CN111661816A - MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof - Google Patents

MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof Download PDF

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CN111661816A
CN111661816A CN202010518407.9A CN202010518407A CN111661816A CN 111661816 A CN111661816 A CN 111661816A CN 202010518407 A CN202010518407 A CN 202010518407A CN 111661816 A CN111661816 A CN 111661816A
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hydrogen storage
metal oxide
grinding
ternary metal
storage material
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CN111661816B (en
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付强
王鸣
张方
杨昆
吕俊囡
秦宏云
于如军
杨列宁
夏先畅
陈霞
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Shineng Hydrogen Technology Co ltd
Shandong University of Technology
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Shandong University of Technology
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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
    • 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
    • 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

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Abstract

The invention belongs to the technical field of hydrogen storage materials, and particularly relates to MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof. The composite hydrogen storage material is MgH2The invention is prepared by mixing ternary metal oxide and graphite as base material and magnetic grinding, and adding ternary metal oxide and graphite particles to coat MgH2The crystal particles form an excellent core-shell structure, have good catalysis and remarkable dynamic performance, and the porosity of the graphite is also favorable for the adsorption of hydrogen, so that the hydrogen absorption efficiency is improved; the addition of the ternary metal oxide and the graphite can effectively eliminate the agglomeration of the hydrogen storage material, thereby achieving the purpose of reducing the particle size of the material particles, and compared with the existing single binary metal oxide, the ternary metal oxide has better dynamic performance, good hydrogen absorption and desorption reversibility and can be circulated for many times at a specific temperatureThe ring can still show better hydrogen storage performance.

Description

MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof
Technical Field
The invention belongs to the technical field of hydrogen storage materials, and particularly relates to MgH2-ternary metal oxide-graphite composite hydrogen storage material and preparation method thereof.
Background
With the continuous development of the global population and economic scale, global energy and environment face a severe situation. Environmental problems and their causes of energy use are constantly being recognized, and not only are the hazards of smog, photochemical smog, acid rain, and the like, but also global climate changes due to elevated atmospheric carbon dioxide concentrations have been identified as a fact of no contention. Therefore, it is urgently needed to develop new energy, how to efficiently utilize hydrogen energy, and solving the problem that storage of hydrogen energy is a key link for popularization and application of the hydrogen energy.
The magnesium metal as a hydrogen storage material has the advantages of small density, high hydrogen storage capacity, abundant resources, low price and the like. Therefore, magnesium-based hydrogen storage alloy is one of the most promising hydrogen storage materials. Alloying is a simple and effective means for improving Mg-based hydrogen storage alloy, and the system design and phase structure regulation of the material directly relate to the quality of the hydrogen storage performance.
However, the existing hydrogen storage materials have the problems of difficult hydrogen absorption and desorption activation, slow hydrogen absorption and desorption speed (namely, poor hydrogen absorption and desorption dynamic performance) and poor hydrogen absorption and desorption thermodynamic performance, and generally the hydrogen can be effectively absorbed and desorbed only at about 350 ℃.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides MgH2The ternary metal oxide-graphite composite hydrogen storage material can obviously improve the cyclic hydrogen storage performance while keeping high hydrogen storage capacity and excellent hydrogen storage kinetic performance, and effectively reduce the problem of material performance degradation after hydrogen absorption and desorption for many times; meanwhile, the invention also provides a preparation method of the polishing slurry, and the magnetic polishing mode is adopted, so that the polishing effect is good, and the working efficiency is high.
MgH of the invention2-ternary metal oxide-graphite composite hydrogen storage material, with MgH2Is prepared by mixing ternary metal oxide and graphite as base material.
The ternary metal oxide is VNbO5、CuCo2O4，MnFe2O4Or Co2NiO, and the NiO is one of the NiO.
The MgH2Has a particle diameter of 50-100 nm.
The composite hydrogen storage material contains 10-15 wt% of ternary metal oxide and has a particle size of 5-50 μm.
The composite hydrogen storage material contains 2-3 wt% of graphite and has a particle size of 10-30 nm.
MgH of the invention2The preparation method of the ternary metal oxide-graphite composite hydrogen storage material comprises the following steps:
(1) under the protective atmosphere of inert gas, MgH2Adding the mixed material of the ternary metal oxide and the graphite powder into a grinding tank of an electromagnetic grinding machine, 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 the electromagnetic grinding machine, driving the magnetic grinding needle to rotate at high speed by 360 degrees after electrifying, and performing high-speed collision grinding with the materials;
(3) and after the grinding is finished, 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 grinding machine is 1800 plus 3600rpm, the interval time of forward and reverse rotation is 0.5h, and the total grinding time is 0.5-30 h.
The electromagnet is arranged around the grinding tank of the electromagnetic grinding machine and consists of an electromagnetic coil and an iron core, and an alternating magnetic field is generated by utilizing the current to drive the magnetic grinding needle in the tank to generate shearing collision with the materials so as to achieve a better grinding effect. The electromagnet is connected with a voltage and current controller and controls the grinding condition in the grinding tank with an alternating current frequency converter.
XRD (X-ray diffraction) characterization shows that the composite hydrogen storage material prepared by the invention contains VNbO5，βMgH2And gamma MgH2And MgH is generated after one-time hydrogen absorption and desorption2Are all converted into β MgH2。
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 MgH2The crystal particles form an excellent core-shell structure, have good catalysis and remarkable dynamic performance, and the porosity of the graphite is also favorable for the adsorption of hydrogen, so that the hydrogen absorption efficiency is improved; the addition of the ternary metal oxide and the graphite can effectively eliminate the agglomeration of the hydrogen storage material, thereby achieving the purpose of reducing the particle size of the material particles.
2. Compared with the existing single binary metal oxide, the binary metal oxide has better dynamic performance and good hydrogen absorption and desorption reversibility, and can still show better hydrogen storage performance after multiple cycles at specific temperature.
3. The invention adopts a magnetic grinding mode and is completed by a magnetic grinding machine, the mixed material is rotated at high speed and violently 360 degrees around a grinding medium by using an alternating magnetic field made by current, the high-speed perfect grinding effect is achieved by violent impact, and compared with the traditional ball grinding, the grinding time can be greatly shortened, thereby improving the working efficiency.
Detailed Description
The present invention will be further described with reference to the following 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 grinding machine and then drying to prepare graphite powder with the particle size of 10 nm;
(2) under the protective atmosphere of inert gas argon, MgH with the particle size of 50nm is added2Mixing with graphite powder with the particle size of 10nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(3) setting parameters of a grinding machine, setting the grinding frequency to be 1800rpm, setting the interval time between positive and negative rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(4) and after grinding for 30 hours, closing the grinder, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
The mass percentage of the graphite in the prepared composite hydrogen storage material is 2 wt%
Comparative example 2
(1) Will V2O5And Nb2O5Mixing at a molar ratio of 1:1, grinding for 12 hr, annealing at 500 deg.C to obtain VNbO with particle diameter of 5 μm5；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 10 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 50nm is added2VNbO having a particle diameter of 5 μm5Mixing with graphite powder with the particle size of 10nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 1800rpm, setting the interval time between positive and negative rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 30 hours, closing the grinder, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
VNbO in the prepared composite hydrogen storage material5The mass percentage of the graphite is 5wt percent, and the mass percentage of the graphite is 2wt percent
Example 1
(1) Will V2O5And Nb2O5Mixing at a molar ratio of 1:1, grinding for 12 hr, annealing at 500 deg.C to obtain VNbO with particle diameter of 5 μm5；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 10 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 50nm is added2VNbO having a particle diameter of 5 μm5Mixing with graphite powder with the particle size of 10nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 1800rpm, setting the interval time between positive and negative rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 30 hours, closing the grinder, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
VNbO in the prepared composite hydrogen storage material5The content of the graphite is 10 wt%, and the content of the graphite is 2 wt%.
Example 2
(1) Will V2O5And Nb2O5Mixed in a molar ratio of 1:1 and ground for 12 hoursThen, VNbO having a particle size of 5 μm was synthesized by annealing at 500 ℃ to5；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 10 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 50nm is added2VNbO having a particle diameter of 5 μm5Mixing with graphite powder with the particle size of 10nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 1800rpm, setting the interval time between positive and negative rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 30 hours, closing the grinder, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
VNbO in the prepared composite hydrogen storage material515 wt% of graphite and 2 wt% of graphite.
Example 3
(1) Mixing CuO and CoO at a molar ratio of 1:1, grinding for 12 hr, annealing at 500 deg.C to obtain CuCo with particle size of 10 μm2O4；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 15 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 50nm is added2CuCo with particle size of 10 mu m2O4Mixing with graphite powder with the particle size of 15nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 2500rpm, setting the forward and reverse rotation operation interval time to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 20 hours, closing the grinder, 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 material2O4The content of the graphite is 10 wt%, and the content of the graphite is 2 wt%.
Example 4
(1) MnO and Fe2O3Mixing at a molar ratio of 1:1, grinding for 12 hr, annealing at 500 deg.C to obtain MnFe powder with particle size of 25 μm2O4；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 20 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 60nm is added2MnFe having a particle size of 25 μm2O4Mixing with graphite powder with the particle size of 20nm, adding the mixture into a grinding tank of an electromagnetic grinding machine, wherein a magnetic grinding needle is arranged in the grinding tank, the mass ratio of the mixture to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 3000rpm, setting the interval time between positive and negative rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 15 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.
MnFe in the prepared composite hydrogen storage material2O4The mass percentage of the graphite is 12 wt%, and the mass percentage of the graphite is 2 wt%.
Example 5
(1) CoO and NiO are mixed according to the molar ratio of 1:1, ground for 12 hours, annealed and synthesized at 500 ℃ and Co with the grain diameter of 45 mu m2NiO；
(2) Grinding the scaly graphite in an electromagnetic grinding machine and then drying to prepare graphite powder with the particle size of 30 nm;
(3) under the protective atmosphere of inert gas argon, MgH with the particle size of 100nm is added2Co having a particle diameter of 45 μm2Mixing NiO and graphite powder with the particle size of 30nm, adding the mixed material into a grinding tank of an electromagnetic grinding machine, arranging a magnetic grinding needle in the grinding tank, wherein the mass ratio of the mixed material to the magnetic grinding needle is 1:20, and sealing a grinding cavity;
(4) setting parameters of a grinding machine, setting the grinding frequency to be 3600rpm, setting the interval time of forward and reverse rotation to be 0.5h, then introducing hydrogen with the pressure of 10MPa, starting the electromagnetic grinding machine, driving the magnetic grinding needle to do high-speed 360-degree rotary motion after electrifying, and performing high-speed collision grinding with materials;
(5) and after grinding for 3 hours, closing the grinder, separating substances in the grinding cavity by using a magnetic object, and extracting a product to obtain the composite hydrogen storage material.
Co in the prepared composite hydrogen storage material2The mass percent of NiO is 15 wt%, and the mass percent of graphite is 3 wt%.
Performance testing
The hydrogen release amount of the composite hydrogen storage material of comparative example 1 without the addition of the ternary metal oxide and the composite hydrogen storage materials of comparative example 2, example 1 and example 2 with the addition of the ternary metal oxide are tested at different temperatures, and the test results are shown in Table 1, and the hydrogen release amount is measured at 160 ℃ and 20bar H2The hydrogen storage amount was measured, and the measurement results are shown in Table 2.
TABLE 1 hydrogen evolution at different temperatures for comparative examples 1-2 and examples 1-2 composite hydrogen storage materials
Figure BDA0002531027390000051
Figure BDA0002531027390000061
TABLE 2 hydrogen storage capacity of comparative examples 1-2 and examples 1-2 composite hydrogen storage materials
Figure BDA0002531027390000062
The composite hydrogen storage material prepared in example 2 was subjected to hydrogen storage/release amount tests at 300 ℃ and 275 ℃ with cycling 10 to 50 times, and the test results are shown in table 3.
TABLE 3 composite Hydrogen storage Material prepared in example 2 with 10-50 cycles of hydrogen storage/desorption
Number of cycles 10 20 30 40 50
Hydrogen storage capacity (wt.%) at 300 deg.C 6 5.8 5.7 5.8 5.8
Hydrogen evolution at 300 ℃ (wt.%) 5.7 5.6 4.9 5.1 5.5
Hydrogen storage at 275 deg.C (wt.%) 5.2 5.4 5.3 5.2 5.1
Hydrogen evolution (wt.%) at 275 deg.C 5.2 5.2 4.9 5.1 5.0
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 (10)

1. MgH2-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the composite hydrogen storage material is MgH2Is prepared by mixing ternary metal oxide and graphite as base material.
2. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the ternary metal oxide is VNbO5、CuCo2O4，MnFe2O4Or Co2NiO, and the NiO is one of the NiO.
3. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the MgH2Has a particle diameter of 50-100 nm.
4. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the mass percentage of the ternary metal oxide in the composite hydrogen storage material is 10-15 wt%.
5. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the particle size of the ternary metal oxide is 5-50 μm.
6. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the particle size of the graphite is 10-30 nm.
7. The MgH of claim 12-ternary metal oxide-graphite composite hydrogen storage material, characterized in that: the mass percentage of the graphite in the composite hydrogen storage material is 2-3 wt%.
8. MgH according to claims 1-72The preparation method of the ternary metal oxide-graphite composite hydrogen storage material is characterized by comprising the following steps: the method comprises the following steps:
(1) under the protective atmosphere of inert gas, MgH2Adding the mixed material of the ternary metal oxide and the graphite powder into a grinding tank of an electromagnetic grinding machine, 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 the electromagnetic grinding machine, and carrying out high-speed collision grinding;
(3) and after the grinding is finished, separating out the magnetic grinding needle to obtain the composite hydrogen storage material.
9. The MgH of claim 82The preparation method of the ternary metal oxide-graphite composite hydrogen storage material is characterized by comprising the following steps: the mass ratio of the mixed material to the magnetic grinding needle in the step (1) is 1: 10-50.
10. The MgH of claim 82The preparation method of the ternary metal oxide-graphite composite hydrogen storage material is characterized by comprising the following steps: in the step (2), the grinding frequency of the electromagnetic grinding machine is 1800 plus 3600rpm, the interval time of forward and reverse rotation is 0.5h, and the total grinding time is 0.5-30 h.
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