CN107934913A - The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping - Google Patents
The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping Download PDFInfo
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- CN107934913A CN107934913A CN201711123813.XA CN201711123813A CN107934913A CN 107934913 A CN107934913 A CN 107934913A CN 201711123813 A CN201711123813 A CN 201711123813A CN 107934913 A CN107934913 A CN 107934913A
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- 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
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Abstract
The invention discloses a kind of composite hydrogen storage material of transition metal fluorides doping, the material is by LiBH4、LiNH2、MgH2It is made with transition metal fluorides mixing machinery ball milling.It puts the initial hydrogen discharging temperature of hydrogen as 90 DEG C ~ 100 DEG C, and second step hydrogen discharging temperature is mainly put hydrogen and completed 180 DEG C ~ 200 DEG C sections at 150 DEG C or so, the wt% hydrogen of 6.5 wt% of composite hydrogen storage material releasing ~ 7.0 when being heated to 200 DEG C.Its preparation method includes：1）Raw material weighs；2）Ball-milling method prepares composite hydrogen storage material.The present invention has the following advantages：1st, there is relatively low hydrogen discharging temperature and a large amount of hydrogen discharging temperatures；2nd, hydrogen desorption capacity is big；3rd, put the induction period that the process that hydrogen is put as the second step of rate constants is greatly decreased in hydrogen process, reduce the hydrogen discharging temperature that second step puts hydrogen, coordinate two steps and put hydrogen process, and hydrogen discharge reaction speed is very fast, the dehydrogenation dynamic performance having had；4th, low raw-material cost, synthetic method, technique are simple.There is certain application prospect in hydrogen storage material field.
Description
Technical field
The present invention relates to the technical field of the hydrogen storage material of new energy materials, is specifically a kind of transition metal fluorides doping
Composite hydrogen storage material preparation method and its application in hydrogen storage material.
Background technology
Hydrogen Energy enjoys common people to close since it has the characteristics that efficient, cleaning, the renewable new energy for being known as 21 century
Note.The development and utilization of Hydrogen Energy is related to the four big key technologies such as preparation, storage, transport and the application of hydrogen, since hydrogen exists
Inflammable, explosive, easy diffusion, and problem, the storing technologies of hydrogen such as volume energy density under normal temperature and pressure is low become hydrogen
It can utilize and move towards practical, scale bottleneck.Therefore, the hydrogen storage technology for developing high-energy-density, high efficiency and safety is to work as
The key issue of modern urgent need to resolve.
In numerous hydrogen storage materials, light-weight metal boron hydride be considered as most promising hydrogen storage material system it
One.Wherein, LiBH4High hydrogen storage capability with 18.3 wt%, is a kind of hydrogen storage material of great potential.But its high thermodynamics
Stability and slow hydrogen desorption kinetics of inhaling can not meet the needs of its practical application.
In recent years, constantly research finds that the combination of amino-compound and boron hydride can effectively improve its dehydrogenation thermodynamics
And dynamic performance.Pinkerton et al. [F. E. Pinkerton, C. P. Meisner, M. S. Meyer, M. P.
Balogh and M. D. Kundrat. Hydrogen desorption exceeding ten weight percent
from the new quaternary hydride Li3BN2H8.Journal of Physical Chemistry B,
2005, 109:6-8.] according to molar ratio 1:2 by LiBH4With LiNH2It is for composite to have prepared new Li-B-N-H systems storage
Hydrogen material.When temperature is heated to ~ 350 DEG C, about 10 wt% of hydrogen desorption capacity of the Li-B-N-H systems.Its hydrogen discharging performance and LiBH4
And LiNH2Compared to being significantly increased, the extensive concern of people is caused.Because it has very high kinetic barrier, hydrogen discharging temperature
Still it is higher, and have NH during heat resolve3Releasing.Tang etc. [W. S. Tang, G. T. Wu, T. Liu,
A. T. S. Wee, C. K. Yong, Z. T. Xiong, A. T. S.Hor, P. Chen. Cobalt-catalyzed
hydrogen desorption from the LiNH2-LiBH4 system. Dalton Trans. 2008:2395-
2399.] it is used as catalyst by adding transition metal, hence it is evident that reduce the hydrogen discharging temperature of Li-B-N-H systems.It is multiple in order to improve
The hydrogen storage property of zoarium system, Yang [J. Yang, A. Sudik, D. J. Siegel, D. Halliday, A. Drews,
R.O. Carter, C. Wolverton,C.J.Lewis, J. W A. Sachtler, J. J. Low, S.
A.Faheem,D.A. Lesch and V OzolinS.A Self-Catalyzing Hydrogen-Storage
Material.Angewandte Chemie International Edition,2008, 47:882-887.] etc. development
With LiBH4、LiNH2And MgH2Compound multicomponent system hydrogen storage system.The system is " self-catalysis " system, is had more preferably
Hydrogen storage property：Its initial hydrogen discharging temperature is 150 DEG C or so, and dynamics and thermodynamic property have also obtained certain improvement；At the same time
NH3Release suppressed.Meanwhile the cycle performance for changing material is also improved.But it also there are following technology to ask
Topic：
1st, initial hydrogen discharging temperature is still higher, higher than 150 DEG C；
2nd, two steps are needed to put hydrogen, first step hydrogen desorption capacity is few, and second step hydrogen discharging temperature is higher, i.e., starts to put hydrogen at 250 DEG C, 320
DEG C degree could be realized and put hydrogen completely.
The content of the invention
The object of the present invention is to provide a kind of transition metal fluorides doping composite hydrogen storage material its preparation method and
Its application in hydrogen storage material.
By containing transition metal fluoride, promote the decomposition of intermediate product in reaction process using transition metal ions,
Hydrogen process is put in control, is on the one hand reduced the whole initial hydrogen discharging temperature for putting hydrogen process, on the other hand, is greatly decreased as rate-determining step
Rapid second step is put the induction period of the process of hydrogen, reduces the hydrogen discharging temperature that second step puts hydrogen, is coordinated two steps and is put hydrogen process, final real
Now largely put hydrogen process to occur below 200 DEG C, realize that hydrogen storage material releases the hydrogen of 7.0wt% at 200 DEG C.
Realizing the concrete technical scheme of the object of the invention is：
The composite hydrogen storage material of transition metal fluorides doping, it is by LiBH4、LiNH2、MgH2Mixed with transition metal fluorides
Mechanical ball mill is made, and the transition metal fluorides are nickel fluoride or cobaltous fluoride, which puts hydrogen, initially put
Hydrogen temperature is 90 DEG C ~ 100 DEG C, and second step hydrogen discharging temperature is mainly put hydrogen and completed in the range of 180 DEG C ~ 200 DEG C at 150 DEG C or so.
It is heated to the hydrogen that composite hydrogen storage material at 200 DEG C releases the wt% of 6.5 wt% ~ 7.0.
The preparation method of the composite hydrogen storage material of transition metal fluorides doping, comprises the following steps：
Step 1）Raw material weighs, by LiBH4、LiNH2、MgH2Mass ratio with transition metal fluorides is 1：2：（0~2）：
（0~0.1）, weigh LiBH4、LiNH2、MgH2And transition metal fluorides, mixing；
Step 2）Ball-milling method prepares composite hydrogen storage material.It is by ratio of grinding media to material（100~200）:1, by abrading-ball and step 1）The original weighed up
Material is put into ball grinder, sealing；Then ball grinder is put into ball mill, sets Ball-milling Time as 1 ~ 3 h, the rotating speed of ball milling for 100 ~
300 r/min, carry out ball milling, obtain the composite hydrogen storage material of transition metal fluorides doping.The whole preparation process exists
Carried out under inert gas conditions.
Through the dehydrogenation experiment detection that heats up, the initial dehydrogenated temperature of composite hydrogen storage material of the invention is 90 DEG C, compares LiBH4-
2LiNH2-MgH2Hydrogen storage material reduces 60 DEG C；And hydrogen discharging rate is substantially accelerated, LiBH at 200 DEG C4-2LiNH2-MgH2-
0.05NiF2Hydrogen storage material and LiBH4-2LiNH2-MgH2-0.05CoF2Hydrogen storage material can put 6.8 wt%'s and 7.0 wt% respectively
Hydrogen, and LiBH4-2LiNH2-MgH2The hydrogen that hydrogen storage material only has 3.3 wt% is released；Reach 8.3 in 300 DEG C of total hydrogen desorption capacities
Wt% and 8.5 wt%.
Test and detect through isothermal dehydrogenation, at 200 DEG C, LiBH in the present invention4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material
Material and LiBH4-2LiNH2-MgH2-0.05CoF2Hydrogen storage material can release the hydrogen of 6.8 wt% and 7.0 wt% in 20 min respectively
Gas, and LiBH4-2LiNH2-MgH2Hydrogen storage material is only capable of releasing the hydrogen of 3.3 wt%.
Therefore, the present invention has the following advantages relative to the prior art：
1st, composite hydrogen storage material of the invention has relatively low hydrogen discharging temperature, starts to put hydrogen at 90-100 DEG C；
2nd, the induction period for the process that hydrogen is put as the second step of rate constants is greatly decreased in the compound composite material of the present invention, reduces by the
Two steps put the hydrogen discharging temperature of hydrogen, i.e., put hydrogen being reduced to 150 DEG C or so by original 250 DEG C or so；
3rd, hydrogen completion is largely put when composite hydrogen storage material of the present invention is heated to 200 DEG C, hydrogen desorption capacity can reach 7.0 wt% or so, have
The dehydrogenation dynamic performance having had；
4th, composite hydrogen storage material of the invention is of low cost, derives from a wealth of sources, synthetic method, technique are simple, are easy to mass produce.
So the present invention has certain application prospect in hydrogen storage material.
Brief description of the drawings：
Fig. 1 is LiBH prepared by Examples 1 and 24-2LiNH2-MgH2-0.05NiF2Hydrogen storage material and LiBH4-2LiNH2-MgH2-
0.05CoF2The temperature programming Hydrogen desorption isotherms of hydrogen storage material；
Fig. 2 is LiBH prepared by Examples 1 and 24-2LiNH2-MgH2-0.05NiF2Hydrogen storage material and LiBH4-2LiNH2-MgH2-
0.05CoF2Hydrogen storage material in 200 DEG C of constant temperature Hydrogen desorption isotherms.
Embodiment
The present invention is described further present invention with reference to Figure of description, but be not to this hair by embodiment
Bright restriction.
Embodiment 1
A kind of composite hydrogen storage material of transition metal fluorides doping, LiBH4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material
Preparation method, comprises the following steps：
Step 1）Raw material weighs：Under the protection of argon gas, 0.088 g LiBH are weighed4、0.1856 g LiNH2、0.1064 g
MgH2With 0.02 g NiF2Powder, totally 0.4 g；
Step 2）Ball-milling method prepares composite hydrogen storage material：It is 200 by ratio of grinding media to material under the protection of argon gas:1, by abrading-ball and step
1）The raw material weighed up is put into ball grinder, sealing；Then ball grinder is put into ball mill, sets rotational speed of ball-mill as 200 rpm, ball milling
Time is 2 h, obtains LiBH4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material.
Embodiment 2
A kind of composite hydrogen storage material of transition metal fluorides doping, LiBH4-2LiNH2-MgH2-0.05CoF2Hydrogen storage material
Preparation method, comprises the following steps：
Step 1）Raw material weighs：Under the protection of argon gas, 0.088 g LiBH are weighed4、0.1856 g LiNH2、0.1064 g
MgH2With 0.02 g CoF2Powder, totally 0.4 g；
Step 2）Ball-milling method prepares composite hydrogen storage material：It is 200 by ratio of grinding media to material under the protection of argon gas:1, by abrading-ball and step
1）The raw material weighed up is put into ball grinder, sealing；Then ball grinder is put into ball mill, sets rotational speed of ball-mill as 200 rpm, ball milling
Time is 2 h, obtains LiBH4-2LiNH2-MgH2-0.05CoF2Hydrogen storage material.
In order to study influence of the different transition metal fluorides to composite hydrogen storage material hydrogen storage property, to Examples 1 and 2 system
The composite hydrogen storage material LiBH of the different transition metal fluorides doping of standby 2 kinds4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material
And LiBH4-2LiNH2-MgH2-0.05CoF2Hydrogen storage material carries out heating dehydrogenation experiment test, and heating rate is 2 DEG C/min.
Experimental result is as shown in Figure 1, can be seen that the composite hydrogen storage material of transition metal fluorides doping from Hydrogen desorption isotherms
Hydrogen discharging performance be effectively improved.Its initial dehydrogenated temperature is 90 DEG C, compares LiBH4-2LiNH2-MgH2Hydrogen storage material it is initial
Desorption temperature reduces 60 DEG C；Largely put hydrogen when being heated to 200 DEG C to terminate, LiBH4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material
Material and LiBH4-2LiNH2-MgH2-0.05CoF2The hydrogen desorption capacity of hydrogen storage material respectively reaches 7.0 wt% and 6.8 wt%；300
DEG C, its hydrogen desorption capacity has respectively reached 8.5 wt% and 8.3 wt%.
The isothermal dehydrogenation experiment of the composite hydrogen storage material of transition metal fluorides doping.
The composite hydrogen storage material of transition metal fluorides doping is subjected to isothermal dehydrogenation experiment at 200 DEG C.Experimental result is such as
Shown in Fig. 2, the LiBH at 200 DEG C4-2LiNH2-MgH2-0.05NiF2Hydrogen storage material and LiBH4-2LiNH2-MgH2-0.05CoF2
Hydrogen storage material can put the hydrogen of 6.8 wt% and 7.0 wt% in 20 min respectively, and LiBH4-2LiNH2-MgH2Hydrogen storage material only has
The hydrogen of 3.3 wt% is released.
Claims (8)
- A kind of 1. composite hydrogen storage material of transition metal fluorides doping, it is characterised in that：The material is by LiBH4、LiNH2、MgH2 It is made with transition metal fluorides mixing machinery ball milling.
- 2. composite hydrogen storage material according to claim 1, it is characterised in that：The transition metal fluorides for nickel fluoride or Cobaltous fluoride.
- 3. composite hydrogen storage material according to claim 1, it is characterised in that：Two step of composite hydrogen storage material puts hydrogen, at the beginning of it Beginning hydrogen discharging temperature is 90 DEG C ~ 100 DEG C, and second step hydrogen discharging temperature mainly puts hydrogen in the range of 180 DEG C ~ 200 DEG C at 150 DEG C or so Complete.
- 4. composite hydrogen storage material according to claim 1, it is characterised in that：When being heated to 200 DEG C, the composite hydrogen-storage material Material can release the hydrogen of the wt% of 6.5 wt% ~ 7.0.
- 5. the preparation method of composite hydrogen storage material according to claim 1, it is characterised in that comprise the following steps：Step 1）Raw material weighs, and LiBH is weighed by the ratio between amount of certain material4、LiNH2、MgH2Mixed with transition metal fluorides Close powder；Step 2）Ball-milling method prepares composite hydrogen storage material, by certain ratio of grinding media to material, by abrading-ball and step 1）The raw material weighed up is put into Ball grinder, sealing；Then ball grinder is put into ball mill, in certain ball milling condition ball milling, obtains transition metal fluorides doping Composite hydrogen storage material.
- 6. preparation method according to claim 5, it is characterised in that：The step 1）LiBH4、LiNH2、MgH2And transition The ratio between amount of material of metal fluoride is LiBH4：LiNH2：MgH2：Transition metal fluorides=1：2：（0~2）：（0~0.1）.
- 7. preparation method according to claim 5, it is characterised in that：The step 2）Ratio of grinding media to material be（100~200）： 1；Ball milling condition is：Ball-milling Time is 1 ~ 3 h, and the rotating speed of ball milling is 100 ~ 300 r/min.
- 8. preparation method according to claim 5, it is characterised in that：The whole preparation process is in inert gas conditions Lower progress.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081383A (en) * | 2018-07-10 | 2018-12-25 | 扬州大学 | The preparation method of transition metal fluorides |
| CN112110426A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Method for synthesizing amino lithium potassium by mechanical ball milling |
| CN112110428A (en) * | 2020-08-25 | 2020-12-22 | 浙江工业大学 | Method for synthesizing amino lithium potassium by solid-solid reaction |
| CN112110427A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Synthesis method of lithium potassium amino fluoride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183312A (en) * | 2011-12-26 | 2013-07-03 | 北京有色金属研究总院 | Li-Mg-B-N-H hydrogen storage material |
| CN103539066A (en) * | 2012-07-13 | 2014-01-29 | 中国科学院大连化学物理研究所 | NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material and preparation method thereof |
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2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183312A (en) * | 2011-12-26 | 2013-07-03 | 北京有色金属研究总院 | Li-Mg-B-N-H hydrogen storage material |
| CN103539066A (en) * | 2012-07-13 | 2014-01-29 | 中国科学院大连化学物理研究所 | NiF2-dopped LiBH4-LiNH2-CaH2 composite hydrogen storage material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081383A (en) * | 2018-07-10 | 2018-12-25 | 扬州大学 | The preparation method of transition metal fluorides |
| CN109081383B (en) * | 2018-07-10 | 2023-08-25 | 扬州大学 | Process for preparing transition metal fluorides |
| CN112110426A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Method for synthesizing amino lithium potassium by mechanical ball milling |
| CN112110427A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Synthesis method of lithium potassium amino fluoride |
| CN112110428A (en) * | 2020-08-25 | 2020-12-22 | 浙江工业大学 | Method for synthesizing amino lithium potassium by solid-solid reaction |
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