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Method for low-heat solid-phase synthesis of AlH3

A low-heat solid phase and mixture technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problem of wasting solvents, achieve low equipment requirements, cheap raw material prices, and save solvents

Active Publication Date: 2016-03-02
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to solve AlCl 3 and LiAlH 4 Synthesis of AlH by Reaction in Solvent 3 The resulting product is AlH 3 ethers and compounds instead of AlH 3 And the problem of wasting solvent, and provide a kind of low heat solid phase synthesis AlH 3 Methods

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  • Method for low-heat solid-phase synthesis of AlH3

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specific Embodiment approach 1

[0020] Specific embodiment one: a kind of low heat solid-phase synthesis AlH of this embodiment 3 The method, described method is carried out under anhydrous anaerobic condition, and concrete steps are as follows:

[0021] 1. Weigh LiAlH with a molar ratio of (4-10):1:1 in the glove box 4 、LiBH 4 and AlCl 3 After mixing, a mixture is obtained;

[0022] 2. Grind the mixture of step 1 in an agate mortar and grind it in a sand bath, and raise the temperature to 65-80°C at a heating rate of 1°C / min;

[0023] 3. Keep the temperature at 65-80°C and continue grinding for 1-3 hours;

[0024] 4. Wash the material obtained after grinding in step 3 with diethyl ether and tetrahydrofuran respectively, then place it in a vacuum drying oven, and dry it for 2 hours at a temperature of 50°C to obtain AlH 3 .

specific Embodiment approach 2

[0025] Specific embodiment two: the difference between this embodiment and specific embodiment one is: LiAlH 4 、LiBH 4 and AlCl 3 The molar ratio of (4~9):1:1. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0026] Specific embodiment three: the difference between this embodiment and specific embodiment one is: LiAlH 4 、LiBH 4 and AlCl 3 The molar ratio of (4~8):1:1. Others are the same as in the first embodiment.

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Abstract

The invention relates to a method for synthesis of AlH3, in particular to a method for low-heat solid-phase synthesis of AlH3, and aims to solve the problems that ester compounds of AlH3 are produced rather than AlH3 when AlCl3 and LiAlH4 react in a solvent to synthesize AlH3 and the solvent is wasted. The method comprises steps as follows: adopting a mixture of LiAlH4, LiBH4 and AlCl3 with the molar ratio being (4-10):1:1 in a glove box, gradually heating the mixture to the temperature of 65-80 DEG C during grinding, and continuously grinding the mixture for 1-3 h at the temperature; washing a sample after the reaction with ethyl ether and tetrahydrofuran respectively, and drying the sample in a vacuum drying oven at the temperature of 50 DEG C for 2h to obtain a product, that is, a target product. The technology is simple, the equipment requirement is low, raw materials are low in price, and a good foundation is laid for preparation of solid-phase AlH3 later; the prepared product can be used as a reducing agent.

Description

technical field [0001] The present invention relates to a kind of non-solvated AlH 3 The preparation method of, be specifically related to a kind of AlCl 3 、LiBH 4 and LiAlH 4 Preparation of AlH by Direct Milling at Low Temperature 3 Methods. Background technique [0002] Energy is an important driving force for a country's industrial growth and economic development. Although the energy used now is still dominated by traditional energy sources such as oil, coal, and natural gas, and this basic energy structure will not change in a short time. However, our current traditional energy situation is already very severe, so the trend of developing and utilizing clean and low-carbon new energy is gradually obvious. [0003] There are many types of new clean energy, including wind energy, solar energy, tidal energy, hydrogen energy and so on. Among these new clean energy sources, hydrogen energy has the following advantages: (1) The use of hydrogen energy does not produce any ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/06
CPCC01B6/06C01P2002/72
Inventor 杨玉林姜艾锋范瑞清李梦茹王华威叶腾凌朱朝阳郑剑庞爱民唐根
Owner HARBIN INST OF TECH