CN115992357A - Preparation method of electrolyte of all-vanadium redox flow battery - Google Patents
Preparation method of electrolyte of all-vanadium redox flow battery Download PDFInfo
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- CN115992357A CN115992357A CN202310105342.9A CN202310105342A CN115992357A CN 115992357 A CN115992357 A CN 115992357A CN 202310105342 A CN202310105342 A CN 202310105342A CN 115992357 A CN115992357 A CN 115992357A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 35
- 239000003792 electrolyte Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229910001456 vanadium ion Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 238000009825 accumulation Methods 0.000 abstract description 3
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 208000003251 Pruritus Diseases 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
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000007803 itching Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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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 relates to the technical field of battery electrolyte preparation, and discloses a preparation method of an all-vanadium redox flow battery electrolyte, which comprises the following preparation steps: the positive electrode and the negative electrode of the electrolytic tank are respectively added with a V 2 O 5 Powder, H 2 C 2 O 4 Fully stirring and mixing the ethanol mixed solution and the dilute sulfuric acid solution at 50-90 ℃ to prepare the VOSO 4 Solution at 40mA/cm 2 ‑120 mA/cm 2 In the electrolysis current density environment, 3.5-valence vanadium ion electrolyte is obtained at the cathode of the electrolytic tank after electrolytic reduction. The invention adds H 2 C 2 O 4 Ethanol mixture, H 2 C 2 O 4 In the reaction process of the ethanol mixed solution, ethanol can be used as a defoaming agent to reduce the problem of bubble accumulation in the reaction kettle, the whole technical scheme has the advantages of relatively low preparation cost, relatively low equipment requirement, one third of consumed electric energy by an electrolysis method and the like, and the whole process is safe and environment-friendly, has no redundant exhaust gas discharge, is more energy-saving and environment-friendly, and has high safety.
Description
Technical Field
The invention relates to the technical field of battery electrolyte preparation, in particular to a preparation method of an all-vanadium redox flow battery electrolyte.
Background
Along with the ordered promotion of 'double carbon' targets in China, the hundred megawatt energy storage power station also pulls open curtains for large-scale construction. The company is arranged around the national industry planning, and a green circular economy all-vanadium industry cluster integrating a vanadium raw material base, a new vanadium material and new vanadium energy is laid out on the basis of a 'vanadium product deep processing national local combined engineering research center'.
At present, two main methods for synthesizing electrolyte of all-vanadium redox flow batteries are as follows: chemical synthesis and electrolysis.
The chemical method adopts vanadium oxide and sulfuric acid solution with certain concentration to heat and fully activate, and then adds reducing agent (S, SO) 2 Etc.) to obtain a low-valence vanadium solution with a certain concentration. The method has the advantages that the reduction substance residues influence the performance of the electrolyte, a large amount of harmful gas is generated in the preparation process, bubbles are accumulated in the reaction kettle, the reaction space is influenced, and the process equipment requirements and the vanadium conversion rate are extremely high.
The electrolytic method generally adopts an electrolytic cell device with a diaphragm or a salt bridge, V vanadium oxide is taken as a raw material, and H containing the V oxide is added into a negative electrode tank of an electrolytic system 2 SO 4 Adding H with the same concentration into the solution and the positive electrode area 2 SO 4 And adding a proper direct current power supply to the anode and the cathode, and reducing vanadium ions on the surface of the negative electrode to obtain a low-valence vanadium ion solution. The method has the advantages that the oxygen evolution reaction occurs at the positive electrode, the concentration of sulfuric acid is increased continuously, the actual production risk is relatively high, and a large amount of electric energy is consumed in the whole process.
Disclosure of Invention
In order to solve the defects of the prior art, the invention discloses a preparation method of an electrolyte of an all-vanadium redox flow battery, and provides a method combining a chemical reduction method and an electrolytic method, which can reduce the preparation cost, reduce the equipment requirement, consume one third of the electric energy as compared with the electrolytic method, and have the advantages of no discharge of redundant waste gas, energy conservation, environmental protection and high preparation safety in the whole process.
The invention discloses a preparation method of an electrolyte of an all-vanadium redox flow battery, which comprises the following preparation steps:
the positive electrode and the negative electrode of the electrolytic tank are respectively added with a V 2 O 5 Powder, H 2 C 2 O 4 Fully stirring and mixing the ethanol mixed solution and the dilute sulfuric acid solution at 50-90 ℃ to prepare the VOSO 4 Solution at 40mA/cm 2 - 120 mA/cm 2 In the electrolysis current density environment, 3.5-valence vanadium ion electrolyte is obtained at the cathode of the electrolytic tank after electrolytic reduction.
Further, adding VOSO with the same volume into the anode and the cathode of the electrolytic tank 4 A solution.
Further, the VOSO 4 The preparation method of the solution comprises the steps of firstly preparing V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 50-90deg.C, and adding H 2 C 2 O 4 Ethanol mixed solution, and obtaining VOSO after 2 hours 4 A solution.
Further, the H 2 C 2 O 4 Ethanol mixture with V 2 O 5 The weight ratio of the powder is 0.55-0.80.
Further, the concentration of the dilute sulfuric acid solution is 3.5mol/l to 4.8mol/l.
Further, an all-vanadium battery pile is adopted in the electrolysis of the electrolytic tank.
The working principle and the beneficial effects of the invention are as follows:
VOSO according to the technical scheme 4 The solution is composed of H 2 C 2 O 4 Raw materials such as ethanol mixed solution, H 2 C 2 O 4 In the reaction process of the ethanol mixed solution, ethanol not only serves as a defoamer to reduce the problem of bubble accumulation in the reaction kettle, but also has the effect of disturbing HSO (high speed oxidation) and is used for obtaining acetic acid after oxidation 4 The balance effect can enhance the stability of the positive electrode electrolyte and effectively avoid the itching reaction of the positive electrode. The technical proposal is that the preparation method is thatThe method has the advantages of low equipment dependence, energy conservation, environmental protection, high safety and the like.
Drawings
FIG. 1 is a graph of performance parameters for a first embodiment of the present invention;
FIG. 2 is a graph of performance parameters for a second embodiment of the present invention;
FIG. 3 is a graph of performance parameters for a third embodiment of the present invention;
FIG. 4 is a graph of performance parameters for a fourth embodiment of the present invention;
fig. 5 is a graph of performance versus four examples of the present invention.
Description of the embodiments
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to solve the problems in the background art, the applicant provides a method combining a chemical synthesis method and an electrolytic method, which can eliminate the technical defects in the background art. The invention discloses a preparation method of an electrolyte of an all-vanadium redox flow battery, which comprises the following preparation steps:
the positive electrode and the negative electrode of the electrolytic tank are respectively added with a V 2 O 5 Powder, H 2 C 2 O 4 Fully stirring and mixing the ethanol mixed solution and the dilute sulfuric acid solution at 50-90 ℃ to prepare the VOSO 4 Solution at 40mA/cm 2 - 120 mA/cm 2 Under the condition of electrolysis current density, 3.5-valence vanadium ion electrolyte is obtained at the cathode of the electrolytic tank after electrolytic reduction. H 2 C 2 O 4 In the reaction process of the ethanol mixed solution, ethanol not only can be used as a defoamer to reduce the problem of bubble accumulation in a reaction kettle, but also can be used for obtaining acetic acid after oxidation and disturbing HSO 4 The balance effect can enhance the stability of the positive electrode electrolyte, effectively avoid the itching reaction of the positive electrode, and the reaction of the positive electrode Is V (IV) +e+ & fwdarw V (V).
Examples
V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 80deg.C for 1 hr, and adding appropriate amount of H 2 C 2 O 4 Stirring the powder for 2 hours to obtain VOSO 4 A solution. The tetravalent vanadium conversion rate is above 96%, and meets the index requirement. Then the electrolyte is subjected to the electrolysis of an all-vanadium battery pile, and the current density is 40mA/cm 2 And (3) carrying out electrolysis in the environment to obtain a solution 1, and carrying out performance test on the assembled all-vanadium redox flow battery by using the solution to evaluate the performance of the electrolyte, wherein the performance parameters are shown in figure 1.
Examples
V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 80deg.C for 1 hr, and adding appropriate amount of H 2 C 2 O 4 Stirring the powder for 2 hours to obtain VOSO 4 A solution. The tetravalent vanadium conversion rate is above 96%, and meets the index requirement. Then the electrolyte is subjected to the electrolysis of an all-vanadium battery pile, and the current density is 80mA/cm 2 And (3) carrying out electrolysis in the environment to obtain a solution 2, and carrying out performance test on the assembled all-vanadium redox flow battery by using the solution to evaluate the performance of the electrolyte, wherein the performance parameters are shown in figure 2.
Examples
V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 80deg.C for 1 hr, and adding appropriate amount of H 2 C 2 O 4 Ethanol mixed solution, and obtaining VOSO after 2 hours 4 A solution. The tetravalent vanadium conversion rate is above 96%, and meets the index requirement. Then the electrolyte is subjected to the electrolysis of an all-vanadium battery pile, and the current density is 40mA/cm 2 And (3) carrying out electrolysis in the environment to obtain a solution 3, and carrying out performance test on the assembled all-vanadium redox flow battery by using the solution to evaluate the performance of the electrolyte, wherein the performance parameters are shown in figure 3.
Examples
V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 80deg.C for 1 hr, and adding appropriate amount of H 2 C 2 O 4 Ethanol mixed solution, and obtaining VOSO after 2 hours 4 A solution. The tetravalent vanadium conversion rate is above 96%, and meets the index requirement. Then the electrolyte is subjected to the electrolysis of an all-vanadium battery pile, and the current density is 80mA/cm 2 Electrolysis under the environment to obtain solution 4, thus dissolvingThe performance of the liquid-assembled all-vanadium redox flow battery was tested to evaluate the electrolyte performance, with performance parameters as shown in fig. 4.
In combination with the four examples, as shown in FIG. 5, it can be seen that H is added 2 C 2 O 4 Mixing the ethanol mixed solution with dilute sulfuric acid and simply adding H 2 C 2 O 4 The powder is mixed with dilute sulfuric acid, the coulomb efficiency and the voltage efficiency can be improved by more than 2%, the energy efficiency can be improved by more than 4%, and the V (V) concentration and the V concentration are improved under the condition that the charging depth (SOC) is 70%.
Finally, it should be noted that: the above embodiments are only for illustrating the present invention and not for limiting the technical solution described in the present invention; thus, while the invention has been described in detail with reference to the various embodiments described above, it will be understood by those skilled in the art that the invention may be modified or equivalents; all technical solutions and modifications thereof that do not depart from the spirit and scope of the present invention are intended to be included in the scope of the appended claims.
Claims (6)
1. The preparation method of the electrolyte of the all-vanadium redox flow battery is characterized by comprising the following steps of: the preparation method comprises the following preparation steps:
the positive electrode and the negative electrode of the electrolytic tank are respectively added with a V 2 O 5 Powder, H 2 C 2 O 4 Fully stirring and mixing the ethanol mixed solution and the dilute sulfuric acid solution at 50-90 ℃ to prepare the VOSO 4 Solution at 40mA/cm 2 - 120 mA/cm 2 In the electrolysis current density environment, 3.5-valence vanadium ion electrolyte is obtained at the cathode of the electrolytic tank after electrolytic reduction.
2. The method for preparing the electrolyte of the all-vanadium redox flow battery, which is disclosed in claim 1, is characterized in that: adding VOSO with the same volume into the anode and the cathode of the electrolytic tank 4 A solution.
3. The method for preparing the electrolyte of the all-vanadium redox flow battery according to claim 2, wherein the method comprises the following steps: the VOSO 4 The preparation method of the solution comprises the steps of firstly preparing V 2 O 5 Mixing the powder with dilute sulfuric acid solution at 50-90deg.C, and adding H 2 C 2 O 4 Ethanol mixed solution, and obtaining VOSO after 2 hours 4 A solution.
4. The method for preparing the electrolyte of the all-vanadium redox flow battery according to claim 3, wherein the method comprises the following steps: the H is 2 C 2 O 4 Ethanol mixture with V 2 O 5 The weight ratio of the powder is 0.55-0.80.
5. The method for preparing the electrolyte of the all-vanadium redox flow battery, which is disclosed in claim 4, is characterized in that: the concentration of the dilute sulfuric acid solution is 3.5mol/l to 4.8mol/l.
6. The method for preparing the electrolyte of the all-vanadium redox flow battery, which is disclosed in claim 1, is characterized in that: and an all-vanadium battery pile is adopted in the electrolysis of the electrolytic tank.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116504994A (en) * | 2023-06-28 | 2023-07-28 | 杭州德海艾科能源科技有限公司 | All-vanadium redox flow battery negative electrode dual-function additive and preparation method and application thereof |
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| 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 |
| CN114447386A (en) * | 2021-12-21 | 2022-05-06 | 陕西华银科技股份有限公司 | Preparation method of all-vanadium redox flow battery electrolyte |
| WO2022114926A1 (en) * | 2020-11-30 | 2022-06-02 | 롯데케미칼 주식회사 | Method for producing electrolyte for vanadium redox flow battery |
| KR20220132971A (en) * | 2021-03-24 | 2022-10-04 | 한국전력공사 | electrolyte for vanadium redox flow battery and the method of preparing the same, vanadium redox flow battery comprising thereof |
| CN115418653A (en) * | 2022-09-14 | 2022-12-02 | 鞍钢集团北京研究院有限公司 | Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction |
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- 2023-02-13 CN CN202310105342.9A patent/CN115992357A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105006585A (en) * | 2015-06-09 | 2015-10-28 | 陈曦 | Preparation method of electrolyte for all-vanadium redox-flow battery |
| 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 |
| WO2022114926A1 (en) * | 2020-11-30 | 2022-06-02 | 롯데케미칼 주식회사 | Method for producing electrolyte for vanadium redox flow battery |
| KR20220132971A (en) * | 2021-03-24 | 2022-10-04 | 한국전력공사 | electrolyte for vanadium redox flow battery and the method of preparing the same, vanadium redox flow battery comprising thereof |
| CN114447386A (en) * | 2021-12-21 | 2022-05-06 | 陕西华银科技股份有限公司 | Preparation method of all-vanadium redox flow battery electrolyte |
| CN115418653A (en) * | 2022-09-14 | 2022-12-02 | 鞍钢集团北京研究院有限公司 | Method for preparing vanadium battery electrolyte by electrolysis through coupling reaction |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116504994A (en) * | 2023-06-28 | 2023-07-28 | 杭州德海艾科能源科技有限公司 | All-vanadium redox flow battery negative electrode dual-function additive and preparation method and application thereof |
| CN116504994B (en) * | 2023-06-28 | 2023-09-29 | 杭州德海艾科能源科技有限公司 | All-vanadium redox flow battery negative electrode dual-function additive and preparation method and application thereof |
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