CN115321595B - Preparation method of hydrated vanadium pentoxide - Google Patents
Preparation method of hydrated vanadium pentoxide Download PDFInfo
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000003780 insertion Methods 0.000 abstract description 5
- 230000037431 insertion Effects 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 4
- 208000005374 Poisoning Diseases 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 231100000572 poisoning Toxicity 0.000 abstract description 3
- 230000000607 poisoning effect Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000008346 aqueous phase Substances 0.000 abstract description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract 1
- 229910001882 dioxygen Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000007774 positive electrode material Substances 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000006230 acetylene black Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical class [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
-
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of hydrated vanadium pentoxide. The invention uses VS 2 As raw material, dioxygen is used in an aqueous phase systemS replacement is carried out on water to synthesize vanadium pentoxide. Then and the rest is H 2 O 2 The reaction produces hydrated vanadium pentoxide. Compared with high temperature thermal oxidation, H is adopted 2 O 2 Oxidation is a green treatment. Simultaneously, the poisoning risk in the synthesis process is reduced; the product is hydrate, the interlayer spacing is larger, the insertion and the extraction of ions are facilitated, the volume expansion is relieved, and the electrochemical performance is good.
Description
Technical Field
The invention belongs to the field of battery materials, and particularly relates to a preparation method of hydrated vanadium pentoxide as a battery material.
Background
The zinc can be used as the anode of the water-based zinc ion battery, and has the advantages of low cost, rich resources, good safety, environmental protection, low oxidation-reduction potential and Zn 2+ Has two charges and high theoretical specific capacity of 820mAh g during electrochemical storage -1 Excellent electrochemical performance has recently received a great deal of attention. And the zinc ion battery has application potential in portable flexible electronic equipment, electric automobiles and other equipment. Finding a suitable cathode material is essential for excavating the great potential of zinc ion batteries.
Currently, vanadium-based, manganese-based, prussian blue analogues and the like are suitable as the positive electrode material of the zinc ion battery. Wherein V is 2 O 5 Vanadium has a tunable layered structure and vanadium has a number of redox states and has been widely studied. The hydrated vanadium pentoxide is formed by inserting water molecules between layers of the vanadium pentoxide, the inserted crystal water molecules can not only increase the interlayer distance, a wide interlayer channel is convenient for the insertion/extraction of ions and the alleviation of volume expansion caused in the circulation process, but also play a role in shielding charges, and meanwhile, the water molecules between layers can also serve as interlayer struts to increase the stability of the structure. The application of the hydrated vanadium pentoxide to the aqueous zinc ion battery can make the zinc ions overcome less obstruction in the process of insertion/extraction. The most similar to the experimental scheme at present is hydrated vanadium pentoxide obtained by treating commercial vanadium pentoxide, but the vanadium pentoxide has high toxicity and is at risk of poisoning in the experimental process.
Disclosure of Invention
The invention aims to provide a preparation method of hydrated vanadium pentoxide aiming at the defects of the prior art.
As one aspect of the invention, the invention is expressed in terms of VS 2 S substitution is carried out by hydrogen peroxide under a water phase system to synthesize vanadium pentoxide. Then and the rest is H 2 O 2 The reaction produces hydrated vanadium pentoxide. Compared with high temperature thermal oxidation, H is adopted 2 O 2 Oxidation is a green treatment. Simultaneously, the poisoning risk in the synthesis process is reduced; the product is hydrate, the interlayer spacing is larger, the insertion and the extraction of ions are facilitated, the volume expansion is relieved, and the electrochemical performance is good.
Specifically, the scheme is as follows: VS (virtual switch) 2 Adding the mixture into hydrogen peroxide solution, uniformly mixing, transferring the mixture into a polytetrafluoroethylene reaction kettle, and heating the mixture for 2 to 3 hours at the temperature of between 120 and 140 ℃ to obtain hydrated vanadium pentoxide; the molar amount of hydrogen peroxide is VS 2 25:1 to 35:1 of the molar amount of the catalyst. In the reaction process, since the bond energy of V-O is higher than V-S, hydrogen peroxide firstly replaces S atoms on the surface of molybdenum disulfide with O atoms, resulting in S-V 4+ Conversion to O-V 4+ The method comprises the steps of carrying out a first treatment on the surface of the As the reaction proceeds, O-V 4+ Further oxidation to O-V 5+ Generating V 2 O 5 。
Further, based on the aqueous phase synthesis system, V is formed by controlling the mass fraction of hydrogen peroxide to be 2-3 percent 2 O 5 Then and the rest is H 2 O 2 The hydrated vanadium pentoxide containing 1.6 crystal water is obtained through the reaction, so that the stability of a crystal structure can be ensured, and the smooth insertion/removal of ions can be ensured.
In certain embodiments of the present application, the VS 2 The preparation method comprises the following steps:
(1) 2mmol of amine metavanadate and 15mmol of thioacetamide were added to the aqueous ammonia solution in sequence and stirred for 1h.
(2) Transferring into a polytetrafluoroethylene reaction kettle, heating for 20 hours at 180 ℃ in an oven, cooling to room temperature, washing with deionized water and ethanol, and drying to obtain VS2.
The invention has the beneficial effects that:
1. the invention is realized by simple H 2 O 2 The hydrated vanadium pentoxide synthesized by the oxidation process has the advantages of low cost and high safety.
2. The hydrated vanadium pentoxide prepared by the method has larger specific surface area, provides a large number of reactive sites, and is beneficial to improving the electrochemical performance of the water-based zinc battery.
Drawings
Fig. 1 is an XRD test pattern of hydrated vanadium pentoxide.
FIG. 2 is a scanned image of hydrated vanadium pentoxide;
FIG. 3 is a high resolution image of hydrated vanadium pentoxide;
FIG. 4 is an EDS diagram of hydrated vanadium pentoxide;
fig. 5A is a magnification test chart, and fig. 5B is a cycle stability test chart.
Detailed Description
The invention is further described below with reference to examples. The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
1. 2ml of concentrated ammonia water was weighed and added to 30ml of deionized water and stirred. 2mmol of amine metavanadate and 15mmol of thioacetamide are weighed and added into the mixed solution in sequence, and the mixed solution is stirred for 1h.
2. Adding the solution into a 50ml polytetrafluoroethylene reaction kettle, heating for 20 hours at 180 ℃ in an oven, cooling to room temperature, washing with deionized water and ethanol, and drying to obtain VS 2 。
3. 1mmolVS to be obtained 2 Adding 40ml of H with mass fraction of 2.3% 2 O 2 Is added to the aqueous solution of (a). Stirring, adding into polytetrafluoroethylene reaction kettle, heating at 120deg.C for 2 hr to obtain hydrated vanadium pentoxide (XRD test shown in figure 1).
The obtained scanned image of the hydrated vanadium pentoxide is shown in fig. 2, and the scanned image shows that the morphology is lamellar, the specific surface area is large, and the contact area of the active material and the electrolyte is increased.
The high resolution image is shown in fig. 3, which shows the interplanar spacing corresponding to the (001) crystal plane of the hydrated vanadium pentoxide, further demonstrating the presence of the hydrated vanadium pentoxide.
EDX images of hydrated vanadium pentoxide are shown in fig. 4, from which a uniform distribution of V and O elements can be seen.
4. The prepared hydrated vanadium pentoxide: acetylene black: PVDF was prepared according to 7:2:1, preparing slurry, stirring for 12 hours, coating the slurry on carbon paper, and then drying in vacuum at 60 ℃ for 12 hours. The positive electrode material, the negative electrode material, the separator and the electrolyte are assembled into a button cell for electrochemical test, the multiplying power test and the cycling stability test are shown in fig. 5, and the initial specific capacity can reach 420mAh/g under the current density of 0.1A/g. Specific capacities of 320, 280, 240 and 200mAh/g can be achieved at current densities of 0.2, 0.5, 1 and 2A/g, a specific capacity of 320mAh/g can still be reached when returning to a current density of 0.1A/g, the material shows better multiplying power performance. The specific capacity of about 250mAh/g can be maintained after the cycle of 650 turns at the current density of 1A/g, the coulombic efficiency is close to 100%, and the cycle stability is excellent.
The third step was the same as the first two steps of Experimental example 1, and H was changed 2 O 2 Is used for the concentration of (a),
1mmolVS to be obtained 2 Adding into 40ml H with mass fraction of 1.5% and 6.5%, respectively 2 O 2 Is added to the aqueous solution of (a). Stirring, adding into a polytetrafluoroethylene reaction kettle, heating at 120 ℃ for 2 hours, respectively preparing electrode slices as comparison samples, assembling into a button cell, and performing electrochemical performance test. As can be seen from FIG. 5, H was used in a mass fraction of 1.5% and 6.5%, both in terms of rate performance and cycle stability 2 O 2 None of the treated samples had a mass fraction of 2.3% H 2 O 2 The treated samples exhibited good performance.
Example 2
Commercially available VS 2 1mmol, added to a solution containing 25mmol of H 2 O 2 Is contained in an aqueous solution (mass fraction of hydrogen peroxide: 2%). Stirring, adding into a polytetrafluoroethylene reaction kettle, heating at 140 ℃ for 2 hours to obtain hydrated vanadium pentoxide (with the same characteristic peak as PDF 40-1296), wherein the obtained hydrated vanadium pentoxide has flaky morphology and large specific surface area. The (001) crystal plane of the hydrated vanadium pentoxide can be seen to correspond to a 1.15nm interplanar distance through a high-resolution image, and the existence of the hydrated vanadium pentoxide is further proved.
The prepared hydrated vanadium pentoxide: acetylene black: PVDF was prepared according to 7:2:1, preparing slurry, stirring for 12 hours, coating the slurry on carbon paper, and then drying in vacuum at 60 ℃ for 12 hours. The positive electrode material, the negative electrode material, the diaphragm and the electrolyte are assembled into a button cell for electrochemical test, rate test and cycle stability test, and the initial specific capacity can reach 406mAh/g under the current density of 0.1A/g. Specific capacities of 311, 268, 224 and 196mAh/g can be achieved at current densities of 0.2, 0.5, 1 and 2A/g, the specific capacity of 309mAh/g can still be achieved when the current density is returned to 0.1A/g, and the better rate capability is shown. The specific capacity of about 219mAh/g can be maintained after the cycle of 650 turns at the current density of 1A/g, the coulombic efficiency is close to 100%, and the cycle stability is excellent.
Example 3
Commercially available VS 2 1mmol, added to a solution containing 25mmol of H 2 O 2 Is contained in the aqueous solution (3% by mass of hydrogen peroxide). Stirring, adding into a polytetrafluoroethylene reaction kettle, heating at 130 ℃ for 3 hours to obtain hydrated vanadium pentoxide (with the same characteristic peak as PDF 40-1296), wherein the obtained hydrated vanadium pentoxide has flaky morphology and large specific surface area. The (001) crystal plane of the hydrated vanadium pentoxide can be seen to correspond to a 1.15nm interplanar distance through a high-resolution image, and the existence of the hydrated vanadium pentoxide is further proved.
The prepared hydrated vanadium pentoxide: acetylene black: PVDF was prepared according to 7:2:1, preparing slurry, stirring for 12 hours, coating the slurry on carbon paper, and then drying in vacuum at 60 ℃ for 12 hours. The positive electrode material, the negative electrode material, the diaphragm and the electrolyte are assembled into a button cell for electrochemical test, rate test and cycle stability test, and the initial specific capacity can reach 416mAh/g under the current density of 0.1A/g. Specific capacities of 309, 254, 221, 189mAh/g can be achieved at current densities of 0.2, 0.5, 1, 2A/g, a specific capacity of 302mAh/g can still be reached when returning to a current density of 0.1A/g, the material shows better multiplying power performance. The specific capacity of about 212mAh/g can be maintained after 650 circles of circulation at the current density of 1A/g, and the coulombic efficiency is close to 100%.
Claims (1)
1. A method for preparing flake hydrated vanadium pentoxide, which is characterized by comprising the following steps: VS (virtual switch) 2 Adding the mixture into a hydrogen peroxide solution with the mass fraction of 2-3%, uniformly mixing, transferring the mixture into a polytetrafluoroethylene reaction kettle, and heating the mixture for 2-3 h at 120-140 ℃ to obtain hydrated vanadium pentoxide V 2 O 5 •1.6H 2 O; molar amount of hydrogen peroxide VS 2 The molar ratio of (2) is: 25: 1-30: 1, a step of; the VS 2 The preparation method comprises the following steps:
(1) Adding 2mmol of ammonium metavanadate and 15mmol of thioacetamide into an ammonia water solution in sequence, and stirring for 1h;
(2) Transferring into a polytetrafluoroethylene reaction kettle, heating for 20 hours at 180 ℃ in an oven, cooling to room temperature, washing with deionized water and ethanol, and drying to obtain VS 2 。
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Citations (6)
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|---|---|---|---|---|
| CN101700909A (en) * | 2009-11-25 | 2010-05-05 | 中国科学技术大学 | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method |
| CN102010004A (en) * | 2010-12-27 | 2011-04-13 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| US20150380732A1 (en) * | 2014-06-30 | 2015-12-31 | Indiana University Research And Technology Corporation | Novel vanadium oxide cathode material |
| CN109399712A (en) * | 2018-12-11 | 2019-03-01 | 联和能源投资控股有限公司 | A method of with hydrogen peroxide clean manufacturing high purity vanadic anhydride |
| CN109830666A (en) * | 2019-02-19 | 2019-05-31 | 珠海光宇电池有限公司 | A kind of vanadic anhydride positive electrode and preparation method and application |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700909A (en) * | 2009-11-25 | 2010-05-05 | 中国科学技术大学 | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method |
| CN102010004A (en) * | 2010-12-27 | 2011-04-13 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN103979608A (en) * | 2014-05-22 | 2014-08-13 | 吉林大学 | Method for preparing hollow core-shell vanadium pentoxide microsphere |
| US20150380732A1 (en) * | 2014-06-30 | 2015-12-31 | Indiana University Research And Technology Corporation | Novel vanadium oxide cathode material |
| CN109399712A (en) * | 2018-12-11 | 2019-03-01 | 联和能源投资控股有限公司 | A method of with hydrogen peroxide clean manufacturing high purity vanadic anhydride |
| CN109830666A (en) * | 2019-02-19 | 2019-05-31 | 珠海光宇电池有限公司 | A kind of vanadic anhydride positive electrode and preparation method and application |
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