CN115036547A - Preparation method of ion-conducting membrane for all-vanadium redox flow battery - Google Patents
Preparation method of ion-conducting membrane for all-vanadium redox flow battery Download PDFInfo
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- CN115036547A CN115036547A CN202210487131.1A CN202210487131A CN115036547A CN 115036547 A CN115036547 A CN 115036547A CN 202210487131 A CN202210487131 A CN 202210487131A CN 115036547 A CN115036547 A CN 115036547A
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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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- 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
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
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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 invention discloses a preparation method of an ion-conducting membrane for an all-vanadium flow battery, relating to the technical field of all-vanadium flow batteries 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 Performing crystallization reaction in a mixed solution of O) and sodium fluoride (NaF), and then placing in NH 4 And (3) washing and calcining the washed and calcined Cl aqueous solution, wherein the calcined flaky alumina carrier is the ion conducting membrane for the all-vanadium flow battery. The invention provides a preparation method of an ion conduction membrane for an all-vanadium redox flow battery, which can be detected according to the comparison table, and the prepared membrane has the advantages of good hydrogen ion selective permeability, vanadium ion permeation resistance, excellent acid resistance stability and the like, and can be applied to the preparation of the ion conduction membrane for the all-vanadium redox flow batteryThe method is used for the all-vanadium flow battery, and can also be used for gas separation, liquid separation or ion separation.
Description
Technical Field
The invention relates to the technical field of all-vanadium redox flow batteries, in particular to a preparation method of an ion conduction membrane for an all-vanadium redox flow battery.
Background
The flow battery is a high-capacity electrochemical energy storage device which uses flowing electrolyte solution as an energy storage medium, has the most remarkable characteristics of capability of realizing independent regulation and control of power and capacity, and has the characteristics of high safety, large energy storage scale, high efficiency, long service life and the like, and has good application prospect in the field of large-scale energy storage. In recent years, the research on flow batteries has been rapidly advanced.
The Vanadium Redox Flow Battery (VRB) adopts electrolytes of the same elements at two poles, avoids cross contamination caused by mutual permeation of different active substances between a positive pole and a negative pole, has the characteristics of long service life, repeatable discharge, high reliability and the like, is rich in Vanadium resource reserves in China, and is considered by the industry and academia to be the most suitable for the development of the China.
The electrolyte of the all-vanadium flow battery generally has strong acidity. The hydrogen ion conduction membrane is one of key materials of the all-vanadium redox flow battery, and on one hand, the membrane separates positive and negative electrolytes so as to avoid cross contamination of positive and negative active ions and self-discharge; and on the other hand, hydrogen ions are allowed to pass through to form an internal circuit of the battery.
At present, high cost still serves as a bottleneck for restricting large-scale popularization and application of the all-vanadium redox flow battery, and the development of a high-performance ion conduction membrane is one of important ways for reducing the cost of the battery and is also a key for promoting the development of the energy storage industry in China.
Therefore, developing an ion conducting membrane with low cost, high mechanical strength, good chemical stability and acid resistance stability, and excellent hydrogen ion permselectivity and vanadium ion permeation resistance is crucial to the development of all-vanadium flow batteries.
Disclosure of Invention
The invention aims to provide a preparation method of an ion conduction membrane for an all-vanadium flow battery, and aims to solve the defects in the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme: a preparation method of an ion conduction membrane for an all-vanadium flow battery comprises the following specific preparation steps:
step one, soaking a clean and dry sheet-shaped alumina carrier in a tetrapropyl ammonium hydride water solution, taking out the alumina carrier after a period of time, and drying the alumina carrier for 1 hour at the temperature of 40 ℃.
Step two, distilled water (H) 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O) and sodium fluoride (NaF) are taken as raw materials, sequentially added into a glass bottle, stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 O is 0.001-0.02, SiO 2 0.0001-0.05 of/H2O, Al 2 (SO 4 ) 3 /H 2 O is 0.00005-0.03, NaF/H 2 O is 0.000005-0.015.
And step three, soaking the flaky alumina carrier obtained in the step one in the mixed solution obtained in the step two again, taking out the flaky alumina carrier after a period of time, putting the flaky alumina carrier into a stainless steel reaction kettle, putting the stainless steel reaction kettle into an oven at a certain temperature for crystallization reaction for a period of time, taking out the flaky alumina carrier after the reaction is finished, growing a thin and compact molecular sieve film on the outer surface of the carrier, washing the carrier by using distilled water, drying the carrier in the oven at 100 ℃, and then calcining the carrier for 6 hours in a high-temperature furnace at 550 ℃, wherein the crystallization temperature of the crystallization reaction is 80-200 ℃, and the reaction time is 2-48 hours.
Step four, placing the flaky alumina carrier obtained in the step three in NH 4 And refluxing the Cl aqueous solution for 2-12h at 60-90 ℃, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ oven, and calcining the sheet alumina carrier for 6h in a 550 ℃ high-temperature furnace, wherein the calcined sheet alumina carrier is the ion-conducting membrane for the all-vanadium flow battery.
Preferably, the sheet alumina carrier in the first step is a porous carrier, and the pore size of the carrier is 100nm-10 μm.
Preferably, the mass fraction of tetrapropylammonium hydroxide in the tetrapropylammonium hydroxide aqueous solution in the first step is 1-30%.
Preferably, the impregnation time of the alumina carrier in the first step is 10-600 s.
Preferably, silica Sol (SiO) in step two 2 ·nH 2 O) SiO 2 The mass fraction is 20-40%.
Preferably, the crystallization temperature of the crystallization reaction in the step three is 100-.
Preferably, the dipping time of the alumina carrier in the step three is 10-600 s.
Preferably, NH in step four 4 NH of aqueous Cl solution 4 The mass fraction of Cl is 5-30%.
Preferably, the ion conducting membrane prepared by the invention is applied to an all-vanadium flow battery.
Preferably, the ion conducting membrane prepared by the invention is used for gas separation, liquid separation or ion separation in the all-vanadium flow battery.
In the technical scheme, the invention provides the following technical effects and advantages:
the invention provides a preparation method of an ion conduction membrane for an all-vanadium redox flow battery, and the ion conduction membrane can be detected according to the comparison table.
Detailed Description
The present invention will be described in further detail below in order to enable those skilled in the art to better understand the technical solution of the present invention.
Example one
The invention provides a preparation method of an ion conduction membrane for an all-vanadium redox flow battery, which comprises the following specific preparation steps:
step one, soaking a clean and dry flake alumina carrier in a 5 wt% tetrapropyl ammonium hydride aqueous solution for 10-600s, and then drying at 40 ℃ for 1h, wherein the alumina carrier is a porous carrier with the pore size of 100nm-10 mu m.
Step two, distilled water (H) 2 O)、Sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O) and sodium fluoride (NaF) are taken as raw materials, sequentially added into a glass bottle, stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 O is 0.01, SiO 2 /H 2 O is 0.02 and Al 2 (SO 4 ) 3 /H 2 O is 0.0005, NaF/H 2 O is 0.0002, silica Sol (SiO) 2 ·nH 2 SiO) of O) 2 The mass fraction is 20-40%.
And step three, soaking the flaky alumina carrier obtained in the step one in the mixed solution obtained in the step two again, taking out the flaky alumina carrier after a period of time, putting the flaky alumina carrier into a stainless steel reaction kettle, putting the stainless steel reaction kettle into an oven at a certain temperature for crystallization reaction for a period of time, taking out the flaky alumina carrier after the reaction is finished, growing a thin and compact molecular sieve film on the outer surface of the carrier, washing the carrier by using distilled water, drying the carrier in the oven at 100 ℃, and then calcining the carrier in a high-temperature furnace at 550 ℃ for 6 hours, wherein the crystallization temperature of the crystallization reaction is 175 ℃ and the reaction time is 12 hours.
Step four, placing the flaky alumina carrier obtained in the step three in 15 wt% of NH 4 And refluxing the mixture in a Cl aqueous solution at 90 ℃ for 6h, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ oven, and calcining the sheet alumina carrier in a 550 ℃ high-temperature furnace for 6h, wherein the calcined sheet alumina carrier is the ion conducting membrane for the all-vanadium flow battery.
Example two
A preparation method of an ion conduction membrane for an all-vanadium flow battery comprises the following specific preparation steps:
step one, soaking a clean and dry flake alumina carrier in a 15 wt% tetrapropyl ammonium hydride aqueous solution for 10-600s, and then drying at 40 ℃ for 1h, wherein the alumina carrier is a porous carrier with the pore size of 100nm-10 mu m.
Step two, distilled water (H) 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O)And sodium fluoride (NaF) as raw materials are sequentially added into a glass bottle and stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 O is 0.01, SiO 2 /H 2 O is 0.02 and Al 2 (SO 4 ) 3 /H 2 O is 0.0005, NaF/H 2 O is 0.0002, silica Sol (SiO) 2 ·nH 2 O) SiO 2 The mass fraction is 20-40%.
And step three, soaking the flaky alumina carrier obtained in the step one in the mixed solution obtained in the step two again, taking out the flaky alumina carrier after a period of time, putting the flaky alumina carrier into a stainless steel reaction kettle, putting the stainless steel reaction kettle into an oven at a certain temperature for crystallization reaction for a period of time, taking out the flaky alumina carrier after the reaction is finished, growing a thin and compact molecular sieve film on the outer surface of the carrier, washing the carrier by using distilled water, drying the carrier in the oven at 100 ℃, and then calcining the carrier in a high-temperature furnace at 550 ℃ for 6 hours, wherein the crystallization temperature of the crystallization reaction is 175 ℃ and the reaction time is 12 hours.
Step four, placing the flaky alumina carrier obtained in the step three in 15 wt% NH 4 And refluxing the Cl aqueous solution for 6h at 90 ℃, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ drying oven, and calcining the sheet alumina carrier for 6h in a 550 ℃ high-temperature furnace, wherein the calcined sheet alumina carrier is the ion conducting membrane for the all-vanadium flow battery.
EXAMPLE III
A preparation method of an ion conduction membrane for an all-vanadium flow battery comprises the following specific preparation steps:
step one, soaking a clean and dry flake alumina carrier in a 5 wt% tetrapropyl ammonium hydride aqueous solution for 10-600s, and then drying at 40 ℃ for 1h, wherein the alumina carrier is a porous carrier with the pore size of 100nm-10 mu m.
Step two, distilled water (H) 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O) and sodium fluoride (NaF) are taken as raw materials, sequentially added into a glass bottle, stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 The content of O is 0.01,SiO 2 /H 2 o is 0.02 and Al 2 (SO 4 ) 3 /H 2 O is 0.00005, NaF/H 2 O is 0.0002, silica Sol (SiO) 2 ·nH 2 O) SiO 2 The mass fraction is 20-40%.
And step three, soaking the sheet alumina carrier obtained in the step one in the mixed solution obtained in the step two again, taking out the sheet alumina carrier after a period of time, putting the sheet alumina carrier into a stainless steel reaction kettle, placing the stainless steel reaction kettle in an oven at a certain temperature for crystallization reaction for a period of time, taking out the sheet alumina carrier after the reaction is finished, growing a thin and compact molecular sieve membrane on the outer surface of the carrier, washing the carrier by distilled water, drying the carrier in the oven at 100 ℃, and calcining the carrier in a high-temperature furnace at 550 ℃ for 6 hours, wherein the crystallization temperature of the crystallization reaction is 175 ℃ and the reaction time is 12 hours.
Step four, placing the flaky alumina carrier obtained in the step three in 15 wt% NH 4 And refluxing the Cl aqueous solution for 6h at 90 ℃, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ drying oven, and calcining the sheet alumina carrier for 6h in a 550 ℃ high-temperature furnace, wherein the calcined sheet alumina carrier is the ion conducting membrane for the all-vanadium flow battery.
Example four
A preparation method of an ion conduction membrane for an all-vanadium flow battery comprises the following specific preparation steps:
step one, soaking a clean and dry flake alumina carrier in a 5 wt% tetrapropyl ammonium hydride aqueous solution for 10-600s, and then drying at 40 ℃ for 1h, wherein the alumina carrier is a porous carrier with the pore size of 100nm-10 mu m.
Step two, distilled water (H) is used 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O) and sodium fluoride (NaF) are taken as raw materials, sequentially added into a glass bottle, stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 O is 0.01, SiO 2 /H 2 O is 0.02 and Al 2 (SO 4 ) 3 /H 2 O is 0.0005, NaF/H 2 O is 0.0002, silica sol(SiO 2 ·nH 2 O) SiO 2 The mass fraction is 20-40%.
And step three, soaking the sheet alumina carrier obtained in the step one in the mixed solution obtained in the step two, taking out the sheet alumina carrier after a period of time, putting the sheet alumina carrier into a stainless steel reaction kettle, placing the stainless steel reaction kettle in an oven at a certain temperature for crystallization reaction for a period of time, taking out the sheet alumina carrier after the reaction is finished, growing a thin and compact molecular sieve membrane on the outer surface of the carrier, washing the carrier by distilled water, drying the carrier in the oven at 100 ℃, and then calcining the carrier in a high-temperature furnace at 550 ℃ for 6 hours, wherein the crystallization temperature of the crystallization reaction is 175 ℃ and the reaction time is 48 hours.
Step four, placing the flaky alumina carrier obtained in the step three in 15 wt% of NH 4 And refluxing the Cl aqueous solution for 6h at 90 ℃, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ drying oven, and calcining the sheet alumina carrier for 6h in a 550 ℃ high-temperature furnace, wherein the calcined sheet alumina carrier is the ion conducting membrane for the all-vanadium flow battery.
TABLE 1 ion conducting film Performance comparison Table prepared by each example
| Stability against acid | Hydrogen ion permselectivity | Resistance to penetration by vanadium ions | |
| Example one | Good taste | Height of | Good taste |
| Example two | Is better | Is higher than | Good for |
| EXAMPLE III | Is excellent in | Is low in | Good taste |
| Example four | Good taste | Is low in | Is excellent in |
In conclusion, the invention provides a preparation method of an ion conduction membrane for an all-vanadium flow battery, and the ion conduction membrane can be detected according to the comparison table, and the membrane prepared by the invention has the advantages of good hydrogen ion selective permeability, vanadium ion permeation resistance, excellent acid resistance stability and the like, can be applied to the all-vanadium flow battery, and can also be used for gas separation, liquid separation or ion separation.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the foregoing description is illustrative in nature and is not to be construed as limiting the scope of the invention as claimed.
Claims (10)
1. A preparation method of an ion conduction membrane for an all-vanadium flow battery is characterized by comprising the following specific preparation steps:
step one, soaking a clean and dry sheet-shaped alumina carrier in a tetrapropyl ammonium hydride aqueous solution, taking out the alumina carrier after a period of time, and drying the alumina carrier for 1 hour at the temperature of 40 ℃.
Step two, distilled water (H) 2 O), sodium hydroxide (NaOH), silica Sol (SiO) 2 ·nH 2 O), aluminum sulfate octadecahydrate (Al) 2 (SO 4 ) 3 ·18H 2 O) and sodium fluoride (NaF) are taken as raw materials, sequentially added into a glass bottle, stirred by a special stirrer until the solution is uniformly mixed, wherein NaOH/H 2 O is 0.001-0.02, SiO 2 0.0001-0.05 of/H2O, Al 2 (SO 4 ) 3 /H 2 O is 0.00005-0.03, NaF/H 2 O is 0.000005-0.015.
And step three, soaking the flaky alumina carrier obtained in the step one in the mixed solution obtained in the step two again, taking out the flaky alumina carrier after a period of time, putting the flaky alumina carrier into a stainless steel reaction kettle, placing the stainless steel reaction kettle in an oven at a certain temperature for crystallization reaction for a period of time, taking out the flaky alumina carrier after the reaction is finished, growing a thin and compact molecular sieve membrane on the outer surface of the carrier, washing the carrier by distilled water, drying the carrier in the oven at 100 ℃, and calcining the carrier in a high-temperature furnace at 550 ℃ for 6 hours, wherein the crystallization temperature of the crystallization reaction is 80-200 ℃, and the reaction time is 2-48 hours.
Step four, placing the flaky alumina carrier obtained in the step three in NH 4 And refluxing the Cl aqueous solution for 2-12h at 60-90 ℃, taking out the sheet alumina carrier, washing the sheet alumina carrier by using distilled water, drying the sheet alumina carrier in a 100 ℃ oven, and calcining the sheet alumina carrier for 6h in a 550 ℃ high-temperature furnace, wherein the calcined sheet alumina carrier is the ion-conducting membrane for the all-vanadium flow battery.
2. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: in the first step, the sheet alumina carrier is a porous carrier, and the pore size of the carrier is 100nm-10 mu m.
3. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: in the first step, the mass fraction of the tetrapropylammonium hydroxide in the tetrapropylammonium hydroxide aqueous solution is 1-30%.
4. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: and in the first step, the dipping time of the alumina carrier is 10-600 s.
5. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: silica Sol (SiO) in the second step 2 ·nH 2 SiO) of O) 2 The mass fraction is 20-40%.
6. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: the crystallization temperature of the crystallization reaction in the third step is 100-.
7. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: in the third step, the impregnation time of the alumina carrier is 10-600 s.
8. The method for preparing the ion conducting membrane for the all-vanadium flow battery according to claim 1, wherein the method comprises the following steps: NH in the fourth step 4 NH of aqueous Cl solution 4 The mass fraction of Cl is 5-30%.
9. Use of an ion-conducting membrane prepared according to claim 1, characterized in that: the ion conducting membrane is applied to an all-vanadium flow battery.
10. Use of an ion-conducting membrane according to claim 9, characterized in that: the ion conducting membrane is used for gas separation, liquid separation or ion separation in an all-vanadium flow battery.
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