Claims

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Application Information

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IPC IPC(8): C01B21/092
Inventor 熊智涛胡大强陈萍
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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