Solid-phase synthesis method of Mg(BH4)2 hydrogen storage material

A technology of solid-phase synthesis and hydrogen storage materials, which is applied in the production of hydrogen, borane/diborane hydride, etc., can solve the problems of low purity of reaction products, high cost of materials, and complicated reaction process, etc. Easy to control, no organic pollution, and simple synthesis method

Inactive Publication Date: 2012-10-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two methods are similar to the synthetic pathway of magnesium hydride-borane adducts, and have the disadvantages of high cost of starting materials, which are not conducive to large-scale production
[0019] In summary, the existing Mg(BH 4 ) 2 The reaction process of the synthesis method is complicated, the reaction is difficult to control, the purity of the reaction product is low, and the disadvantages such as high cost cannot meet the requirements of its large-scale application.

Method used

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  • Solid-phase synthesis method of Mg(BH4)2 hydrogen storage material
  • Solid-phase synthesis method of Mg(BH4)2 hydrogen storage material
  • Solid-phase synthesis method of Mg(BH4)2 hydrogen storage material

Examples

Experimental program
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Effect test

Embodiment 1

[0038] In a glove box filled with Ar gas, the MgB 2 Respectively with 1wt%, 2wt%, 3wt%, 5wt%, 8wt%, 10wt%, 12wt%, 15wt% of Sc, Ti, V, Fe, Co, Ni, Zr, Nb, Mo, Ru, Pd, Pt, Mix Rh and Hf powder, put it into a stainless steel ball mill tank that can be sealed and has an on-off valve. After the ball mill tank is evacuated, fill it with 80-100 atm hydrogen, and perform ball milling on a planetary ball mill under a high-pressure hydrogen atmosphere. The ratio is 50:1, the rotation speed is 500rpm, and the ball milling time is 24-36h. The samples after ball milling were tested by FTIR. The results showed that all ball milled products were at 1000-1400 and 2200-2400cm -1 Mg(BH 4 ) 2 The characteristic infrared absorption peak of Mg(BH 4 ) 2 Formation. figure 1 MgB shown 2 - FTIR spectrum of the product after high pressure ball milling of 12wt% Ni. Products at 1127, 1163, 1233, 2226, 2292, 2388cm -1 6 Mg(BH 4 ) 2 characteristic infrared absorption peaks.

Embodiment 2

[0040] In a glove box filled with Ar gas, the MgB 2 Respectively with 1wt% Sc-2wt% Ti, 2wt% Sc-1wt% Ti, 2wt% Ti-3wt% V, 2wt% V-1wt% Co, 3wt% Fe-1wt% Ni, 3wt% Zr-4wt% Nb, 4wt%Mo-1wt%Ti, 5wt%Ru-2wt%Pd, 1wt%Pd-2wt%Pt, 6wt%Rh-2wt%Hf, 1wt%Sc-2wt%Ti-3wtV, 2wt%Fe-3wt%Co- 2wt%Ni, 3wt%Zr-2wt%Nb-5wt%Mo, 2wt%Ru-3wt%Pd-4wt%Pt, 3wt%Rh-2wt%Hf-6wt%V powder mixed, can be sealed, with a switch The stainless steel ball milling tank of the valve, after the ball milling tank is evacuated, is filled with 85 atm of hydrogen, and under the high-pressure hydrogen atmosphere, ball milling is carried out on a planetary ball mill with a ball-to-material ratio of 75:1, a rotating speed of 480 rpm, and a ball milling time of 32 hours. The samples after ball milling were tested by FTIR, and the results are listed in Table 1. It can be seen from the data in the table that all ball milling products are at 1000-1400 and 2200-2400cm -1 Mg(BH 4 ) 2 The characteristic infrared absorption peak of Mg(BH 4 ) ...

Embodiment 3

[0044] In a glove box filled with Ar gas, the MgB 2 -MgH 2 The mixture of 2wt%, 4wt%, 6wt%, 8wt%, 10wt% of ScF 3 , ScCl 3 、ScI 3 、TiF 3 、TiF 4 、TiCl 3 、TiCl 4 、TiI 4 , VF 3 , VF 4 , VCl 3 , VCl 4 , VBr 3 、CoCl 2 , FeCl 3 、NiCl 2 , YCl 3 , ZrCl 4 , NbCl 5 、MoCl 3 、MoCl 5 、MoF 6 、RuBr 3 、RuI 3 , RhCl 3 , HfCl 4 , PdCl 2 , PtCl 2 , PtCl 4 、LaCl 3 , CeCl 4 Mix and put it into a stainless steel ball mill tank that can be sealed and has a switch valve. After the ball mill tank is evacuated, it is filled with 30-80 atm of hydrogen respectively. : 1, the rotating speed is 450rpm, and the ball milling time is 36-48h. The products after ball milling were subjected to FTIR and volumetric hydrogen release tests respectively. The results showed that all the ball milled products were -1 The characteristic infrared absorption peaks of Mg(BH4)2 appear in the wavenumber range, showing that Mg(BH4) 4 ) 2 The hydrogen release of all samples occurred in the range...

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Abstract

The invention discloses a solid-phase synthesis method of a Mg(BH4)2 hydrogen storage material. Magnesium boride or a mixture of magnesium boride and magnesium hydride is used as a starting material to carry out a mechanochemical reaction in high pressure hydrogen atmosphere, with a catalyst selected from one or more of a transition metal, a transition metal halide, a transition metal hydride and a transition metal oxide, so as to prepare the Mg(BH4)2. The preparation method of the Mg(BH4)2 hydrogen storage material of the invention has advantages of simple synthetic method, easily controlled reaction process, low cost and no organic pollution.

Description

technical field [0001] The invention relates to the technical field of synthesis of hydrogen storage materials, in particular to a Mg(BH 4 ) 2 Solid phase synthesis of hydrogen storage materials. Background technique [0002] Mg(BH 4 ) 2 It is one of the research hotspots of hydrogen storage materials at present. It has the advantages of large hydrogen storage capacity (14.9wt.%), low hydrogen desorption temperature, and reversible hydrogen absorption and desorption. It will play an important role in the development of hydrogen economy; at the same time, Mg(BH 4 ) 2 It has strong reducibility, can replace some reducing agents widely used now, and has great application prospects in the chemical industry. [0003] At present, for Mg(BH 4 ) 2 The development of synthetic technology mainly focuses on the ion exchange reaction to synthesize Mg(BH 4 ) 2 , Magnesium boride hydrogenation to Mg(BH 4 ) 2 , Magnesium hydride and BH 3 The substance addition reaction of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/21C01B3/02
Inventor 刘永锋杨燕京高明霞潘洪革
Owner ZHEJIANG UNIV
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