CN111661816B - MgH 2 Ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof - Google Patents
MgH 2 Ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof Download PDFInfo
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- CN111661816B CN111661816B CN202010518407.9A CN202010518407A CN111661816B CN 111661816 B CN111661816 B CN 111661816B CN 202010518407 A CN202010518407 A CN 202010518407A CN 111661816 B CN111661816 B CN 111661816B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
- B24B1/005—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes using a magnetic polishing agent
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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
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- Y02E60/32—Hydrogen storage
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Abstract
The invention belongs to the technical field of hydrogen storage materials, and in particular relates to MgH 2 Ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof. The composite hydrogen storage material adopts MgH 2 The invention is prepared by mixing ternary metal oxide and graphite as base materials and magnetically grinding and compounding, and the ternary metal oxide is coated with MgH by adding ternary metal oxide and graphite particles 2 The crystal particles form an excellent core-shell structure, have good catalytic effect and remarkable dynamic performance, and the porosity of the graphite is also beneficial to the adsorption of hydrogen and improves the hydrogen absorption efficiency; the addition of the ternary metal oxide and the graphite can effectively eliminate the agglomeration of the hydrogen storage material, so that the purpose of reducing the particle size of the material particles is achieved, and compared with the existing single binary metal oxide, the ternary metal oxide has better dynamic performance and good reversibility of hydrogen absorption and desorption, and can still show better hydrogen storage performance after multiple cycles at a specific temperature.
Description
Technical Field
The invention belongs to the technical field of hydrogen storage materials, and in particular relates to MgH 2 Ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof.
Background
With the continued development of global population and economic scale, global energy and environment are facing severe situations. Environmental problems and causes thereof due to the use of energy are continuously recognized, and not only are hazards such as smoke, photochemical smog and acid rain, but also global climate change caused by the increase of the concentration of carbon dioxide in the atmosphere are recognized as the fact of no contention. Therefore, development of new energy sources is needed, and how to efficiently utilize hydrogen energy is a key link for solving the problem of hydrogen energy storage.
The metal magnesium as one kind of hydrogen storing material has the advantages of small density, high hydrogen storing capacity, rich resource, low cost, etc. Therefore, the magnesium-based hydrogen storage alloy is one of the most promising hydrogen storage materials. Alloying is a simple and effective means for improving the Mg-based hydrogen storage alloy, and the system design and the phase structure regulation of the material are directly related to the advantages and disadvantages of the hydrogen storage performance.
However, the existing hydrogen storage materials have the problems of difficult hydrogen absorption and desorption activation, low hydrogen absorption and desorption speed (namely, poor hydrogen absorption and desorption dynamic performance) and poor hydrogen absorption and desorption thermodynamic performance, and the effective hydrogen absorption and desorption can be realized only at about 350 ℃.
Disclosure of Invention
The invention aims to solve the technical problems that: overcomes the defects of the prior art and provides an MgH 2 The ternary metal oxide-graphite composite hydrogen storage material can obviously improve the cyclic hydrogen storage performance while maintaining the high hydrogen storage amount and excellent hydrogen storage dynamic performance, and effectively reduce the degradation problem of the material performance after repeated hydrogen absorption and desorption; meanwhile, the invention also provides a preparation method of the magnetic grinding type grinding machine, which adopts a magnetic grinding mode, and has good grinding effect and high working efficiency.
MgH according to the invention 2 Ternary metal oxide-graphite composite hydrogen storage material prepared by MgH 2 As base material, mixAnd combining the ternary metal oxide and graphite.
The ternary metal oxide is VNbO 5 、CuCo 2 O 4 ，MnFe 2 O 4 Or Co 2 One of NiO.
The MgH 2 The particle size of (2) is 50-100nm.
The mass percentage of the ternary metal oxide in the composite hydrogen storage material is 10-15wt% and the grain diameter is 5-50 mu m.
The mass percentage of graphite in the composite hydrogen storage material is 2-3wt% and the particle size is 10-30nm.
MgH according to the invention 2 -preparation method of ternary metal oxide-graphite composite hydrogen storage material, comprising the following steps:
(1) Under the protection atmosphere of inert gas, mgH is added 2 Adding the mixed material of the ternary metal oxide and the graphite powder into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, and a grinding cavity is sealed;
(2) Introducing hydrogen with the pressure of 5-15MPa, starting an electromagnetic grinder, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after electrifying to perform high-speed collision grinding with materials;
(3) And after finishing grinding, separating out the magnetic grinding needle to obtain the composite hydrogen storage material.
The mass ratio of the mixed material to the magnetic grinding needle in the step (1) is 1:10-50, preferably 1:20.
In the step (2), the grinding frequency of the electromagnetic grinder is 1800-3600rpm, the interval time between the forward and reverse running is 0.5h, and the total grinding time is 0.5-30h.
An electromagnet is arranged around the grinding tank of the electromagnetic grinder, the electromagnet consists of an electromagnetic coil and an iron core, and an alternating magnetic field is generated by utilizing current to drive a magnetic grinding needle in the tank to produce shearing collision with materials so as to achieve a good grinding effect. The electromagnet is connected with the voltage and current controller and is connected with the AC frequency converter to control the grinding condition in the grinding tank.
XRD characterization shows that the composite hydrogen storage material prepared by the invention contains VNbO 5 ，βMgH 2 And gamma MgH 2 MgH after one-time hydrogen absorption and desorption 2 Are all converted into beta MgH 2 。
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adds ternary metal oxide and graphite particles, and the ternary metal oxide coats MgH 2 The crystal particles form an excellent core-shell structure, have good catalytic effect and remarkable dynamic performance, and the porosity of the graphite is also beneficial to the adsorption of hydrogen and improves the hydrogen absorption efficiency; the addition of the ternary metal oxide and the graphite can effectively eliminate the agglomeration of the hydrogen storage material, so that the purpose of reducing the particle size of the material particles is achieved.
2. Compared with the existing single binary metal oxide, the invention has better dynamic performance and good reversibility of hydrogen absorption and desorption, and can still show better hydrogen storage performance after multiple cycles at a specific temperature.
3. The invention adopts a magnetic grinding mode, is completed by a magnetic grinder, utilizes an alternating magnetic field made by current to enable the mixed material to rotate around a grinding medium at a high speed and violently for 360 degrees, achieves a high-speed perfect grinding effect by violent impact, and can greatly shorten the grinding time compared with the traditional ball mill, thereby improving the working efficiency.
Detailed Description
The invention is further illustrated below with reference to examples.
All the raw materials used in the examples are commercially available unless otherwise specified.
Comparative example 1
(1) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 10 nm;
(2) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 Mixing with graphite powder with particle size of 10nm, adding the mixture into grinding tank of electromagnetic grinder, wherein magnetic grinding needle is arranged in the grinding tank, and mixing the mixture with magnetic grinding needleThe mass ratio of (2) is 1:20, and the grinding cavity is sealed;
(3) Setting grinding parameters, setting the grinding frequency to 1800rpm, enabling the interval time between forward and reverse running to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(4) After grinding for 30 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
The mass percentage of graphite in the prepared composite hydrogen storage material is 2wt%
Comparative example 2
(1) Will V 2 O 5 And Nb (Nb) 2 O 5 Mixing at a molar ratio of 1:1, grinding for 12 hours, annealing at 500 ℃ to synthesize VNbO with a particle size of 5 μm 5 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 10 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 VNbO with particle size of 5 μm 5 Mixing with graphite powder with the particle size of 10nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 1800rpm, enabling the interval time between forward and reverse running to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) After grinding for 30 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
VNbO in the prepared composite hydrogen storage material 5 The mass percentage of the graphite is 5wt%, and the mass percentage of the graphite is 2wt%
Example 1
(1) Will V 2 O 5 And Nb (Nb) 2 O 5 Mixing at a molar ratio of 1:1, grinding for 12 hours, annealing at 500 ℃ to synthesize VNbO with a particle size of 5 μm 5 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 10 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 VNbO with particle size of 5 μm 5 Mixing with graphite powder with the particle size of 10nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 1800rpm, enabling the interval time between forward and reverse running to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) After grinding for 30 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
VNbO in the prepared composite hydrogen storage material 5 The mass percentage of the graphite is 10wt%, and the mass percentage of the graphite is 2wt%.
Example 2
(1) Will V 2 O 5 And Nb (Nb) 2 O 5 Mixing at a molar ratio of 1:1, grinding for 12 hours, annealing at 500 ℃ to synthesize VNbO with a particle size of 5 μm 5 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 10 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 VNbO with particle size of 5 μm 5 Mixing with graphite powder with the particle size of 10nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 1800rpm, enabling the interval time between forward and reverse running to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) After grinding for 30 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
VNbO in the prepared composite hydrogen storage material 5 The mass percentage of the graphite is 15wt%, and the mass percentage of the graphite is 2wt%.
Example 3
(1) CuO and CoO are mixed in a molar ratio of 1:1 and ground for 12 hours, and annealed at 500 ℃ to synthesize CuCo with a particle size of 10 μm 2 O 4 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 15 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 CuCo with particle size of 10 μm 2 O 4 Mixing with graphite powder with the particle size of 15nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 2500rpm, enabling the interval time between forward and reverse movement to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) And after grinding for 20 hours, closing the grinding machine, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
CuCo in the prepared composite hydrogen storage material 2 O 4 The mass percentage of the graphite is 10wt%, and the mass percentage of the graphite is 2wt%.
Example 4
(1) MnO and Fe 2 O 3 Mixing at a molar ratio of 1:1, grinding for 12 hours, annealing at 500 ℃ for synthesis,MnFe with particle size of 25 mu m 2 O 4 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 20 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 60nm is prepared 2 MnFe with particle size of 25 mu m 2 O 4 Mixing with graphite powder with the particle size of 20nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 3000rpm, enabling the interval time between forward and reverse movement to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) After grinding for 15 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
MnFe in the prepared composite hydrogen storage material 2 O 4 The mass percentage of the graphite is 12wt%, and the mass percentage of the graphite is 2wt%.
Example 5
(1) CoO and NiO were mixed in a molar ratio of 1:1 and ground for 12 hours, and annealed at 500℃to synthesize Co having a particle size of 45. Mu.m 2 NiO；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 30 nm;
(3) MgH with the grain diameter of 100nm is processed under the protection atmosphere of inert gas argon 2 Co with particle size of 45 μm 2 Mixing NiO and graphite powder with the particle size of 30nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting grinding frequency to be 3600rpm, enabling the interval time between positive and negative movement to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) After grinding for 3 hours, the grinding machine is closed, the magnetic objects are used for separating substances in the grinding cavity, and the products are extracted, so that the composite hydrogen storage material is obtained.
Co in the prepared composite hydrogen storage material 2 The mass percentage of NiO is 15wt%, and the mass percentage of graphite is 3wt%.
Performance testing
The comparative example 1 composite hydrogen storage material without ternary metal oxide added, and the comparative example 2, example 1 and example 2 composite hydrogen storage materials with ternary metal oxide added were subjected to tests of hydrogen release amounts at different temperatures, the test results are shown in Table 1, at 160℃and 20bar H 2 The test of hydrogen storage amount was carried out as follows, and the test results are shown in Table 2.
TABLE 1 Hydrogen release amount at different temperatures for comparative examples 1-2 and example 1-2 composite hydrogen storage materials
Table 2 Hydrogen storage amount of the composite hydrogen storage materials of comparative examples 1 to 2 and examples 1 to 2
The composite hydrogen storage material prepared in example 2 was circulated 10 to 50 times, and the hydrogen storage/release amount was tested at 300 c and 275 c, and the test results are shown in table 3.
TABLE 3 cycle 10-50 times hydrogen storage/release amount of composite hydrogen storage material prepared in example 2
| Number of cycles | 10 | 20 | 30 | 40 | 50 |
| Hydrogen storage at 300 ℃ (wt.%) | 6 | 5.8 | 5.7 | 5.8 | 5.8 |
| Hydrogen evolution at 300 ℃ (wt.%) | 5.7 | 5.6 | 4.9 | 5.1 | 5.5 |
| 275 ℃ hydrogen storage (wt.%) | 5.2 | 5.4 | 5.3 | 5.2 | 5.1 |
| Hydrogen evolution at 275 ℃ (wt.%) | 5.2 | 5.2 | 4.9 | 5.1 | 5.0 |
Of course, the foregoing is merely preferred embodiments of the present invention and is not to be construed as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and those skilled in the art will appreciate that the present invention is capable of equally varying and improving within the spirit and scope of the present invention.
Claims (1)
1. MgH (MgH) 2 -preparation method of ternary metal oxide-graphite composite hydrogen storage material, comprising the following steps:
(1) CuO and CoO are mixed in a molar ratio of 1:1 and ground for 12 hours, and annealed at 500 ℃ to synthesize CuCo with a particle size of 10 μm 2 O 4 ；
(2) Grinding the scaly graphite in an electromagnetic grinder, and drying to prepare graphite powder with the particle size of 15 nm;
(3) Under the protection atmosphere of inert gas argon, mgH with the particle diameter of 50nm is prepared 2 CuCo with particle size of 10 μm 2 O 4 Mixing with graphite powder with the particle size of 15nm, adding the mixed material into a grinding tank of an electromagnetic grinder, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) Setting grinding parameters, setting the grinding frequency to 2500rpm, enabling the interval time between forward and reverse movement to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting an electromagnetic grinding machine, and driving a magnetic grinding needle to perform high-speed 360-degree rotary motion after the electromagnetic grinding machine is electrified to perform high-speed collision grinding with materials;
(5) And after grinding for 20 hours, closing the grinding machine, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
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