CN106698347A - Lithium-sodium dual-alkali metal aluminum-hydrogen compound and synthesis method thereof - Google Patents

Lithium-sodium dual-alkali metal aluminum-hydrogen compound and synthesis method thereof Download PDF

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CN106698347A
CN106698347A CN201611166388.8A CN201611166388A CN106698347A CN 106698347 A CN106698347 A CN 106698347A CN 201611166388 A CN201611166388 A CN 201611166388A CN 106698347 A CN106698347 A CN 106698347A
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powder
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hydrogen
lithium
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CN106698347B (en
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张耀
范小路
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Southeast University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/24Hydrides containing at least two metals; Addition complexes thereof
    • C01B6/243Hydrides containing at least two metals; Addition complexes thereof containing only hydrogen, aluminium and alkali metals, e.g. Li(AlH4)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

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Abstract

The invention discloses lithium-sodium dual-alkali metal aluminum-hydrogen compound and a synthesis method thereof. The lithium-sodium dual-alkali metal aluminum-hydrogen compound has a single cubic structure and has the chemical formula of LixNa3-xAlH6, wherein x is 0.9-1.3. The lithium-sodium dual-alkali metal aluminum-hydrogen compound has high proportion hydrogen storage capacity and fast hydrogen absorption rate. The preparation method for the lithium-sodium dual-alkali metal aluminum-hydrogen compound comprises the following steps: mixing Li3AlH6 and Na3AlH6 according to the molar ratio of 0.9:2.1-1.3:1.7, and ball-milling for 10-30 h at a speed of 400 rpm-500 rpm, to obtain LixNa3-xAlH6, wherein x is 0.9-1.3; Li toms and Na atoms in the structure occupy gaps of an AlH6 octahedron, and the Li toms and the Na atoms are replaced with each other along with the different ratio of the Li toms and the Na atoms. The method is simple and easy to implement, and is suitable for mass commercial production; the optimum proportion hydrogen storage capacity is high, the initial dehydrogenation temperature is low, and the hydrogen absorption rate is obviously improved.

Description

A kind of double composite alkali aluminum hydrogen compounds of lithium sodium and its synthetic method
Technical field
The present invention relates to the double composite alkali aluminum hydrogen compounds of lithium sodium and its synthetic method, belong to hydrogen storage material field.
Technical background
With developing rapidly for human society, the energy increasingly becomes the bottleneck of restriction Human Sustainable Development.Traditional energy Source material is mainly fossil energy oil, coal, natural gas etc..However, with the long-term use of such energy and material, it is natural Environment has also suffered serious destruction.Acid rain, haze, greenhouse effects etc. all have with the use of traditional energy material it is close can not The contact for dividing, the environment moment for the survival of mankind suffer from threat.Although the regenerative resources such as wind energy, solar energy are in certain journey The pressure that fossil energy is brought to environment is alleviated on degree, but most of regenerative resource can not directly meet human society To the demand of the energy.
Hydrogen Energy is undoubtedly the green energy resource that a kind of calorific value is high, pollution-free, can be recycled, be the long-term sustainable development of the mankind and Existence is provided may.Hydrogen Energy has immeasurable prospect in industries such as motor vehicle, aviations.Hydrogen storage has gaseous high pressure to store up The technical approach such as hydrogen, liquid low temperature hydrogen storage, solid-state hydrogen storage, wherein, solid-state hydrogen storage is that one kind is reacted using hydrogen storage material with hydrogen The chemical hydrogen storage technology of generation solid solution and hydride, compared with first two physics hydrogen storage technology, with hydrogen-storage density is big, transport Convenient and safe advantage, is increasingly valued by people and favors.Wherein, light metal complex hydrides hydrogen storage system such as boron hydrogen Compound system, alanate system, amides system etc., due to being all made up of lightweight element, its theoretical hydrogen storage capability will The solid hydrogen-storing alloy more traditional than other is much higher, and puts hydrogen decomposition temperature with relatively low, is solid-state storage in recent years The main direction of studying of hydrogen Material Field.
It is wherein especially practical the most considerable with alanate system.But LiAlH4It is irreversible, NaAlH4Although it is reversible but It is that its suction hydrogen dynamic performance is poor, reversal condition is more harsh, as the bottleneck for restricting its popularization and application.LiNa2AlH6It is reversible Property is good, but its initial dehydrogenated temperature is of a relatively high, and dehydrogenation rate is to be improved.
The content of the invention
Technical problem:It is an object of the present invention to provide a kind of double composite alkali aluminum hydrogen compounds of lithium sodium, the compound hydrogen storage capability Height, initial dehydrogenated temperature is low, and hydrogen-absorption speed is significantly improved.
It is a further object to provide a kind of synthetic method of the double composite alkali aluminum hydrogen compounds of lithium sodium, the method letter It is single easy, it is adaptable to high-volume commodity production.
Technical scheme:The invention provides a kind of double composite alkali aluminum hydrogen compounds of lithium sodium, the double composite alkali aluminum hydrogenations of the lithium sodium The chemical formula of compound is LixNa3-xAlH6, x=0.9~1.3, with single cubic structure, Li atoms and Na atoms in the structure Occupy AlH6Octahedral gap;As Li atoms are different from Na atomic ratios, Li atoms and Na atom phase double replacements.
Wherein:
Described chemical formula is LixNa3-xAlH6Best performance is Li1.3Na1.7AlH6
The initial dehydrogenated temperature of the double composite alkali aluminum hydrogen compounds of described lithium sodium is 150 DEG C~250 DEG C, and 1000s inhales hydrogen and holds It is 2.0wt%~2.25wt% to measure, and 300 DEG C of amount of dehydrogenation is 3.0wt%~3.45wt%.
Present invention also offers a kind of synthetic method of the double composite alkali aluminum hydrogen compounds of lithium sodium, the method includes following step Suddenly:
Step one, according to mol ratio 0.9:2.1~1.3:1.7 by Li3AlH6Powder and Na3AlH6Powder mixes, and is mixed Close powder;
Step 2, the mixed-powder for obtaining step one carry out ball milling, and Li is obtainedxNa3-xAlH6Powder, wherein x=0.9~ 1.3。
Wherein:
Li described in step one3AlH6Powder preparation method is as follows:According to mol ratio 2:1 weighs LiH powder and LiAlH4Powder , in being fitted into ball grinder under ar gas environment, be loaded into ball grinder on ball mill afterwards by end, and grinding is obtained Li3AlH6Powder, institute State mill ball quality and LiH powder and LiAlH in ball grinder4The ratio of the gross mass of both powder is 30:1~80:1, the grinding The rotating speed of machine is 400rpm~500rpm, a length of 5h~10h during grinding.
Na described in step one3AlH6Powder preparation method is as follows:According to mol ratio 2:1 weighs NaH powder and NaAlH4Powder , in being fitted into ball grinder under ar gas environment, be loaded into ball grinder on ball mill afterwards by end, and grinding is obtained Na3AlH6Powder, institute State mill ball quality and NaH powder and NaAlH in ball grinder4The ratio of the gross mass of both powder is 30:1~80:1, the grinding The rotating speed of machine is 400rpm~500rpm, a length of 10h-30h during grinding.
Mechanical milling process described in step 2 is:By Li3AlH6Powder and Na3AlH6Powder loads ball milling under ar gas environment In tank, ball grinder is loaded on ball mill afterwards, grinding is obtained Na3AlH6Powder, wherein x=0.9~1.3, the ball grinder Middle mill ball quality and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1~80:1, the grinder Rotating speed is 400rpm~500rpm, a length of 10h~30h during grinding.
The double composite alkali aluminum hydrogen compound Li of described lithium sodium1.3Na1.7AlH6, the 1000s hydrogen-absorption speeds of the compound are obvious Higher than hydroaluminium LiNa2AlH6
Beneficial effect:The present invention compared with prior art, with advantages below:
The double composite alkali aluminum hydrogen compound molecular weight of lithium sodium prepared by the present invention are relatively low, thus hydrogen storage capability is relatively Height, initial dehydrogenated temperature is substantially reduced, and is inhaled hydrogen discharging rate and is significantly improved, and is widely used in portable and stationary hydrogen energy equipment.
The response path of the synthetic method of the double composite alkali aluminum hydrogen compounds of lithium sodium that the present invention is provided is relatively easy, and synthesis is produced Thing purity is high, simple for process, can be widely applied to the production of hydrogen storage material.
Brief description of the drawings
Fig. 1, LixNa3-xAlH6Ball milling synthetic sample X-ray diffractogram, wherein x=0.9~1.3;
Fig. 2, LixNa3-xAlH6Cell parameter is with lithium atom mol ratio change curve;
Fig. 3, LixNa3-xAlH6Desorption by heating curve under 5 DEG C/min heating rates, 300 DEG C of vacuum states;
Fig. 4, under the conditions of 234 DEG C, -5MPa hydrogen pressures, LixNa3-xAlH6It is bent that pure phase dehydrogenation product 1000s inhales hydrogen dynamics Line.
Specific embodiment
By LiH powder and LiAlH4Powder is according to mol ratio 2:1 ratio, in ar gas environment lower-weighing and loads ball milling Tank, abrading-ball is mass ratio 30 with abrasive material ratio:1~80:1.It is loaded on star-like ball mill, with rotating speed 400rpm~500rpm ball millings 5h~10h is obtained Li3AlH6Powder is stand-by.
By NaH powder and NaAlH4Powder is according to mol ratio 2:1 ratio is in ar gas environment lower-weighing and loads ball grinder, Abrading-ball is mass ratio 30 with abrasive material ratio:1~80:1.It is loaded on star-like ball mill, with rotating speed 400rpm~500rpm ball millings 10h-30h is obtained Na3AlH6Powder is stand-by.
By obtained Li3AlH6With Na3AlH6Powder is according to 0.9:2.1~1.3:1.7 molar ratio mixed-powders, It is fitted into ball grinder under ar gas environment, abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1~ 80:1.Grinding jar is loaded on star-like ball mill afterwards, Li is obtained with rotating speed 400rpm~500rpm ball millings 10h~30hxNa3- xAlH6Powder, Li is determined through XRD testsxNa3-xAlH6Pure phase (x=0.9~1.3).
The hydrogen storage property test of sample uses Xihua special type gas-solid reaction test equipment (PCT), the liter of main test sample Temperature desorption TPD, suction hydrogen dynamics, all test samples load process and are carried out under glove box ar gas environment.To hydrogen storage material Hydrogen storage property test is carried out, in glove box ar gas environment lower-weighing is fitted into the sample cell of PCT equipments no less than 0.2g samples.Dress After carrying sample cell, vacuum is extracted to below 0.093MPa with vavuum pump, with 5 degrees/min of heating rate test program desorption by heating Curve (TPD, as shown in Figure 3).In 234 DEG C of insulations after the completion of desorption, plus 5MPa hydrogen presses test material hydrogen sucking function (such as Fig. 4 institutes Show).Sample Li can respectively be drawn by Fig. 3, Fig. 41.3Na1.7AlH6For desorption temperature is minimum, hydrogen storage capability is maximum, 1000s inhales hydrogen The double composite alkali aluminum hydride hydrogen storage system samples of the most fast Li~Na of speed.
Example 1
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 0.9:2.1 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, wherein abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1. Ball grinder is loaded on star-like ball mill afterwards, Li is obtained with rotating speed 400rpm ball millings 10h0.9Na2.1AlH6Powder, through XRD Test determines Li0.9Na2.1AlH6Pure phase, tests its hydrogen storage property in a manner described, and desorption temperature is 210 DEG C~260 DEG C.
Example 2
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.0:2.0 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, wherein abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 40:1. Ball grinder is loaded on star-like ball mill afterwards, Li is obtained with the ball milling 15h of rotating speed 4301.0Na2.0AlH6Powder, tests through XRD Determine Li1.0Na2.0AlH6Pure phase, tests its hydrogen storage property in a manner described, and desorption temperature is 210 DEG C~260 DEG C.
Example 3
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.1:1.9 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, wherein abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 50:1. Ball grinder is loaded on star-like ball mill afterwards, Li is obtained with rotating speed 460rpm ball millings 20h1.1Na1.9AlH6Powder, through XRD Test determines Li1.1Na1.9AlH6Pure phase, tests its hydrogen storage property in a manner described, and desorption temperature is 210 DEG C~260 DEG C.
Example 4
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.2:1.8 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, wherein Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 65:1.Afterwards will Ball grinder is loaded on star-like ball mill, and Li is obtained with rotating speed 480rpm ball millings 25h1.2Na1.8AlH6Powder, it is true through XRD tests Determine Li1.2Na1.8AlH6Pure phase, tests its hydrogen storage property in a manner described, and desorption temperature is 200 DEG C~260 DEG C.
Example 5
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.3:1.7 mixed-powders, in ar gas environment In lower loading ball grinder, wherein Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 80:1.Afterwards by ball milling It is canned to be downloaded on star-like ball mill, Li is obtained with rotating speed 500rpm ball millings 30h1.3Na1.7AlH6Powder, tests through XRD and determines Li1.3Na1.7AlH6Pure phase, tests its hydrogen storage property in a manner described, and desorption temperature is 150 DEG C~250 DEG C, such as Fig. 3 and Fig. 4 institutes Show Li1.3Na1.7AlH6Hydrogen-absorption speed and dehydrogenation capacity are up to optimal proportion.
Example 6
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.4:1.6 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, wherein abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1 ~80:1.Ball grinder is loaded on star-like ball mill afterwards, is obtained with rotating speed 400rpm~500rpm ball millings 10~30 hours Li1.4Na1.6AlH6Powder, Li is determined through XRD tests1.4Na1.6AlH6Thing calculates the visible pure phase scope of cell parameter through jade X between 0.9~1.3, as shown in Fig. 2 in x=1.4, shown Li1.4Na1.6AlH6Non- pure phase.
Example 7
By obtained Li3AlH6With Na3AlH6Powder is according to Li~Na mol ratios 1.5:1.5 prepare mixed-powder, in argon gas It is fitted into ball grinder under environment, with abrading-ball and Li3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1~ 80:1.Ball grinder is loaded on star-like ball mill afterwards, is obtained with rotating speed 400rpm~500rpm ball millings 10h~30 hour Li1.5Na1.5AlH6Powder, Li is determined through XRD tests1.5Na1.5AlH6Sample contains NaAlH4, as shown in x=1.5 in Fig. 1 Li1.5Na1.5AlH6Non- pure phase.

Claims (6)

1. double composite alkali aluminum hydrogen compounds of a kind of lithium sodium, it is characterised in that:The chemical formula of the double composite alkali aluminum hydrogen compounds of the lithium sodium It is LixNa3-xAlH6, x=0.9~1.3, with single cubic structure, Li atoms and Na atoms occupy AlH in the structure6Octahedral The gap of body, as Li atoms are different from Na atomic ratios, Li atoms and Na atom phase double replacements.
2. double composite alkali aluminum hydrogen compounds of a kind of lithium sodium as claimed in claim 1, it is characterised in that:Described chemical formula LixNa3-xAlH6Best performance is Li1.3Na1.7AlH6
3. double composite alkali aluminum hydrogen compounds of a kind of lithium sodium as claimed in claim 1, it is characterised in that:The double alkali gold of described lithium sodium Category hydroaluminium, the initial dehydrogenated temperature of the compound is 150 DEG C~250 DEG C, 1000s hydrogen absorption capacities be 2.0wt%~ 2.25wt%, 300 DEG C of amount of dehydrogenation is 3.0wt%~3.45wt%.
4. the synthetic method of the double composite alkali aluminum hydrogen compounds of a kind of lithium sodium as claimed in claim 1, it is characterised in that:The method Comprise the following steps:
Step one, according to mol ratio 0.9:2.1~1.3:1.7 by Li3AlH6Powder and Na3AlH6Powder mixes, and obtains mixed powder End;
Step 2, the mixed-powder for obtaining step one carry out ball milling, and Li is obtainedxNa3-xAlH6Powder, wherein x=0.9~1.3.
5. the synthetic method of the double composite alkali aluminum hydrogen compounds of a kind of lithium sodium as claimed in claim 4, it is characterised in that:Step 2 Described mechanical milling process is:By Li3AlH6Powder and Na3AlH6During powder is fitted into ball grinder under ar gas environment, afterwards by ball milling Canned to be downloaded on ball mill, grinding is obtained LixNa3-xAlH6Powder, wherein x=0.9~1.3.
6. the synthetic method of the double composite alkali aluminum hydrogen compounds of a kind of lithium sodium as claimed in claim 5, it is characterised in that:The ball Mill ball quality and Li in grinding jar3AlH6Powder and Na3AlH6The ratio of the gross mass of both powder is 30:1~80:1, the grinding The rotating speed of machine is 400rpm~500rpm, a length of 10h~30h during grinding.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7837976B2 (en) * 2005-07-29 2010-11-23 Brookhaven Science Associates, Llc Activated aluminum hydride hydrogen storage compositions and uses thereof
CN102530872A (en) * 2010-12-08 2012-07-04 中国科学院金属研究所 Multi-metal ammonia borane compound hydrogen storage material and preparation and composite hydrogen release method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
FENGHUAI WANG ET AL.: "Formation Reactions and the Thermodynamics and Kinetics of Dehydrogenation Reaction of Mixed Alanate Na2LiAlH6", 《JOURNAL OF PHYSICAL CHEMISTRY C》 *
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