CN105776132A - Method for cheaply and extensively preparing nitrogen-based metal compound hydrogen storage material - Google Patents
Method for cheaply and extensively preparing nitrogen-based metal compound hydrogen storage material Download PDFInfo
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- CN105776132A CN105776132A CN201410784903.3A CN201410784903A CN105776132A CN 105776132 A CN105776132 A CN 105776132A CN 201410784903 A CN201410784903 A CN 201410784903A CN 105776132 A CN105776132 A CN 105776132A
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Abstract
The invention discloses a method for extensively preparing a nitrogen-based metal compound hydrogen storage material. The nitrogen-based metal compound hydrogen storage material is obtained through uniform mixing, calcining, deamination and hydrogenation with one or two or more of a metallic element, a metal hydride and a metal nitrogen-based compound as a host material and other compounds as an assistant. The metal nitrogen-based compounds can be one or two or more of a metal amino compound, a metal imino compound and a metal nitrogen compound. The metal element can be a group I-III metal or an early transition metal. The nitrogen-based metal compound hydrogen storage material can be safety, cheaply and extensively prepared through the method, so the preparation cost of the nitrogen-based metal compound hydrogen storage material is greatly reduced. The cheap hydrogen storage material provides extremely important guidance for civilianization and practicalization of hydrogen storage systems.
Description
Technical field
The present invention relates to the application in hydrogen storage technology field of a kind of method inexpensively preparing nitrilo metallic compound hydrogen storage material, especially safety inexpensively prepares nitrilo metallic compound hydrogen storage material on a large scale.
Background technology
The environmental pollution that the carbon energy and materials such as coal, oil, natural gas are day by day exhausted and adjoint serious in their use procedure.Energy depletion and the big problem of environmental pollution amount this just force the green energy resource of sustainable development that people go exploitation new, such as wind energy, solar energy, bioenergy, Hydrogen Energy etc..Wherein Hydrogen Energy is because of its rich reserves, the high (142MJkg of mass energy density-1), by-product (water) environmental protection is pollution-free and enjoys the favor of people.Therefore greatly develop hydrogen energy source and contribute to alleviating the day by day urgent energy, environment and social problem including alleviating environmental pollution, alleviate global warming, alleviating the war etc. caused because the local energy is uneven.The restriction applicable Main Bottleneck of hydrogen is hydric safe, efficient, cheap storage at present.Existing hydrogen storage mode mainly includes high-pressure hydrogen storing, liquid hydrogen storage, solid-state hydrogen storage.Wherein solid-state hydrogen storage be the mode by chemical reaction or physical absorption by hydrogen storage in solid-state material, its energy density is high and safety is good, it is believed that be the most promising a kind of hydrogen storage mode.The lightweight high capacity solid hydrogen storage material being made up of light element, such as boron hydride, alanate, nitrilo compound etc., theoretical hydrogen storage capability is above 5wt%, and this brings hope for solid-state hydrogen storage material.Wherein nitrilo compound hydrogen storage material is owing to its hydrogen storage content is big and inhales factors such as putting hydrogen condition gentleness, and very likely becomes the hydrogen storage material of a new generation's practical application.Such as Mg (NH2)2-2LiH system, its gravimetric hydrogen storage density is 5.6wt%；Its enthalpy～40kJ (molH2)-1According to model Hough Equation for Calculating known its discharge 1 atmospheric equilibrium hydrogen pressure needed for temperature be about 90 DEG C, this is very identical with Proton Exchange Membrane Fuel Cells (PEMFC) operating temperature；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.Nitrilo compound hydrogen storage process generally involves nitrilo metallic compound and metal hydride, and study mechanism thinks the metal N-H key (H in nitrilo metallic compoundδ+)With the metal-H key (H in metal hydrideδ-) between strong interaction be nitrilo metal compound objects system release hydrogen driving force.So in nitrilo metal compound objects system certain embodiments there is H in general requirement simultaneouslyδ+And Hδ-The H of two kinds of different electronegativity.At present, the metal hydride species on market is more various, it is common that obtained by the hydrogenation of metal simple-substance high-temperature fusion；But the ammonobase classes of compounds in nitrilo metallic compound is relatively deficient, its common synthetic method has the various ways such as the direct ammonification of metal, metal hydride ammonification or metal nitride hydrogenation, and generally its course of processing is complicated and be difficult to form pure ammonobase compound so ammonobase compound is expensive.If metal hydride lithium LiH (Sigma) price of hydrogen storage rank is at～83 pieces/gram；The metal amino lithium LiNH of hydrogen storage rank2(Sigma) price is at～80 pieces/gram；Additionally go back on some amino-compound market and cannot directly obtain, such as amino magnesium (Mg (NH2)2, it is estimated that the laboratory of amino magnesium synthesis price is at～150 pieces/gram.General light vehicle-mounted hydrogen storage system requires that its reversible hydrogen storage capacity is 5Kg, with the hydrogen storage material of current most vehicular applications prospect: Mg (NH2)2-2LiH system (5.6wt%) is example, then want the～Mg (NH of 90Kg2)2-2LiH sample.Mg (NH is prepared with current laboratory2)2The price (Sigma) buying LiH with commercialization calculates, then only the price of hydrogen storage material is just up to 1,200,000 RMB, so being difficult to practical or being difficult to the common peopleization.Therefore this patent proposes a kind of method that safety inexpensively prepares nitrilo metallic compound hydrogen storage material on a large scale.
Summary of the invention
The present invention make every effort to provide a kind of simple to operate, safety is high, with low cost, the method for preparing nitrilo metallic compound hydrogen storage material on a large scale.Particular content is, adopts the multi-steps such as Homogeneous phase mixing, calcining, deamination, hydrogenation inexpensively to prepare nitrilo metallic compound hydrogen storage material on a large scale, thus advancing the practical of nitrilo metallic compound hydrogen storage material.Can also a certain step in preparation process or add auxiliary agent in a few step process and improve the hydrogen storage property of nitrilo metallic compound hydrogen storage material.
Aforesaid metal (M) is 1-3 race main group metal or early transition metal.After its formation nitride, corresponding formula is: MNxHy (0 < x≤10,0 < y≤20).
The material that whole or a certain composition in aforesaid builders or a certain composition are formed in mixing, calcining, deamination, hydrogenation process, and these materials can act on nitrilo metallic compound hydrogen storage material and form noval chemical compound or solid solution.Main auxiliary agent has: metal simple-substance, metal hydride, metal-oxide, metal hydroxides, metal nitride, metal halide, metallic boron hydrides, metal boron hydronitrogen etc..
The laboratory preparation manipulation process of the present invention: weigh metal or metal hydride material of main part or its auxiliary agent in the glove box of inert atmosphere, being encased in special ball grinder, (ball grinder is ball grinder salable, pressure, on cover equipped with the valve connected in tank, for passing in tank or discharging gas) seal, in tank body, pour into ammonia or liquefied ammonia or other gas such as hydrogen, argon, carbon dioxide etc. subsequently.Being installed on planetary ball mill and start ball milling, the speed setting of ball mill is 50～400rpm, and the pellet mass ratio of ball milling is: 0.1～20.Sample after ball milling is complete, transfers to after taking out in the voltage-resistant reactor of sealing and calcine under ammonia atmosphere in glove box, and its calcining heat is different according to the difference of used metal, its temperature 100～600 DEG C.Sample after calcining is placed in deamination under vacuum or low ammonia dividing potential drop, and the sample after deamination is hydrogenated with under hydrogen or hydrogen mixed gas atmosphere, thus obtaining nitrilo metallic compound hydrogen storage material.
The present invention has the following advantages:
1. adopt this method safety inexpensively can prepare nitrilo metallic compound hydrogen storage material on a large scale from cheap metal simple-substance through simple ball milling, calcining, deamination and hydrogenation.
2. adopt this method can directly prepare pure nitrilo metallic compound hydrogen storage material and can also prepare the nitrilo metallic compound hydrogen storage material of admixed with additives.
3. adopt this method to prepare nitrilo metallic compound without directly contacting poisonous and harmful dust or gas, whole process safety strong operability.
The method technique preparing nitrilo metallic compound hydrogen storage material that the present invention proposes is simple, safe and reliable, can greatly reduce cost, can prepare hydrogen storage material on a large scale.The practical application of Hydrogen Energy is had extremely important value and significance by the hydrogen storage material of inexpensive safety.
Accompanying drawing explanation
Fig. 1. Li-N-H (LiNH prepared by this law2-LiH) system hydrogenation after dehydrogenation inhale hydrogen curve chart.
Fig. 2. Li-Mg-N-H (Mg (NH prepared by this law2)2-2LiH) system hydrogenation after dehydrogenation inhale hydrogen curve chart.
Detailed description of the invention
The present invention is with metal simple-substance or metal hydride for material of main part, simultaneously can interpolation auxiliary agent in material of main part in the past, by obtaining nitrilo metallic compound hydrogen storage material after the steps such as mix homogeneously, calcining, deamination, hydrogenation, thus extensive inexpensive safety prepare nitrilo metallic compound hydrogen storage material.Below by way of specific embodiment, the present invention is described in detail, it is pointed out that the invention is not limited in these embodiments following, be also not limited to laboratory operation.
Embodiment 1: preparation Li-N-H (LiNH2-LiH) system
(1) in glove box, weigh a certain amount of lithium metal such as 70g, be subsequently adding in ball grinder, be subsequently injected into 10-120atm ammonia or liquefied ammonia.
(2) by after the described addition lithium metal of step (1) and ammonia, it is placed on planetary ball mill by ball grinder 100～200rpm mixing 1-20h, makes part metals lithium and ammonia react generation Lithamide. simultaneously.
(3) sample that step (2) mixed takes out and is placed in voltage-resistant reactor ammonification, and ammonification temperature is between 50～350 DEG C；Time 1-50h；Also can (> 50h for a long time) repeat step (2) until all lithium metals are changed into Lithamide..
(4) the Lithamide. sample as obtained after step (3) ammonification carries out temperature programming (fixing heating rate) deamination test (TPD-MS) and determines its deamination temperature, and selects suitable temperature (200～500 DEG C) to carry out deamination.
(5) as the sample after step (4) deamination carries out hydroprocessing；Hydrogenation pressure > 2atm；Hydrogenation temperature > 150 DEG C.
(6) after being hydrogenated with such as step (5), the dehydrogenation of Li-N-H system inhales hydrogen result as shown in Figure 1.
Embodiment 2: preparation Li-Mg-N-H (Mg (NH2)2-nLiH) system
(1) in glove box, the lithium metal of a certain amount of magnesium metal and corresponding amount is weighed (such as Mg (NH2)2The mol ratio of-2LiH system then Mg and Li is 1:2, such as 38g altogether), be subsequently adding in ball grinder, be subsequently injected into ammonia (> 5atm) or liquefied ammonia.
(2) by after the described addition magnesium metal of step (1), lithium metal and ammonia, it is placed on planetary ball mill by ball grinder 50～200rpm and is mixed for more than 1h until uniformly, make part metals lithium or magnesium and ammonia react simultaneously and generate Lithamide. or amino magnesium.
(3) sample that step (2) mixed takes out and is placed in voltage-resistant reactor ammonification, and ammonification temperature is between 150～400 DEG C；
(4) sample as obtained after step (3) ammonification carries out temperature programming deamination test (TPD-MS) and determines its deamination temperature, and selects suitable temperature 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, carry out inhaling dehydrogenation cycle after hydrogenation is full and finally can obtain Mg (NH2)2-nLiH system.
(6) Li-Mg-N-H (Mg (NH after being hydrogenated with such as step (5)2)2-2LiH) system dehydrogenation inhale hydrogen result as shown in Figure 2.
Embodiment 3: prepare the KH Li-Mg-N-H (Mg (NH modified2)2-nLiH-yKH) system
(1) in glove box, the lithium metal of a certain amount of magnesium metal and corresponding amount and metallic potassium are weighed (such as Mg (NH2)2The mol ratio of-1.9LiH-0.1KH system then Mg and Li and K is 1:1.9:0.1, such as gross weight 41.2g), be subsequently adding in ball grinder, be subsequently injected into ammonia (> 2atm) or liquefied ammonia.
(2) by after the described addition magnesium metal of step (1), lithium metal, metallic potassium and ammonia, the mixing that is placed on planetary ball mill by ball grinder 50～200rpm > 1h, until mix homogeneously, make part metals lithium, metallic potassium or magnesium and ammonia react generation Lithamide., potassamide or amino magnesium simultaneously.
(3) sample that step (2) mixed takes out and is placed in voltage-resistant reactor ammonification, and ammonification temperature is between 150～400 DEG C；
(4) sample as obtained after step (3) ammonification carries out temperature programming deamination test (TPD-MS) and determines its deamination temperature, and selects suitable temperature 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, be hydrogenated with saturated carry out inhaling dehydrogenation cycle after can obtain Mg (NH2)2-nLiH-yKH system.
Claims (9)
1. the method preparing nitrilo metallic compound hydrogen storage material, it is characterised in that:
It is mixed into material of main part with one or two or more kinds in metal simple-substance, metal hydride or metal nitrogen based compound, with other compound for auxiliary agent, obtains nitrilo metallic compound hydrogen storage material by Homogeneous phase mixing, calcining, deamination, hydrogenation.
2. the method for claim 1, it is characterised in that: described metal nitrogen based compound can be one or two or more kinds mixing in metal amide, metal imido compound or nitride metal compound.
3. method as claimed in claim 1 or 2, it is characterized in that: described metal (M) is 1-3 race main group metal or early transition metal (IVB-VIIB metal, mainly has: one or two or more kinds in Sc, Ti, V, Cr, Mn, Zr, Nb, Mo etc.)；After its formation nitrogenate, corresponding formula is: MNxHy (0 < x≤10,0 < y≤20).
4. the method for claim 1, it is characterised in that: described auxiliary agent can be one or two or more kinds in metal hydride, metal-oxide, metal hydroxides, metal nitride, metal halide, metallic boron hydrides, metal boron hydronitrogen etc.；The material that whole or a certain composition in described auxiliary agent or a certain composition are formed in mixing, calcining, deamination, hydrogenation process, and these materials can act on nitrilo metallic compound hydrogen storage material；The mol ratio of auxiliary agent and material of main part is 1:100～10:1.
5. method as claimed in claim 4, it is characterised in that: the metal in described auxiliary agent is one or more in 1-3 race main group metal or transition metal, one or two or more kinds such as K, Na, Co, Cr, V, in Zr etc.；Metal in described metal hydride, metal-oxide, metal hydroxides, metal nitride, metal halide is the one (one or two or more kinds in Sc, Ti, V, Cr, Mn, Zr, Nb, Mo etc.) in 1-3 race main group metal or transition metal, and its formula is: MXn, 0 < n≤7, X is one or two or more kinds in H, O, OH, N, F, Cl, Br, I etc.；The metal source in metallic boron hydrides and metal boron hydronitrogen one in 1-3 race main group metal or transition metal, its formula is: M (BH4)n,0<n≤10；M(BH4)x(NH2)y,0<x≤10,0<y≤20。
6. method as claimed in claim, it is characterised in that: mixed uniformly mode is: mechanical ball milling, mechanical agitation, smashing or grinding；When using planetary ball mill, rotational speed of ball-mill is 50～400rpm, and the pellet mass ratio of ball milling is 0.1～20.
7. the method for claim 1, it is characterised in that: during calcining, gas pressure is 0.5～120atm, calcining heat 50～600 DEG C, calcination time 0.5～300h；Calcination atmosphere can be then ammonia atmosphere can also be the mixing atmosphere of ammonia；When ammonia is mixing gas, mixing gas can be NH3: X mixing composition (X=H2、N2, one or two or more kinds in He, Ne, Ar, Ke, Xe), the mol ratio that wherein ammonia accounts for is 10%～100%；The mol ratio of total ammonia amount and metal or metal hydride is 0.1～80.
8. the method for claim 1, it is characterised in that: deamination temperature 100～500 DEG C, deamination time 0.5～100h.
9. the method for claim 1, it is characterized in that: in hydrogenation process in its hydrogen can be pure hydrogen can also be hydrogen and ammonia, nitrogen, argon etc. one or two or more kinds mixing gas, in mixing gas, the volumetric concentration of other gas outside dehydrogenation gas is less than 99%；The volume content of hydrogen is 1% to 100%；Hydrogenation hydrogen pressure 5～700atm, hydrogenation temperature 80～300 DEG C, hydrogenation time 0.02～10h.
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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 |
| CN112062110A (en) * | 2020-08-14 | 2020-12-11 | 浙江工业大学 | Method for synthesizing binary metal amino compound |
| CN112079331A (en) * | 2020-08-20 | 2020-12-15 | 浙江工业大学 | Synthesis method of metal-nitrogen-hydrogen system hydrogen storage material |
| CN112110426A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Method for synthesizing amino lithium potassium by mechanical ball milling |
| CN112978679A (en) * | 2019-12-12 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of multi-metal hydrogen-containing compound |
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Cited By (7)
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| 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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