CN104638288A - Electrochemical preparation method of 3.5 valence vanadium electrolyte - Google Patents
Electrochemical preparation method of 3.5 valence vanadium electrolyte Download PDFInfo
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- CN104638288A CN104638288A CN201310542929.2A CN201310542929A CN104638288A CN 104638288 A CN104638288 A CN 104638288A CN 201310542929 A CN201310542929 A CN 201310542929A CN 104638288 A CN104638288 A CN 104638288A
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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
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
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Abstract
The invention belongs to the fields of chemical engineering and industry, and especially relates to a preparation method of an all vanadium redox flow battery electrolyte. The method adopts an electrolysis device, adopts a chemically and electrochemically combined technology to reduce high valence vanadium, and a vanadium (IV) raw material is reduced through parts of electric energy and a reducing agent for reducing vanadium (V) to prepare a highly pure 3.5 valence vanadium solution. The 3.5 valence vanadium can be directly used as the all vanadium redox flow battery positive and negative electrolyte, and the electrolyte can realize positive electrode and negative electrode coupling after initial charge, can be used without an activation process, and is an all vanadium redox flow electrolyte product with a best valence. The method has the characteristics of short preparation flow, low electric energy consumption and high product purity, and easily realizes continuous production.
Description
Technical field
The present invention relates to a kind of preparation method of all-vanadium redox flow battery electrolyte, particularly a kind of electrochemical preparation method of 3.5 valency V electrolytes.The employing electrolysis unit of the method, adopts the way that electrochemistry and electronation combine, and consumes the reducing agent of part electric energy and reducible 5 valency vanadium, with 4 valency vanadium for highly purified 3.5 valency vanadium solutions prepared by raw material.3.5 valency vanadium can be directly applied for all-vanadium flow battery both positive and negative polarity, and can reach both positive and negative polarity coupling after initial charge, can use without the need to experiencing activation process, be the all-vanadium flow electrolyte product of optimum valence state.The method has the feature that preparation flow is short, consumption electric energy is low, product purity is high.
Technical background
Flow battery is a kind of large-scale energy storage device, under flow regime, realize energy storage with active material, exoergic makes feature, a series of progress is obtained over nearly 30 years, particularly in recent years, along with the development of the regenerative resources such as wind and solar energy, the extensive energy storage feature of flow battery shows its excellent development prospect.Be developed so far, existing multiple system, wherein, all-vanadium flow battery system is system the most ripe at present.
The both positive and negative polarity of all-vanadium flow battery is respectively V
5+/ V
4+and V
3+/ V
2+electricity is right, and in traditional handicraft, the general 4 valency V electrolytes that adopt are as raw material.For this reason, during first Application, in positive pole tank, inject the tetravalence V electrolyte doubling negative solution, after charging complete, then the positive pole liquid of half is poured out, just can complete the both positive and negative polarity valence state of battery and the coupling of material.And 3.5 valency electrolyte are without the need to experience activation, initial charge can reach the coupling of both positive and negative polarity valence state and material, can directly use, and will become the first-selected product of following commercial fluid cell electrolyte.
Existing patent is the mixed dissolution in sulfuric acid solution by vanadic oxide and vanadium trioxide mostly, carries out chemistry and electrochemical reduction, and preparation becomes three ~ tetravalence vanadium solution.Patent (ZL03159533.2) is on the basis that vanadic oxide and vanadium trioxide 1:1 mix, and adopt the method for electrolysis to be reduced by electrolyte, preparation becomes trivalent and tetravalence vanadium ratio is the mixture of 1:1.Vanadium trioxide and vanadic oxide mix according to the ratio of 1.5 ~ 2.5:1 by patent (application number 200610038914.2), and high-temperature roasting, obtains many vfanadium compound, then sulfuric acid is added, preparation becomes three ~ tetravalence V electrolyte, and wherein, tetravalence vanadium is greater than 50% of total vanadium.Patent (application number 200910171737.3), also by vanadic oxide and vanadium trioxide sulfuric acid dissolution, adds organic substance reducing agent simultaneously, obtains three ~ tetravalence vanadium solution.Patent (ZL200710188392.9) adopts trivalent vanadium to prepare electrolyte of vanadium redox battery.Vanadium trioxide is mixed with sulfuric acid, puts into tube furnace, at the temperature lower calcination of 100 ~ 300 degree, utilize air that part trivalent vanadium is oxidized into tetravalence, obtain the mixture of each half of three tetravalences.
In above-mentioned various methods, adopt vanadic oxide, vanadium trioxide powder or the mixture of the two more, be dissolved in strong acid, by the reaction under hot conditions, prepare V electrolyte.The raw material of these class methods is barium oxide, and feed preparation process is complicated, expensive, should be not suitable for the large-scale production of electrolyte.
Summary of the invention
The object of the present invention is to provide a kind of electrochemical preparation method of 3.5 valency V electrolytes.Be different from the preparation method of existing fluid cell electrolyte, thinking of the present invention is: adopt the way that electrochemistry and electronation combine, in electrolytic cell, control both positive and negative polarity rate of charge and electrolysis electricity, 4 valency vanadium are become 3.5 valencys at cathodic reduction, 4 valency vanadium are oxidized into 5 valencys at positive pole simultaneously, subsequently, electrolyte liquid is released, inject 4 new valency vanadium liquid, reducing agent is added in anode electrolyte, 5 valency vanadium reduction are become 4 valencys, so can realize reusing of anode electrolyte, and 3.5 continuous seepage of valency vanadium, and the method has preparation flow short, consumption electric energy is low, the feature that product purity is high.
Of the present inventionly to be implemented as follows: in the electrochemical preparation method of this 3.5 valency V electrolyte, a kind of novel electrolysis unit adopted, positive pole and the negative electrolyte solution amberplex of this device are separated, flow between solution reservoir and battery under pump promotes respectively, there is oxidation or reduction reaction in both positive and negative polarity electrolyte on catalysis electrode again; In this electrolysis unit, using 4 valency vanadium of moiety volume as anode electrolyte, using 4 valency vanadium of a volume as electrolyte liquid, under the condition of impressed current, control electrolysis electricity, negative solution is reduced to 3.5 valencys by 4 valencys, positive solution is oxidizing to 5 valencys by 4 valencys.After electrolysis, after being released by 3.5 valency vanadium solutions of negative pole, then add 4 valency vanadium of same volume, meanwhile, add reducing agent at positive pole and 5 valency vanadium are reduced to 4 valencys, repeat last electrolysis.
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, amberplex is cation-exchange membrane or anion-exchange membrane.
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, anode catalytic electrode is more than one in material with carbon element, stereotype, titanium plate, tantalum plate, nail-plate, iridium plate, and negative pole catalysis electrode is more than one in material with carbon element, stereotype, titanium plate, tantalum plate, nail-plate, iridium plate; Material with carbon element is graphitization or non-graphitized sheet material, porous carbon felt, carbon paper or porous charcoal sheet material, and wherein the pore diameter range of porous material is at 1 ~ 200 μm.
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, the volume of anode electrolyte and the volume ratio of electrolyte liquid are 1.5 ~ 1.1:2; The average decomposition voltage of monocell is at below 1.8V.
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, the electrolyte solution of positive pole and negative pole is 4 valency vanadium solutions, electrolyte solution supporting electrolyte is more than one in sulfuric acid, hydrochloric acid, perchloric acid, and the concentration of electrolyte solution vanadium is 1.5 ~ 2.5 moles often liter;
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, the electric current of electrolysis depends on the electrode area of electrolytic cell, and electrolytic current density is 50 ~ 400mA cm
-2; The terminal of electrolysis is controlled by electrolysis electricity, and the amount of substance of electrolyte liquid active material vanadium is 1, then electrolysis electricity is about 13.4 ~ 14.7Ah electrolysis termination.
In the electrochemical preparation method of 3.5 valency V electrolytes of the present invention, the amount of positive pole reducing agent is controlled by the amount of substance of vanadium, the amount of substance of negative electrode active material vanadium is 1, and the chemical dosage ratio that this reducing agent and vanadium react is m, then the amount of substance that reducing agent adds is 1 ~ 1.1m mol.
Beneficial effect of the present invention:
1, the preparation method that the present invention proposes adopts electrolysis unit, but it is different from the industry of tradition electroreduction, positive pole negative pole all adopts electrolyte solution of the same race, effectively reduce cross pollution, the electrode potential of positive pole reaction is lower than oxygen evolution potential, effectively reduce groove pressure, not only reduce energy consumption, and reduce the requirement of positive plate sludge proof.
2, positive pole 5 valency vanadium is reduced to 4 valencys by proposition reducing agent of the present invention, can reach the recycling of anode electrolyte, meanwhile, coordinates the charging of negative solution, discharging, easily accomplishes scale production.
Accompanying drawing explanation
Fig. 1. electrolysis unit
In figure: 1. electrolytic cell, 2. positive pole fluid reservoir, 3. negative pole fluid reservoir, 4. positive pole feed liquor tank, 5. negative pole feed liquor tank, 6. negative pole goes out flow container, 7. magnetic drive pump, 8. three-way solenoid valve, 9. pipeline, 10. potentiostat.
Embodiment
Example 1
By 11 liters of 1.6MVOSO
4+ 3MH
2sO
4solution injects positive pole tank, by 20 liters of 1.6MVOSO
4+ 3MH
2sO
4solution injects cathode pot, and the electrode area of electrolytic cell is 0.9m
2, adopt nafionl15 film separate electrolysis cell, use constant-current electrolysis mode, under the current density of 180 peaces, carry out constant-current electrolysis, control flume is pressed in 1.8V, otherwise reduces Faradaic current, after electrolysis electricity reaches 428.8Ah, stop electrolysis, the negative pole vanadium liquid of 3.5 valencys is released, refills 20 liters of 1.6MVOSO
4+ 3MH
2sO
4solution, meanwhile, adds water and hydrazine 4.8M in positive pole liquid, after reacting completely, repeats electrolysis last time.
Example 2
By 11 liters of 2.0MVOSO
4+ 3MH
2sO
4solution injects positive pole tank, by 20 liters of 2.0MVOSO
4+ 3MH
2sO
4solution injects cathode pot, and the electrode area of electrolytic cell is 0.9m
2, adopt nafionl15 film separate electrolysis cell, use constant-current electrolysis mode, under the current density of 180 peaces, carry out constant-current electrolysis, control flume is pressed in 1.8V, otherwise reduces Faradaic current, after electrolysis electricity reaches 536Ah, stop electrolysis, the negative pole vanadium liquid of 3.5 valencys is released, refills 20 liters of 2.0MVOSO
4+ 3MH
2sO
4solution, meanwhile, adds water and hydrazine 6.0M in positive pole liquid, after reacting completely, repeats electrolysis last time.
Claims (7)
1. the electrochemical preparation method of a valency V electrolyte, it is characterized in that the step of the method is as follows: adopt a kind of electrolysis unit, this device is by electrolytic cell (1), positive pole fluid reservoir (2), negative pole fluid reservoir (3), positive pole feed liquor tank (4), negative pole feed liquor tank (5), negative pole goes out flow container (6), magnetic drive pump (7), control valve (8), pipeline (9) and power supply (10) are formed, wherein positive pole feed liquor tank (4) is connected to positive pole fluid reservoir (2) and promotes by magnetic drive pump (7) the positive polar region that anode electrolyte flows through electrolytic cell (1) by pipeline (9), negative pole feed liquor tank (5) is connected to negative pole fluid reservoir (3) and promotes by magnetic drive pump (7) the negative pole district that electrolyte liquid flows through electrolytic cell (1) by pipeline (9), negative pole is gone out flow container (6) and is connected to negative pole fluid reservoir (3) and is promoted by crossing magnetic drive pump (7), for taking out electrolyte liquid at the end of electrolysis by pipeline (9) and three-way control valve (8), electrolytic cell (1) is by end plate (11), collector electrode (12), barrier (13), catalysis electrode (14), barrier film (15) and bipolar plates (16) composition, positive polar region collector electrode (12), positive pole separates grid (13) and positive polar region catalysis electrode (14) forms positive polar region, negative pole district collector electrode (12), negative pole separates grid (13) and composition negative pole district of negative pole district catalysis electrode (14), positive polar region separated by barrier film (15) and negative pole district forms single electrolytic cell, multiple single electrolytic cell is connected into electrolytic cell (1) by bipolar plates (16), anode electrolyte and electrolyte liquid are separated by barrier film (15), flow between the positive polar region of positive pole fluid reservoir (2) and electrolytic cell (1) and between negative pole fluid reservoir (3) and electrolytic cell (1) negative pole district under magnetic drive pump (7) promotes respectively, in this electrolysis unit, using 4 valency vanadium solutions of moiety volume as anode electrolyte, using 4 valency vanadium solutions of a volume as electrolyte liquid, under the function of current that power supply (10) provides, control electrolysis electricity, the vanadium of electrolyte liquid is reduced to 3.5 valencys by 4 valencys, the vanadium of anode electrolyte is oxidizing to 5 valencys by 4 valencys.After electrolysis, after being released by 3.5 valency vanadium solutions of negative pole, then add 4 valency vanadium of same volume, meanwhile, add reducing agent at positive pole and 5 valency vanadium are reduced to 4 valencys, repeat last electrolysis.
2. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, is characterized in that amberplex is cation-exchange membrane or anion-exchange membrane.
3. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, it is characterized in that anode catalytic electrode is more than one in material with carbon element, stereotype, titanium plate, tantalum plate, nail-plate, iridium plate, negative pole catalysis electrode is more than one in material with carbon element, stereotype, titanium plate, tantalum plate, nail-plate, iridium plate; Material with carbon element is graphitization or non-graphitized sheet material, porous carbon felt, carbon paper or porous charcoal sheet material, and wherein the pore diameter range of porous material is at 1 ~ 200 μm.
4. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, is characterized in that the volume of anode electrolyte and the volume ratio of electrolyte liquid are 1.5 ~ 1.1:2; The average decomposition voltage of monocell is at below 1.8V.
5. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, it is characterized in that the electrolyte solution of positive pole and negative pole is 4 valency vanadium solutions, electrolyte solution supporting electrolyte is more than one in sulfuric acid, hydrochloric acid, perchloric acid, and the concentration of electrolyte solution vanadium is 1.5 ~ 2.5 moles often liter.
6. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, it is characterized in that the electric current of electrolysis depends on the electrode area of electrolytic cell, electrolytic current density is 50 ~ 400mA cm
-2; The terminal of electrolysis is controlled by electrolysis electricity, and the amount of substance of electrolyte liquid active material vanadium is 1, then electrolysis electricity is about 13.4 ~ 14.7Ah electrolysis termination.
7. the electrochemical preparation method of a kind of 3.5 valency V electrolytes according to claim 1, it is characterized in that the amount of positive pole reducing agent is controlled by the amount of substance of vanadium, the amount of substance of negative electrode active material vanadium is 1, the chemical dosage ratio that this reducing agent and vanadium react is m, then the amount of substance that reducing agent adds is 1 ~ 1.1m mol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108023109A (en) * | 2017-12-08 | 2018-05-11 | 湖南省银峰新能源有限公司 | A kind of preparation method of 3.5 valency pure hydrochloric acid system V electrolyte of high energy |
| CN109669142A (en) * | 2017-09-28 | 2019-04-23 | 大连融科储能技术发展有限公司 | A kind of method and system for the migration of real-time monitoring all-vanadium flow battery vanadium |
| CN110867602A (en) * | 2019-11-01 | 2020-03-06 | 四川星明能源环保科技有限公司 | Preparation method of solid vanadium electrolyte |
| CN116231023B (en) * | 2023-02-21 | 2023-08-18 | 沈阳恒久安泰环保与节能科技有限公司 | Preparation method of 3.5-valent hydrochloric acid system and 3.5-valent sulfuric acid system vanadium electrolyte |
| RU2803292C1 (en) * | 2022-04-01 | 2023-09-12 | Общество с ограниченной ответственностью "Инэнерджи" (ООО "Инэнерджи") | Method for producing an electrolyte for a vanadium flow redox battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101619465A (en) * | 2008-07-02 | 2010-01-06 | 中国科学院大连化学物理研究所 | Method for preparing vanadium battery solution or adjusting capacity and special device thereof |
| CN102468499A (en) * | 2010-11-04 | 2012-05-23 | 新奥科技发展有限公司 | Regeneration method for waste liquor of all-vanadium flow battery |
-
2013
- 2013-11-06 CN CN201310542929.2A patent/CN104638288A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101619465A (en) * | 2008-07-02 | 2010-01-06 | 中国科学院大连化学物理研究所 | Method for preparing vanadium battery solution or adjusting capacity and special device thereof |
| CN102468499A (en) * | 2010-11-04 | 2012-05-23 | 新奥科技发展有限公司 | Regeneration method for waste liquor of all-vanadium flow battery |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2017128969A1 (en) * | 2016-01-28 | 2017-08-03 | 中国科学院过程工程研究所 | System and method for producing 3.5-valent highly pure vanadium electrolyte |
| CN106257728B (en) * | 2016-01-28 | 2018-01-12 | 中国科学院过程工程研究所 | A kind of system and method for producing the high-purity V electrolyte of 3.5 valencys |
| RU2695083C1 (en) * | 2016-01-28 | 2019-07-19 | Инститьют Оф Процесс Инжиниринг, Чайнис Академи Оф Сайнсис | System and method of obtaining high-purity vanadium electrolyte with valence of 3,5 |
| CN109669142A (en) * | 2017-09-28 | 2019-04-23 | 大连融科储能技术发展有限公司 | A kind of method and system for the migration of real-time monitoring all-vanadium flow battery vanadium |
| CN108023109A (en) * | 2017-12-08 | 2018-05-11 | 湖南省银峰新能源有限公司 | A kind of preparation method of 3.5 valency pure hydrochloric acid system V electrolyte of high energy |
| CN110867602A (en) * | 2019-11-01 | 2020-03-06 | 四川星明能源环保科技有限公司 | Preparation method of solid vanadium electrolyte |
| RU2803292C1 (en) * | 2022-04-01 | 2023-09-12 | Общество с ограниченной ответственностью "Инэнерджи" (ООО "Инэнерджи") | Method for producing an electrolyte for a vanadium flow redox battery |
| CN116231023B (en) * | 2023-02-21 | 2023-08-18 | 沈阳恒久安泰环保与节能科技有限公司 | Preparation method of 3.5-valent hydrochloric acid system and 3.5-valent sulfuric acid system vanadium electrolyte |
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Application publication date: 20150520 |