Preparation method of hydrogen storage material of borane ammonia compound

A technology for hydrogen storage materials and compounds, applied in chemical instruments and methods, hydrogen production, metal hydrides, etc., can solve the problems of low sample purity, complicated preparation process, and low synthesis yield, and achieve non-toxic raw materials and methods The effect of simple and easy operation and cheap raw materials

Inactive Publication Date: 2012-07-11
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a borane ammonia compound hydrogen storage material, which solves the complex preparation process of DADB and the use of toxic gas raw materials B in the prior art. 2 h 6 , low synthetic yield, low sample purity, unsuitable for large-scale preparation, etc.

Method used

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  • Preparation method of hydrogen storage material of borane ammonia compound
  • Preparation method of hydrogen storage material of borane ammonia compound
  • Preparation method of hydrogen storage material of borane ammonia compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] NaBH 4 and NH 4 F is the starting material, the molar ratio is 1:1, and the mixture of DADB / 2NaF is prepared by mechanical ball milling method; then the by-product NaF in the ball milled sample is removed by dissolving, filtering, deammonizing and other steps with liquid ammonia as solvent, A white DADB powder was obtained as follows:

[0021] The raw material used is: NaBH 4 (purity 98%, ~200 mesh), NH 4 F (purity 98%, ~200 mesh).

[0022] NaBH in an argon atmosphere glove box 4 / NH 4 The F mixture and stainless steel balls were put into a stainless steel ball mill jar, sealed with a cover and placed on a Fritsch 7 planetary ball mill for 3 hours. The ball milling atmosphere is high-purity argon (purity 99.9999%), the initial pressure is 1 atmosphere, and the mass ratio of balls to materials is about 100:1. Put the ball-milled sample into a three-necked round-bottomed flask filled with liquid ammonia solvent, stir ultrasonically for 30 minutes, then let it stand...

Embodiment 2

[0026] Take LiBH 4 and NH 4 Cl is the starting material, the molar ratio is 1:1, the ball milling time is 1 hour, and the rest of the preparation conditions are the same as in Example 1.

[0027] The raw material used is: LiBH 4 (purity 98%, ~200 mesh), NH 4 Cl (purity 98%, ~200 mesh).

[0028] X-ray diffraction test conditions are the same as in Example 1. image 3 gives (a) LiBH 4 / NH 4 X-ray diffraction pattern of Cl ball-milled sample and (b) DADB after purification. The results showed that LiBH 4 / NH 4 The Cl mixture reacts completely according to the stoichiometric ratio during the ball milling process to form a mixture of DADB and LiCl, the X-ray diffraction pattern of DADB and the results reported in the literature [1.S.G.Shore and K.W. Inorg.Chem.1964, 3, 914-915] consistent; the liquid ammonia purification method can effectively remove the by-product LiCl, and finally obtain a white DADB powder sample with a particle size of about 300 mesh, a purity of ≥98%...

Embodiment 3

[0031] Take LiBH 4 and (NH 4 ) 2 SO 4 as the starting material, the molar ratio is 2:1, the ball milling time is 2 hours, and the rest of the preparation conditions are the same as in Example 1.

[0032] The raw material used is: LiBH 4 (purity 98%, ~200 mesh), (NH 4 ) 2 SO 4 (purity 98%, ~200 mesh).

[0033] X-ray diffraction test conditions are the same as in Example 1. Figure 5 gives (a)2LiBH 4 / (NH 4 ) 2 SO 4 The X-ray diffraction pattern of the ball-milled sample and (b) DADB after purification. The results showed that 2LiBH 4 / (NH 4 ) 2 SO 4 During the ball milling process, the mixture reacted completely according to the stoichiometric ratio to form DADB and Li 2 SO 4 The mixture, the X-ray diffraction pattern of DADB and the results reported in the literature [1.S.G.Shore and K.W. Inorg.Chem.1964,3,914-915] consistent; adopting the liquid ammonia purification method can effectively remove the by-product Li 2 SO 4 , finally obtained a white DADB po...

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Abstract

The invention relates to the field of hydrogen storage materials, in particular to a preparation method of a hydrogen storage material of a borane ammonia compound, which aims at resolving the problem in the prior art that the existing hydrogen storage material is complex in preparation process, utilizes toxic raw material B2H6, and is low in compounding rate, low in sample purity, not suitable for large-scale preparation and the like. The borane ammonia compound comprises boron, nitrogen and hydrogen, the molecular formula of the borane ammonia compound is [(NH3)2BH2](BH4), and the abbreviation is DADB. The special operation steps include utilizing the mixture of metal borohydride M(BH4)x and ammonium salt (NH4)yL as an initial raw material, adopting the mechanical ball milling method toprepare a mixture of DADB and MyLx; and (2) utilizing the mixture of the DADB and the MyLx as the initial raw material and adopting a liquid ammonia solvent to conduct dissolving, filtering and ammonia removing steps to remove by-product MyLx and obtain a pure DADB powder sample. The preparation method is simple and easy to implement, capable of preparing a high-purity DADB compound in high yieldand suitable for scale preparation, and the raw materials are low in cost and non-toxic.

Description

Technical field [0001] The invention relates to the field of hydrogen storage materials, in particular to a method for preparing a borane ammonia compound hydrogen storage material. Background technique [0002] Hydrogen energy is an efficient, clean, and renewable secondary energy source, which provides an ideal alternative energy source for solving global problems such as energy, climate, and environment. However, the large-scale commercial application of hydrogen energy faces a series of technical challenges in hydrogen production, hydrogen storage / transportation, and hydrogen utilization. The "bottleneck" link that can be exploited. Among the existing hydrogen storage methods, material-based solid-state hydrogen storage is significantly superior to high-pressure hydrogen containers and cryogenic liquid hydrogen in terms of operational safety and hydrogen storage volume density, so it is regarded as the most promising hydrogen storage method. Among the known hydrogen st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/13C01B3/06
CPCY02E60/36
Inventor 王平方占召康向东
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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