CN106450401B - A method of vanadic sulfate is prepared using discarded V electrolyte - Google Patents
A method of vanadic sulfate is prepared using discarded V electrolyte Download PDFInfo
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- CN106450401B CN106450401B CN201610993930.0A CN201610993930A CN106450401B CN 106450401 B CN106450401 B CN 106450401B CN 201610993930 A CN201610993930 A CN 201610993930A CN 106450401 B CN106450401 B CN 106450401B
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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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 present invention provides a kind of methods for preparing vanadic sulfate using discarded V electrolyte.The method includes the steps: determine volume for V in the high price anode electrolyte of vanadium battery of V4+Concentration C1、V5+Concentration C2With sulfate ion SO4 2‑Concentration CS；V is added2O5, V2O5The range of the amount n of substance is according to C1、C2And CSIt is determined with V；Reducing agent is added and carries out reduction reaction, after reaction, filtering；Acquired solution is subjected to dehydration crystallization, oxygen vanadium sulfate crystals are made.Method of the invention can fully achieve electrolyte of vanadium redox battery and recycle, and vanadium cell operating cost is effectively reduced, and vanadium recovery can be made to be greater than 90%, and operation is simple for method.
Description
Technical field
The present invention relates to vanadium chemical fields, more particularly, are related to a kind of high price vanadium cell anolyte for utilizing and discarding
The method that liquid prepares vanadic sulfate.
Background technique
With the development of new energy, vanadium cell is widely noticed as big promising energy-storage battery.Electrolyte of vanadium redox battery is
The important component of vanadium cell, is the energy carrier of battery, and the energy storage key of vanadium cell is in electrolyte, and in longtime running
Positive and negative anodes mismatch can occur, energy imbalance leads to the problem of cannot continuing to run, increases operating cost, as vanadium cell is led
The development in domain, the recycling of depleted electrolytes start the concerned issue as vanadium cell industry.
The existing method for preparing vanadic sulfate using depleted electrolytes recycling is electrolysed (ginseng after having addition vanadic anhydride again
Examine the Chinese patent " method for preparing vanadic sulfate using failure electrolyte of vanadium redox battery " of Publication No. CN105406098A), and
Vanadic anhydride is first made to be restored with organic reagent (with reference to a kind of Chinese patent " utilization of Publication No. CN102983346A again
The method of the electrolyte for vanadium cell extracting sulfuric acid vanadyl of failure "), both operating procedures are complicated, and long flow path is at high cost, cannot
Large-scale application.
Summary of the invention
It is above-mentioned existing in the prior art it is an object of the present invention to solving for the deficiencies in the prior art
One or more problems.For example, one of the objects of the present invention is to provide one kind can recycle waste electrolyte in batches, realize
The method of electrolyte recycled.
To achieve the goals above, the present invention provides a kind of methods for preparing vanadic sulfate using discarded V electrolyte.
The method includes the steps: determine volume for V in the high price anode electrolyte of vanadium battery of V4+Concentration C1、V5+Concentration C2And sulfate radical
Ion SO4 2-Concentration CS；V is added2O5, V2O5The range of the amount n of substance is according to C1、C2And CSIt is determined with V；Reducing agent is added to carry out
Reduction reaction；Filtering；Dehydration crystallization is carried out to filtrate, oxygen vanadium sulfate crystals are made.
Compared with prior art, electrolyte of vanadium redox battery can be fully achieved according to the method for the present invention to recycle, effectively
Vanadium cell operating cost is reduced, vanadium recovery can be made to be greater than 90%, and operation is simple for method.
Specific embodiment
Hereinafter, according to the present invention utilize will be described in detail in conjunction with exemplary embodiment and discards V electrolyte (i.e.
Discarded electrolyte of vanadium redox battery) method for preparing vanadic sulfate.
Vanadium cell can generate vanadium ion migration, the oxidation of cathode divalent vanadium ion, cathode liberation of hydrogen etc. due to long-play,
Positive and negative anodes concentration of electrolyte is caused to differ, energy mismatches, and it is superfluous especially to show as positive pentavalent vanadium ion, or even reduce electrolysis
Fluid viscosity, generation precipitating etc., influence the normal operation of battery, so the processing of depleted electrolytes is mainly high price vanadium anode electricity
The processing for solving liquid (also known as high price anode electrolyte of vanadium battery), vanadium is tetravalence and pentavalent and deposits when anode electrolyte energy storage, at high price
Anode electrolyte of vanadium battery refers to the positive liquid of four pentavalents mixing.
The method according to the present invention for preparing vanadic sulfate using discarded V electrolyte be discarded high price vanadium cell just
Five oxidations two are added in pole electrolyte (also known as discarded V electrolyte, discarded electrolyte of vanadium redox battery or failure electrolyte of vanadium redox battery)
Then reducing agent is added in vanadium, by redox reaction by vanadium ion by high-valence state V5+It is reduced to lower valency V4+, then to gained
Solution carries out dehydration crystallization, to obtain oxygen vanadium sulfate crystals.
In an exemplary embodiment of the present invention, the side that V electrolyte prepares vanadic sulfate is discarded in utilization of the invention
Method is comprising steps of determine volume for content of vanadium, V complete in the high price anode electrolyte of vanadium battery of V4+Concentration C1、V5+Concentration C2And sulphur
Acid ion SO4 2-Concentration CS；V is added into high price anode electrolyte of vanadium battery2O5, V2O5The range of the amount n of substance is according to C1、
C2And CSIt is determined with V；Reducing agent is added and carries out reduction reaction；Filtering；Dehydration crystallization is carried out to filtrate, obtains vanadic sulfate crystalline substance
Body.
In the present embodiment, using high price anode electrolyte of vanadium battery as raw material, pass through potentiometric titration, uv-spectrophotometric
Method or chemical method determine full content of vanadium, V in high price anode electrolyte of vanadium battery4+Concentration C11、V5+Concentration C12And sulfate ion
SO4 2-Concentration CS。
In the present embodiment, V is added into high price anode electrolyte of vanadium battery2O5, addition opportunity is that it is added in reducing agent
Before, V2O5The range of the amount n of substance determines according to the following formula: 0≤n≤(CS-C2/2-C1) × V, wherein the unit of n is mol, V's
Unit is L, C1、C2And CSUnit be mol/L.
In the present embodiment, reducing agent is added under room temperature (room temperature, such as 25 degree), and the additional amount of reducing agent is according to C12, V and
N is determined, i.e., according to pentavalent vanadium ion V in high price anode electrolyte of vanadium battery5+With addition V2O5Amount determine that reducing agent exists
Guarantee V5+It is reduced to V4+Under the premise of it is slightly excessive.The terminal of reduction reaction is that solution becomes pure blue, and reduction reaction temperature is not
More than 90 DEG C, it is preferred that reduction temperature is 60~80 DEG C.The reduction reaction time is related with other reaction conditions, according to reaction
Type, amount and the concentration of object determines that is, fixed reaction condition determines the reaction time later.Solid V2O5Just with high price vanadium cell
Reaction kettle is first added in pole electrolyte, is then passed through reducing agent after mixing, and wherein the addition of gaseous reducing agent is through entire reduction
Reaction process is not added at one time；Reducing agent includes S, SO2、H2S、H2O2、H2SO3And H2C2O4At least one of；Reduction
After reaction, residue obtained return reduction step next time is filtered, filtering is residue obtained to contain portion of residual V2O5And/or its
His solid impurity.By after filtering gained filtrate carry out dehydration crystallization process are as follows: by after filtering gained filtrate carry out heating concentration or
Oxygen vanadium sulfate crystals are precipitated in decrease temperature crystalline, crystallization；Preferably, heating concentration is carried out under vacuum conditions, wherein vacuum degree 0.05
~0.09Mpa；Acquired solution returns to reduction step next time after dehydration crystallization.
In the present embodiment, depleted electrolytes are high price anode electrolyte of vanadium battery, and all-vanadium ionic is dense in depleted electrolytes
Degree is 1.5~2.0mol/L, and sulfate ion concentration is 4.0~5.0mol/L.Oxygen vanadium sulfate crystals impurity content is made
Less than 1%, sulfuric acid content and crystal water content are added ingredient with material and have fluctuation, and sulfuric acid content is less than 30%, crystal water content
Less than 40%, single vanadium recovery is greater than 90%, and whole process is lost without vanadium.
The above exemplary embodiments for a better understanding of the present invention carry out further it below with reference to specific example
Explanation.
Example 1
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, and measuring full content of vanadium in electrolyte with potentiometric titration is
1.7mol/L, V4+Concentration C1For 0.7mol/L, V5+Concentration C2For 1.0mol/L, sulfate radical SO4 2-Concentration CSFor 4.1mol/L.?
Excessive SO is passed through under room temperature2Gas, solution becomes blue after reacting 4h, and heating concentration under vacuum conditions, obtains after solution filtering
To oxygen vanadium sulfate crystals, the rate of recovery of vanadium is 95%, H in gained crystal2SO4Content is 21%, crystal water content 35%.
Example 2
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, and measuring full content of vanadium in electrolyte with chemical method is
1.7mol/L, V4+Concentration C11For 0.7mol/L, V5+Concentration C2For 1.0mol/L, sulfate radical SO4 2-Concentration CSFor 4.1mol/L.?
1kgV is added in electrolyte2O5, wherein V2O5The amount n of substance determines range: 0≤n≤(C according to the following formulaS-C2/2-C1) × V, i.e., 0
≤ n≤14.5mol, corresponding V2O5Mass range is 0~2.6kg.Excess S is added at normal temperature, solution becomes blue after reacting 8h
Color, heating concentration under vacuum conditions after solution filtering obtain oxygen vanadium sulfate crystals, and the rate of recovery of vanadium is 92%, gained crystal
Middle H2SO4Content is 10%, crystal water content 38%.
Example 3
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, measures full vanadium in electrolyte with ultraviolet spectrophotometry and contains
Amount is 1.7mol/L, V4+Concentration C11For 0.7mol/L, V5+Concentration C2For 1.0mol/L, sulfate radical SO4 2-Concentration CSFor 4.1mol/
L.2.5kgV is added in the electrolytic solution2O5, wherein V2O5The amount n of substance determines range: 0≤n≤(C according to the following formulaS-C2/2-C1)
× V, i.e. 0≤n≤14.5mol, corresponding V2O5Mass range is 0~2.6kg.It is passed through excessive H at normal temperature2S gas, reaction
Solution becomes blue after 8h, and heating concentration under vacuum conditions, obtains oxygen vanadium sulfate crystals, the rate of recovery of vanadium is after solution filtering
90%, H in gained crystal2SO4Content is 0%, crystal water content 38%.
Example 4
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, measures full vanadium in electrolyte with ultraviolet spectrophotometry and contains
Amount is 1.8mol/L, V4+Concentration C11For 0.9mol/L, V5+Concentration C2For 0.9mol/L, sulfate radical SO4 2-Concentration CSFor 4.5mol/
L.1.5kgV is added in the electrolytic solution2O5, wherein V2O5The amount n of substance determines range: 0≤n≤(C according to the following formulaS-C2/2-C1)
× V, i.e. 0≤n≤15.8mol, corresponding V2O5Mass range is 0~2.87kg.It is passed through excessive H at normal temperature2O2, reaction
Solution becomes blue after 7.5h, and heating concentration under vacuum conditions, obtains oxygen vanadium sulfate crystals, the rate of recovery of vanadium after solution filtering
It is 91%, H in gained crystal2SO4Content is 10%, crystal water content 40%.
Example 5
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, and measuring full content of vanadium in electrolyte with chemical method is
1.9mol/L, V4+Concentration C11For 1.2mol/L, V5+Concentration C2For such as 0.7mol/L, sulfate radical SO4 2-Concentration CSFor 4.7mol/
L.2.2kgV is added in the electrolytic solution2O5, wherein V2O5The amount n of substance determines range: 0≤n≤(C according to the following formulaS-C2/2-C1)
× V, i.e. 0≤n≤15.8mol, corresponding V2O5Mass range is 0~2.87kg.It is passed through excessive H at normal temperature2SO3, reaction
Solution becomes blue after 8.5h, and heating concentration under vacuum conditions, obtains oxygen vanadium sulfate crystals, the rate of recovery of vanadium after solution filtering
It is 92%, H in gained crystal2SO4Content is 10%, crystal water content 38%.
Example 6
Taking volume V is the high price anode electrolyte of vanadium battery of 5L, measures full vanadium in electrolyte with ultraviolet spectrophotometry and contains
Amount is 2.0mol/L, V4+Concentration C11For 1.0mol/L, V5+Concentration C2For 1.0mol/L, sulfate radical SO4 2-Concentration CSFor 4.9mol/
L.2.8kgV is added in the electrolytic solution2O5, wherein V2O5The amount n of substance determines range: 0≤n≤(C according to the following formulaS-C2/2-C1)
× V, i.e. 0≤n≤17mol, corresponding V2O5Mass range is 0~3.1kg.It is passed through excessive H at normal temperature2C2O4, reaction
Solution becomes blue after 7.5h, and heating concentration under vacuum conditions, obtains oxygen vanadium sulfate crystals, the rate of recovery of vanadium after solution filtering
It is 93%, H in gained crystal2SO4Content is 10%, crystal water content 38%.
Reducing agent cited by the present invention includes SO2、S、H2S、H2O2、H2SO3And H2C2O4One of, however these are only
It is example, other suitable reducing agents as known in the art can be used.
In conclusion the advantages of V electrolyte low-cost high-efficiency recoverying and utilizing method of the invention includes: that (1) can be achieved
Journey is lost without vanadium, is all recycled.(2) single vanadium recovery can be greater than 90%.(3) operating process is simple and easy, convenient big
Scale is promoted.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (5)
1. a kind of method for preparing vanadic sulfate using discarded V electrolyte, the depleted electrolytes are high price vanadium cell anode electricity
Solve liquid, which is characterized in that described method includes following steps:
Determine volume for V in the high price anode electrolyte of vanadium battery of V4+Concentration C1、V5+Concentration C2With sulfate ion SO4 2-Concentration
CS；
V is added2O5, V2O5The range of the amount n of substance is according to C1、C2、CSIt is determined with V；
Reducing agent is added and carries out reduction reaction, the reaction temperature of the reduction reaction is 60~80 DEG C；
Filtering；
Dehydration crystallization is carried out to filtrate, obtains oxygen vanadium sulfate crystals；The dehydration crystallization process are as follows: to after filtering gained filtrate into
Oxygen vanadium sulfate crystals are precipitated in row heating concentration, crystallization, and the heating concentration carries out under vacuum conditions；
Wherein, reducing agent is added at normal temperature；
The V2O5The range of the amount n of substance determines according to the following formula:
0≤n≤(CS-C2/2-C1) × V,
Wherein, the unit of n is mol, and the unit of V is L, C1、C2And CSUnit be mol/L.
2. the method according to claim 1 for preparing vanadic sulfate using discarded V electrolyte, which is characterized in that the height
All-vanadium ionic concentration is 1.5~2.0mol/L in valence anode electrolyte of vanadium battery, and sulfate ion concentration is 4.0~5.0mol/
L。
3. the method according to claim 1 for preparing vanadic sulfate using discarded V electrolyte, which is characterized in that described to go back
Former agent includes S, SO2、H2S、H2O2、H2SO3And H2SO3At least one of.
4. the method according to claim 1 for preparing vanadic sulfate using discarded V electrolyte, which is characterized in that described true
Determine high price anode electrolyte of vanadium battery V4+Concentration C1、V5+Concentration C2With sulfate ion SO4 2-Concentration CSBy potentiometric titration,
Ultraviolet spectrophotometry or chemical method execute.
5. the method according to claim 1 for preparing vanadic sulfate using discarded V electrolyte, which is characterized in that the crystalline substance
The impurity content of body is less than 1%, and sulfuric acid content is less than 30%, and crystal water content is less than 40%.
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| CN109301300B (en) * | 2018-09-27 | 2021-07-06 | 成都先进金属材料产业技术研究院有限公司 | Method for adjusting vanadium valence state in vanadium battery electrolyte |
| CN111313071A (en) * | 2018-12-11 | 2020-06-19 | 中国科学院大连化学物理研究所 | All-vanadium redox flow battery negative electrode electrolyte and method for reducing negative electrode vanadium ion migration |
| CN117142519B (en) * | 2023-10-30 | 2024-01-02 | 寰泰储能科技股份有限公司 | Method, device and application for recycling vanadyl hydroxide from waste vanadium electrolyte |
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| CN102983346A (en) * | 2012-12-04 | 2013-03-20 | 中国科学院金属研究所 | Method for preparing vanadyl sulfate from electrolyte for failure vanadium cell |
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| CN104181158A (en) * | 2014-08-22 | 2014-12-03 | 武钢集团昆明钢铁股份有限公司 | Method for measuring concentration of tetravalent and pentavalent vanadium ions in vanadium battery electrolyte |
| CN105406098A (en) * | 2015-12-24 | 2016-03-16 | 湖南汇锋高新能源有限公司 | Method for preparing vanadyl sulfate by using failure vanadium cell electrolyte |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1491898A (en) * | 2002-09-25 | 2004-04-28 | 攀枝花钢铁有限责任公司钢铁研究院 | Process for preparinbg vanadylic sulfate and use |
| CN103420415A (en) * | 2012-05-15 | 2013-12-04 | 攀钢集团攀枝花钢钒有限公司 | Preparation method of vanadyl sulfate |
| CN102983346A (en) * | 2012-12-04 | 2013-03-20 | 中国科学院金属研究所 | Method for preparing vanadyl sulfate from electrolyte for failure vanadium cell |
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Effective date of registration: 20201210 Address after: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee after: SICHUAN PAN YAN TECHNOLOGY Co.,Ltd. Address before: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee before: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. |