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Method for inducing and synthesis gamma-Ca(BH4)2 through mechanical force

A technology of hydrogen storage material and mechanical force, applied in chemical instruments and methods, borane/diborane hydride, hydrogen and other directions, can solve problems such as difficult synthesis, and achieve low production cost, high efficiency, and easy reaction process. control effect

Active Publication Date: 2017-01-11
南通南京大学材料工程技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, γ-Ca(BH 4 ) 2 Compared with the α-phase and β-phase, it has better kinetic properties, but the single-phase γ-Ca(BH 4 ) 2 The synthesis of
At present, there is no effective and controllable synthesis of single-phase γ-Ca(BH 4 ) 2 preparation method

Method used

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  • Method for inducing and synthesis gamma-Ca(BH4)2 through mechanical force
  • Method for inducing and synthesis gamma-Ca(BH4)2 through mechanical force
  • Method for inducing and synthesis gamma-Ca(BH4)2 through mechanical force

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In a glove box filled with argon, with CaCl 2 and NaBH 4 Weigh 10g CaCl with a molar ratio of 1:2 2 and NaBH 4 , stirred magnetically under 200ml THF solvent for 2h, the resulting solution was transferred to a stainless steel reactor, kept at 90°C for 5h, and after filtration, the resulting clear solution was placed in a dynamic vacuum for 10 -3 bar, temperature 55 ° C conditions to remove the solvent treatment, the reaction precursor Ca(BH 4 ) 2 • THF.

[0033] Weigh 5g homemade Ca (BH 4 ) 2 THF precursor, put into the ball mill tank (stainless steel tank with on-off valve) with grinding balls, at 5bar H 2 Under the condition of atmosphere and 40°C, the obtained precursor was subjected to high-energy ball milling with a ball-to-material ratio of 80:1, a ball milling speed of 300 rpm, and a ball milling time of 12 hours. Ball milled product at 150°C, dynamic vacuum 10 -6 Under the condition of bar, heat treatment for 6h, the preparation of γ-Ca(BH 4 ) 2 .

...

Embodiment 2

[0036] In a glove box filled with argon, with CaCl 2 and NaBH 4 Weigh 10g CaCl with a molar ratio of 1:2 2 and NaBH 4 , stirred magnetically under 200ml THF solvent for 3h, the resulting solution was transferred to a stainless steel reactor, kept at 100°C for 3h, and after filtration, the resulting clear solution was placed in a dynamic vacuum for 10 -4 bar, temperature of 50 ° C conditions to remove the solvent treatment, the reaction precursor Ca(BH 4 ) 2 • THF.

[0037] Weigh 5g homemade Ca (BH 4 ) 2 THF precursors, put into a ball mill jar with balls at 2 bar N 2 Under the condition of atmosphere and 40°C, the obtained precursor was subjected to high-energy ball milling with a ball-to-material ratio of 100:1, a ball milling speed of 250 rpm, and ball milling times of 12h, 16h, and 20h, respectively. Ball milled product at 140°C, dynamic vacuum 10 -3 Under the condition of bar, heat treatment for 10h, Ca(BH 4 ) 2 .

[0038] figure 2 It is the XRD pattern of th...

Embodiment 3

[0043] In a glove box filled with argon, with CaCl 2 and NaBH 4 Weigh 10g CaCl with a molar ratio of 1:2 2 and NaBH 4 , stirred magnetically under 200ml THF solvent for 3h, the resulting solution was transferred to a stainless steel reactor, kept at 80°C for 6h, and after filtration, the resulting clear solution was placed in a dynamic vacuum for 10 -5 bar, temperature 45 ° C conditions to remove the solvent treatment, the reaction precursor Ca(BH 4 ) 2 •THF.

[0044] Weigh 5g homemade Ca (BH 4 ) 2 Put the THF precursor into a ball milling tank with balls, and carry out high-energy ball milling on the obtained precursor under the condition of 2bar Ar atmosphere and 50°C, the ball-to-material ratio is 80:1, the ball milling speed is 300rpm, 12h, 16h and 20h respectively. Ball milled product at 100°C, dynamic vacuum 10 -4 Under the condition of bar, heat treatment for 6 hours, Ca(BH 4 ) 2 .

[0045] image 3 It is a scanning electron microscope picture of the produc...

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Abstract

The invention discloses a method for inducing and synthesis gamma-Ca(BH4)2 through mechanical force. A Ca(BH)2 precursor, namely Ca(BH4)2.THF, is synthesized through the solvothermal method to serve as an initial reactant, mechanical force is introduced under certain atmosphere, pressure and condition conditions for mechanical force induction and activation, the Ca(BH4)2.THF activated product is processed by means of an adduct-free ligand, and single-phase gamma-Ca(BH4)2 excellent in hydrogen storage property is obtained. The preparation method has the advantages that production equipment is simple, operation is easy, reaction conditions are safe and reliable, the reaction process is easy to control, production cost is low, the production period is short, and product performance is stable.

Description

technical field [0001] The invention relates to the field of hydrogen storage materials, in particular to a mechanically induced synthesis of γ-Ca(BH 4 ) 2 Methods for hydrogen storage materials. Background technique [0002] Calcium borohydride (Ca(BH 4 ) 2 ) hydrogen storage material has high mass hydrogen storage density (11.5wt%), volume hydrogen storage density (130kg-H 2 / m 3 ), and excellent thermodynamic properties (theoretical decomposition enthalpy is only 32kJ / mol H 2 ), so that its operating temperature at 1 bar equilibrium decomposition pressure is lower than 100°C, and it can theoretically release 9.6wt% hydrogen (higher than the requirements of the US Department of Energy (DOE) and the International Energy Agency (IEA) greater than 5.5wt%), It has been the focus of research in the field of hydrogen storage at home and abroad in the past ten years. [0003] Crystallographic studies showed that Ca(BH 4 ) 2 It has three different crystal forms, which are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/21C01B3/00
CPCC01B3/001C01B6/21C01P2002/72C01P2004/03Y02E60/32
Inventor 顾坚任华仇叶云宋帅
Owner 南通南京大学材料工程技术研究院
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