CN112079331A - Synthesis method of metal-nitrogen-hydrogen system hydrogen storage material - Google Patents
Synthesis method of metal-nitrogen-hydrogen system hydrogen storage material Download PDFInfo
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- CN112079331A CN112079331A CN202010845728.XA CN202010845728A CN112079331A CN 112079331 A CN112079331 A CN 112079331A CN 202010845728 A CN202010845728 A CN 202010845728A CN 112079331 A CN112079331 A CN 112079331A
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- 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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- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
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- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the field of material synthesis, and particularly relates to a synthesis method of a metal-nitrogen-hydrogen storage material. The invention discloses a method for synthesizing a hydrogen storage material of a metal-nitrogen-hydrogen system by utilizing mechanical ball milling, aiming at the problems of few existing synthesis methods, high required cost and the like of the metal-nitrogen-hydrogen system. The method comprises the steps of taking metal lithium as a raw material, and carrying out mechanical ball milling in an ammonia atmosphere to further synthesize the Li-N-H system hydrogen storage material. The invention utilizes mechanical ball milling to synthesize the Li-N-H system hydrogen storage material, has simple process and low energy consumption, and provides a new method for the industrialized synthesis application of the existing metal-nitrogen-hydrogen system.
Description
Technical Field
The invention belongs to the field of material synthesis, and mainly relates to a synthesis method of a metal-nitrogen-hydrogen system hydrogen storage material.
Background
The metal amide and the metal hydride are important compounds in the hydrogen storage material, and have good application prospect when being used as the hydrogen storage material. The lithium-nitrogen-hydrogen system composed of two lithium compounds has the advantages of low reaction enthalpy (-45kJ/mol) and the like as a classical hydrogen storage system due to the strong hydrogen storage capacity (6.5 wt%). Experimental tests show that LiNH is used as a catalyst2The Li-N-H system formed by the LiH binary hydrogen storage material is heated to 300 ℃ and the hydrogen release amount can reach about 5 wt%. Currently, LiNH is prepared2The LiH method has more related reports, but all the methods are complicated and inconvenient, and have byproducts which influence the purity. The following methods are known to prepare hydrogen storage materials of metal-nitrogen-hydrogen system: (1) direct use of commercially available LiNH2LiH is used as a raw material to be subjected to 1:1 ball milling mixing, and the cost requirement is high. (2) Reacting LiH with NH at room temperature3Ball milling in situ to generate LiNH2And then the resultant LiNH is subjected to2Mixing with LiH at a molar ratio of 1:1, and ball milling to obtain LiNH2And LiNH2+ hydrogen release properties of LiH [ J ]]Journal of university of Risk of Lanzhou, 2007(05):1-5.]. The above method has a disadvantage of high production cost.
Because the metal-nitrogen-hydrogen system has wide application in hydrogen storage materials, the hydrogen storage system obtained by simply mixing two phases has high cost. Therefore, the invention provides a method for synthesizing a metal-nitrogen-hydrogen system hydrogen storage material.
Disclosure of Invention
The invention aims to solve the problems and provide a simple and efficient method for synthesizing a metal-nitrogen-hydrogen system hydrogen storage material in situ.
The invention leads metal lithium and ammonia gas to react after mechanical ball milling to generate the Li-N-H system hydrogen storage material. The specific technical scheme is as follows:
a method for synthesizing a metal-nitrogen-hydrogen system hydrogen storage material comprises the following steps:
(1) under the protection of inert gas, adding a certain amount of metal lithium into a ball milling tank, adding grinding balls according to a certain ball-to-material ratio, and then sealing the ball milling tank;
(2) vacuumizing the ball milling tank, and then introducing ammonia gas into the ball milling tank;
(3) filling the ball milling tank filled with the ammonia gas on a ball mill, and performing ball milling reaction at a certain rotating speed for a certain time;
(4) after the reaction is finished, discharging gas in the ball milling tank, vacuumizing, taking out a product under an inert atmosphere, and performing post-treatment to obtain LiNH2-a LiH hydrogen storage material.
The inert atmosphere in the steps (1) and (4) is a gas which does not react with the reactant and the product, and specifically is any one or mixture of argon and helium.
The ball-material ratio in the step (1) is (20-80): 1, and the ball-material ratio refers to the ratio of the mass of the grinding balls to the mass of the materials.
The molar ratio of the introduced amount of the ammonia gas to the metallic lithium in the step (2) is 1 (2-4).
The ball milling rotating speed in the step (3) is 200-500 r/min, and the ball milling time is 6-48 h.
The post-treatment in the step (4) is to sieve the product by a 200-600 mesh sieve and remove excessive metal by a solid-solid separation mode to obtain LiNH2-a LiH hydrogen storage material.
In the invention, the chemical equation related to the synthesis method is as follows:
2Li+NH3→LiNH2+LiH
compared with the prior art, the invention has the following beneficial effects:
the synthesis method of the metal-nitrogen-hydrogen system hydrogen storage material takes metal lithium and ammonia gas as raw materials, and synthesizes the metal-nitrogen-hydrogen system hydrogen storage material in situ, thereby being more convenient and efficient and having lower cost.
Drawings
Fig. 1 is an XRD pattern of the synthesized lithium-nitrogen-hydrogen storage material of example 1.
Detailed Description
The technical solution of the present invention is further described below by using specific examples, but the scope of the present invention is not limited thereto.
Example 1
Under argon atmosphere, 0.7g of metallic lithium was weighed out in a ball-to-feed ratio of 60:1 and placed in a sealed ball-milling jar. Then, after the ball milling tank is vacuumized, 0.85g of NH is introduced3And performing ball milling reaction on the mixture for 12 hours on a ball mill at the rotating speed of 500 r/min. And after the reaction is finished, collecting the gas in the ball milling tank, and vacuumizing again. Then taking out the lithium-ion battery under the argon atmosphere, sieving the lithium-ion battery by using a 400-mesh sieve, and removing excessive metallic lithium in a solid-solid separation mode to obtain the LiNH with the molar ratio of 1:12And LiH. Figure 1 is the XRD pattern of the product.
Example 2
Under argon atmosphere, 1.4g of lithium metal is weighed out in a ball-to-feed ratio of 20:1 and placed in a sealed ball-milling tank. Then the ball milling pot was evacuated and 1.7g of NH was added3And performing ball milling reaction on the mixture for 48 hours on a ball mill at the rotating speed of 400 r/min. And after the reaction is finished, collecting the gas in the ball milling tank, and vacuumizing again. Then taking out the lithium-ion battery under the argon atmosphere, sieving the lithium-ion battery by using a 600-mesh sieve, and removing excessive metallic lithium in a solid-solid separation mode to obtain the LiNH with the molar ratio of 1:12And LiH.
Example 3
Under a helium atmosphere, 0.7g of metallic lithium was weighed out in a ball-mill jar sealed at a ball-to-feed ratio of 80: 1. After the ball milling pot was evacuated, 0.85g of NH was introduced3And performing ball milling reaction on the mixture for 6 hours on a ball mill at the rotating speed of 500 r/min. And after the reaction is finished, collecting the gas in the ball milling tank, and vacuumizing again. Then taking out under helium atmosphere, and sieving with 200 mesh sieveRemoving excessive metallic lithium by solid-solid separation to obtain LiNH with a molar ratio of 1:12And LiH.
Example 4
Under the mixed atmosphere of argon and helium, 0.7g of metallic lithium is weighed with the ball-to-material ratio of 60:1 and is filled into a sealed ball milling tank. After the ball milling pot was evacuated, 0.85g of NH was introduced3And performing ball milling reaction on the mixture for 24 hours on a ball mill at the rotating speed of 200 r/min. And after the reaction is finished, collecting the gas in the ball milling tank, and vacuumizing again. Then taking out the lithium-ion battery in a mixed atmosphere of argon and helium, sieving the lithium-ion battery by using a 500-mesh sieve, and removing excessive metallic lithium in a solid-solid separation mode to obtain the LiNH with the molar ratio of 1:12And LiH.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
Claims (7)
1. A method for synthesizing a metal-nitrogen-hydrogen system hydrogen storage material is characterized by mainly comprising the following steps:
(1) under the protection of inert gas, adding a certain amount of metal lithium into a ball milling tank, adding grinding balls according to a certain ball-to-material ratio, and then sealing the ball milling tank;
(2) vacuumizing the ball milling tank, and then introducing ammonia gas into the ball milling tank;
(3) the ball milling tank is arranged on a ball mill, and ball milling reaction is carried out for a certain time at a certain rotating speed;
(4) after the reaction is finished, discharging gas in the ball milling tank, vacuumizing, taking out a product under an inert atmosphere, and performing post-treatment to obtain LiNH2-a LiH hydrogen storage material.
2. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: in the steps (1) and (4), the inert atmosphere is any one or mixture of argon and helium.
3. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: the ball-material ratio in the step (1) is (20-80): 1.
4. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: the molar ratio of the introduced amount of the ammonia gas to the metallic lithium in the step (2) is 1 (2-4).
5. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: the ball milling rotating speed in the step (3) is 200-500 r/min, and the ball milling time is 6-48 h.
6. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: the post-treatment in the step (4) is to sieve the product by a 200-600 mesh sieve and remove excessive metal by means of solid-solid separation to obtain LiNH2-a LiH hydrogen storage material.
7. The method for synthesizing a hydrogen storage material of metal-nitrogen-hydrogen system according to claim 1, wherein: the chemical equation involved in the synthesis method is as follows:
2Li+NH3→LiNH2+LiH。
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