CN102502490A - Preparation method of Mg(AlH4)2 hydrogen storage system - Google Patents

Preparation method of Mg(AlH4)2 hydrogen storage system Download PDF

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Publication number
CN102502490A
CN102502490A CN2011103398731A CN201110339873A CN102502490A CN 102502490 A CN102502490 A CN 102502490A CN 2011103398731 A CN2011103398731 A CN 2011103398731A CN 201110339873 A CN201110339873 A CN 201110339873A CN 102502490 A CN102502490 A CN 102502490A
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ball
alh
hydrogen storage
storage system
alloy
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王一菁
袁华堂
焦丽芳
闫超
刘光
李丽
仇方圆
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Nankai University
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Nankai University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a preparation method of a Mg(AlH4)2 hydrogen storage system, comprising the following steps of: weighing Ti powder and B powder according to a mol ratio ranging from 1: 1.8 to 1: 2.4; adding the Ti powder and the B powder into a ball-milling pot according to a ball-material mass ratio of 20: 1, and carrying out ball-milling under the protection of an argon gas for 80-140 hours to prepare a Ti-B alloy; respectively adding the Ti-B alloy and NaAlH4 with contents which are 1-10 mol% and 1-20 mol% of those of Mg(AlH4)2, and the Mg(AlH4)2 into the ball-milling pot, wherein the mass ratio of the ball to the material is 40: 1; and carrying out the ball-milling and mixing the materials under the protection of the argon gas for 1-5 hours to prepare the Mg(AlH4)2 hydrogen storage system. According to the invention, a hydrogen-releasing peak temperature of the Mg(AlH4)2 hydrogen storage system is only 94 DEG C, namely the hydrogen is released at a temperature of about 40 DEG C and the temperature is reduced by about 60 DEG C compared with the temperature in the process without a catalyst; and furthermore, the preparation method provided by the invention has the advantages of simplicity in operation, simple equipment and moderate operation conditions.

Description

A kind of Mg (AlH 4) 2The preparation method of hydrogen storage system
Technical field
The present invention relates to a kind of Mg (AlH 4) 2The preparation method of hydrogen storage system belongs to the hydrogen storage material field.
Background technology
Along with the aggravation of global energy dilemma, Hydrogen Energy has received global generally attention as reproducible secondary clean energy.The stored safely of hydrogen is the key that Hydrogen Energy is utilized, and solid-state hydride hydrogen storage technology is a kind of ideal hydrogen storage technology, and rare earth hydrogen storage alloy has low suction hydrogen discharging temperature and dynamic performance preferably, but its hydrogen storage capability is lower, has only about 1.5wt%.In recent years, the light metal hydrogenate and the complex hydrides that have a higher hydrogen storage capability (more than the 5wt%) become a research focus.
Hydrogen storage material will be applied to actual production, just needs lower hydrogen discharging temperature.But the hydrogen storage material hydrogen discharging temperature that some hydrogen-storage amounts are bigger at present is all higher, for example the MgH in the metal hydride 2, have the higher theoretical hydrogen storage capability of 7.6wt%, but need be about 320 ℃ could releasing hydrogen gas, the requirement of actual application below 100 ℃ head and shoulders above, even add catalyzer, its hydrogen discharging temperature is still more than 200 ℃; NaAlH in the metal coordinate hydride for another example 4, having the theoretical hydrogen storage capability of 7.4wt%, hydrogen discharging temperature can be reduced to about 160 ℃ after adding catalyzer about 190 ℃, but that this hydrogen discharging temperature still exceeds requirement of actual application is too many.
Mg (AlH comparatively speaking 4) 2It is the lower metal coordinate hydride of a kind of hydrogen discharging temperature; About 150 ℃, and have the theoretical hydrogen storage capability of 9.3wt%, because of the hydrogen discharging temperature of itself just lower in all kinds of hydrogen storage materials; And hydrogen storage capability is bigger; Be the bigger hydrogen storage material of a kind of potentiality to be exploited, catalyzer is one of approach that reduces its hydrogen discharging temperature, adds TiCl 3Its hydrogen discharging temperature is reduced to about 120 ℃, but this temperature still also have a segment distance apart from application request.
Also find no more effective catalyst at present.
Summary of the invention
The object of the present invention is to provide a kind of Mg (AlH 4) 2The preparation method of hydrogen storage system.
The present invention is achieved in that a kind of Mg (AlH 4) 2The preparation method of hydrogen storage system comprises:
1) preparation of catalyzer Ti-B alloy
With Ti powder and B powder in molar ratio 1:1.8-1:2.4 take by weighing and by ball material mass ratio 20:1, throw in ball grinder ball milling 80-140h under argon shield, prepare said Ti-B alloy;
2) Mg (AlH 4) 2The preparation of hydrogen storage system
With said Ti-B alloy, NaAlH 4Press Mg (AlH respectively 4) 21 ~ 10mol% and 1 ~ 20mol% and Mg (AlH 4) 2Put in the ball grinder, ball material mass ratio 40:1, ball mill mixing 1-5h under argon shield makes said Mg (AlH 4) 2Hydrogen storage system.
Wherein, the rotating speed of ball mill is 450r/min said step 1), 2).
Mg (the AlH of the present invention's preparation 4) 2Hydrogen storage system is with respect to simple Mg (AlH 4) 2Decompose hydrogen discharging temperature and reduce greatly, first puts the hydrogen peak temperature is merely 94 ℃, nearly 60 ℃ of reduction amplitude, and promptly begin to put hydrogen at 40 ℃, satisfy the temperature requirement of practical application; And operating process is easy, and equipment is simple, and operational condition is gentle.
Description of drawings
Fig. 1 is the XRD figure of the prepared Ti-B alloy of the embodiment of the invention;
Fig. 2 is prepared Ti-B alloy and NaAlH of the embodiment of the invention 4Concerted catalysis Mg (AlH 4) 2The TPD figure that divides liberation hydrogen;
Fig. 3 is to be prepared Ti-B alloy and NaAlH of the embodiment of the invention 4Concerted catalysis Mg (AlH 4) 2The TPD figure that divides liberation hydrogen.
Embodiment
Embodiment 1
1), Ti powder and B powder are mixed according to mol ratio 1:2,20:1 places ball grinder according to ball material mass ratio, charges into the normal pressure argon gas in jar, obtains the Ti-B alloy with rotating speed ball milling 140h in ball mill of 450r/min;
2), the Ti-B alloy of gained is pressed Mg (AlH 4) 25mol%, NaAlH 4Press Mg (AlH 4) 220mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 5h makes said Mg (AlH 4) 2Hydrogen storage system.
To gained Mg (AlH 4) 2Hydrogen storage system materials carries out temperature programmed desorption(TPD) (TPD) test, and Fig. 2 is gained Mg (AlH 4) 2The TPD figure of hydrogen storage system materials shows this Ti-B alloy and NaAlH 4Mg (the AlH of concerted catalysis 4) 2First puts the hydrogen peak temperature is merely 94 ℃.
Embodiment 2
The Ti-B alloy of embodiment 1 preparation is pressed Mg (AlH 4) 21mol%, NaAlH 4Press Mg (AlH 4) 210mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 3h makes said Mg (AlH 4) 2Hydrogen storage system.
Embodiment 3
The Ti-B alloy of embodiment 1 preparation is pressed Mg (AlH 4) 25mol%, NaAlH 4Press Mg (AlH 4) 218mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 1h makes said Mg (AlH 4) 2Hydrogen storage system.
Embodiment 4
1), Ti powder and B powder are mixed according to mol ratio 1:1.8,20:1 places ball grinder according to ball material mass ratio, charges into the normal pressure argon gas in jar, obtains the Ti-B alloy with rotating speed ball milling 80h in ball mill of 450r/min;
2), the Ti-B alloy of gained is pressed Mg (AlH 4) 28mol%, NaAlH 4Press Mg (AlH 4) 29mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 3h makes said Mg (AlH 4) 2Hydrogen storage system.
Embodiment 5
The Ti-B alloy of embodiment 4 preparations is pressed Mg (AlH 4) 28mol%, NaAlH 4Press Mg (AlH 4) 220mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 5h makes said Mg (AlH 4) 2Hydrogen storage system.
Embodiment 6
The Ti-B alloy of embodiment 4 preparations is pressed Mg (AlH 4) 29mol%, NaAlH 4Press Mg (AlH 4) 29mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, and ball milling time 3h makes said Mg (AlH 4) 2Hydrogen storage system.
Embodiment 7
1, Ti powder and B powder are mixed according to mol ratio 1:2.2, place ball grinder, charge into the normal pressure argon gas in jar, obtain the Ti-B alloy with rotating speed ball milling 100h in ball mill of 450r/min according to the ball material mass ratio of 20:1.
2, the Ti-B alloy of gained is pressed Mg (AlH 4) 210mol%, NaAlH 4Press Mg (AlH 4) 210mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 5h.
The gained material is carried out the TPD test, and Fig. 3 is the TPD figure of gained material, shows this Ti-B alloy and NaAlH 4Mg (the AlH of concerted catalysis 4) 2First to put the hydrogen peak temperature be 115 ℃.
Embodiment 8
The Ti-B alloy of embodiment 7 preparations is pressed Mg (AlH 4) 21mol%, NaAlH 4Press Mg (AlH 4) 210mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 3h.
Embodiment 9
The Ti-B alloy of embodiment 7 preparations is pressed Mg (AlH 4) 210mol%, NaAlH 4Press Mg (AlH 4) 210mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 1h.
Embodiment 10
1, Ti powder and B powder are mixed according to mol ratio 1:2.4,20:1 places ball grinder according to ball material mass ratio, charges into the normal pressure argon gas in jar, obtains the Ti-B alloy with rotating speed ball milling 100h in ball mill of 450r/min.
2, the Ti-B alloy of gained is pressed Mg (AlH 4) 210mol%, NaAlH 4Press Mg (AlH 4) 21mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 1h.
Embodiment 11
The Ti-B alloy of embodiment 10 preparations is pressed Mg (AlH 4) 25mol%, NaAlH 4Press Mg (AlH 4) 220mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 3h.
Embodiment 12
The Ti-B alloy of embodiment 10 preparations is pressed Mg (AlH 4) 210mol%, NaAlH 4Press Mg (AlH 4) 220mol%, with Mg (AlH 4) 2Drop into ball grinder, ball material mass ratio 40:1 charges into the normal pressure argon gas in the ball grinder, drum's speed of rotation 450r/min, ball milling time 5h.

Claims (2)

1. Mg (AlH 4) 2The preparation method of hydrogen storage system is characterized in that, may further comprise the steps:
1) preparation of catalyzer Ti-B alloy
With Ti powder and B powder in molar ratio 1:1.8-1:2.4 take by weighing and by ball material mass ratio 20:1, throw in ball grinder ball milling 80-140h under argon shield, prepare said Ti-B alloy;
2) Mg (AlH 4) 2The preparation of hydrogen storage system
With said Ti-B alloy, NaAlH 4Press Mg (AlH respectively 4) 21 ~ 10mol% and 1 ~ 20mol% and Mg (AlH 4) 2Put in the ball grinder, ball material mass ratio 40:1, ball mill mixing 1-5h under argon shield makes said Mg (AlH 4) 2Hydrogen storage system.
2. Mg (AlH according to claim 1 4) 2The preparation method of hydrogen storage system is characterized in that, step 1), 2) in drum's speed of rotation be 450r/min.
CN2011103398731A 2011-11-01 2011-11-01 Preparation method of Mg(AlH4)2 hydrogen storage system Pending CN102502490A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417786A (en) * 2008-11-21 2009-04-29 包头稀土研究院 La15Fe77B8 type hydrogen storage alloy and use thereof
CN101554992A (en) * 2009-05-22 2009-10-14 南开大学 Method for preparing light metal complex hydrides by catalyzing boride and applications thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417786A (en) * 2008-11-21 2009-04-29 包头稀土研究院 La15Fe77B8 type hydrogen storage alloy and use thereof
CN101554992A (en) * 2009-05-22 2009-10-14 南开大学 Method for preparing light metal complex hydrides by catalyzing boride and applications thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杨桂玲等: "非金属与金属的协同作用对镁基储氢合金电化学性能的影响", 《物理化学学报》 *
闫超等: "NaAlH_4与TiB_2对Mg_AlH_4_2放氢温度的影响", 《南开大学学报（自然科学版）》 *

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Application publication date: 20120620