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In-situ preparation method of nanometer magnesium hydride

An in-situ preparation of magnesium hydride technology, applied in the field of hydrogen storage materials and nanomaterials, can solve the problems of unfavorable applications and reduce the hydrogen storage capacity of materials, and achieve the effect of maintaining capacity, high hydrogen storage capacity and avoiding side effects

Active Publication Date: 2019-08-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To avoid nano MgH 2 Particle growth or agglomeration in the preparation requires the introduction of a large amount of carbon, mesoporous silicon and other carrier materials to disperse the nano-products, which will significantly reduce the hydrogen storage capacity of the material, which is not conducive to practical application

Method used

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  • In-situ preparation method of nanometer magnesium hydride
  • In-situ preparation method of nanometer magnesium hydride
  • In-situ preparation method of nanometer magnesium hydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The preparation of embodiment 1 nanometer magnesium hydride

[0059] (1) Put 500mg of anhydrous magnesium chloride and 500mg of lithium hydride in an argon atmosphere glove box, put them into ball mill jars respectively, and ball mill them at a speed of 350 rpm for 3 hours.

[0060] (2) In an argon atmosphere glove box, take a total of 600mg of ball-milled anhydrous magnesium chloride and lithium hydride (molar ratio 1:2), put it into a 250ml flask, then inject 150ml of ultra-dry tetrahydrofuran into the flask, and stir for 30min , to be fully dissolved magnesium chloride.

[0061] (3) Insert the ultrasonic rod into the flask, keep the end of the ultrasonic rod in the middle of the mixture in the flask, and perform ultrasonic treatment with an output power of 210W. During the ultrasonic process, in order to keep the temperature of the sample from rising too high, continuous ultrasonic for half an hour must be intermittent for half an hour , accumulatively processed for...

Embodiment 2

[0080] The preparation of the nano-magnesium hydride sample of embodiment 2Ti catalytic doping

[0081] (1) Anhydrous magnesium chloride (500 mg) and lithium hydride (500 mg) were placed in a ball mill jar respectively in an argon atmosphere glove box, and ball milled at a speed of 350 rpm for 3 hours.

[0082] (2) In an argon atmosphere glove box, take a total of 600 mg of ball-milled anhydrous magnesium chloride and lithium hydride (molar ratio 1:2) and titanium tetrachloride (TiCl 4 ) (16.4 μL), put into a 250ml flask, then inject 100ml ultra-dry cyclohexane into the flask and stir for 30min, the ratio of the present embodiment, the molar ratio of Ti catalyst to magnesium chloride is 0.03:1.

[0083] (3) Insert the ultrasonic rod into the flask, keep the end of the ultrasonic rod in the middle of the mixture in the flask, and perform ultrasonic treatment with an output power of 210W. During the ultrasonic process, in order to keep the temperature of the sample from rising t...

Embodiment 3

[0099] The preparation of the nano-magnesium hydride sample of embodiment 3V catalytic doping

[0100] The same as the preparation method of Example 2, the difference is that the transition metal catalyst used is: vanadium trichloride VCl 3 , Table 1 lists the corresponding raw material ratio and key process, the sample named nano-MgH 2 -0.03V.

[0101] Table 1 nano-MgH 2 -0.03V sample preparation process and raw material ratio

[0102] Ultrasonic power (W) Ultrasonic time (h) MgCl 2 +LiH(mg)

VCl 3 (mg)

210 6 600 24

[0103] From Figure 12 In a, it can be seen that the sample only contains magnesium and vanadium elements. The weak oxygen signal and carbon signal come from carbon and oxygen pollution in the air or a small amount of organic solvent residue, indicating that the main phase of the sample is magnesium hydride, and a small amount of vanadium is used as a catalyst. ;From Figure 12 It can be seen in b that the V2p of the titan...

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Abstract

The invention discloses an in-situ preparation method of nanometer magnesium hydride. The method comprises the steps that under protection of an inert atmosphere, magnesium chloride and lithium hydride are added into an organic solvent, and through stirring, organic turbid liquid of a mixture is obtained; the organic turbid liquid is subjected to ultrasonic treatment, a chemical reaction of the mixture is promoted, and after the reaction is finished, filtration is conducted; a solid reaction product is washed, centrifuged and dried, remaining organic matter is removed, and the nanometer magnesium hydride is obtained. According to the preparation method, the energy provided by the cavitation effect, generated in a liquid medium, of ultrasonic waves is used for promoting the chemical reaction between the magnesium chloride and the lithium hydride, due to the fact that compared with traditional energy supply through heating and mechanical force, the cavitation effect can provide a large amount of energy instantaneously in a quite small range, the prepared product particles cannot easily become large, and the breaking effect of the ultrasonic waves is utilized for inhibiting nanometerparticle aggregation; the side effects caused by addition of various carrier materials for inhibiting growth of the particles are avoided, therefore the nanoscale magnesium hydride is obtained, and the effective hydrogen storage capacity of the product is increased.

Description

technical field [0001] The invention relates to the technical field of hydrogen storage materials and nanometer materials, in particular to an in-situ preparation method of nanometer magnesium hydride. Background technique [0002] The intensification of the energy crisis and the deterioration of the earth's environment have prompted human beings to accelerate the development of renewable and clean energy. Hydrogen energy has attracted people's attention for its abundant reserves and clean and pollution-free features. At present, the bottleneck restricting the hydrogen economy is mainly the storage and transportation of hydrogen, and the development of solid hydrogen storage materials based on chemical hydrogen storage is known as the most effective way to solve the problem of on-board hydrogen storage. [0003] MgH 2 It is a typical light metal hydride hydrogen storage material, its theoretical hydrogen storage capacity is as high as 7.6wt%, and its reversibility is good,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/04C01B6/24C01B3/00B82Y30/00
CPCC01B6/04C01B6/24C01B3/001B82Y30/00Y02E60/32C01B3/0026B82Y40/00C01P2002/72C01P2002/85C01P2002/89C01P2004/03C01P2004/04C01P2004/64
Inventor 刘永锋张欣潘洪革高明霞
Owner ZHEJIANG UNIV
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