CN110963461A - Metal oxide and porous material composite hydrogen storage material and preparation method thereof - Google Patents
Metal oxide and porous material composite hydrogen storage material and preparation method thereof Download PDFInfo
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- CN110963461A CN110963461A CN201911411873.0A CN201911411873A CN110963461A CN 110963461 A CN110963461 A CN 110963461A CN 201911411873 A CN201911411873 A CN 201911411873A CN 110963461 A CN110963461 A CN 110963461A
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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
Abstract
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a metal oxide and porous material composite hydrogen storage material and a preparation method thereof. The metal oxide and porous material composite hydrogen storage material is formed by compounding magnesium hydride, a porous material and a metal oxide, wherein the weight ratio of the magnesium hydride to the porous material to the metal oxide is 100-10:5-0.1: 1-0.05. Grinding mixed metal oxide particles by taking magnesium hydride as a base material to obtain an activated magnesium hydride material; and mixing the activated magnesium hydride material with a porous material, and performing ball milling or compression to obtain the composite hydrogen storage material. According to the invention, the nanoscale metal oxide particles are added and simultaneously compounded with the porous material, so that the hydrogenation speed of the magnesium-based composite powder in the hydrogen-charging ball-milling process can be accelerated, and the hydrogenation speed is combined with the excellent pore channels, the high surface area and other properties of the porous material, so that the hydrogen storage material has good characteristics in the aspects of hydrogen adsorption and desorption kinetics.
Description
Technical Field
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a metal oxide and porous material composite hydrogen storage material and a preparation method thereof.
Background
So far, the main examples of the metal hydrogen storage materials that have been studied relatively frequently are: (1) with LaNi5A rare earth system AB of5A type alloy; (2) AB type hydrogen storage alloy represented by TiFe, (3) ZrV2Is a representative AB2A type Laves phase hydrogen storage alloy; (4) with LaNi3Novel AB of the type3A hydrogen storage alloy of type; (5) with Mg2A represented by Ni2A type B hydrogen storage alloy. Although LaNi5Type and LaNi3The alloy has excellent hydrogen absorption and desorption dynamic performance and lower hydrogen absorption and desorption temperature, but the hydrogen absorption weight is lower (only about 1.5 percent); 1.8-2.2 wt% of TiFe system, and the activation process is difficult; the Laves phase series alloy has long activation period, low hydrogen storage amount and high price. Mg (magnesium)2The hydrogen absorption weight ratio of the Ni-based magnesium-based alloy is also only 3.6%. According to the indexes (working pressure of 1-10 atm; reversible hydrogen storage capacity of 4-5 wt%) of hydrogen storage material for automobile proposed in recent years, the hydrogen storage material should satisfy the above three indexes at the same time, especially storage temperature of 273-373KThe hydrogen weight ratio is 4-5%, and a novel metal hydrogen storage material needs to be further researched and explored. Magnesium is a most promising candidate metal hydrogen storage material with the advantages of high hydrogen storage capacity (7.6% by weight), abundant resources, low price, no pollution and the like. However, magnesium has not been practically used up to now due to its high hydrogen absorption and desorption temperature and poor kinetic properties. Chinese patent CN1204282C discloses a material with high hydrogen storage capacity, which improves the hydrogen charging and discharging kinetics and thermodynamic property of pure magnesium hydrogen storage material to a certain extent, but because nickel which does not absorb hydrogen is added, the hydrogen absorption capacity is reduced, and because nickel is relatively expensive, the cost of the material is increased.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, provides a metal oxide and porous material composite hydrogen storage material, can obviously improve the hydrogen storage kinetic performance of the magnesium hydrogen storage material while keeping high hydrogen storage capacity, and also obviously reduces the hydrogen storage temperature. Meanwhile, the invention also provides a preparation method of the compound, which is scientific and reasonable and is suitable for industrial production.
The metal oxide and porous material composite hydrogen storage material is formed by compounding magnesium hydride, a porous material and a metal oxide, wherein the weight ratio of the magnesium hydride to the porous material to the metal oxide is 100-10:5-0.1: 1-0.05.
The particle size of the magnesium hydride is 16.5-20.5 nm.
The porous material is graphite or SiO2、Al2O3One or more of A-type molecular sieve, X-type molecular sieve, Y-type molecular sieve or MFI molecular sieve. The particle size of the porous material is 5-50 μm.
The metal oxide is α -Fe2O3、TiO2、CeO2、Cr2O3、CuO、Mn2O3Or Sc2O3One or more of them, the particle size is 10-30 nm.
The preparation method of the metal oxide and porous material composite hydrogen storage material comprises the following steps:
(1) grinding mixed metal oxide particles by taking magnesium hydride as a base material to obtain an activated magnesium hydride material;
(2) and mixing the activated magnesium hydride material with a porous material, and performing ball milling or compression to obtain the composite hydrogen storage material.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the nano-scale metal oxide particles are added, so that the hydrogenation speed of the magnesium-based composite powder in the hydrogen-charging ball-milling process can be accelerated, and the reduction of the particle size of magnesium hydride is facilitated; nanocrystalline MgH coated by metal oxide2The core-shell structure with excellent synergistic effect is formed, the catalyst has good catalysis and remarkable dynamic performance, the hydrogen storage reaction speed can be improved, the micro-area heat release is controlled, and the metal oxide effectively eliminates a hydrogen storage reactant Mg (OH)2And further achieve the purpose of full hydrolysis reaction.
2. The invention uses the porous material with adjustable aperture as the carrier, and compounds the magnesium hydride and the porous material, so that the hydrogen storage performance of the magnesium hydride is combined with the excellent pore channels, high surface area and other performances of the porous material, and the hydrogen storage material has good characteristics in the aspects of hydrogen adsorption and desorption kinetics.
Detailed Description
The present invention will be further described with reference to the following examples.
The starting materials used in the examples are commercially available unless otherwise specified.
Example 1
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material and mixed with metal oxide particles, and the mass percentage of each component in the mixture is that the magnesium hydride accounts for 99 percent and the α -Fe accounts for2O31 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Mixing the activated magnesium hydride material with graphite with the particle size of 15 mu m according to the mass ratio of 100:1, and compressing by a granulator to obtain the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min at the normal temperature of 25 ℃ to release hydrogen with 75 percent of theoretical hydrogen storage amount, and the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min at the temperature of 50 ℃ to release hydrogen with 98 percent of theoretical hydrogen storage amount.
Example 2
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material, mixed with metal oxide particles, and the mass percentage of each component in the mixture is as follows: 98% magnesium hydride, TiO22 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Mixing the obtained activated magnesium hydride material with active Al with particle size of 5 μm2O3Mixing the raw materials according to the mass ratio of 100:1, and compressing the mixture by a granulator to obtain the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min at the normal temperature of 25 ℃ to release hydrogen with 73.8 percent of theoretical hydrogen storage amount, and the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min at the temperature of 50 ℃ to release hydrogen with 98.8 percent of theoretical hydrogen storage amount.
Example 3
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material, mixed with metal oxide particles, and the mass percentage of each component in the mixture is as follows: 97% of magnesium hydride, CeO23 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Mixing the obtained activated magnesium hydride material with SiO with particle size of 15 μm2Mixing at a mass ratio of 100:0.5, and granulating with a granulatorAnd (4) compressing to obtain the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min at the normal temperature of 25 ℃ to release hydrogen with the theoretical hydrogen storage amount of 71.6 percent, and the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min at the temperature of 50 ℃ to release hydrogen with the theoretical hydrogen storage amount of 97.8 percent.
Example 4
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material, mixed with metal oxide particles, and the mass percentage of each component in the mixture is as follows: 97% of magnesium hydride, Cr2O33 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Treating the A-type molecular sieve with the particle size of 5 microns in a muffle furnace at 300 ℃ for 15 hours under a vacuum condition, and then cooling to room temperature; mixing the treated A-type molecular sieve with the obtained activated magnesium hydride material, wherein the weight ratio of the magnesium hydride to the molecular sieve material is 100:0.5, and then absorbing and releasing hydrogen for 5 times at 200 ℃ to form diffusion, thus obtaining the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, at the normal temperature of 25 ℃, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min to release hydrogen with 77.7 percent of theoretical hydrogen storage amount, and at the temperature of 50 ℃, the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min to release hydrogen with 98.9 percent of theoretical hydrogen storage amount.
Example 5
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material, mixed with metal oxide particles, and the mass percentage of each component in the mixture is as follows: 97% of magnesium hydride, Cr2O33 percent; performing hydrogen charging ball milling on the mixture in a ball mill, performing hydrogen charging (0.4MPa) ball milling for 80h in a planetary ball mill with a ball-material ratio of 20:1 and a ball milling rotation speed of 180r/min to obtain the activated hydrogenationThe particle size of the magnesium material is 28-60 nm.
Processing an X-type molecular sieve with the particle size of 5 mu m in a muffle furnace at 300 ℃ for 15 hours under a vacuum condition, and then cooling to room temperature; mixing the treated X-type molecular sieve with the obtained activated magnesium hydride material, wherein the weight ratio of the magnesium hydride to the molecular sieve material is 100:0.5, and then absorbing and releasing hydrogen for 10 times at 200 ℃ to form diffusion, thus obtaining the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in seawater for 15min at the normal temperature of 25 ℃ to release hydrogen with 73.2 percent of theoretical hydrogen storage amount, and the composite magnesium hydride hydrogen storage material is hydrolyzed in seawater for 15min at the temperature of 50 ℃ to release hydrogen with 97.7 percent of theoretical hydrogen storage amount.
Example 6
The metal oxide and porous material composite hydrogen storage material takes magnesium hydride as a base material, mixed with metal oxide particles, and the mass percentage of each component in the mixture is as follows: 97% of magnesium hydride, Cr2O33 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Treating a Y-type molecular sieve with the particle size of 25 mu m in a muffle furnace at 300 ℃ for 15 hours under a vacuum condition, and then cooling to room temperature; mixing the treated Y-type molecular sieve with the obtained activated magnesium hydride material, wherein the weight ratio of the magnesium hydride to the molecular sieve material is 100:0.5, and then absorbing and releasing hydrogen for 10 times at 200 ℃ to form diffusion, thus obtaining the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min at the normal temperature of 25 ℃ to release hydrogen with 78.9 percent of theoretical hydrogen storage amount, and the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min at the temperature of 50 ℃ to release hydrogen with 99.0 percent of theoretical hydrogen storage amount.
Example 7
The metal oxide and the porousThe composite hydrogen storage material is prepared with magnesium hydride as base material and mixed metal oxide grains, and the mixture includes magnesium hydride 99 wt% and α -Fe2O31 percent; and (3) performing hydrogen-charging ball milling on the mixture in a ball mill, and performing hydrogen-charging (0.4MPa) ball milling for 80h in a planetary ball mill, wherein the ball-to-material ratio is 20:1, the ball milling rotation speed is 180r/min, and the particle size of the obtained activated magnesium hydride material is 28-60 nm.
Treating an MFI molecular sieve with the particle size of 50 mu m in a muffle furnace at 300 ℃ for 15 hours under a vacuum condition, and then cooling to room temperature; and mixing the treated MFI molecular sieve with the obtained activated magnesium hydride material, wherein the weight ratio of the magnesium hydride to the molecular sieve material is 100:0.5, and then absorbing and releasing hydrogen for 15 times at 200 ℃ to form diffusion, thus obtaining the composite hydrogen storage material.
The hydrolysis speed of the obtained composite magnesium hydride hydrogen storage material is obviously improved along with the temperature rise, the composite magnesium hydride hydrogen storage material is hydrolyzed in secondary distilled water for 15min at the normal temperature of 25 ℃ to release hydrogen with 78.6 percent of theoretical hydrogen storage amount, and the composite magnesium hydride hydrogen storage material is hydrolyzed in the secondary distilled water for 15min at the temperature of 50 ℃ to release hydrogen with 99.1 percent of theoretical hydrogen storage amount.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (7)
1. A metal oxide and porous material composite hydrogen storage material is characterized in that: the magnesium hydride, the porous material and the metal oxide are compounded in a weight ratio of 100-10:5-0.1: 1-0.05.
2. The metal oxide and porous material composite hydrogen storage material of claim 1, wherein: the porous material is graphite or SiO2、Al2O3A type molecular sieve and X type molecular sieveOne or more of Y-type molecular sieve or MFI molecular sieve.
3. The metal oxide and porous material composite hydrogen storage material of claim 1, wherein: the particle size of the magnesium hydride is 16.5-20.5 nm.
4. The metal oxide and porous material composite hydrogen storage material of claim 1, wherein: the particle size of the porous material is 5-50 μm.
5. The metal oxide and porous material composite hydrogen storage material as claimed in claim 1, wherein the metal oxide is α -Fe2O3、TiO2、CeO2、Cr2O3、CuO、Mn2O3Or Sc2O3One or more of (a).
6. The metal oxide and porous material composite hydrogen storage material of claim 1, wherein: the particle size of the metal oxide is 10-30 nm.
7. A method for preparing the metal oxide and porous material composite hydrogen storage material of claim 1, which is characterized in that: the method comprises the following steps:
(1) grinding mixed metal oxide particles by taking magnesium hydride as a base material to obtain an activated magnesium hydride material;
(2) and (2) mixing the activated magnesium hydride material obtained in the step (1) with a porous material, and performing ball milling or compression to obtain the composite hydrogen storage material.
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| CN111661816A (en) * | 2020-06-09 | 2020-09-15 | 世能氢电科技有限公司 | MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof |
| CN111850366A (en) * | 2020-06-12 | 2020-10-30 | 榆林学院 | Oxide-loaded magnesium-nickel alloy hydrogen storage composite material and preparation method thereof |
| CN111940719A (en) * | 2020-08-11 | 2020-11-17 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Nano magnesium-based hydrogen storage material and preparation method thereof |
| CN113753854A (en) * | 2020-12-31 | 2021-12-07 | 厦门大学 | Hydrogen storage fuel with straight hole structure and preparation method thereof |
| CN113979406A (en) * | 2021-11-09 | 2022-01-28 | 上海超高环保科技股份有限公司 | Method for sintering hydrogen storage material by using nano particles |
| CN114044487A (en) * | 2021-12-08 | 2022-02-15 | 上海超高环保科技股份有限公司 | Method for manufacturing corrugated rare earth hydrogen storage material |
| WO2023082551A1 (en) * | 2021-11-12 | 2023-05-19 | 江苏科技大学 | Composite hydrogen storage material, preparation method therefor, and application thereof |
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| CN111661816A (en) * | 2020-06-09 | 2020-09-15 | 世能氢电科技有限公司 | MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof |
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| CN111850366A (en) * | 2020-06-12 | 2020-10-30 | 榆林学院 | Oxide-loaded magnesium-nickel alloy hydrogen storage composite material and preparation method thereof |
| CN111850366B (en) * | 2020-06-12 | 2021-06-18 | 榆林学院 | Oxide-loaded magnesium-nickel alloy hydrogen storage composite material and preparation method thereof |
| CN111940719A (en) * | 2020-08-11 | 2020-11-17 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Nano magnesium-based hydrogen storage material and preparation method thereof |
| CN113753854A (en) * | 2020-12-31 | 2021-12-07 | 厦门大学 | Hydrogen storage fuel with straight hole structure and preparation method thereof |
| CN113979406A (en) * | 2021-11-09 | 2022-01-28 | 上海超高环保科技股份有限公司 | Method for sintering hydrogen storage material by using nano particles |
| WO2023082551A1 (en) * | 2021-11-12 | 2023-05-19 | 江苏科技大学 | Composite hydrogen storage material, preparation method therefor, and application thereof |
| CN114044487A (en) * | 2021-12-08 | 2022-02-15 | 上海超高环保科技股份有限公司 | Method for manufacturing corrugated rare earth hydrogen storage material |
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| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Ming Inventor after: Zhao Zengdian Inventor after: Xia Xianchang Inventor after: Hao Xiaoming Inventor after: Fu Qiang Inventor after: Zhang Fang Inventor after: Yu Rujun Inventor after: Guanfeng Steel Inventor after: Chen Yanyan Inventor after: Yang Kun Inventor after: Lv Junnan Inventor after: Yang Liening Inventor before: Wang Ming Inventor before: Zhao Zengdian Inventor before: Xia Xianchang Inventor before: Hao Xiaoming Inventor before: Fu Qiang Inventor before: Zhang Fang Inventor before: Yu Rujun Inventor before: Guanfeng Steel Inventor before: Chen Yanyan Inventor before: Yang Kun Inventor before: Lv Junnan Inventor before: Yang Liening |