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A kind of method for preparing aluminum hydride

A technology of aluminum hydride and aluminum hydride, applied in chemical instruments and methods, metal hydride, hydrogen, etc., can solve the problems of difficult purification of ammonium aluminum hydride intermediate, low yield of aluminum hydride, and cost of a large amount of ether, etc. Achieve the effects of large product particles, fast synthesis rate, and improved reaction efficiency

Active Publication Date: 2022-03-08
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Aiming at the problems that the preparation method in the prior art requires a large amount of ether and the cost is high, the intermediate aluminum hydride is difficult to purify, the yield of aluminum hydride is low, and the particles are fine, etc., the technical solution of the present invention is: a method for preparing aluminum hydride, using Quaternary ammonium salt, alkali metal aluminum hydride and halogenated hydrocarbon are raw materials, comprising the following steps:

Method used

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  • A kind of method for preparing aluminum hydride
  • A kind of method for preparing aluminum hydride
  • A kind of method for preparing aluminum hydride

Examples

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Embodiment 1

[0030] Under nitrogen protection, weigh 1.56g LiAlH 4 (0.0411mol) in a 500mL three-necked flask, add 150mL of anhydrous toluene, add about 50g of zirconia grinding medium with a particle size of 0.8mm in the three-necked flask, and install a reflux condenser and a constant pressure dropping funnel, and stir vigorously 1h; then weigh 15.95g of purified dioctadecyldimethylammonium chloride (0.0274mol) into a 250mL flask with a branch, add 150mL of anhydrous toluene, heat and stir in an oil bath at 50°C Dissolve; then, transfer the dioctadecyldimethylammonium chloride solution to a constant pressure dropping funnel, and drop it into a three-necked bottle within 30 minutes; after the addition, react at 60°C for 24 hours; the next day, let it stand After cooling, filter through a sand core funnel twice to remove the precipitate and recycle the zirconia grinding medium to obtain a toluene solution of quaternary ammonium aluminum hydride.

[0031] Weigh 0.05gC 60 In the toluene sol...

Embodiment 2

[0033] The crystallization aid is the ground aluminum trihydride seed, and the others are the same as in the examples. The yield is 35%.

Embodiment 3

[0035]It is basically the same as Example 1, except that 1-2 mL of ether is added to the toluene solution of benzyl chloride, and is added dropwise to the toluene solution of quaternary ammonium aluminum hydride along with the benzyl chloride solution, and the reflux state is maintained. Steam out at the end. The yield was 37%.

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Abstract

The invention discloses a method for preparing aluminum hydride, which uses quaternary ammonium salts, alkali metal aluminum hydrides and halogenated hydrocarbons as raw materials, and comprises the following steps: (1) under a nitrogen atmosphere, the aluminum hydride is equipped with magnetic stirring, reflux condensation Add alkali metal aluminum hydride and spherical inorganic oxide grinding medium to the reactor of tube and constant pressure dropping funnel, then add anhydrous aromatic hydrocarbon, and stir for 0.5-1h; transfer the aromatic hydrocarbon solution of quaternary ammonium salt to the constant pressure dropping funnel Add it dropwise to the reactor, continue to stir, and react at 25-60°C for 6-24 hours; let it stand for cooling, and filter to obtain the aromatic hydrocarbon solution of quaternary ammonium aluminum hydride; (2) Add the crystallization aid to the quaternary ammonium aluminum hydride In the aromatic hydrocarbon solution of the compound, add the aromatic hydrocarbon solution of halogenated hydrocarbon dropwise, and a precipitate is formed; after the dropwise addition, continue to stir for 2 to 5 hours, a large amount of white precipitate forms, filter, wash, and vacuum dry to obtain a white solid product. The method has the advantages of simple process, safe operation, high yield and easy production expansion.

Description

technical field [0001] The invention relates to a synthesis method of aluminum hydride and belongs to the field of new energy. Background technique [0002] One of the major challenges in finding solutions for hydrogen energy applications is the development of solid-state hydrogen storage media for vehicles. As a new type of hydrogen storage material, aluminum trihydride has a mass hydrogen storage of 10.08%, a volume hydrogen storage of 1.486g / mL (about twice the volume of liquid hydrogen), and a modified hydrogen release temperature lower than 100°C. With the rise of hydrogen fuel cells, especially low-temperature proton exchange membrane fuel cells, research on aluminum hydride has received more and more attention. [0003] There are many methods for synthesizing aluminum hydride reported at home and abroad. The main method is to prepare solvated aluminum hydride diethyl ether complex first, and then synthesize non-solvated aluminum hydride with different crystal forms t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B3/00C01B6/06
CPCC01B3/0031C01B6/06Y02E60/32
Inventor 李文江夏宇邢校辉常伟林于文杰王建伟薛金强尚丙坤
Owner LIMING RES INST OF CHEM IND
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