CN106145031A - A kind of LiNH improving hydrogen storage property2the preparation method of LiH hydrogen storage material - Google Patents
A kind of LiNH improving hydrogen storage property2the preparation method of LiH hydrogen storage material Download PDFInfo
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- CN106145031A CN106145031A CN201610522104.8A CN201610522104A CN106145031A CN 106145031 A CN106145031 A CN 106145031A CN 201610522104 A CN201610522104 A CN 201610522104A CN 106145031 A CN106145031 A CN 106145031A
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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
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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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
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Abstract
A kind of LiNH improving hydrogen storage property2The preparation method of LiH hydrogen storage material, belongs to solid state chemistry hydrogen storage technology field, by the LiNH of doping RbF2Carry out ball-milling treatment under an atmosphere of hydrogen with the mixture of LiH, obtain LiNH2LiH hydrogen storage material.The RbF that the present invention adds is substantially improved LiNH as catalyst2The method of the hydrogen desorption performance of LiH system, has obtained relatively low putting hydrogen peak temperature and put hydrogen initial temperature, makes hydrogen storage material hydrogen discharging temperature in advance, accelerates hydrogen discharging rate.
Description
Technical field
The invention belongs to solid state chemistry hydrogen storage technology field, particularly to LiNH2The height that-LiH system hydrogen storage property improves
The exploration of effect catalyst.
Background technology
In sustainable development and friendly environment society, find one cleaning and the high-octane energy is even more important.Because of hydrogen
The most only produce water, so becoming the most attracting no pollution energy.Although the hydrogen reserves as lightweight element
Abundant and there is high-energy-density, but extensively the utilizing and limited by hydrogen storage mode of Hydrogen Energy.Two kinds of traditional hydrogen storage
Mode, also because having relatively low bulk density, is difficulty with the actual application of vehicle-mounted hydrogen storage.And the appearance of solid-state hydrogen storage technology, change
It is apt to current situation.Especially for lightweight element hydrogen storage system, it is achieved that the solid-state of high weight and high volume density is stored up safely
Hydrogen.
There are metal hydrogen storage, carbonaceous material hydrogen storage method etc. for solid-state hydrogen storage, but experiment proof can not meet well
The needs of the vehicle-mounted hydrogen storage of business.Therefore, people start to turn to research some light-weight metal, such as alkali metal lithium, sodium or potassium
Compound.Since Chen Ping in 2002 et al. has delivered the nitride of lithium metal on Nature first can be relative with amides
About 320 ° C of relatively low temperature reversibly inhale to be put hydrogen capacity and reaches 11.5wt%, Metal-N-H system hydrogen storage material and obtained greatly
Development.Relative to other solid hydrogen storage materials, the amides of light metal particularly lithium and magnesium is put with suction greatly at hydrogen storage capability
The low these two aspects of hydrogen temperature has advantage, is to be hopeful most to reach the target that International Energy Agency proposes, thus meets hydrogen fuel
The application requirement of battery car.In the lithium of lightweight, boron, nitrogen, magnesium, Li3N owing to having the highest hydrogen storage content (10.4wt%) and
Receive much attention.LiNH2Can be 200～300 DEG C of reversible hydrogen adsorption and desorptions (-6wt%) after-LiH mixing.Therefore, LiNH2-LiH system
By vast researcher as the primary study development object of hydrogen storage material.
In order to improve LiNH2Suction/the hydrogen discharging performance of-LiH system, TiCl is added in existing people's research in this Li-N-H system3
And relevant potassium compound such as KH, KX(wherein X are F, Cl or Br) etc., find to add the suction for improving Li-N-H system/put
Hydrogen dynamic performance has preferable catalytic effect, can greatly improve LiNH2The dynamic performance of hydrogen is put in the suction of-LiH system.
Summary of the invention
Present invention aim at proposing a kind of LiNH that can be effectively improved hydrogen storage property2The preparation side of-LiH hydrogen storage material
Method.
The technical scheme is that the LiNH of doping RbF2Ball milling is carried out under an atmosphere of hydrogen with the mixture of LiH
Process, obtain LiNH2-LiH hydrogen storage material.
The RbF that the present invention adds is substantially improved LiNH as catalyst2The method of the hydrogen desorption performance of-LiH system,
Put hydrogen peak temperature to relatively low and put hydrogen initial temperature, make hydrogen storage material hydrogen discharging temperature in advance, accelerate hydrogen discharging rate.
In a hydrogen atmosphere, ball-milling treatment has obtained the size doped crystal granule up to Nano grade to the present invention so that
The RbF of doping can preferably be distributed to LiNH2With LiH sample, make reaction complete with adding, thus accelerate hydrogen discharge reaction
Carry out, LiNH can be significantly improved2The dehydrogenation kinetics of-LiH system.
Further, the doping of RbF of the present invention accounts for 1～10 mol% of described mixture.Different dopings
RbF can reduce LiNH to varying degrees2-LiH system desorption temperature, improves dehydrogenation rate, but can reduce LiNH accordingly2-
The hydrogen storage content of LiH system.Improving LiNH2-LiH system hydrogen storage property and on the basis of ensureing its hydrogen storage ability, selects RbF's
Doping, in the range of 1～10 mol%, experiments prove that different RbF doping is to LiNH2-LiH system dehydrogenation
Impact finds, the LiNH when RbF doping reaches 1 mol%2-LiH system dehydrogenation peak temperature is 256 DEG C, with undoped than fall
Low 24 DEG C；The LiNH when RbF doping reaches 5 mol%2-LiH system dehydrogenation peak temperature is 211 DEG C, with undoped than reducing
69℃；The LiNH when RbF doping reaches 10 mol%2-LiH system dehydrogenation peak temperature is 200 DEG C, with undoped than reducing
80℃.Considering hydrogen discharging temperature and hydrogen storage ability, 5 mol%RbF that adulterate are optimum, it is thus achieved that minimum puts hydrogen peak value
Temperature, minimum dehydrogenation initial temperature: 120 DEG C, with undoped than reducing by 70 DEG C.Meanwhile, the releasing to ammonia also has suppression
Effect.
It is highly preferred that the doping of described RbF accounts for 5 mol% of described mixture.Condition at doping 5 mol% RbF
Under, obtain relatively low hydrogen desorption temperature and hydrogen desorption speed, meanwhile, having of a relatively high hydrogen storage content is 3.6wt%.
Described LiNH2It is 1: 1 with the mixing quality ratio of LiH.Chen Ping et al. proposes Li in 2002 on " Nature " first3N
Can reversibly store the hydrogen of 10wt%, hereafter Li-N-H system hydrogen storage material receives significant attention: Li3N+2H2↔Li2NH+
LiH+H2↔LiNH2+2LiH.And Li2NH+H2↔LiNH2+ LiH reaction system is due to its of a relatively high hydrogen storage content (6.5wt%)
And relatively low reaction activity becomes one of hydrogen storage material of hot topic.Therefore, the LiNH of 1:1 is selected2Come with the mixture of LiH
Research LiNH2The hydrogen storage property of-LiH system.
In order to suppress LiNH2During ball milling, generation Li is reacted with LiH2NH and H2, select at higher hydrogen
0.6MPa) carry out ball milling pretreatment under power.
Accompanying drawing explanation
Fig. 1 is LiNH2X-ray diffractogram after the ball milling of-LiH doping different proportion RbF.
Fig. 2 is LiNH2The thermal desorption mass spectrum of sample after-LiH doping different proportion RbF ball milling.
Fig. 3 is LiNH2-LiH non-impurity-doped, adulterate 5 mol% RbF samples Hydrogen desorption isotherms at 200 DEG C.
Fig. 4 is LiNH2-LiH non-impurity-doped, adulterate 5 mol% RbF samples Hydrogen desorption isotherms at 300 DEG C.
Detailed description of the invention
One, embodiment 1:
1, ball milling LiNH2-LiH biased sample: in argon glove box, weighs 0.3g by LiNH2With LiH crystal with 1: 1 mass
Load in the ball grinder containing 20 rustless steel steel balls than the sample of mixing composition.Then from glove box, take out ball grinder, fill
Enter 0.6MPa hydrogen, and ball grinder is symmetrically arranged in planetary ball mill, ball-milling treatment 2 under the rotating speed of 450 revs/min
Hour.
2, after ball milling, sample carries out hydrogen desorption test: in argon glove box, reclaims LiNH after ball milling2Mix with LiH
Sample, takes LiNH after 13mg ball milling2Carrying out hydrogen desorption test with LiH biased sample by caloic combined instrument, gas signal is examined
Survey as H2And NH3, condition is argon gas atmosphere, 50～600 DEG C, and heating rate is 5k/min.Non-impurity-doped LiNH can be obtained2-LiH
The hydrogen of putting of system initiates and peak temperature.
3, after ball milling, sample carries out hydrogen desorption kinetics test: in argon glove box, after taking 150mg ball milling respectively
LiNH2At 200 DEG C and 300 DEG C, isothermal hydrogen desorption experiment is carried out by PCT with LiH biased sample.Non-impurity-doped can be obtained
LiNH2-LiH system hydrogen discharging rate at 200 DEG C and 300 DEG C and hydrogen desorption capacity.
Two, embodiment 2:
1, with 1: 1 mass ratio by LiNH2First mix with LiH, then the 1mol% RbF that adulterates, obtain the LiNH of doping RbF2With
LiH mixed crystal.
The LiNH of doping RbF2With LiH mixed crystal: in argon glove box, weigh the LiNH of 0.3g doping RbF2With
LiH mixed crystal loads in the ball grinder containing 20 rustless steel steel balls.Then from glove box, take out ball grinder, be filled with
0.6MPa hydrogen, and ball grinder is symmetrically arranged in planetary ball mill, under the rotating speed of 450 revs/min, ball-milling treatment 2 is little
Time.
2, after ball milling, sample carries out hydrogen desorption test: in argon glove box, and adulterate after reclaiming ball milling 1 mol% RbF
LiNH2And LiH(1:1) biased sample, the LiNH of the 1 mol% RbF that adulterates after taking 13mg ball milling2With LiH biased sample by heat
Matter combined instrument carries out hydrogen desorption test, and gas signal is detected as H2And NH3, condition is argon gas atmosphere, 50-600 DEG C, and heat up speed
Rate is 5k/min.Can be obtained adulterating the LiNH of 1 mol% RbF2The hydrogen of putting of-LiH system initiates and peak temperature.
3, after ball milling, sample carries out hydrogen desorption kinetics test: in argon glove box, mixes after taking 150mg ball milling respectively
The LiNH of miscellaneous 1 mol% RbF2At 200 DEG C and 300 DEG C, isothermal hydrogen desorption experiment is carried out by PCT with LiH biased sample.
Can be obtained adulterating the LiNH of 1 mol% RbF2-LiH system hydrogen discharging rate at 200 DEG C and 300 DEG C and hydrogen desorption capacity.
Three, embodiment 3:
1, with 1: 1 mass ratio by LiNH2First mix with LiH, then the 5mol% RbF that adulterates, obtain the LiNH of doping RbF2With
LiH mixed crystal.
The LiNH of doping RbF2With LiH mixed crystal: in argon glove box, weigh the LiNH of 0.3g doping RbF2With
LiH mixed crystal loads in the ball grinder containing 20 rustless steel steel balls.Then from glove box, take out ball grinder, be filled with
0.6MPa hydrogen, and ball grinder is symmetrically arranged in planetary ball mill, under the rotating speed of 450 revs/min, ball-milling treatment 2 is little
Time.
2, after ball milling, sample carries out hydrogen desorption test: in argon glove box, and adulterate after reclaiming ball milling 5 mol% RbF
LiNH2With LiH biased sample, the LiNH of the 5 mol% RbF that adulterate after taking 13mg ball milling2Joined by caloic with LiH biased sample
Carrying out hydrogen desorption test with instrument, gas signal is detected as H2And NH3, condition is argon gas atmosphere, 50～600 DEG C, and heating rate is
5k/min.Can be obtained adulterating the LiNH of 5 mol% RbF2The hydrogen of putting of-LiH system initiates and peak temperature.
3, after ball milling, sample carries out hydrogen desorption kinetics test: in argon glove box, mixes after taking 150mg ball milling respectively
The LiNH of miscellaneous 5 mol% RbF2At 200 DEG C and 300 DEG C, isothermal hydrogen desorption experiment is carried out by PCT with LiH biased sample.
Can be obtained adulterating the LiNH of 5 mol% RbF2-LiH system hydrogen discharging rate at 200 DEG C and 300 DEG C and hydrogen desorption capacity.
Four, embodiment 4:
1, with 1: 1 mass ratio by LiNH2First mix with LiH, then the 10mol% RbF that adulterates, obtain the LiNH of doping RbF2With
LiH mixed crystal.
The LiNH of doping RbF2With LiH mixed crystal: in argon glove box, weigh the LiNH of 0.3g doping RbF2With
LiH mixed crystal loads in the ball grinder containing 20 rustless steel steel balls.Then from glove box, take out ball grinder, be filled with
0.6MPa hydrogen, and ball grinder is symmetrically arranged in planetary ball mill, under the rotating speed of 450 revs/min, ball-milling treatment 2 is little
Time.
2, after ball milling, sample carries out hydrogen desorption test: in argon glove box, and adulterate after reclaiming ball milling 10 mol% RbF
LiNH2With LiH biased sample, the LiNH of the 10 mol% RbF that adulterate after taking 13mg ball milling2Joined by caloic with LiH biased sample
Carrying out hydrogen desorption test with instrument, gas signal is detected as H2And NH3, condition is argon gas atmosphere, 50～600 DEG C, and heating rate is
5k/min.Can be obtained adulterating the LiNH of 10 mol% RbF2The hydrogen of putting of-LiH system initiates and peak temperature.
3, after ball milling, sample carries out hydrogen desorption kinetics test: in argon glove box, mixes after taking 150mg ball milling respectively
The LiNH of miscellaneous 10 mol% RbF2At 200 DEG C and 300 DEG C, isothermal hydrogen desorption experiment is carried out by PCT with LiH biased sample.
Can be obtained adulterating the LiNH of 10 mol% RbF2-LiH system hydrogen discharging rate at 200 DEG C and 300 DEG C and hydrogen desorption capacity.
Five, test result analysis:
Fig. 1 is LiNH2XRD comparison diagram after the ball milling of-LiH doping different proportion RbF, marks by contrasting the XRD of several materials
Quasi-card, finds that the characteristic peak of the RbF in doped samples is more and more obvious along with RbF adds the increase of percentage ratio.Meanwhile, make
With Debye-Scherrer formula analysis through the sample particle size of ball milling pretreatment up to Nano grade so that RbF, LiNH2、
Being more uniformly distributed of LiH mixing.
Fig. 2 is LiNH2The thermal desorption mass spectrum of sample after-LiH doping different proportion RbF ball milling, when RbF doping reaches 5
LiNH during mol%2-LiH system dehydrogenation peak temperature is 211 DEG C, and with undoped than reducing by 69 DEG C, dehydrogenation initial temperature is 120
DEG C, reduce by 70 DEG C.
Fig. 3 and Fig. 4 is LiNH2-LiH non-impurity-doped, adulterate 5 mol% RbF samples at 200 DEG C and 300 DEG C to put hydrogen bent
Line, when relatively lower temp 200 DEG C, adulterates 5 mol% RbF sample hydrogen discharging rates and hydrogen desorption capacity is substantially better than non-impurity-doped sample
Product.Time at 300 DEG C, the 5 mol% RbF sample hydrogen desorption capacities that adulterate reach 3.6wt%, but less than non-impurity-doped sample hydrogen desorption capacity, explanation
Doping RbF can reduce LiNH to a certain extent2The hydrogen storage content of-LiH system.
Comprehensive hydrogen desorption temperature, speed and hydrogen storage content consider, the 5 mol% RbF samples that adulterate are optimum, can significantly improve
LiNH2The hydrogen desorption performance of-LiH system, compared with other outstanding catalyst of at present report, we obtain minimum puts hydrogen
Peak temperature and put hydrogen initial temperature, is more nearly the hydrogen storage standard that International Energy Agency in 2015 is formulated, distance solid-state hydrogen storage
Business is applied closer to a step.
Claims (5)
1. the LiNH improving hydrogen storage property2The preparation method of-LiH hydrogen storage material, it is characterised in that: by doping RbF's
LiNH2Carry out ball-milling treatment under an atmosphere of hydrogen with the mixture of LiH, obtain LiNH2-LiH hydrogen storage material.
Method the most according to claim 1, it is characterised in that the doping of described RbF accounts for the 1～10 of described mixture
mol%。
Method the most according to claim 2, it is characterised in that the doping of described RbF accounts for 5 mol% of described mixture.
4. according to method described in claim 1 or 2 or 3, it is characterised in that described LiNH2It is 1: 1 with the mixing quality ratio of LiH.
Method the most according to claim 1, it is characterised in that described atmosphere of hydrogen condition is 0.6MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107161946A (en) * | 2017-05-16 | 2017-09-15 | 上海大学 | Li N H system hydrogen storage materials and preparation method thereof |
| CN107188121A (en) * | 2017-06-16 | 2017-09-22 | 扬州大学 | A kind of improved LiNH2LiH composite hydrogen storage materials and the method for improving hydrogen storage property |
| CN107253697A (en) * | 2017-06-16 | 2017-10-17 | 扬州大学 | A kind of multi-walled carbon nanotube that adulterates improves the Li of hydrogen storage property3N hydrogen storage materials and preparation method thereof |
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| CN1876561A (en) * | 2005-06-10 | 2006-12-13 | 中国科学院金属研究所 | Li-Mg-N-H hydrogen storage material and process for preparing same |
| 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 |
| CN104925751A (en) * | 2015-06-18 | 2015-09-23 | 扬州大学 | Preparing method for improving LiH-NH<3> hydrogen storing system dehydrogenizing kinetics |
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| CN1876561A (en) * | 2005-06-10 | 2006-12-13 | 中国科学院金属研究所 | Li-Mg-N-H hydrogen storage material and process for preparing same |
| 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 |
| CN104925751A (en) * | 2015-06-18 | 2015-09-23 | 扬州大学 | Preparing method for improving LiH-NH<3> hydrogen storing system dehydrogenizing kinetics |
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| CHAO LI等: "Improved Hydrogen-Storage Thermodynamics and Kinetics for an RbF-Doped Mg(NH2)2–2LiH System", 《CHEM. ASIAN J》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107161946A (en) * | 2017-05-16 | 2017-09-15 | 上海大学 | Li N H system hydrogen storage materials and preparation method thereof |
| CN107188121A (en) * | 2017-06-16 | 2017-09-22 | 扬州大学 | A kind of improved LiNH2LiH composite hydrogen storage materials and the method for improving hydrogen storage property |
| CN107253697A (en) * | 2017-06-16 | 2017-10-17 | 扬州大学 | A kind of multi-walled carbon nanotube that adulterates improves the Li of hydrogen storage property3N hydrogen storage materials and preparation method thereof |
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Application publication date: 20161123 |