CN114156515A - Preparation method of vanadyl sulfate electrolyte prepared from vanadium slag - Google Patents
Preparation method of vanadyl sulfate electrolyte prepared from vanadium slag Download PDFInfo
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- CN114156515A CN114156515A CN202111309136.7A CN202111309136A CN114156515A CN 114156515 A CN114156515 A CN 114156515A CN 202111309136 A CN202111309136 A CN 202111309136A CN 114156515 A CN114156515 A CN 114156515A
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- Prior art keywords
- vanadium
- vanadyl sulfate
- leaching
- sulfate electrolyte
- sulfuric acid
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 62
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002893 slag Substances 0.000 title claims abstract description 39
- 239000003792 electrolyte Substances 0.000 title claims abstract description 33
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 229940041260 vanadyl sulfate Drugs 0.000 title claims abstract description 30
- 229910000352 vanadyl sulfate Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000002386 leaching Methods 0.000 claims abstract description 42
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 28
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000012074 organic phase Substances 0.000 claims abstract description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- -1 vanadium inorganic compound Chemical class 0.000 abstract description 2
- 239000013543 active substance Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/186—Regeneration by electrochemical means by electrolytic decomposition of the electrolytic solution or the formed water product
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
- Y02E60/50—Fuel cells
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the field of vanadium batteries, in particular to a method for preparing vanadyl sulfate electrolyte prepared from vanadium slag. Stirring and mixing vanadium slag and concentrated sulfuric acid to obtain leaching slag and leaching liquid, filtering the leaching slag for multiple times to obtain the leaching liquid, adding activated carbon into the leaching liquid, adsorbing for multiple times, filtering to obtain high-purity leaching liquid, extracting vanadium element by using P204, enabling the vanadium element to enter an organic phase, back-extracting the organic phase by using dilute sulfuric acid, enabling vanadium to enter an extraction liquid, adding ammonium chloride to obtain ammonium metavanadate, and filtering for multiple times to obtain high-purity ammonium metavanadate, so that vanadium pentoxide with high purity is obtained, and the quality of vanadyl sulfate electrolyte is improved. The invention provides a preparation method of vanadyl sulfate electrolyte prepared from vanadium slag, which is characterized in that vanadium slag is used for extracting vanadium element into an organic phase, and then the vanadium element is separated from other elements in the vanadium slag through back extraction of sulfuric acid to generate a vanadium inorganic compound, generate ammonium metavanadate and prepare vanadium pentoxide so as to prepare vanadyl sulfate electrolyte.
Description
Technical Field
The invention relates to the field of vanadium batteries, in particular to a method for preparing vanadyl sulfate electrolyte prepared from vanadium slag.
Background
With the development and application of renewable energy, the large-scale high-efficiency energy storage technology becomes a hotspot for research and development in the energy field, and the all-vanadium redox flow energy storage system has huge application prospects in the fields of solar energy, wind energy storage and grid connection, power grid peak regulation, remote power supply systems, uninterruptible power supplies and the like due to the advantages of no pollution, long service life, high energy efficiency, simple maintenance and the like, although the research of foreign vanadium batteries has entered into a practical stage, the stability of high-concentration vanadium electrolyte, the electrode material, the electrochemical activity thereof and the optimization of system structure are one of main factors restricting the commercial operation development of the vanadium electrolyte, wherein the preparation of the vanadium electrolyte is the core of the all-vanadium redox flow energy storage system, the vanadium electrolyte special for the vanadium battery is an active substance for starting electrochemical reaction in the vanadium battery, and the electrolyte requires higher stability and conductivity, the battery energy is stored in the form of electrolyte, the electrolyte used in the preparation method of vanadyl sulfate electrolyte in the prior art is prepared by directly dissolving vanadyl sulfate in sulfuric acid, but vanadyl sulfate is high in price and preparation difficulty, and impurities are more during preparation, so that the using effect of the electrolyte is poor.
Disclosure of Invention
The invention provides a preparation method of vanadyl sulfate electrolyte prepared from vanadium slag, which is characterized in that vanadium slag is used for extracting vanadium element into an organic phase, and then back extraction is carried out by sulfuric acid to separate the vanadium element from other elements in the vanadium slag, so as to generate a high-concentration vanadium inorganic compound, generate ammonium metavanadate and prepare vanadium pentoxide by using the ammonium metavanadate.
The technical scheme adopted by the invention is a method for preparing vanadyl sulfate electrolyte prepared from vanadium slag, which is characterized by comprising the following steps of:
the method comprises the following steps: stirring and mixing the vanadium slag and concentrated sulfuric acid;
step two: stirring the mixture for 3-5 days under the condition of heat preservation to obtain ore pulp;
step three: standing the ore pulp obtained in the second step to obtain leaching residues and leaching liquid, filtering the leaching residues for multiple times to obtain the leaching liquid, adding active carbon into the leaching liquid, adsorbing for multiple times, and filtering to obtain high-purity leaching liquid;
step four: mixing the high-purity leachate with vanadium slag, stirring and leaching, and separating out crude leachate and leaching slag;
step five: extracting the rough leachate, adding an extracting agent and a diluent, shaking for 10 minutes, and allowing vanadium to enter an organic phase;
step six: carrying out back extraction on the organic phase by using 3 mol/L dilute sulfuric acid, adding vanadium into an extract liquor, and adding ammonium chloride into the extract liquor to obtain ammonium metavanadate;
step seven: dissolving ammonium metavanadate for many times, filtering and refining to obtain high-purity ammonium metavanadate;
step eight: washing high-purity ammonium metavanadate with water, and dehydrating to obtain vanadium pentoxide powder;
step nine: mixing vanadium pentoxide powder with dilute sulfuric acid to obtain vanadyl sulfate electrolyte.
In the fifth step, the extractant is P204.
The dilute sulfuric acid concentration is 3 mol per liter.
The solvent used in the preparation process is deionized water.
And in the fifth step, the diluent is sulfonated kerosene.
The refining process in the seventh step specifically comprises the following steps: adding the rough ammonium metavanadate into deionized water, dissolving at high temperature, adding active carbon, adsorbing impurities for three times, and filtering to obtain high-purity ammonium metavanadate.
In the step nine, the mixing proportion of the vanadium pentoxide powder and the dilute sulfuric acid is that 3 mol per liter of dilute sulfuric acid is added into 1 mol per liter of vanadyl sulfate solution.
The invention has the beneficial effects that:
the invention provides a method for preparing vanadyl sulfate electrolyte by using vanadium slag, which comprises the steps of stirring and mixing vanadium slag and concentrated sulfuric acid to obtain leaching slag and leaching solution, filtering the leaching slag for multiple times to obtain the leaching solution, adding activated carbon into the leaching solution, adsorbing for multiple times, filtering to obtain high-purity leaching solution, extracting vanadium element by using P204, enabling the vanadium element to enter an organic phase, carrying out back extraction on the organic phase by using dilute sulfuric acid, adding vanadium into the extraction solution, adding ammonium chloride to obtain ammonium metavanadate, and filtering for multiple times to obtain high-purity ammonium metavanadate, so that vanadium pentoxide with higher purity is obtained, and the quality of the vanadyl sulfate electrolyte is improved.
Detailed Description
Example 1:
the method aims to solve the problems that the existing product has simple and rough process and high cleaning cost, the anion active agent residue cannot be thoroughly cleaned due to slight negligence of cleaning times or non-standard cleaning, the human body cannot be irreversibly damaged, the anion active agent residue generated in the cleaning process is irreversible to the natural damage, the anion active agent residue cannot be treated by natural decomposition or biodegradation, the only decomposition method is chemical decomposition and the like.
The invention provides a method for preparing vanadyl sulfate electrolyte prepared from vanadium slag, which is characterized by comprising the following steps of:
the method comprises the following steps: stirring and mixing the vanadium slag and concentrated sulfuric acid;
step two: stirring the mixture for 3-5 days under the condition of heat preservation to obtain ore pulp;
step three: standing the ore pulp obtained in the second step to obtain leaching residues and leaching liquid, filtering the leaching residues for multiple times to obtain the leaching liquid, adding active carbon into the leaching liquid, adsorbing for multiple times, and filtering to obtain high-purity leaching liquid;
step four: mixing the high-purity leachate with vanadium slag, stirring and leaching, and separating out crude leachate and leaching slag;
step five: extracting the rough leachate, adding an extracting agent and a diluent, shaking for 10 minutes, and allowing vanadium to enter an organic phase;
step six: carrying out back extraction on the organic phase by using 3 mol/L dilute sulfuric acid, adding vanadium into an extract liquor, and adding ammonium chloride into the extract liquor to obtain ammonium metavanadate;
step seven: dissolving ammonium metavanadate for many times, filtering and refining to obtain high-purity ammonium metavanadate;
step eight: washing high-purity ammonium metavanadate with water, and dehydrating to obtain vanadium pentoxide powder;
step nine: mixing vanadium pentoxide powder with dilute sulfuric acid to obtain vanadyl sulfate electrolyte.
In the fifth step, the extractant is P204.
The dilute sulfuric acid concentration is 3 mol per liter.
The solvent used in the preparation process is deionized water.
And in the fifth step, the diluent is sulfonated kerosene.
The refining process in the seventh step specifically comprises the following steps: adding the rough ammonium metavanadate into deionized water, dissolving at high temperature, adding active carbon, adsorbing impurities for three times, and filtering to obtain high-purity ammonium metavanadate.
In the step nine, the mixing proportion of the vanadium pentoxide powder and the dilute sulfuric acid is that 3 mol per liter of dilute sulfuric acid is added into 1 mol per liter of vanadyl sulfate solution.
According to the method for preparing the vanadyl sulfate electrolyte by using the vanadium slag, the vanadium slag and concentrated sulfuric acid are stirred and mixed to obtain leaching slag and leaching solution, the leaching slag is filtered for multiple times to obtain the leaching solution, activated carbon is added into the leaching solution for multiple times of adsorption and filtration to obtain high-purity leaching solution, P204 is used for extracting vanadium element to enable the vanadium element to enter an organic phase, then the organic phase is subjected to back extraction by using dilute sulfuric acid, vanadium enters an extraction solution, ammonium chloride is added to obtain ammonium metavanadate, and high-purity ammonium metavanadate is obtained after multiple times of filtration to obtain high-purity vanadium pentoxide, so that the quality of the vanadyl sulfate electrolyte is improved.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A method for preparing vanadyl sulfate electrolyte prepared from vanadium slag is characterized by comprising the following steps:
the method comprises the following steps: stirring and mixing the vanadium slag and concentrated sulfuric acid;
step two: stirring the mixture for 3-5 days under the condition of heat preservation to obtain ore pulp;
step three: standing the ore pulp obtained in the second step to obtain leaching residues and leaching liquid, filtering the leaching residues for multiple times to obtain the leaching liquid, adding active carbon into the leaching liquid, adsorbing for multiple times, and filtering to obtain high-purity leaching liquid;
step four: mixing high-purity vanadium slag leachate, stirring and leaching, and separating out crude leachate and leaching slag;
step five: extracting the rough leachate, adding an extracting agent and a diluent, shaking for 10 minutes, and allowing vanadium to enter an organic phase;
step six: carrying out back extraction on the organic phase by using 3 mol/L dilute sulfuric acid, adding vanadium into an extract liquor, and adding ammonium chloride into the extract liquor to obtain ammonium metavanadate;
step seven: dissolving ammonium metavanadate for many times, filtering and refining to obtain high-purity ammonium metavanadate;
step eight: washing high-purity ammonium metavanadate with water, and dehydrating to obtain vanadium pentoxide powder;
step nine: mixing vanadium pentoxide powder with dilute sulfuric acid to obtain vanadyl sulfate electrolyte.
2. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 1, is characterized in that: in the fifth step, the extractant is P204.
3. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 1, is characterized in that: the dilute sulfuric acid concentration is 3 mol per liter.
4. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 1, is characterized in that: the solvent used in the preparation process is deionized water.
5. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 4, wherein the method comprises the following steps: and in the fifth step, the diluent is sulfonated kerosene.
6. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 5, wherein the method comprises the following steps: the refining process in the seventh step specifically comprises the following steps: adding the rough ammonium metavanadate into deionized water, dissolving at high temperature, adding active carbon, adsorbing impurities for three times, and filtering to obtain high-purity ammonium metavanadate.
7. The method for preparing the vanadyl sulfate electrolyte prepared from the vanadium slag according to claim 1, is characterized in that: in the step nine, the mixing proportion of the vanadium pentoxide powder and the dilute sulfuric acid is that 3 mol per liter of dilute sulfuric acid is added into 1 mol per liter of vanadyl sulfate solution.
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CN202111309136.7A CN114156515A (en) | 2021-11-06 | 2021-11-06 | Preparation method of vanadyl sulfate electrolyte prepared from vanadium slag |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2024119104A3 (en) * | 2022-12-01 | 2024-08-02 | U.S. Vanadium, Llc | Dehydrated electrolyte for a vanadium redox flow battery |
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CN101585553A (en) * | 2009-07-06 | 2009-11-25 | 云南俊驰环保科技有限公司 | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium |
CN103401010A (en) * | 2013-08-13 | 2013-11-20 | 湖南省银峰新能源有限公司 | Method for preparing electrolytes of all-vanadium flow battery |
CN103505903A (en) * | 2012-06-25 | 2014-01-15 | 中国人民解放军63971部队 | Two-stage extraction preparation method for high-purity vanadyl sulfate solution |
CN104409760A (en) * | 2014-10-21 | 2015-03-11 | 国网电力科学研究院武汉南瑞有限责任公司 | Method for preparing electrolyte solution for vanadium battery through dissolving vanadium oxide |
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KR20180103340A (en) * | 2017-03-09 | 2018-09-19 | 한국과학기술연구원 | Anion exchange membrane for vanadium redox flow battery and vanadium redox flow battery comprising thereof |
-
2021
- 2021-11-06 CN CN202111309136.7A patent/CN114156515A/en active Pending
Patent Citations (6)
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CN101585553A (en) * | 2009-07-06 | 2009-11-25 | 云南俊驰环保科技有限公司 | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium |
CN103505903A (en) * | 2012-06-25 | 2014-01-15 | 中国人民解放军63971部队 | Two-stage extraction preparation method for high-purity vanadyl sulfate solution |
CN103401010A (en) * | 2013-08-13 | 2013-11-20 | 湖南省银峰新能源有限公司 | Method for preparing electrolytes of all-vanadium flow battery |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2024119104A3 (en) * | 2022-12-01 | 2024-08-02 | U.S. Vanadium, Llc | Dehydrated electrolyte for a vanadium redox flow battery |
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