CN103606694A - Preparation method for commercial vanadium battery electrolyte - Google Patents
Preparation method for commercial vanadium battery electrolyte Download PDFInfo
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- CN103606694A CN103606694A CN201310568546.2A CN201310568546A CN103606694A CN 103606694 A CN103606694 A CN 103606694A CN 201310568546 A CN201310568546 A CN 201310568546A CN 103606694 A CN103606694 A CN 103606694A
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- 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
- H01M8/20—Indirect fuel cells, e.g. fuel cells with redox couple being irreversible
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0002—Aqueous electrolytes
- H01M2300/0005—Acid electrolytes
- H01M2300/0011—Sulfuric acid-based
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a preparation method for commercial vanadium battery electrolyte. According to the preparation method, vanadium electrolyte is prepared by one step through a chemical method; the preparation method comprises the following steps: dissolving raw materials containing vanadium by using an alkali; adjusting a pH (Potential of Hydrogen) value by acid-alkali regulation; repeatedly precipitating the vanadium to remove impurity elements; then roasting to obtain an oxide of the vanadium; finally, dissolving the oxide of the vanadium by using concentrated sulfuric acid to obtain the vanadium electrolyte. With the adoption of the method, impurities including iron, chrome, silicon, manganese and the like can be removed effectively and a process flow is shortened; the vanadium yield is improved, the impurity content is reduced and the process flow is shortened; the product purity can also be improved. The preparation method for the commercial vanadium battery electrolyte has important meanings on production technology levels and market competitiveness of the vanadium electrolyte; the method has good economic benefits and social benefits.
Description
Technical field
The present invention relates to battery manufacture field, especially a kind of preparation method of electrolyte of vanadium redox battery.
Background technology
In existing liquid energy-storage technology, because having, the advantage such as the harmless deep discharge of adjustable, the large electric current of stored energy capacitance and power, long service life, Operation and Maintenance are simple, environmental protection receives much attention vanadium redox battery (abbreviation vanadium cell).Along with the development of correlation technique, it is practical that vanadium cell just progressively moves towards.Vanadium cell is mainly comprised of three parts: electrode material, battery diaphragm, electrolyte, so its development is also mainly subject to the restriction of these three aspects.Wherein electrolyte is the core of vanadium cell, and the quality of electrolyte has directly determined the energy storage capacity of vanadium cell, finds the suitable method of preparing electrolyte of vanadium redox battery to develop important in inhibiting to vanadium cell.
Although the technology of preparing of existing V electrolyte is varied, greatly mainly with V
2o
5or V
2o
3for raw material, adopt chemical method or electrochemical electrolysis method or both combinations to prepare V electrolyte.But it is slow and in reduction process, generally need to add the reducing agent of picture oxalic acid, sulphur and so on that chemical method is prepared the dissolution velocity of solid in the process of electrolyte, this class material is difficult for eradicating, have and remain on a small quantity in electrolyte, affect the useful life of chemical property and the battery of V electrolyte.Although and electrochemical process technique is simple, add additive that impurity ion content in electrolyte is increased in electrolytic process, cause the charge-discharge performance of electrolyte to reduce, meanwhile anode electrode is easily corroded, and increases preparation cost.
A kind of electrolytic preparation method of all-vanadium redox flow battery electrolyte is provided in patent 03159533.2, this method adopts and in the sulfuric acid solution of 1:1, adds successively vanadium trioxide, vanadic oxide to obtain vanadic sulfate solution, then adds the additives such as sodium sulphate, polyoxyethylene nonylphenol ether to carry out electrolysis and obtains the electrolyte of vanadium redox battery that trivalent vanadium and tetravalence vanadium respectively account for total vanadium 50%.
Patent 200710188392.9 provides a kind of preparation method of whole vanadium oxide reduction battery electrolytic solution, this method be after vanadium trioxide and the concentrated sulfuric acid are mixed by a certain percentage in electric tube furnace after 100-300 ℃ of calcining, be dissolved in dilute sulfuric acid, obtain the electrolyte of vanadium redox battery that trivalent vanadium and tetravalence vanadium respectively account for total vanadium 50%.
Patent 200510075608.1 provides a kind of full vanadium ion fluid cell electrolyte and preparation method, the qualified vanadium liquid of this method Yi Fan factory is raw material, with sulfuric acid, regulate and take liquid sulfur dioxide after pH value and reduce as reducing agent, then with sodium carbonate, regulate pH value to obtain vanadium dioxide precipitation, to precipitate in water-soluble, sulfuric acid, ethanolic solution, add additive, then electrolysis obtains the electrolyte of vanadium redox battery that trivalent vanadium and tetravalence vanadium respectively account for total vanadium 50%.
Some problems that the preparation method of above-mentioned V electrolyte also exists, are mainly manifested in:
(1) course of reaction adds additive: additive exerts an influence to the conductivity of solution and chemical property, can cause the hydration of going of vanadium oxygen hydrated ion in solution, is unfavorable for the dissolving of vanadium.
(2) reaction process is loaded down with trivial details: in course of reaction, the electrolyte of vanadium redox battery that respectively accounts for total vanadium 50% for obtaining trivalent vanadium and tetravalence vanadium needs electrolysis, has increased like this reaction process, has improved preparation cost.
(3) impurity content is high: the impurity contents such as V electrolyte institute iron content prepared by the experimental raw of using according to above-mentioned patent, chromium, silicon are higher, and the useful life important of these impurity to battery.
Therefore, how preparing to utilize and prepare qualified commercial V electrolyte compared with abbreviated system condition, is the difficult problem that existing commercial V electrolyte preparation method faces.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of electrolyte of vanadium redox battery, is a kind ofly to prepare that impurity content is low, the simple method for preparing vanadium cell electrolyte of technique.
For solving the problems of the technologies described above, the technical solution used in the present invention is: will containing vanadium raw materials with alkali heavy molten after, regulate the precipitation repeatedly of pH value, to remove impurity element wherein, then by roasting, obtain the oxide of vanadium, finally with the concentrated sulfuric acid by the oxide dissolution of vanadium, can obtain commercial V electrolyte.
Processing step of the present invention is:
(1) will with alkali lye, dissolve containing vanadium raw materials, regulate pH value 7.5～10, and add cleaner to carry out removal of impurities;
(2) filtrate after removal of impurities regulates pH value 1.5～3.0, and heating precipitation, obtains ammonium poly-vanadate/ammonium metavanadate;
(3) after ammonium poly-vanadate/ammonium metavanadate is dissolved with alkali, regulate pH value 1.5～3.0, precipitation again, obtains two heavy ammonium poly-vanadate/ammonium metavanadates;
(4) two heavy ammonium poly-vanadate/ammonium metavanadate roastings under reducibility gas, obtain the oxide of vanadium;
(5) oxide of vanadium mixes with the concentrated sulfuric acid, and stirring and dissolving can obtain V electrolyte.
Adopt after present technique, generally through twice precipitation, can obtain the vanadium product that qualified applicable V electrolyte is produced, if defective, can be through precipitation more frequently to reduce the impurity of vanadium product special use, obtain being applicable to the vanadium product that V electrolyte is produced, the precipitation process of precipitation process repeatedly can be greater than secondary.
Alkali in step of the present invention (1) is mixture, ammoniacal liquor, ammonia or the liquefied ammonia of NaOH, potassium hydroxide, NaOH and potassium hydroxide.
Cleaner in step of the present invention (1) is aluminium salt cleaner, and described aluminium salt comprises all aluminum soluble salts such as aluminum sulfate, aluminium chloride, sodium metaaluminate.
Reducibility gas in step of the present invention (4) is hydrogen or ammonia; Described sintering temperature is 500～800 ℃.
Of the present invention is the vanadium products such as ammonium metavanadate, ammonium poly-vanadate, vanadic oxide, vanadium trioxide and composition thereof containing vanadium raw materials.
The beneficial effect that adopts technique scheme to produce is:
(1) improve the purity of V electrolyte: because existing used for all-vanadium redox flow battery V electrolyte impurity is as higher in iron, silicon equal size, the useful life of greatly having limited battery; And adopt the present invention to fire highly purified barium oxide after purifying containing vanadium raw materials, can effectively remove the impurity such as iron, chromium, silicon, manganese.
(2) reduce production costs: the present invention adopts chemical method one step to prepare V electrolyte, has shortened technological process, can effectively reduce costs.
Therefore, adopt after the present invention, not only can improve vanadium yield, reduce impurity content, shortened process, thereby reduce the production cost of V electrolyte, improve product purity.To improving production technology level and the market competitiveness of V electrolyte, have great importance, the present invention has good economic benefit and social benefit.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
Embodiment 1: shown in Fig. 1, the preparation method's of this electrolyte of vanadium redox battery concrete technology is as described below.
Take ammonium poly-vanadate as raw material, add NaOH to be dissolved, filtrate is regulated to pH value 9, add aluminum sulfate to carry out removal of impurities.After removal of impurities, filtrate is regulated to pH value 1.5, add the heat sink ammonium poly-vanadate that obtains.Then by ammonium poly-vanadate with ammoniacal liquor heavy molten after, regulate the heavy ammonium poly-vanadate of pH value 2.0, after filtering, drying, in the situation that passing into ammonia, fire vanadium trioxide in 800 ℃, then by vanadium trioxide and concentrated sulfuric acid mix and blend, add high purity water to dissolve after filtration, obtain V electrolyte.Gained V electrolyte impurity content Al<17ppm, Na<15ppm, Fe<15ppm, Ca<15ppm, K<10ppm, Cr<5ppm, other impurity contents are all less than 2ppm.
Embodiment 2: the preparation method's of this electrolyte of vanadium redox battery concrete technology is as described below.
Take ammonium poly-vanadate as raw material, the in the situation that of heating, add ammoniacal liquor to be dissolved, filtrate is regulated to pH value 7.5, add sodium metaaluminate to carry out removal of impurities.After removal of impurities, filtrate is regulated to pH value 1.9, add the heat sink ammonium poly-vanadate that obtains.Then by ammonium poly-vanadate with ammoniacal liquor heavy molten after, regulate the heavy ammonium poly-vanadate of pH value 2.3, after filtering, drying, in the situation that passing into ammonia, fire vanadium trioxide in 800 ℃, then by vanadium trioxide and concentrated sulfuric acid mix and blend, add high purity water to dissolve after filtration, obtain V electrolyte.Gained V electrolyte impurity content Al<17ppm, Na<15ppm, Fe<15ppm, Ca<15ppm, K<10ppm, Cr<5ppm, other impurity contents are all less than 2ppm.
Embodiment 3: the preparation method's of this electrolyte of vanadium redox battery concrete technology is as described below.
Take vanadic oxide as raw material, add potassium hydroxide to be dissolved, filtrate is regulated to pH value 8-9, add aluminium chloride to carry out removal of impurities.After removal of impurities, filtrate is regulated to pH value 10, add the heat sink ammonium poly-vanadate that obtains.Then by ammonium poly-vanadate with potassium hydroxide heavy molten after, regulate the heavy ammonium poly-vanadate of pH value 2.3, after filtering, drying, in the situation that passing into ammonia, fire vanadium trioxide in 800 ℃, then by vanadium trioxide and concentrated sulfuric acid mix and blend, add high purity water to dissolve after filtration, obtain V electrolyte.Gained V electrolyte impurity content Al<17ppm, Na<16ppm, Fe<15ppm, Ca<25ppm, K<10ppm, Cr<5ppm, other impurity contents are all less than 2ppm.
Embodiment 4: take vanadic oxide as raw material, add NaOH to be dissolved, filtrate is regulated to pH value 10, add aluminum sulfate to carry out removal of impurities.After removal of impurities, filtrate is regulated to pH value 2.1, add the heat sink ammonium poly-vanadate that obtains.Then by ammonium poly-vanadate with ammoniacal liquor heavy molten after, regulate the heavy ammonium poly-vanadates of pH value 3, filter, at 500 ℃, fire vanadic oxide after oven dry, then by vanadic oxide vanadium and concentrated sulfuric acid mix and blend, add reducing agent to obtain tetravalence vanadium vanadic sulfate solution.Gained V electrolyte impurity content Si<10ppm, Cr<5ppm, Fe<25ppm, other impurity contents are all less than 10ppm.
Claims (8)
1. the preparation method of a commercial electrolyte of vanadium redox battery, it is characterized in that: will containing vanadium raw materials with alkali heavy molten after, regulate the precipitation repeatedly of pH value, to remove impurity element wherein, then by roasting, obtain the oxide of vanadium, finally with the concentrated sulfuric acid by the oxide dissolution of vanadium, can obtain commercial V electrolyte.
2. the preparation method of commercial electrolyte of vanadium redox battery according to claim 1, is characterized in that, its processing step is:
(1) will with alkali lye, dissolve containing vanadium raw materials, regulate pH value 7.5～10, and add cleaner to carry out removal of impurities;
(2) filtrate after removal of impurities regulates pH value 1.5～3.0, and heating precipitation, obtains ammonium poly-vanadate/ammonium metavanadate;
(3) after ammonium poly-vanadate/ammonium metavanadate is dissolved with alkali, regulate pH value 1.5～3.0, precipitation again, obtains two heavy ammonium poly-vanadate/ammonium metavanadates;
(4) two heavy ammonium poly-vanadate/ammonium metavanadate roastings under reducibility gas, obtain the oxide of vanadium;
(5) oxide of vanadium mixes with the concentrated sulfuric acid, and stirring and dissolving can obtain V electrolyte.
3. the preparation method of electrolyte of vanadium redox battery according to claim 2, is characterized in that: alkali used is mixture, ammoniacal liquor, ammonia or the liquefied ammonia etc. of NaOH, potassium hydroxide, NaOH and potassium hydroxide.
4. the preparation method of electrolyte of vanadium redox battery according to claim 2, is characterized in that the cleaner in step (1) is aluminium salt cleaner, comprises all aluminum soluble salts such as aluminum sulfate, aluminium chloride, sodium metaaluminate.
5. the preparation method of electrolyte of vanadium redox battery according to claim 2, is characterized in that the precipitation process of precipitation process repeatedly can be greater than secondary.
6. the preparation method of electrolyte of vanadium redox battery according to claim 2, is characterized in that: the reducibility gas in described step (4) is hydrogen or ammonia.
7. the preparation method of electrolyte of vanadium redox battery according to claim 2, is characterized in that: in described step (4), sintering temperature is 500～800 ℃.
8. according to the preparation method of the electrolyte of vanadium redox battery described in claim 1-2 any one, it is characterized in that: described is the vanadium products such as ammonium metavanadate, ammonium poly-vanadate, vanadic oxide, vanadium trioxide and composition thereof containing vanadium raw materials.
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Cited By (16)
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|---|---|---|---|---|
| CN104388683A (en) * | 2014-12-08 | 2015-03-04 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
| CN104538660A (en) * | 2014-12-25 | 2015-04-22 | 河北钢铁股份有限公司承德分公司 | Preparation method of high-purity vanadium oxide suitable for all-vanadium flow battery |
| CN106257728A (en) * | 2016-01-28 | 2016-12-28 | 中国科学院过程工程研究所 | A kind of system and method producing 3.5 valency high purity vanadium electrolyte |
| CN106257727A (en) * | 2016-01-28 | 2016-12-28 | 中国科学院过程工程研究所 | A kind of system and method preparing the high-purity electrolyte of vanadium cell |
| CN106257725A (en) * | 2016-01-28 | 2016-12-28 | 中国科学院过程工程研究所 | A kind of system and method preparing high activity all-vanadium flow battery specific valence state electrolyte |
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| CN106257726A (en) * | 2016-01-28 | 2016-12-28 | 中国科学院过程工程研究所 | A kind of system and method producing high-purity high-activity V electrolyte |
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| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| US10099939B2 (en) | 2015-01-30 | 2018-10-16 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium pentoxide powder |
| US10112846B2 (en) | 2015-01-30 | 2018-10-30 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium tetraoxide powder |
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| CN109136555A (en) * | 2018-08-30 | 2019-01-04 | 东北大学 | Electroreduction produces the oxide precursor of V-Ti and the preparation method of flower ball-shaped ammonium poly-vanadate |
| CN111200149A (en) * | 2018-11-19 | 2020-05-26 | 大连融科储能技术发展有限公司 | Formula and process of electrolyte for all-vanadium redox flow battery |
| CN114180624A (en) * | 2021-12-23 | 2022-03-15 | 大连博融新材料有限公司 | Method for preparing high-purity vanadium by separating vanadium and ammonium serving as ammonium metavanadate raw materials |
| CN114180624B (en) * | 2021-12-23 | 2024-01-23 | 大连融科储能集团股份有限公司 | Method for preparing high-purity vanadium by separating ammonium metavanadate raw material vanadium and ammonium |
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