CN103280591B - A kind of manufacture method of solid electrolyte for vanadium flow battery - Google Patents
A kind of manufacture method of solid electrolyte for vanadium flow battery Download PDFInfo
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- CN103280591B CN103280591B CN201310198369.3A CN201310198369A CN103280591B CN 103280591 B CN103280591 B CN 103280591B CN 201310198369 A CN201310198369 A CN 201310198369A CN 103280591 B CN103280591 B CN 103280591B
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- solid electrolyte
- vanadium
- electrolyte
- reaction
- product
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 40
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003792 electrolyte Substances 0.000 claims abstract description 21
- 230000035484 reaction time Effects 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 230000007423 decrease Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 8
- 238000002821 scintillation proximity assay Methods 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 6
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 230000004044 response Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 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 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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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- Fuel Cell (AREA)
- Secondary Cells (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of manufacture method of solid electrolyte for vanadium flow battery, comprise first by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 3L/min ~ 20L/min
2, and controlling reaction temperature at 300 DEG C ~ 900 DEG C, the reaction time is 0.5h ~ 4h, obtains V
4o
7product; Again by V
4o
7product and the concentrated sulfuric acid, SPA are carry out hybrid reaction at 1: 2.347: 0.07 ~ 1: 3.52: 0.104 according to weight ratio, and control reaction temperature at 100 DEG C ~ 500 DEG C, and the reaction time is 30min ~ 300min, obtains blocks of solid electrolyte; Be finally carry out hybrid reaction at 4: 4.2 ~ 4: 6.4 by blocks of solid electrolyte and pure water according to weight ratio, and control reaction temperature at 50 DEG C ~ 150 DEG C, the reaction time is 20 minutes, obtains electrolyte.Invention increases production efficiency, decrease cost of transportation, the Vanadium valence in electrolyte can be controlled simultaneously accurately.
Description
Technical field
The present invention relates to battery solid electrolyte technical field, more particularly, particularly a kind of manufacture method of solid electrolyte for vanadium flow battery.
Background technology
Current manufacture electrolyte of vanadium redox battery has following three kinds of methods.One is direct electrolysis method, namely adopts the V that asymmetric electrolytic tank electrolysis reduces in dilution heat of sulfuric acid
2o
5, obtain electrolyte, it is low to there is production efficiency in it, and there is the process problem of anode waste electrolyte.Two is first chemical method, then electrolysis, first by V
2o
5in dilute sulfuric acid, be reduced into the vanadic sulfate solution of 4 valencys by reducing agents such as oxalic acid, then with electrolysis tank, the vanadic sulfate electrolysis of solutions of this 4 valency be reduced into electrolyte for vanadium cell.Three is chemical methods, as: the method that US Patent No. 5587132 provides dissolves V with the dilute sulfuric acid of 60C ~ 150C
2o
3, this course of dissolution needs more than 5 hours, then obtains 3 valency vanadic sulfate solution, and with oxalic acid and dilute sulfuric acid and V
2o
5reaction acquisition 4 valency vanadic sulfate solution, again 3 valency vanadic sulfate solution and 4 valency vanadic sulfate solution equal proportions are mixed to get the electrolyte of 3.5 valencys, but its shortcoming existed is: it is slow that the method exists reaction speed, cause production efficiency low, dissolve not exclusively, and the 3.5 valency V electrolytes that final products need can not accurately control within 3.5+/-0.03.Meanwhile, another adopts the Chinese patent CN2007101883929 of chemical method to provide three vanadium oxide (VO
3) concentrated sulfuric acid that is dissolved in 100C ~ 300C temperature obtains green vfanadium compound, this vfanadium compound is dissolved in dilution heat of sulfuric acid and obtains electrolyte; But its shortcoming existed is: three vanadium oxides of the method definition, concept obfuscation, and science does not have molecular formula be VO
3material exist, for the key component vanadium of the electrolyte produced valence state and application also do not illustrate.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of solid electrolyte for vanadium flow battery, it is high and accurately can control the advantage of Vanadium valence between 3.5+/-0.03 of final products that the method has production efficiency.
A manufacture method for solid electrolyte for vanadium flow battery, comprises the following steps:
The first step: by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 3L/min ~ 20L/min
2, and controlling reaction temperature at 300 DEG C ~ 900 DEG C, the reaction time is 0.5 hour ~ 4 hours, obtains V
4o
7product; Its chemical equation is: 2 V
2o
5+ 3H
2=V
4o
7+ 3H
2o;
Second step: by the V obtained in the first step
4o
7product and the concentrated sulfuric acid, SPA are that 1:2.347:0.07 ~ 1:3.52:0.104 carries out hybrid reaction according to weight ratio, and control reaction temperature at 100 DEG C ~ 500 DEG C, and the reaction time is 30min ~ 300min, obtains blocks of solid electrolyte;
3rd step: be that 4:4.2 ~ 4:6.4 carries out hybrid reaction according to weight ratio by the blocks of solid electrolyte obtained in second step and pure water, and control reaction temperature at 50 DEG C ~ 150 DEG C, reaction time is 10 ~ 80min, obtaining vanadium concentration is 1.4mol/L ~ 2.1mol/L, Vanadium valence is 3.5+/-0.03 valency, sulfate concentration is 3.4mol/L ~ 5.2mol/L, and phosphate concentration is the electrolyte of 0.01mol/L ~ 0.3mol/L, and its chemical equation is: V
4o
7+ 5H
2sO
4=V
2(SO
4)
3+ 2VOSO
4+ 5H
2o.
Like this, owing to obtaining V from above-mentioned second step
2(SO
4)
3and VOSO
4be water-soluble substances, soluble in water, controlling Vanadium valence in the present invention is that namely the principle of 3.5+/-0.03 valency is: work as V
2(SO
4)
3and VOSO
4these two kinds of materials are according to the water-soluble electrolyte that can obtain vanadium cell and use of equimolar ratio.
According to a preferred embodiment of the invention: the V obtained in the described first step
4o
7in product, vanadium content is 64.2% ~ 64.8%.
Compared with prior art, beneficial effect of the present invention is: 1, adopt V
4o
7with strong sulfuric acid response, make reaction speed very fast, and then improve production efficiency; 2, when when extensive use electrolyte, blocks of solid electrolyte decreases packing of product demand and long-distance transport cost, decreases the solution disclosure risk in shipping storage process and processing cost; 3, by blocks of solid electrolyte rapid solution in pure water, can produce satisfactory Vanadium valence between 3.5+/-0.03 finished product electrolyte.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.And the concentration of the concentrated sulfuric acid adopted in all embodiments is 98%, density is 1.84g/ml; The concentration of phosphoric acid is 85%, and density is 1.685g/ml.
embodiment one.
The present embodiment provides a kind of manufacture method of solid electrolyte for vanadium flow battery, and it comprises the following steps:
The first step: prepare 50 kilograms and analyze pure powdery V
2o
5, and by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 12L/min
2, and controlling reaction temperature at 620 DEG C, the reaction time is 2 hours, obtains V
4o
7product, and control V
4o
7in product, vanadium content is 64.2%;
Second step: by the V obtained in the first step
4o
7product and the concentrated sulfuric acid, SPA are that 1:2.934:0.087 carries out hybrid reaction according to weight ratio, and control reaction temperature at 280 DEG C, reaction time is 180 minutes, and obtain green blocks of solid electrolyte, the valence state simultaneously chemically examining the vanadium of solid electrolyte is 3.5 valencys; Particularly, in the present embodiment, homemade raw material dish can be adopted, load 1000 grams of V
4o
7, pour 1630 milliliters of concentrated sulfuric acids and 50 milliliters of SPAs into, then raw material dish sent in tunnel calcining kiln;
3rd step: be that 4:5.3 carries out hybrid reaction in acid-resistant reacting kettle according to weight ratio by the blocks of solid electrolyte obtained in second step and pure water, can select solid electrolyte 4000 grams, pure water 5300 grams; And controlling reaction temperature at 90 DEG C, the reaction time is 20 minutes, and needs to stir in course of reaction; After question response, obtaining vanadium concentration is 1.7mol/L, and Vanadium valence is 3.5 valencys, sulfate concentration 4.3 mol/L, and the electrolyte of phosphate concentration 0.1 mol/L; Finally by experiment, adopt the electrolyte that method of the present invention is obtained, load in vanadium cell test macro and test.Voltage efficiency 80%, coulombic efficiency 97%.
embodiment two.
The present embodiment provides a kind of manufacture method of solid electrolyte for vanadium flow battery, and it comprises the following steps:
The first step: prepare 50 kilograms and analyze pure powdery V
2o
5, and by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 3L/min
2, and controlling reaction temperature at 300 DEG C, the reaction time is 4 hours, obtains V
4o
7product, and control V
4o
7in product, vanadium content is 64.2%;
Second step: by the V obtained in the first step
4o
7product and the concentrated sulfuric acid, SPA are that 1:2.347:0.07 carries out hybrid reaction according to weight ratio, and control reaction temperature at 100 DEG C, reaction time is 300 minutes, and obtain green blocks of solid electrolyte, the valence state simultaneously chemically examining the vanadium of solid electrolyte is 3.5 valencys; Concrete, in the present embodiment, homemade raw material dish can be adopted, load 1000 grams of V
4o
7, pour 1304 milliliters of concentrated sulfuric acids and 40 milliliters of SPAs into, then raw material dish sent in tunnel calcining kiln; Be that 4:4.2 carries out hybrid reaction in acid-resistant reacting kettle by the blocks of solid electrolyte obtained in second step and pure water according to weight ratio, solid electrolyte 4000 grams can be selected, pure water 4200 grams; And controlling reaction temperature at 50 DEG C, the reaction time is 60 minutes, and needs to stir in course of reaction; After question response, obtaining vanadium concentration is 1.45 mol/L, and Vanadium valence is 3.52 valencys, sulfate concentration 3.6 mol/L, and the electrolyte of phosphate concentration 0.013 mol/L; Finally by experiment, adopt the electrolyte that the method for this enforcement is obtained, load in vanadium cell test macro and test.Its voltage efficiency 81%, coulombic efficiency 99 %.
embodiment three.
The present embodiment provides a kind of manufacture method of solid electrolyte for vanadium flow battery, and it comprises the following steps:
The first step: prepare 50 kilograms and analyze pure powdery V
2o
5, and by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 20L/min
2, and controlling reaction temperature at 900 DEG C, the reaction time is 0.5 hour, obtains V
4o
7product, and control V
4o
7in product, vanadium content is 64.5 %;
Second step: by the V obtained in the first step
4o
7product and the concentrated sulfuric acid, SPA are that 1:3.52:0.104 carries out hybrid reaction according to weight ratio, and control reaction temperature at 500 DEG C, reaction time is 30 minutes, and obtain green blocks of solid electrolyte, the valence state simultaneously chemically examining the vanadium of solid electrolyte is 3.5 valencys; Concrete, in the present embodiment, homemade raw material dish can be adopted, load 1000 grams of V
4o
7, pour 1956 milliliters of concentrated sulfuric acids and 60 milliliters of SPAs into, then raw material dish sent in tunnel calcining kiln;
3rd step: be that 4:6.4 carries out hybrid reaction in acid-resistant reacting kettle according to weight ratio by the blocks of solid electrolyte obtained in second step and pure water, can select solid electrolyte 4000 grams, pure water 6400 grams; And controlling reaction temperature at 150 DEG C, the reaction time is 10 minutes, and needs to stir in course of reaction; After question response, obtaining vanadium concentration is 2.06 mol/L, and Vanadium valence is 3.47 valencys, sulfate concentration 5.15 mol/L, and the electrolyte of phosphate concentration 0.27 mol/L; Finally by experiment, adopt the electrolyte that the method for this enforcement is obtained, load in vanadium cell test macro and test.Its voltage efficiency 79 %, coulombic efficiency 97 %.
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (2)
1. a manufacture method for solid electrolyte for vanadium flow battery, is characterized in that, comprises the following steps:
The first step: by V
2o
5put into tunnel calcining kiln, and pass into H with the speed of 3L/min ~ 20L/min
2, and controlling reaction temperature at 300 DEG C ~ 900 DEG C, the reaction time is 0.5h ~ 4h, obtains V
4o
7product;
Second step: by the V obtained in the first step
4o
7product and the concentrated sulfuric acid, SPA are that 1:2.347:0.07 ~ 1:3.52:0.104 carries out hybrid reaction according to weight ratio, and control reaction temperature at 100 DEG C ~ 500 DEG C, and the reaction time is 30min ~ 300min, obtains blocks of solid electrolyte;
3rd step: be that 4:4.2-4:6.4 carries out hybrid reaction according to weight ratio by the blocks of solid electrolyte obtained in second step and pure water, and control reaction temperature at 50 DEG C ~ 150 DEG C, reaction time is 10 ~ 80min, obtaining vanadium concentration is 1.4mol/L ~ 2.1mol/L, Vanadium valence is 3.5+/-0.03 valency, sulfate concentration 3.4mol/L ~ 5.2mol/L, and the electrolyte of phosphate concentration 0.01mol/L ~ 0.3mol/L.
2. the manufacture method of solid electrolyte for vanadium flow battery according to claim 1, is characterized in that: the V obtained in the described first step
4o
7in product, vanadium content is 64.2% ~ 64.8%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310198369.3A CN103280591B (en) | 2013-05-25 | 2013-05-25 | A kind of manufacture method of solid electrolyte for vanadium flow battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310198369.3A CN103280591B (en) | 2013-05-25 | 2013-05-25 | A kind of manufacture method of solid electrolyte for vanadium flow battery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103280591A CN103280591A (en) | 2013-09-04 |
| CN103280591B true CN103280591B (en) | 2015-08-19 |
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|---|---|---|---|
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106257726B (en) * | 2016-01-28 | 2018-03-23 | 中国科学院过程工程研究所 | A kind of system and method for producing high-purity high-activity V electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09180745A (en) * | 1995-12-28 | 1997-07-11 | Nippon Chem Ind Co Ltd | Manufacture of vanadium electrolyte |
| JP2003157882A (en) * | 2001-11-21 | 2003-05-30 | Sumitomo Electric Ind Ltd | Operation method of redox flow battery |
| CN102354762B (en) * | 2011-09-30 | 2015-09-30 | 承德万利通实业集团有限公司 | A kind of preparation method of high-purity vanadium battery electrolyte |
| CN102881931A (en) * | 2012-09-26 | 2013-01-16 | 清华大学 | Phosphorus-containing all-vanadium redox flow battery anode electrolyte |
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Effective date of registration: 20240719 Address after: No. 101-1, Mancheng Commercial Street, Lianjie Town, Weiyuan County, Neijiang City, Sichuan Province 642450 Patentee after: Sichuan Development Xingxin Vanadium Energy Technology Co.,Ltd. Country or region after: China Address before: No.5, Checheng East 6th Road, Chengdu Economic and Technological Development Zone (Longquanyi District), Sichuan 610000 Patentee before: SICHUAN XINGMING ENERGY ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Country or region before: China |
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