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Method for preparing lithium borohydride by room-temperature solid-phase ball milling

A lithium borohydride, room temperature solid-phase technology, applied in the field of preparation of high-capacity hydrogen storage materials, can solve problems such as hindering the formation of LiBH4, difficulty in recycling boron resources, and restrictions on large-scale applications, so as to achieve controllable reaction process and source of raw materials Wide range of effects suitable for large-scale production and use

Active Publication Date: 2018-07-17
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, whether it is thermochemical method or high energy ball milling method, LiBH 4 The yields are all lower than 30%, and the research shows that the chemical inertness of elemental boron, that is, the stronger B-B bond, is the hindrance to LiBH 4 Key Factors Generated
[0012] In summary, the current commercial LiBH 4 It is generally prepared by the action of sodium borohydride and lithium chloride, and the synthesis of sodium borohydride needs to consume a large amount of precious metal sodium, and the three wastes are seriously polluted. Although this wet chemical method has a high yield, it has high production costs and technical problems. Complex and difficult to recycle boron resources and other issues, which limit its large-scale application as a hydrogen storage material in vehicle-mounted hydrogen storage
However, the thermochemical method and high-energy ball milling method developed in recent years not only consume a lot of energy but also have a low yield, so it is difficult to be practically applied in industrial production.

Method used

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  • Method for preparing lithium borohydride by room-temperature solid-phase ball milling
  • Method for preparing lithium borohydride by room-temperature solid-phase ball milling
  • Method for preparing lithium borohydride by room-temperature solid-phase ball milling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Prepare lithium borohydride by solid phase ball milling at room temperature, the steps are as follows:

[0059] At room temperature, in a glove box with 0.1MPa argon atmosphere, take Mg and LiBO 2 2H 2 O (the molar ratio is 5:1) is mixed, put into the ball mill pot and seal it, and then place it on a high-energy pendulum ball mill (QM-3C) for ball milling. The rotation speed is 1200 rpm, the ball milling time is 20 hours, the operation mode is alternate restart, each operation is 30 minutes and then pauses for 30 minutes, so alternately;

[0060] After the ball milling, use distilled diethyl ether to dissolve and extract the mixture after the ball milling and filter to obtain a clear filtrate. After the clear filtrate is vacuum-dried, a white powder is obtained;

[0061] The resulting white powder was mixed with commercial LiBH 4 (95%) XRD comparison picture as shown figure 2 shown by figure 2 It can be seen that the obtained white powder is high-purity lithium ...

Embodiment 2

[0064] Prepare lithium borohydride by solid phase ball milling at room temperature, the steps are as follows:

[0065] At room temperature, in a glove box with 0.1MPa argon atmosphere, take Mg and LiBO 2 2H 2 O (the molar ratio is 4.5:1) mixed, put into the ball mill pot and seal it, then put it on the high-energy pendulum type ball mill (QM-3C) for ball milling, the ball-to-material ratio is 50:1, the ball milling speed is 1200 rpm, ball milling The time is 5 hours, and the operation mode is to restart alternately, and stop for 30 minutes after each operation for 30 minutes, and so on alternately.

[0066] The infrared spectrum of the mixture after ball milling is shown as Figure 4 As shown by the curve a in the Figure 4 From the curve a in the figure, we can see that in the infrared spectrum curve 2200~2400cm -1 and 1125cm -1 The peak that appears at corresponds to the vibrational absorption peak of the B-H bond, proving the generation of lithium borohydride.

[0067...

Embodiment 3

[0069] Prepare lithium borohydride by solid phase ball milling at room temperature, the steps are as follows:

[0070] At room temperature, in a glove box with 0.1MPa argon atmosphere, take Mg and LiBO 2 2H 2 O (the molar ratio is 4.5:1) mixed, put into the ball mill pot and seal it, then put it on the high-energy pendulum type ball mill (QM-3C) for ball milling, the ball-to-material ratio is 50:1, the ball milling speed is 1200 rpm, ball milling The time is 10h, and the operation mode is alternate restart, each time running for 30 minutes and then stopping for 30 minutes, so alternately.

[0071] The infrared spectrum of the mixture after ball milling is shown as Figure 4 shown in curve b, with Figure 7 The curve a in is consistent, given by Figure 4 From the curve b in the figure, we can see that in the infrared spectrum curve 2200~2400cm -1 and 1125cm -1 The peak that appears at corresponds to the vibrational absorption peak of the B-H bond, proving the generation ...

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Abstract

The invention discloses a method for preparing lithium borohydride by room-temperature solid-phase ball milling. The method comprises the following steps: under a non-oxidizing atmosphere at room temperature, uniformly mixing a magnesium-containing reducing agent with a lithium metaborate-containing reducing material, carrying out solid-phase ball milling, and carrying out separation and purification to obtain the lithium borohydride. The preparation method provided by the invention has the advantages of simple process, controllable and adjustable reaction process, mild reaction conditions, low energy consumption, low cost, high yield, no pollution, good safety and realization of cyclic utilization of boron resources, and has important practical significance.

Description

technical field [0001] The invention relates to a method for preparing a high-capacity hydrogen storage material, in particular to a method for preparing lithium borohydride by solid phase ball milling at room temperature. Background technique [0002] Energy is the material basis for the development and development of human production and social activities, as well as the basis for human survival. With the rapid development of human society, the demand for energy is increasing day by day. In the past few decades, human beings have exploited and utilized fossil fuels indiscriminately, which has made human beings now face a huge energy crisis and environmental crisis, which has brought great potential to human society. Sustained development poses a great threat. Facing the double pressure of increasingly severe energy crisis and environmental pollution, it is imminent to develop new sustainable green energy. As a clean and abundant renewable energy, hydrogen energy is consi...

Claims

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Application Information

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IPC IPC(8): C01B6/21C01B3/00
CPCC01B3/001C01B6/21C01P2002/72C01P2002/82Y02E60/32C01B6/17C01B3/065Y02E60/36C01P2002/74C01P2006/80
Inventor 欧阳柳章陈康王辉刘江文朱敏
Owner SOUTH CHINA UNIV OF TECH
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