CN115159459B - V-based 4 Nb 18 O 55 Catalytic lifting of MgH 2 Method for hydrogen storage performance - Google Patents
V-based 4 Nb 18 O 55 Catalytic lifting of MgH 2 Method for hydrogen storage performance Download PDFInfo
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- CN115159459B CN115159459B CN202210776033.XA CN202210776033A CN115159459B CN 115159459 B CN115159459 B CN 115159459B CN 202210776033 A CN202210776033 A CN 202210776033A CN 115159459 B CN115159459 B CN 115159459B
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 60
- 239000001257 hydrogen Substances 0.000 title claims abstract description 60
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000003860 storage Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 32
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000003795 desorption Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000004005 microsphere Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000012265 solid product Substances 0.000 claims description 2
- 238000004729 solvothermal method Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 7
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 150000002431 hydrogen Chemical class 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 18
- 230000002441 reversible effect Effects 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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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
- 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
- C01B6/04—Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B01J35/51—
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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 material preparation, and particularly relates to a V-based material 4 Nb 18 O 55 Catalytic lifting of MgH 2 A method for hydrogen storage performance. The method comprises the following steps: first, preparing V by combining solvothermal treatment and heat treatment in two steps 4 Nb 18 O 55 A catalyst; the prepared catalyst is reacted with MgH 2 Performing hydrogenation ball milling and mixing to prepare a composite material; the composite material is subjected to hydrogen absorption and desorption test, so that V can be shown 4 Nb 18 O 55 High performance catalysis. The invention adopts simple process to prepare high-performance V 4 Nb 18 O 55 Catalyst and use for catalyzing MgH 2 Storing hydrogen, and the prepared composite material has the temperature of absorbing and releasing hydrogen relative to pure MgH 2 Greatly reduced and complete rehydrogenation at room temperature can be achieved.
Description
Technical Field
The invention belongs to the technical field of material preparation, and in particular relates to a method for improving MgH 2 A method for hydrogen storage performance.
Background
The energy problem is a big problem faced by the current social development, and the problems of limited reserves of fossil energy and environmental pollution are increasingly remarkable in restriction of economic growth and improvement of people's life. As a clean energy source, hydrogen energy has various advantages such as cleanliness, no pollution, reproducibility, and high energy density, and is considered as one of the best energy sources for future low-carbon energy systems. However, commercialization of hydrogen energy is limited by its lack of safe and efficient efficiencyAnd high mass and volumetric hydrogen storage densities are required, fortunately solid hydrogen storage materials have high hydrogen storage capacities and lower requirements for hydrogen storage vessels relative to liquid or gaseous hydrogen storage modes. Magnesium dihydroxide (MgH) as one of the most studied solid hydrogen storage materials 2 ) It has the advantages of high quality hydrogen storage capacity (7.6 wt%), good reversibility, rich Mg content, etc., but at the same time it also has high thermodynamic stability and kinetic barrier, resulting in its reversible hydrogen storage temperature typically being up to 400 ℃ or higher. Research shows that the dynamic barrier can be effectively reduced by doping transition metal, thereby reducing MgH 2 Wherein Nb is the reversible hydrogen absorption and desorption temperature of 2 O 5 Is a representative catalyst. At present for Nb 2 O 5 The catalyst studies are mainly as follows: modification of Nb with N by ball milling 2 O 5 Or MgH can be effectively prepared by preparing composite metal oxide to realize multi-element multivalent catalytic environment and the like 2 But still the actual operating temperature exceeds 250 c.
Disclosure of Invention
The invention aims to provide the MgH for improving the MgH with simple process and excellent effect 2 A method for hydrogen storage performance.
The invention provides a lifting MgH 2 The hydrogen storage performance is obtained by using V modified Nb-based catalyst 4 Nb 18 O 55 Then with MgH 2 The composite material prepared by doping has excellent hydrogen storage performance as a hydrogen storage material, and meets the requirements of production and scientific research.
The invention provides a lifting MgH 2 The hydrogen storage performance method comprises the following specific steps:
(1) Preparation of porous V 4 Nb 18 O 55 Microsphere:
weighing a Nb source and a V source with the mol ratio of 9:2, wherein the Nb source is NbCl 5 The V source is NH 4 VO 3 Dissolving the two in 50-70 ml of isopropanol, stirring after ultrasonic treatment, and transferring to a non-polytetrafluoroethylene liner after all the two are dissolvedCarrying out solvothermal reaction for 12-36 h in a stainless steel reaction kettle at 180-220 ℃ in an oven; washing the product for more than three times by using absolute ethyl alcohol after the reaction is finished, and drying the solid product separated by centrifugation in a vacuum oven at the temperature of 50-90 ℃; calcining the product in air at 550-700 ℃ for 2-5 h after complete drying to obtain porous V 4 Nb 18 O 55 A microsphere;
(2) The prepared V is subjected to anhydrous and anaerobic atmosphere 4 Nb 18 O 55 With MgH 2 Mixing and then placing the mixture into a ball milling tank with a valve for ball milling; wherein V is 4 Nb 18 O 55 Is MgH 2 1-25% of the weight, wherein the ball-to-material ratio is set to be (80-120): 1; then charging hydrogen pressure not lower than 40 atm, ball milling for 12-24 hours at a rotating speed of 300-500 rpm, and obtaining a composite material; the composite material has excellent hydrogen storage performance.
Transferring the composite material into PCT, and testing the temperature rise program to be 2-15 ℃/min, and releasing all hydrogen at 220-240 ℃ for 10-15 min to obtain about 5.9-6.1 wt.% hydrogen. After the composite material is subjected to hydrogen desorption, hydrogen desorption test is carried out at room temperature, the hydrogen desorption background pressure is set to be 30-50 atm, and more than 90% of the composite material can be hydrogenated within 8-16 h at room temperature after dehydrogenation.
The invention has the following remarkable advantages:
(1) The process is simple and the synthesis is convenient;
(2) The process has low requirements on equipment and is easy to realize;
(3) The obtained composite material has excellent hydrogen absorption and desorption performance, higher reversible hydrogen capacity and commercial application prospect.
Drawings
FIG. 1 is a porous V 4 Nb 18 O 55 XRD spectrum of the microspheres.
FIG. 2 is a porous V 4 Nb 18 O 55 SEM image of microspheres.
FIG. 3 is a non-isothermal hydrogen release profile of a composite material.
Fig. 4 is a graph of the room temperature hydrogen absorption curve of the composite.
Fig. 5 is an isothermal hydrogen release profile of the composite at different temperatures.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1 Hydrogen evolution test of composite materials
Weigh 30 mg V 4 Nb 18 O 55 MgH of 270 mg 2 Then put into a ball milling tank, then add about 36 g stainless steel balls for ball milling and mixing, the ball milling time is 12 h, and hydrogen pressure of 45 atm is filled into the ball milling tank. After ball milling is finished, a ball milling tank is opened in a glove box, then 25 mg composite material powder is scraped and put into a PCT test sample chamber, after loading is finished, vacuumizing treatment is carried out, testing is started when the pressure is lower than 0.001 Mpa, the temperature raising program is set to be from 25 ℃, the temperature is raised to 300 ℃ through 2 ℃/min, and pure MgH is obtained 2 The sample test mode of (2) is consistent, the temperature rise cut-off temperature is set to 400 ℃, and the hydrogen release curves of the two are shown in figure 3.
Under the same test conditions, the initial hydrogen release temperature of the composite material added with the catalyst is reduced to 165 ℃ relative to pure MgH 2 The hydrogen release temperature is reduced by more than 120 ℃, the peak temperature of the composite material is 220 ℃, and 97% of hydrogen in the system is released before 240 ℃.
Example 2 hydrogenation test of composite materials
Weigh 30 mg V 4 Nb 18 O 55 MgH of 270 mg 2 Then put into a ball milling tank, then add about 36 g stainless steel balls for ball milling and mixing, the ball milling time is 12 h, and hydrogen pressure of 45 atm is filled into the ball milling tank. After ball milling is finished, a ball milling tank is opened, a sample is scraped, during hydrogenation test, a composite material of about 100 mg is weighed in a glove box, after rapid temperature rise is carried out until hydrogen release is complete, the system is vacuumized again, after the temperature is reduced to room temperature, the test is started when the pressure is lower than 0.001 Mpa, the hydrogenation test is started, the hydrogen background pressure is set to 50 atm, the hydrogenation time is set to 12 h, and the hydrogenation curve of the composite material is shown in fig. 4. The sample after hydrogen release can absorb 5.64 and wt percent of hydrogen at room temperature, which is equivalent to 94 percent of the hydrogen storage amount of the system.
Example 3 isothermal hydrogen evolution test of composite materials
Weigh 30 mg V 4 Nb 18 O 55 MgH of 270 mg 2 Then put into a ball milling tank, then add about 36 g stainless steel balls for ball milling and mixing, the ball milling time is 12 h, and hydrogen pressure of 45 atm is filled into the ball milling tank. After ball milling is finished, a ball milling tank is opened, a sample is scraped, when isothermal hydrogen discharge test is carried out, a composite material of about 25 mg is weighed in a glove box, the composite material is filled into a reactor, when the pressure is lower than 0.001 Mpa, the test is started, the system is rapidly heated to the temperature to be tested (180-260 ℃) and then is subjected to heat preservation, as shown in FIG. 5, the isothermal hydrogen discharge test of the composite material is carried out, the sample can realize complete hydrogen discharge within 5 min at 260 ℃, and 1.2,3.5 and 5.2 wt% of hydrogen can be released within 30 min at the temperature as low as 180, 200 and 220 ℃.
Reference to the literature
[1] K. F. Aguey-Zinsou, J. R. Ares-Fernandez, Energy Environ. Sci.2010, 3, 526.
[2] Z. Q. Lan, H. Fu, R. L. Zhao, H. Z. Liu, W. Z. Zhou, H. Ning, J. Guo, Chem. Eng. J.2022, 431, 133985.
[3] K. Wang, X. Zhang, Z. Ren, X. Zhang, J. Hu, M. Gao, H. Pan, Y. Liu, Energy Stor. Mater.2019, 23, 79.
[4] K. C. Xian, M. H. Wu, M. X. Gao, S. Wang, Z. L. Li, P. Y. Gao, Z. H. Yao, Y. F. Liu, W. P. Sun, H. G. Pan, Small. 2022, 2107013.
[5] L. Zhang, K. Wang, Y. Liu, X. Zhang, J. Hu, M. Gao, H. Pan, Nano Res.2020, 14, 148。
Claims (2)
1. V-based 4 Nb 18 O 55 Catalytic lifting of MgH 2 The method for storing hydrogen is characterized by comprising the following specific steps:
(1) Preparation of porous V 4 Nb 18 O 55 Microsphere:
weighing a Nb source and a V source with the mol ratio of 9:2, wherein the Nb source is NbCl 5 The V source is NH 4 VO 3 Dissolving the two in 50-70 ml of isopropanol, stirring after ultrasonic treatment, transferring the solution to a stainless steel reaction kettle with a polytetrafluoroethylene lining after complete dissolution, and carrying out solvothermal reaction for 12-36 h at 180-220 ℃ in an oven; washing the product for more than three times by using absolute ethyl alcohol after the reaction is finished, and drying the solid product separated by centrifugation in a vacuum oven at the temperature of 50-90 ℃; calcining the product in air at 550-700 ℃ for 2-5 h after complete drying to obtain porous V 4 Nb 18 O 55 A microsphere;
(2) The prepared V is subjected to anhydrous and anaerobic atmosphere 4 Nb 18 O 55 With MgH 2 Mixing and then placing the mixture into a ball milling tank with a valve for ball milling; wherein V is 4 Nb 18 O 55 Is MgH 2 1-25% of the weight, wherein the ball-to-material ratio is set to be (80-120): 1; then charging hydrogen pressure not lower than 40 atm, ball milling for 12-24 hours at a rotating speed of 300-500 rpm, and obtaining a composite material; the composite material has excellent hydrogen storage performance, the composite material is transferred into PCT, the test heating program is 2-15 ℃/min, and the whole hydrogen of the composite material can be released within 10-15 min at 220-240 ℃;
after the composite material is subjected to hydrogen desorption, hydrogen desorption test is carried out at room temperature, the hydrogen desorption background pressure is set to be 30-50 atm, and after dehydrogenation, more than 90% of the composite material is hydrogenated within 8-16 h at room temperature.
2. A composite material prepared by the method of claim 1.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110116990A (en) * | 2019-04-10 | 2019-08-13 | 浙江大学 | A kind of in-situ preparation method of nanometer of magnesium hydride |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110116990A (en) * | 2019-04-10 | 2019-08-13 | 浙江大学 | A kind of in-situ preparation method of nanometer of magnesium hydride |
| WO2020207188A1 (en) * | 2019-04-10 | 2020-10-15 | 浙江大学 | Method for in-situ preparation of nano-magnesium hydride |
Non-Patent Citations (2)
| Title |
|---|
| "Rapid and durable electrochemical storage behavior enabled by V4Nb18O55 beaded nanofibers:a joint theoretical and experimental study";Shangshu Qian et al;《J. Mater. Chem. A》;第6卷;第17389–17400页 * |
| "Remarkable hydrogen storage properties of MgH2 doped with VNbO5";Antonio Valentoni et al;《Phys. Chem. Chem. Phys》;第20卷;第4100-4108页 * |
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