CN110342458A - Composite hydrogen storage material, preparation method and application - Google Patents
Composite hydrogen storage material, preparation method and application Download PDFInfo
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- CN110342458A CN110342458A CN201910612688.1A CN201910612688A CN110342458A CN 110342458 A CN110342458 A CN 110342458A CN 201910612688 A CN201910612688 A CN 201910612688A CN 110342458 A CN110342458 A CN 110342458A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
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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
- Y02E60/32—Hydrogen storage
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Abstract
The invention discloses a kind of TiH1.971Adulterate MgH2Composite hydrogen storage material, preparation method and application, the composite hydrogen storage material include TiH1.971Powder and MgH2, TiH1.9711wt%~the 15wt% for accounting for composite hydrogen storage material gross mass, by changing TiH1.971The Ball-milling Time and doping ratio of powder studies MgH2Hydrogen storage property.The present invention provides MgH2There is composite material good low temperature to inhale hydrogen desorption kinetics performance and higher sucking/placing hydrogen amount, and preparation method is simple, and cost of material is low, both can be applied to the hydrogen source etc. of protable power unit, fuel cell, has been also applied for large-scale development application.
Description
Technical field
The present invention relates to hydrogen storage materials, and in particular to a kind of composite hydrogen storage material, preparation method and application.
Background technique
The energy is the power of the national economic development, is the important way uplifted the people's living standard.Society is being constantly progressive
With development, energy technology is also in breakthrough of constantly bringing forth new ideas, from the exploitation and use of fossil energy, to the innovation of current new energy
With research, change each time is all in the living standard for improving the people.But due to the limitation of technology, fossil energy or society
The energy relied primarily on accounts for world energy sources use 80%.However fossil energy consumption is increasingly sharpened, including the card by heat engine
When promise circulation carries out energy conversion, there are low efficiencys for it, cause a large amount of energy loss, in addition can also generate CO2, nitrogen oxides
Atmospheric environment and water quality are polluted with sulfide etc..Therefore replacing traditional fossil energy using renewable energy is social hair
The inexorable trend of exhibition.And Hydrogen Energy is just an ideal instead of the energy, can be generated after burning very big thermal energy (1.25 ×
105The heat of kJ can be obtained by 1kg combustion of hydrogen), and combustion product is also relatively cleaner, is a kind of high-quality cleaning renewable energy
Source, and green non-pollution, acquiring way are extensive.Hydrogen Energy is that electric energy is directly converted energy by fuel cell, conversion
There is no the constraint of Carnot cycle in process, thus improves efficiency.
However, being widely used for hydrogen depend on storing it in a kind of safe and efficient and cheap mode, great Jia Dou
It begins to focus on and is dedicated to research and development new material relevant to hydrogen storage, new technology.So far, the liquid hydrogen in hydrogen storage technology
Storing technology, LIGHTWEIGHT HIGH-PRESSURE HYDROGEN TANK technology and Metal hydride systems hydrogen storage technology are in hydrogen-burning automobile or electronic vapour
Successful operation on vehicle.Compared to storage of liquid hydrogen technology and LIGHTWEIGHT HIGH-PRESSURE HYDROGEN TANK technology, Metal hydride systems hydrogen storage technology
Safety is good, and volume hydrogen-storage density is high, so becoming the method for a more attractive using hydride hydrogen-storing.
Magnesium is a kind of very strong hydrogen storage material of hydrogen-absorbing ability, resourceful, low in cost.Improve the effective of magnesium hydrogen storage property
Method is that magnesium and other hydrogen storage compounds is compound.Compared to other metal hydrides, MgH2Hold up to the quality storage of 7.6wt%
Hydrogen density, relatively cheap price, reserves abundant and good reversible hydrogen storage performance, but MgH2It need to be at 300 DEG C or more
Hydrogen release can be effectively inhaled, hydrogen discharging temperature is high, and MgH2High thermodynamic stability and slowly inhale hydrogen desorption kinetics performance limit
Its practical application.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of composite hydrogen storage material, preparation method and applications, solve existing
Current material cannot hydrogen storage at low temperature, the problem of hydrogen storage low efficiency.
Technical solution: composite hydrogen storage material of the present invention, including TiH1.971And MgH2, wherein TiH1.971It accounts for described multiple
Close 1%~15wt% of hydrogen storage material gross mass.
The preparation method of composite hydrogen storage material of the present invention, comprising the following steps:
(1) by TiH1.971Powder is mixed with oleic acid, oleyl amine and heptane, with the revolving speed continuous ball milling 10~60 of 300~500rpm
h；
(2) sample clean after ball milling, after standing remove supernatant liquor, liquid will be instilled after remaining solid carrying out washing treatment
Pipe；
(3) by sample centrifugation, the dry, evacuation after washing, TiH can be obtained1.97Particle；
(4) TiH that will be obtained1.97Particle and MgH2After mixing in an inert atmosphere ball milling to get arrive composite hydrogen-storage material
Material.
Wherein TiH in the step (1)1.97Volume ratio with oleic acid, oleyl amine and heptane is 1:0.33~1:10~1:20.
In order to increase the contact area of steel ball and hydrogen storage material, reduce the particle of hydrogen storage material, the step (1) in ball milling
Middle TiH1.971Mass ratio with the steel ball for ball milling is 1:45~60.
It is cleaned in the step (2) using oleic acid, oleyl amine and mixed solvent in heptan, wherein TiH1.97With oleic acid, oleyl amine
Volume ratio with heptane is 1:0.33~1:10~1:50.
The time that sample is stood in the step (2) is 10~30min, is washed using wine clear to the remaining solid,
It is 5~10 times with the number of ethanol wash.
Centrifugal rotational speed is 8000~10000rpm in the step (3), and the time is 6~10min.
Inert atmosphere finger pressure is the high-purity argon gas atmosphere less than 0.1MPa in the step (4), and the time of ball milling is 1
~6h, ball mill revolution speed are 300~500rpm.
Composite hydrogen storage material of the present invention exists according to the composite hydrogen storage material that the preparation method is prepared
Application as hydrogen storage material.
The utility model has the advantages that: there is composite hydrogen storage material of the invention good low temperature to inhale hydrogen desorption kinetics performance and higher
Sucking/placing hydrogen amount can inhale hydrogen at room temperature；The hydrogen release that heats up is the experimental results showed that doping 5wt%-c-TiH1.971Composite material exist
175 DEG C of beginning hydrogen releases, when temperature is increased to 300 DEG C, can discharge the hydrogen of 6.7wt%.In addition, preparation method letter of the present invention
It is single, it is easy to operate, it can need to only be prepared using mechanical ball mill technology at room temperature, and TiH1.971Preparation it is easy, it is easy to operate,
Cost of material is low, both can be applied to the hydrogen source etc. of protable power unit, fuel cell, has been also suitable for large-scale development and answers
With.
Detailed description of the invention
Fig. 1 is Ball-milling Time to MgH2The influence of the heating hydrogen discharging performance of hydrogen storage material；
Fig. 2 is doping ratio to MgH2The influence of the heating hydrogen discharging performance of hydrogen storage material；
Fig. 3 is MgH2/ 5wt%-c-TiH1.971The heating Hydrogen desorption isotherms (2 DEG C/min of heating rate) of composite hydrogen storage material；
Fig. 4 is doped catalyst TiH1.971The XRD spectra (2 θ=20~80 °) of material
Fig. 5 is MgH2/ 5wt%-c-TiH1.971Hydrogen curve (1 DEG C/min of heating rate) is inhaled in the heating of composite hydrogen storage material；
Fig. 6 is doped catalyst TiH1.971Composite hydrogen storage material constant temperature Hydrogen desorption isotherms；
Fig. 7 is doped catalyst TiH1.971The XRD spectra (2 θ=20~80 °) of composite hydrogen storage material constant temperature hydrogen release.
Specific embodiment
Invention is further explained with reference to the accompanying drawings and examples.
Embodiment 1
Ball-milling Time is studied to TiH1.971Improve MgH2The influence of heating hydrogen discharging performance:
TiH is prepared first1.97Particle: by TiH1.971Powder is mixed with oleic acid, oleyl amine and heptane, TiH1.971With oleic acid, oleyl amine
Volume ratio with heptane is 1:0.33~1:10~1:20, with revolving speed the continuous ball milling 10~60h, TiH of 300~500rpm1.971
Mass ratio with the steel ball for ball milling is 1:45~60；Supernatant liquor is removed after sample clean, standing after ball milling, it will be remaining
Solid carrying out washing treatment after instill liquid line and cleaned using oleic acid, oleyl amine and mixed solvent in heptan, wherein oleic acid, oleyl amine and
The volume ratio of heptane is 1:0.33~1:10~1:50, and heptane amount is too many in order to prevent, it is difficult to it is sufficiently mixed with material, so point
To instill twice, it is carried out to rock mixing after instilling every time, be sucked out, carry out secondary instillation, finally drips oleic acid, oleyl amine
Enter in liquid line；By sample centrifugation, the dry, evacuation after washing, TiH can be obtained1.97Particle；
By the TiH of 5wt%1.971It is mixed into the MgH of 95wt%2Middle carry out ball milling.With the mass ratio of ratio of grinding media to material 40:1, in ball milling
It is put into the ball of 40g in tank, is put into the sample of 1g, wherein the TiH in each tank1.971Ball-milling Time is different, in 10~60h model
It is that 450rpm makes ball grinder positive and negative alternate run 30min, but need to stall 6min when alternately with revolving speed in enclosing.Ball milling two is small
Shi Hou takes out ball grinder, smashs to pieces to the sample to agglomerate in tank.Then at ball milling two hours, sample is taken out, is sealed and is put into hand
It prevents from aoxidizing in casing.
The catalyst composite system 150~250mg of sample for adulterating different Ball-milling Times is weighed in casing respectively.Sample is put
After entering device, evacuates, stop leakage in the roof, start to test, be warming up to 450 DEG C by program with the rate of 2 DEG C/min.
According to the TiH of 10~60h of ball milling1.971Powder Hydrogen desorption isotherms are as shown in Figure 1, comparison shows through Ball-milling Time
Change, TiH1.971To MgH2Hydrogen discharging performance has significant difference, increases Ball-milling Time, can significantly reduce MgH2Initial hydrogen discharging temperature
And hydrogen discharging rate can be improved, and obtain TiH1.971Ball-milling Time with optimal catalytic activity is 60h.
Embodiment 2
Doping ratio is studied to TiH1.971Improve MgH2The influence of heating hydrogen discharging performance:
With the TiH of ball milling 60h1.971Shared ratio is 1wt%~15wt% and MgH2Mixing and ball milling.With ratio of grinding media to material 40:
1 mass ratio is put into the sample of 2g, equally marks, and is that 450rpm makes ball grinder positive and negative alternate run 30min with revolving speed,
But 6min need to be stalled when alternately.After two hours of ball milling, the sample to agglomerate in tank is smashed to pieces；Then at ball milling two hours,
Sample is taken out, is sealed in glove box.
Catalyst composite system 150~250mg of sample of doping 1~15wt% ratio is weighed in casing respectively.Sample
After being put into device, evacuates, stop leakage in the roof, start to test, be warming up to 450 DEG C by program with the rate of 2 DEG C/min.
The Hydrogen desorption isotherms comparison of the composite material of different proportion doping as shown in Figure 2, doping ratio is different as the result is shown
The difference for causing catalytic effect is adulterating 1~5wt%TiH1.971In, it is improved along with doping ratio, initial hydrogen discharging temperature tool
It is significantly reduced, hydrogen discharging rate also improves, and improves dynamic performance.Adulterating 7~15wt%TiH1.971In, along with
The raising of ratio, the trend that initial hydrogen discharging temperature has been improved, but than pure MgH2Initial hydrogen discharging temperature significantly reduces.TiH1.971
Doping ratio optimize to obtain the MgH that performance is obviously improved2+ 5wt%-c-TiH1.971Compound system (c represents ball milling 60h).
Fig. 3 is MgH2/ 5wt%-c-TiH1.971Composite hydrogen storage material from room temperature to 450 DEG C at heating Hydrogen desorption isotherms, from
Fig. 3 is it is found that MgH2/ 5wt%-c-Ti composite hydrogen storage material can discharge the hydrogen of 6.7wt% to 300 DEG C in 175 DEG C of beginning hydrogen releases
Gas can significantly reduce hydrogen discharging temperature, improve hydrogen desorption kinetics performance.
5wt%-c-TiH is doped with to preparation1.971The MgH of (c represents ball milling 60h)2Material carry out XRD object phase table
Sign.This characterization is carried out with X-ray diffractometer.
XRD characterization result is as shown in figure 4, main object mutually remains as MgH in display material2, but widthization occurs for spectral peak, says
Bright MgH2Partial size scale has obtained biggish reduction；There is the presence of simple substance Mg simultaneously, illustrates the MgH produced2Hydrogen content do not reach
To perfect condition；In addition there is TiH1.971Spectral peak, however peak value be it is very small, illustrate TiH1.971With the presence of stabilized condition.
Test MgH2/ 5wt%-c-TiH1.971The heating hydrogen sucking function of composite material:
It takes 150~250mg of sample to be put into device in glove box, evacuates, stop leakage in the roof, start to test, by program with 1
DEG C/rate of min is warming up to 450 DEG C.Curve test is put followed by sky, a steel ball is taken to be put into device, evacuates, picks up
Leakage, starts to test, is warming up to 450 DEG C of by program with the rate of 1 DEG C/min.
Using the hydrogen sucking function of " constant volume-pressure differential method " measurement composite hydrogen storage material.Pure MgH is known from Fig. 52Start at 150 DEG C
Hydrogen is inhaled, 380 DEG C of hydrogen that can inhale 7.33wt% are warming up to, levels off to theoretical hydrogen desorption capacity；MgH2+ 5wt%-c-TiH1.971In room temperature
Under can inhale hydrogen, be warming up to 177 DEG C, the trend for inhaling hydrogen tends towards stability, pass through doping TiH1.971Suction hydrogen can be significantly reduced
Temperature improves hydrogen-absorption speed, improves and inhales hydrogen dynamic performance.
Test MgH2/ 5wt%-c-TiH1.971The constant temperature hydrogen discharging performance of composite material:
It takes 150~250mg of sample to be put into device in glove box, evacuates, stop leakage in the roof, start to test, into 32~33bar
Hydrogen, be warming up to 300 DEG C by program with the rate of 5 DEG C/min, keep the temperature 85min.Open vacuum pump, be deflated to 7bar with
Under, reactor is closed, it opens and evacuates 10s, 7s opens low biography, and 8s opens dilatation, and 9s, which is closed, to be evacuated, and 10s closes reactor, is then remembered
Record test.
Using the constant temperature hydrogen discharging performance of " constant volume-pressure differential method " measurement composite hydrogen storage material.As a result as shown in fig. 6, passing through
After 300 DEG C of constant temperature hydrogen release, in 10min, hydrogen desorption capacity has had reached 6.34wt%, and hydrogen release power performance significantly improves.
Catalyst TiH is doped with to preparation1.971MgH2Composite material material constant temperature hydrogen release carries out XRD object and mutually characterizes.
This characterization is carried out with X-ray diffractometer, as a result as shown in fig. 7,
After the constant temperature hydrogen release by 300 DEG C, main object is mutually Mg to XRD characterization in material as the result is shown, but spectral peak is sent out
Raw constriction, illustrates that Mg partial size scale is improved；There is MgH simultaneously2Presence, illustrate MgH2There is no complete hydrogen release to reach ideal
Hydrogen release；In addition there is TiH1.971Spectral peak, however peak value be it is very small, illustrate TiH1.971With the presence of stabilized condition.
Claims (9)
1. a kind of composite hydrogen storage material, which is characterized in that including TiH1.971And MgH2, wherein TiH1.971Account for the composite hydrogen-storage material
Expect 1wt%~15wt% of gross mass.
2. the preparation method of composite hydrogen storage material as described in claim 1, which comprises the following steps:
(1) by TiH1.971Powder is mixed with oleic acid, oleyl amine and heptane, with 10~60h of revolving speed continuous ball milling of 300~500rpm；
(2) sample clean after ball milling, after standing remove supernatant liquor, liquid line will be instilled after remaining solid carrying out washing treatment；
(3) by sample centrifugation, the dry, evacuation after washing, TiH can be obtained1.97Particle；
(4) TiH that will be obtained1.97Particle and MgH2After mixing in an inert atmosphere ball milling to get arrive composite hydrogen storage material.
3. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that in the step (1)
TiH1.971Volume ratio with oleic acid, oleyl amine and heptane is 1:0.33~1:10~1:20.
4. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that in the step (1)
TiH1.971Mass ratio with the steel ball for ball milling is 1:45~60.
5. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that used in the step (2)
Oleic acid, oleyl amine and mixed solvent in heptan are cleaned, wherein the volume ratio of oleic acid, oleyl amine and heptane is 1:0.33~1:10~1:
50。
6. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that sample in the step (2)
The time of standing is 10~30min, is washed using wine clear to the remaining solid, is 5~10 times with the number of ethanol wash.
7. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that centrifugation in the step (3)
Revolving speed is 8000~10000rpm, and the time is 6~10min.
8. the preparation method of composite hydrogen storage material according to claim 2, which is characterized in that inertia in the step (4)
Atmosphere finger pressure is high-purity argon gas atmosphere less than 0.1MPa, and the time of ball milling is 1~6h, ball mill revolution speed is 300~
500rpm。
9. composite hydrogen storage material as described in claim 1 is prepared according to the described in any item preparation methods of claim 2-8
Obtained composite hydrogen storage material is in the application as hydrogen storage material.
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| CN111533086A (en) * | 2020-05-11 | 2020-08-14 | 中国科学院长春应用化学研究所 | Short-process preparation method for rapidly activating hydrogen storage alloy by using hydrogen-containing compound |
Citations (1)
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| CN109467048A (en) * | 2018-12-27 | 2019-03-15 | 江苏科技大学 | Composite hydrogen storage material and its preparation method and application |
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| CN109467048A (en) * | 2018-12-27 | 2019-03-15 | 江苏科技大学 | Composite hydrogen storage material and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| JANGIR, MUKESH, ET AL.: "The enhanced de/re‐hydrogenation performance of MgH2 with TiH2 additive", 《INTERNATIONAL JOURNAL OF ENERGY RESEARCH》 * |
| LIU, TONG, ET AL.: "Enhanced hydrogen storage properties of magnesium by the synergic catalytic effect of TiH1.971 and TiH1.5 nanoparticles at room temperature", 《JOURNAL OF POWER SOURCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533086A (en) * | 2020-05-11 | 2020-08-14 | 中国科学院长春应用化学研究所 | Short-process preparation method for rapidly activating hydrogen storage alloy by using hydrogen-containing compound |
| CN111533086B (en) * | 2020-05-11 | 2023-12-01 | 中国科学院长春应用化学研究所 | Short-flow preparation method for rapidly activating hydrogen storage alloy by utilizing hydrogen-containing compound |
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Application publication date: 20191018 Assignee: Center for technology transfer Jiangsu University of Science and Technology Assignor: JIANGSU University OF SCIENCE AND TECHNOLOGY Contract record no.: X2021980006173 Denomination of invention: Composite hydrogen storage material, preparation method and application thereof Granted publication date: 20210406 License type: Common License Record date: 20210714 |
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