CN106395902A - Method for preparing vanadium pentoxide by utilizing invalid vanadium battery positive pole electrolyte - Google Patents
Method for preparing vanadium pentoxide by utilizing invalid vanadium battery positive pole electrolyte Download PDFInfo
- Publication number
- CN106395902A CN106395902A CN201610994018.7A CN201610994018A CN106395902A CN 106395902 A CN106395902 A CN 106395902A CN 201610994018 A CN201610994018 A CN 201610994018A CN 106395902 A CN106395902 A CN 106395902A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- electrolyte
- vanadic anhydride
- pentavalent
- anode electrolyte
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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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 58
- 239000003792 electrolyte Substances 0.000 title claims abstract description 55
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910001456 vanadium ion Inorganic materials 0.000 claims abstract description 24
- 239000012065 filter cake Substances 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
Classifications
-
- 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
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Fuel Cell (AREA)
Abstract
The invention provides a method for preparing vanadium pentoxide by utilizing invalid vanadium battery positive pole electrolyte. The method comprises the following steps that the invalid vanadium battery positive pole electrolyte is led into a vanadium battery positive pole, charging pre-oxidation is performed to obtain electrolyte of pentavalent vanadium ions; evaporation and concentration are conducted on the electrolyte of pentavalent vanadium ions, and then standing is performed to form mixed liquid containing a pentavalent vanadium precipitate; the mixed liquid is filtered, and a filter cake is dried and grinded to obtain vanadium pentoxide powder. By the adoption of the method, recycle of vanadium electrolyte is achieved, and the produced vanadium pentoxide is high in purity and can be continuously used for preparing electrolyte and other purposes or used as a catalyst.
Description
Technical field
The present invention relates to vanadium battery field, more particularly, it is related to a kind of anode electrolyte of vanadium battery system using inefficacy
The method of standby vanadic anhydride.
Background technology
Vanadium cell full name vanadium oxide reduction flow battery, has long service life, capacity is big, power is big, security performance is high
Etc. series of advantages.Based on its unique advantage, the applicable field of vanadium energy storage system is wide.It can be used as hospital, work
The local emergency service facility such as factory, military base and office block；Also by supplementing in gas station or electrolyte can be changed in fact
" quickly recharging " of existing vehicle；Can be used as the power supply system of communication, radio repeater station, railway information instruction, military equipment etc.
System；Can be used as the airborne power supply of the vehicles such as industrial truck, fork truck, delivery vehicle, bus, submarine；Apply also for side
Remote area home electric power system and the supporting energy storage device of solar energy, wind energy；Especially can be applicable to extensive energy storage system
System and peak load regulation network.
When in sulfuric acid system, vanadium cell just extremely (VO2)SO4 -/VOSO4Electricity is right, and negative pole is V3+/V2+Electricity is right, and battery fills
After electricity, positive electrode material is V5+Solion, negative pole is V2+Solion；After electric discharge, positive and negative electrode is respectively V4+And V3+Ion is molten
Liquid.V5+And V4+Ion is in an acidic solution respectively with VO2 +Ion and VO2+Ionic species exists.Electrolyte of vanadium redox battery is through vanadium electricity
After pond is recycled for a long time, vanadium ion concentration and sulfuric acid concentration severe overweight, vanadium ion valence state mismatch, or even generation precipitation etc.
Phenomenon, and then cannot use.
Content of the invention
For the deficiencies in the prior art, an object of the present invention is to solve present in above-mentioned prior art
One or more problems.For example, an object of the present invention is to provide a kind of vanadium cell anolyte recycling and losing efficacy
The method of liquid.
To achieve these goals, a kind of anode electrolyte of vanadium battery using inefficacy that provides of the present invention prepares five oxygen
The method changing two vanadium, the method comprising the steps of：The anode electrolyte of vanadium battery of inefficacy is passed through vanadium cell positive pole carry out
Charge and pre-oxidize, obtain the electrolyte of pentavalent vanadium ion；The electrolyte of pentavalent vanadium ion is evaporated concentrating, then stands,
Form the mixed liquor having containing pentavalent vanadium precipitation；Filter mixed liquor, and filter cake is dried and grinds, obtain vanadic anhydride powder
Body.
The anode electrolyte of vanadium battery that utilization according to the present invention was lost efficacy prepares an enforcement of the method for vanadic anhydride
Example, in the anode electrolyte of vanadium battery of inefficacy, vanadium ion concentration can be 1.6mol/L.
The anode electrolyte of vanadium battery that utilization according to the present invention was lost efficacy prepares an enforcement of the method for vanadic anhydride
Example, the electrolyte of described pentavalent vanadium ion is concentrated by evaporation and is more than 3.0mol/L to vanadium ion concentration.
The anode electrolyte of vanadium battery that utilization according to the present invention was lost efficacy prepares an enforcement of the method for vanadic anhydride
Example, described evaporation-concentration step includes：On electric furnace heat pentavalent vanadium ion electrolyte to be boiling for stir.
The anode electrolyte of vanadium battery that utilization according to the present invention was lost efficacy prepares an enforcement of the method for vanadic anhydride
Example, the time of standing can be 24～48h.
Compared with prior art, the method preparing vanadic anhydride using the anode electrolyte of vanadium battery losing efficacy, not only real
Showed the recycling of V electrolyte, and the purity of vanadium pentoxide producing be high, can continue for prepare electrolyte or
Person is used for other purposes such as catalyst, has actual application value.
Specific embodiment
Hereinafter, the vanadium cell positive pole utilization describing in detail with reference to exemplary embodiment according to the present invention being lost efficacy
The method that vanadic anhydride prepared by electrolyte.
The present invention (is also called vanadium cell inefficacy electrolyte, electrolysis of losing efficacy using the anode electrolyte of vanadium battery having lost efficacy
Liquid, inefficacy V electrolyte), inefficacy electrolyte is mainly tetravalence vanadium and the mixed solution of pentavalent vanadium composition, is made wherein by charging
Tetravalent vanadium ion V4+It is changed into pentavalent vanadium ion V5+, then heat concentration so that the pentavalent vanadium in solution is precipitated out, stand one section
Filtering drying after time, you can obtain vanadic anhydride.
In one exemplary embodiment of the present invention, the anode electrolyte of vanadium battery that the utilization of the present invention was lost efficacy prepares five
The method of V 2 O comprises the following steps：
(1) tetravalent vanadium ion pre-oxidation：By the anode electrolyte of vanadium battery of inefficacy be passed through vanadium cell positive pole be charged pre-
Oxidation, obtains the electrolyte of pentavalent vanadium ion.
Wherein, in the electrolyte of inefficacy, the concentration of vanadium ion can be 1.6mol/L.
(2) pentavalent vanadium ion precipitation：The electrolyte of pentavalent vanadium ion is evaporated concentrating, then stands, formation has
Mixed liquor containing pentavalent vanadium precipitation.
In the present example embodiment, after battery being charged, resulting solution (i.e. step (1) resulting solution) is taken out, in electric furnace
On be heated to seething with excitement and be stirred continuously, when vanadium ion concentration is concentrated by evaporation to more than 3.0mol/L, taking off standing 24～48h.
(3) preparation of vanadic anhydride：Solidliquid mixture (mixed liquor containing pentavalent vanadium precipitation) to step (2) gained enters
Row filters, and obtains vanadic anhydride powder by after filter cake drying grinding.
Above-mentioned example embodiment for a better understanding of the present invention, is carried out to it with reference to specific example further
Explanation.
Vanadium cell positive pole inefficacy electrolyte is charged and pre-oxidizes, prepare 10L pentavalent electrolyte (1#Electrolyte) for future use,
Electrolyte needs low temperature to store.
Example 1
Measure 500ml 1#Electrolyte, being concentrated by evaporation and continue stirring until liquor capacity on electric furnace is 270ml；By gained
Solution filters after taking off standing 24h, dries, obtains filter cake 43.69g, calculating vanadium yield is 60.01%, and gained filter cake is ground
Mill, obtains vanadic anhydride powder.
Example 2
Measure 1000ml 1#Electrolyte, being concentrated by evaporation and continue stirring until liquor capacity on electric furnace is 530ml；By institute
Obtain after solution takes off standing 48h and filter, dry, obtain filter cake 94.82g, calculating vanadium yield is 65.12%, by gained filter cake
Grind, obtain vanadic anhydride powder.
Example 3
Measure 2000ml 1#Electrolyte, being concentrated by evaporation and continue stirring until liquor capacity on electric furnace is 800ml；By institute
Obtain after solution takes off standing 96h and filter, dry, obtain filter cake 210.71g, calculating vanadium yield is 72.36%, by gained filter cake
Grind, obtain vanadic anhydride powder.
In sum, the present invention had using the method that vanadic anhydride prepared by vanadium cell inefficacy electrolyte following excellent
Point：
(1) with the electrolyte that lost efficacy as raw material it is achieved that resource reclaim recycles.
(2) it is not necessary to extra addition precipitation during vanadic anhydride is prepared for raw material with inefficacy electrolyte
Step, process is simple, low cost, application easy to spread.
(3) purity of vanadium pentoxide prepared by is high, and vanadium recovery is higher, and technique is suitable to industrialized production.
Although above by describing the present invention with reference to exemplary embodiment, those skilled in the art should be clear
Chu, in the case of the spirit and scope being limited without departing from claim, can be carried out respectively to the exemplary embodiment of the present invention
Plant modifications and changes.
Claims (5)
1. a kind of prepare the method for vanadic anhydride it is characterised in that methods described using the anode electrolyte of vanadium battery losing efficacy
Comprise the following steps：
The anode electrolyte of vanadium battery of inefficacy is passed through vanadium cell positive pole be charged pre-oxidizing, obtains the electrolysis of pentavalent vanadium ion
Liquid；
The electrolyte of pentavalent vanadium ion is evaporated concentrating, then stands, form the mixed liquor having containing pentavalent vanadium precipitation；
Filter mixed liquor, and filter cake is dried and grinds, obtain vanadic anhydride powder.
2. the method preparing vanadic anhydride using the anode electrolyte of vanadium battery losing efficacy according to claim 1, it is special
Levy and be, in the anode electrolyte of vanadium battery of described inefficacy, vanadium ion concentration is 1.6mol/L.
3. the method preparing vanadic anhydride using the anode electrolyte of vanadium battery losing efficacy according to claim 1, it is special
Levy and be, the electrolyte of described pentavalent vanadium ion is concentrated by evaporation and is more than 3.0mol/L to vanadium ion concentration.
4. the method preparing vanadic anhydride using the anode electrolyte of vanadium battery losing efficacy according to claim 1, it is special
Levy and be, described evaporation-concentration step includes：On electric furnace heat pentavalent vanadium ion electrolyte to be boiling for stir.
5. the method preparing vanadic anhydride using the anode electrolyte of vanadium battery losing efficacy according to claim 1, it is special
Levy and be, the time of standing is 24～48h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610994018.7A CN106395902B (en) | 2016-11-11 | 2016-11-11 | A kind of method that anode electrolyte of vanadium battery using failure prepares vanadic anhydride |
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| CN201610994018.7A CN106395902B (en) | 2016-11-11 | 2016-11-11 | A kind of method that anode electrolyte of vanadium battery using failure prepares vanadic anhydride |
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| CN106395902B CN106395902B (en) | 2018-01-26 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109301300A (en) * | 2018-09-27 | 2019-02-01 | 成都先进金属材料产业技术研究院有限公司 | The method for adjusting Vanadium valence in electrolyte of vanadium redox battery |
| CN109721101A (en) * | 2019-01-02 | 2019-05-07 | 成都先进金属材料产业技术研究院有限公司 | Vanadium cell failure electrolyte prepares V2O5The method of nano-powder |
| CN112408477A (en) * | 2020-11-30 | 2021-02-26 | 鞍钢集团北京研究院有限公司 | Method for preparing vanadium dioxide from failure vanadium battery positive electrolyte |
| CN114031114A (en) * | 2021-11-12 | 2022-02-11 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery |
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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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2016
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Patent Citations (2)
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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 |
| CN102983379A (en) * | 2012-12-04 | 2013-03-20 | 中国科学院金属研究所 | Method for preparing vanadium pentoxide from ineffective electrolyte for vanadium battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109301300A (en) * | 2018-09-27 | 2019-02-01 | 成都先进金属材料产业技术研究院有限公司 | The method for adjusting Vanadium valence in electrolyte of vanadium redox battery |
| 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 |
| CN109721101A (en) * | 2019-01-02 | 2019-05-07 | 成都先进金属材料产业技术研究院有限公司 | Vanadium cell failure electrolyte prepares V2O5The method of nano-powder |
| CN112408477A (en) * | 2020-11-30 | 2021-02-26 | 鞍钢集团北京研究院有限公司 | Method for preparing vanadium dioxide from failure vanadium battery positive electrolyte |
| CN114031114A (en) * | 2021-11-12 | 2022-02-11 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery |
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| CN106395902B (en) | 2018-01-26 |
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Effective date of registration: 20220727 Address after: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Patentee after: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE 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. |
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Application publication date: 20170215 Assignee: SICHUAN PAN YAN TECHNOLOGY Co.,Ltd. Assignor: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Contract record no.: X2024980003062 Denomination of invention: A Method for Preparing Vanadium Pentoxide by Utilizing Defective Cathode Electrolyte of Vanadium Batteries Granted publication date: 20180126 License type: Exclusive License Record date: 20240322 |