CN105776132B - An inexpensive and large-scale method for preparing nitrogen-based metal compound hydrogen storage materials - Google Patents
An inexpensive and large-scale method for preparing nitrogen-based metal compound hydrogen storage materials Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 83
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 83
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 78
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 33
- 239000011232 storage material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 21
- 150000002736 metal compounds Chemical class 0.000 title abstract 5
- 239000002184 metal Substances 0.000 claims abstract description 51
- 229910052751 metal Inorganic materials 0.000 claims abstract description 51
- 230000009615 deamination Effects 0.000 claims abstract description 22
- 238000006481 deamination reaction Methods 0.000 claims abstract description 22
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 47
- 229910021529 ammonia Inorganic materials 0.000 claims description 23
- 150000001728 carbonyl compounds Chemical class 0.000 claims description 21
- 239000011777 magnesium Substances 0.000 claims description 19
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 12
- 150000001875 compounds Chemical class 0.000 abstract description 10
- 229910052987 metal hydride Inorganic materials 0.000 abstract description 7
- 150000004681 metal hydrides Chemical class 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 abstract description 2
- 150000003624 transition metals Chemical class 0.000 abstract description 2
- 125000001841 imino group Chemical group [H]N=* 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910017464 nitrogen compound Inorganic materials 0.000 abstract 1
- 150000002830 nitrogen compounds Chemical class 0.000 abstract 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
- 238000004176 ammonification Methods 0.000 description 11
- 238000006356 dehydrogenation reaction Methods 0.000 description 6
- AFRJJFRNGGLMDW-UHFFFAOYSA-N lithium amide Chemical compound [Li+].[NH2-] AFRJJFRNGGLMDW-UHFFFAOYSA-N 0.000 description 6
- KOHUATWNGBDXMV-UHFFFAOYSA-N [Mg]N Chemical compound [Mg]N KOHUATWNGBDXMV-UHFFFAOYSA-N 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910006425 Li—N—H Inorganic materials 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- -1 alanate Chemical compound 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 125000002648 azanetriyl group Chemical group *N(*)* 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 229910010277 boron hydride Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- BKZIMGJXBVAXMP-UHFFFAOYSA-N azanide;gold(1+) Chemical compound [Au]N BKZIMGJXBVAXMP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Hydrogen, Water And Hydrids (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了一种大规模制备氮基金属化合物储氢材料的方法。以金属单质、金属氢化物或金属氮基化合物中的一种或二种以上混合为主体材料，以其它化合物为助剂，通过均匀混合、煅烧、脱氨、加氢获得氮基金属化合物储氢材料。所述的金属氮基化合物可以是金属氨基化合物、金属亚氨基化合物或金属氮化合物中的一种或二种以上混合。所述金属单质为1‑3族主族金属或是前过渡金属。用此法可以安全、廉价、大规模制备氮基金属化合物储氢材料，使氮基金属化合物储氢材料的制备成本大幅度降低。廉价的储氢材料对储氢体系民用化和实用化具有极其重要的指导价值。The invention discloses a method for large-scale preparation of nitrogen-based metal compound hydrogen storage materials. Using one or more of metal element, metal hydride or metal nitrogen-based compound as the main material, and other compounds as auxiliary agents, nitrogen-based metal compounds are obtained by uniform mixing, calcination, deamination, and hydrogenation. Hydrogen storage Material. The metal nitrogen-based compound may be one or a mixture of two or more metal amino compounds, metal imino compounds or metal nitrogen compounds. The metal element is a main group metal of Group 1-3 or a pre-transition metal. Using this method, the nitrogen-based metal compound hydrogen storage material can be prepared safely, cheaply and on a large scale, and the preparation cost of the nitrogen-based metal compound hydrogen storage material can be greatly reduced. Inexpensive hydrogen storage materials have extremely important guiding value for the civilianization and practical application of hydrogen storage systems.
Description
Technical field
The present invention relates to one kind inexpensively to prepare the method for nitrogen metal carbonyl compound hydrogen storage material in hydrogen storage technology field
Using especially safe cheap large scale preparation nitrogen metal carbonyl compound hydrogen storage material.
Background technique
With serious in the increasingly depleted and use process at them of the carbon such as coal, petroleum, natural gas energy and material
Environmental pollution.Energy depletion and the big problem of environmental pollution amount this just force people to go to develop the green energy of new sustainable development
Source, such as wind energy, solar energy, biological energy source, Hydrogen Energy.Wherein Hydrogen Energy is because of its rich reserves, mass energy density height (142MJkg-1)、
The green and pollution-free and favor by people of by-product (water).Therefore greatly develop hydrogen energy source facilitate alleviate it is increasingly urgent
The energy, environment and social concern --- including mitigating environmental pollution, alleviate global warming, mitigate because the local energy is uneven
Caused by war etc..Restricting the applicable main bottleneck of hydrogen at present is hydric safe, efficient, cheap storage.Existing storage
Hydrogen mode mainly includes high-pressure hydrogen storing, liquid hydrogen storage, solid-state hydrogen storage.Wherein solid-state hydrogen storage is by chemical reaction or physical absorption
Mode by hydrogen storage in solid-state material, energy density is high and safety is good, it is considered to be most promising one
Kind hydrogen storage mode.The lightweight high capacity solid hydrogen storage material being made of light element, such as boron hydride, alanate, nitrogen base chemical combination
Object etc., theoretical hydrogen storage capability are above 5wt%, this brings hope for solid-state hydrogen storage material.Wherein nitrilo compound hydrogen storage material
Material very likely becomes the hydrogen storage material of practical application of new generation since its hydrogen storage content is big and inhales the factors such as hydrogen release mild condition
Material.Such as Mg (NH2)2- 2LiH system, gravimetric hydrogen storage density 5.6wt%；Its enthalpy~40kJ (molH2)-1According to model Hough
Temperature needed for it discharges 1 atmospheric equilibrium hydrogen pressure known to equation calculation is about 90 DEG C, this and Proton Exchange Membrane Fuel Cells
(PEMFC) operating temperature is coincide very much；Mg (NH simultaneously2)2- 2LiH system good cycling stability, stable operation in dry air,
So being considered as a kind of hydrogen storage material of most vehicular applications prospect.Nitrogen is generally involved during nitrilo compound hydrogen storage
Metal carbonyl compound and metal hydride, and mechanism study thinks the metal N-H key (H in nitrogen metal carbonyl compoundδ+)With gold
Belong to the metal-H key (H in hydrideδ-) between strong interaction be nitrogen metal carbonyl compound system release hydrogen driving force.
So generally requiring to exist simultaneously H in nitrogen metal carbonyl compound system certain embodimentsδ+And Hδ-The H of two kinds of different electronegativity.Mesh
Before, metal hydride species in the market are more various, usually obtained by the hydrogenation of metal simple-substance high-temperature fusion；But nitrogen fund
The ammonobase classes of compounds belonged in compound is relatively deficient, and common synthetic method has the direct ammonification of metal, gold
Belong to hydride ammonification or metal nitride adds the diversified forms such as hydrogen, its general process is complicated and is difficult to form pure amino gold
Belong to compound so ammonobase compound is expensive.If metal hydride lithium LiH (Sigma) price of hydrogen storage rank is~83
Block/gram；The metal amino lithium LiNH of hydrogen storage rank2(Sigma) price is in~80 pieces/gram；In addition some amino-compound cities are gone back
It can not be directly obtained on, such as amino magnesium (Mg (NH2)2, according to the laboratory synthesis price of reckoning amino magnesium in~150 pieces/gram.One
As light vehicle-mounted hydrogen storage system to require its reversible hydrogen storage capacity be 5Kg, with the most hydrogen storage material of vehicular applications prospect at present: Mg
(NH2)2For -2LiH system (5.6wt%), then want the~Mg (NH of 90Kg2)2- 2LiH sample.Mg is prepared with current laboratory
(NH2)2It is calculated with the price (Sigma) of commercialization purchase LiH, then only the price of hydrogen storage material is as high as 1,200,000 RMB,
So being difficult to functionization or being difficult to the common peopleization.Therefore this patent proposes a kind of cheap large scale preparation nitrogen based metallization of safety
The method for closing object hydrogen storage material.
Summary of the invention
The present invention makes every effort to provide a kind of easy to operate, highly-safe, low in cost, large scale preparation nitrogen metal carbonyl compound
The method of hydrogen storage material.Particular content is inexpensively prepared on a large scale using multi-steps such as uniform mixing, calcining, deamination plus hydrogen
Nitrogen metal carbonyl compound hydrogen storage material, to promote the functionization of nitrogen metal carbonyl compound hydrogen storage material.It can also prepare
Auxiliary agent is added during a certain step or a few steps in journey to improve the hydrogen storage property of nitrogen metal carbonyl compound hydrogen storage material.
Metal (M) above-mentioned is 1-3 race main group metal or early transition metal.It forms corresponding general formula after nitride
Are as follows: MNxHy (0 < x≤10,0 < y≤20).
Whole or a certain ingredients or a certain ingredient in aforesaid builders are formed in mixing, calcining, deamination, the hydrogenation process
Substance, and these substances can act on nitrogen metal carbonyl compound hydrogen storage material and form noval chemical compound or solid solution.Mainly help
Agent has: metal simple-substance, metal hydride, metal oxide, metal hydroxides, metal nitride, metal halide, metal boron
Hydride, metal boron hydronitrogen etc..
Laboratory preparation manipulation process of the invention: metal or metal hydride owner are weighed in the glove box of inert atmosphere
Body material or its auxiliary agent, are encased in special ball grinder that (ball grinder is salable, pressure-resistant ball grinder, is equipped on cover and tank
The valve of interior connection, for gas to be passed through or be discharged into tank) sealing, then poured into tank body ammonia liquefied ammonia or its
Its gas such as hydrogen, argon gas, carbon dioxide etc..It is installed on planetary ball mill and starts ball milling, the revolving speed of ball mill is set as
50~400rpm, the pellet mass ratio of ball milling are as follows: 0.1~20.Sample after ball milling is complete is transferred to after taking out in glove box
It is calcined under ammonia atmosphere in the voltage-resistant reactor of sealing, calcination temperature is different according to the difference of used metal, temperature
100~600 DEG C of degree.Calcined sample is placed in vacuum or low ammonia divides lower deamination, and the sample after deamination is in hydrogen or hydrogen
Add hydrogen under gas mixed atmosphere, to obtain nitrogen metal carbonyl compound hydrogen storage material.
The present invention has the following advantages:
1. using this method by simple ball milling, calcining, deamination and hydrogen can be added from cheap metal simple-substance
The cheap large scale preparation nitrogen metal carbonyl compound hydrogen storage material of safety.
2. can directly prepare pure nitrogen metal carbonyl compound hydrogen storage material using this method can also prepare admixed with additives
Nitrogen metal carbonyl compound hydrogen storage material.
3. preparing nitrogen metal carbonyl compound without directly contacting poisonous and harmful dust or gas, whole process using this method
Safe operation is strong.
The method and process proposed by the present invention for preparing nitrogen metal carbonyl compound hydrogen storage material is simple, securely and reliably, can be very big
Cost is reduced, can be prepared on a large scale hydrogen storage material.The hydrogen storage material of inexpensive safety has the practical application of Hydrogen Energy of crucial importance
Value and significance.
Detailed description of the invention
Li-N-H (the LiNH of Fig. 1 this law preparation2- LiH) system adds the dehydrogenation after hydrogen to inhale hydrogen curve graph.
Li-Mg-N-H (Mg (the NH of Fig. 2 this law preparation2)2- 2LiH) system adds the dehydrogenation after hydrogen to inhale hydrogen curve graph.
Specific embodiment
Present invention material based on metal simple-substance or metal hydride, while auxiliary agent can be added into material of main part,
By be uniformly mixed, calcining, deamination, plus hydrogen and etc. rear acquisitions nitrogen metal carbonyl compound hydrogen storage material, thus on a large scale inexpensively
Safety prepares nitrogen metal carbonyl compound hydrogen storage material.The present invention is described in detail below by way of specific embodiment, is needed
It is pointed out that the invention is not limited to these following embodiments, is also not limited to laboratory operation.
Embodiment 1: preparation Li-N-H (LiNH2- LiH) system
(1) a certain amount of lithium metal such as 70g is weighed in glove box, is then added in ball grinder, is subsequently injected into 10-
120atm ammonia or liquefied ammonia.
(2) by after step (1) described addition lithium metal and ammonia, ball grinder is placed in 100 on planetary ball mill~
200rpm mixing 1-20h, while part metals lithium is reacted with ammonia and generates lithium amide.
(3) the sample taking-up that step (2) mixes is placed on ammonification in voltage-resistant reactor, ammonification temperature is 50~350
Between DEG C；Time 1-50h；(> 50h) step (2) can also be repeated until all lithium metals are changed into lithium amide for a long time.
(4) it is surveyed as lithium amide sample obtained after step (3) ammonification carries out temperature programming (fixed heating rate) deamination
Examination (TPD-MS) determines its deamination temperature, and selects (200~500 DEG C) progress deaminations of suitable temperature.
(5) as the sample after step (4) deamination carries out hydroprocessing；Hydrogenation pressure > 2atm；Hydrogenation temperature > 150 DEG C.
(6) the dehydrogenation suction hydrogen result such as Li-N-H system behind step (5) plus hydrogen is as shown in Figure 1.
Embodiment 2: preparation Li-Mg-N-H (Mg (NH2)2- nLiH) system
(1) lithium metal (such as Mg (NH of a certain amount of magnesium metal and corresponding amount is weighed in glove box2)2- 2LiH system is then
The molar ratio of Mg and Li is 1:2, such as in total 38g), it is then added in ball grinder, is subsequently injected into ammonia (> 5atm) or liquefied ammonia.
(2) by after step (1) described addition magnesium metal, lithium metal and ammonia, ball grinder is placed on planetary ball mill
50~200rpm is mixed for more than 1h until uniform, while reacts part metals lithium or magnesium with ammonia and generating lithium amide or amino
Magnesium.
(3) the sample taking-up that step (2) mixes is placed on ammonification in voltage-resistant reactor, ammonification temperature is 150~400
Between DEG C；
(4) its deamination is determined as sample obtained after step (3) ammonification carries out the test of temperature programming deamination (TPD-MS)
Temperature, and suitable temperature is selected to carry out deamination (150~500 DEG C).
(5) as the sample after step (4) deamination carries out hydroprocessing, hydrogenation pressure > 10atm；Hydrogenation temperature > 120 DEG C add
Suction dehydrogenation cycle is carried out after hydrogen is full finally can be obtained Mg (NH2)2- nLiH system.
(6) such as Li-Mg-N-H (Mg (NH behind step (5) plus hydrogen2)2- 2LiH) system dehydrogenation inhale hydrogen result it is as shown in Figure 2.
Embodiment 3: the Li-Mg-N-H (Mg (NH of KH modification is prepared2)2- nLiH-yKH) system
(1) lithium metal and metallic potassium (such as Mg (NH of a certain amount of magnesium metal and corresponding amount are weighed in glove box2)2-
The molar ratio of 1.9LiH-0.1KH system then Mg and Li and K is that such as total weight 41.2g) ball grinder is then added in 1:1.9:0.1
In, it is subsequently injected into ammonia (> 2atm) or liquefied ammonia.
(2) by after step (1) described addition magnesium metal, lithium metal, metallic potassium and ammonia, ball grinder is placed in planetary ball
50~200rpm mixing > 1h on grinding machine until being uniformly mixed, while making part metals lithium, metallic potassium or magnesium react life with ammonia
At lithium amide, potassamide or amino magnesium.
(3) the sample taking-up that step (2) mixes is placed on ammonification in voltage-resistant reactor, ammonification temperature is 150~400
Between DEG C；
(4) its deamination is determined as sample obtained after step (3) ammonification carries out the test of temperature programming deamination (TPD-MS)
Temperature, and suitable temperature is selected to carry out deamination (60~500 DEG C).
(5) as the sample after step (4) deamination carries out hydroprocessing, hydrogenation pressure > 5atm；Hydrogenation temperature > 80 DEG C add hydrogen
Saturation can be obtained Mg (NH after carrying out suction dehydrogenation cycle2)2- nLiH-yKH system.
Claims (5)
1. a kind of method for preparing nitrogen metal carbonyl compound hydrogen storage material, it is characterised in that:
One kind material based on metal simple-substance lithium and/or magnesium by uniformly mixing, calcining in ammonia atmosphere, deamination, adds hydrogen
Nitrogen metal carbonyl compound hydrogen storage material is obtained afterwards.
2. the method as described in claim 1, it is characterised in that: mixed uniformly mode are as follows: mechanical ball mill, mechanical stirring, powder
Pure or grinding；When with planetary ball mill, rotational speed of ball-mill is 50 ~ 400 rpm, and the pellet mass ratio of ball milling is 0.1 ~ 20.
3. the method as described in claim 1, it is characterised in that: gas pressure is 0.5 ~ 120 atm, calcination temperature 50 when calcining
~ 600 °C, 0.5 ~ 300h of calcination time；Calcination atmosphere is then the mixed gas atmosphere of ammonia atmosphere either ammonia；Work as ammonia
When atmosphere is mixed gas, mixed gas is NH3: X mixing forms, wherein X=H2、N2, He, Ne, Ar, Ke, one of Xe or
Two kinds or more, the molar ratio that wherein ammonia accounts for is 10% ~ 100%；The molar ratio of total ammonia amount and metal is 0.1 ~ 80.
4. the method as described in claim 1, it is characterised in that: 100 ~ 500 °C of deamination temperature, 0.5 ~ 100h of deamination time.
5. the method as described in claim 1, it is characterised in that: its hydrogen is pure hydrogen either hydrogen and ammonia, nitrogen in hydrogenation process
Or one or two or more kinds of mixed gas in argon, the volumetric concentration of other gases in mixed gas in addition to hydrogen are
99% or less；Add hydrogen hydrogen press 5 ~ 700 atm, 80 ~ 300 °C of hydrogenation temperature, 0.02 ~ 10 h of hydrogenation time.
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| CN111252733A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Preparation method of multi-element metal hydride |
| CN112978679B (en) * | 2019-12-12 | 2022-11-22 | 中国科学院大连化学物理研究所 | Preparation method of multi-metal hydrogen-containing compound |
| CN112062110A (en) * | 2020-08-14 | 2020-12-11 | 浙江工业大学 | A kind of synthetic method of binary metal amide |
| CN112110426B (en) * | 2020-08-20 | 2022-06-03 | 浙江工业大学 | Method for synthesizing amino lithium potassium by mechanical ball milling |
| CN112079331B (en) * | 2020-08-20 | 2022-06-03 | 浙江工业大学 | Synthesis method of metal-nitrogen-hydrogen system hydrogen storage material |
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