CN108899568A - A kind of all-vanadium flow battery amberplex and preparation method thereof - Google Patents
A kind of all-vanadium flow battery amberplex and preparation method thereof Download PDFInfo
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- CN108899568A CN108899568A CN201810733917.0A CN201810733917A CN108899568A CN 108899568 A CN108899568 A CN 108899568A CN 201810733917 A CN201810733917 A CN 201810733917A CN 108899568 A CN108899568 A CN 108899568A
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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
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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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 kind of all-vanadium flow battery amberplexes and preparation method thereof.The present invention obtains the solution that mass concentration is 8~12% by the way that the polyether sulfone after sulfonation to be dissolved in dimethyl acetamide, phosphotungstic acid hydrate is added into the solution, mass concentration of the phosphotungstic acid hydrate in the solution is 7%, 90~95 DEG C and mechanical stirring 2.5~3.5 hours are heated to, mixed solution is obtained；Above-mentioned mixed solution is cast on clean glass plate, solvent is heated to evaporate to obtain by the glass plate of film uniform fold, by the glass plate of uniform fold first at 80 DEG C dry 10h, be then warming up to 100 DEG C of dry 10h, be cooled to room temperature after, by film from glass plate isolated all-vanadium flow battery amberplex.All-vanadium flow battery amberplex of the present invention shows extremely low vanadium ion permeability and good battery performance, has excellent performance, and manufacturing cost is cheap, has good commercial application prospect.
Description
Technical field
The invention belongs to battery technology field more particularly to a kind of all-vanadium flow battery amberplex and its preparation sides
Method.
Background technique
All-vanadium flow battery is a kind of efficient electrochemical energy storage materials, and the electrolyte containing active material vanadium ion is
Power storage medium is stored in outside batteries storage tank.Vanadium electrolyte solution enters pile by the circulatory system, in electrode table
Redox reaction occurs for face.When electric discharge, battery plus-negative plate potential difference is reduced, and chemical energy is converted into electric energy；When charging, battery
Positive and negative anodes potential difference increases, and electric energy is converted into chemical energy, to realize the storage and release of electric energy.
However, vanadium redox flow battery so far could not large-scale commercial applications application maximum bottleneck, be one ion of important component therein
Stability, selective penetrated property and its cost of exchange membrane fail the requirement for reaching business energy-storage battery.Therefore, exploitation performance it is good,
Amberplex at low cost is most important to the development of vanadium redox flow battery, also to China's Resources for construction economizing type and environmental-friendly
Type society is of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of all-vanadium flow battery amberplexes and preparation method thereof, it is intended to solve
The problem of vanadium redox flow battery amberplex selectivity.
The invention is realized in this way a kind of preparation method of all-vanadium flow battery amberplex, this method include with
Lower step：
(1) polyether sulfone after sulfonation is dissolved in and obtains the solution that mass concentration is 8~12% in dimethyl acetamide, it is past
Phosphotungstic acid hydrate is added in the solution, mass concentration of the phosphotungstic acid hydrate in the solution is 8%, is heated to 90~95
DEG C and mechanical stirring 2.5~3.5 hours, obtain mixed solution；
(2) above-mentioned mixed solution is cast on clean glass plate, is heated to solvent and evaporates to obtain uniformly to be covered by film
The glass plate of uniform fold is first dried 10h at 80 DEG C, is then warming up to 100 DEG C of dry 10h, is cooled to by the glass plate of lid
After room temperature, film is separated from glass plate.
Preferably, in step (1), the sulfonation process of the polyether sulfone is specially：
A, 10 grams of polyether sulfone powder are slowly added to the H that 100ml mass concentration is 98%2SO4In solution；
B, 20ml camphorsulfonic acid at room temperature, is added dropwise to H by the speed of 2~4 seconds/drop2SO4In solution, it is added dropwise
After reaction solution is poured into ice water, mechanical stirring terminate reaction；
C, will terminate the product after reacting is wash with distilled water 7 to pH value, obtains sulfonation within dry 12 hours at 80 DEG C
Polyether sulfone afterwards.
Preferably, in step (1), the mass concentration of sulfonated polyether sulfone is 10% in the solution.
Preferably, in step (2), the process that the film is separated from glass plate is：By glass be immersed in from
Make thin film separation in sub- water, the film after separation is rinsed, drying.
Compared with the prior art the shortcomings that and deficiency, the invention has the advantages that：
(1) all-vanadium flow battery amberplex of the present invention shows extremely low vanadium ion permeability and good battery
Performance, the low level-one of vanadium ion permeability ratio Nafion112 film；
(2) vanadium redox flow battery of exchange membrane of the present invention is applied, capacitance loss significantly reduces, and coulombic efficiency (is greater than
98%), while there is higher higher energy efficiency (85%), it is high than Nafion112 film (85.7% and 79.3%)；
(3) in self discharge test, exchange membrane of the present invention is shown in the Duration Ratio of open electric circuit decaying
Nafion112 film is 1.5 times long；
(4) exchange membrane of the present invention has excellent performance, and manufacturing cost is cheap, before having good business application
Scape.
Detailed description of the invention
Fig. 1 is the measuring device of vanadium permeability；
Fig. 2 is the scanning electron microscope (SEM) photograph of invention all-vanadium flow battery amberplex；Wherein, Fig. 2 a is S1.0T0.0Film；Fig. 2 b
For S0.9T0.1Film；Fig. 2 c is S0.6T0.4Film；
Fig. 3 is Nafion112, S1.0T0.0And S0.6T0.4The comparison result of the vanadium ion permeability of film；
Fig. 4 is the ion selectivity comparison result of each film；
Fig. 5 is with Nafion112 film and S0.6T0.4Film (37mAcm-2) be vanadium redox flow battery obtained by material charge and discharge it is bent
Line comparison result.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments,
The present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1
(1) 10 grams of polyether sulfone powder are slowly added to the H that 100ml mass concentration is 98%2SO4In solution；In room temperature
Under, 20ml camphorsulfonic acid is added dropwise to H by the speed of 2~4 seconds/drop2SO4In solution, by reaction solution after completion of dropwise addition
It pours into ice water, mechanical stirring terminates reaction；It is wash with distilled water 7 to pH value that the product after reacting, which will be terminated, at 80 DEG C
Obtain the polyether sulfone after sulfonation within dry 12 hours；
(2) polyether sulfone after sulfonation is dissolved in and obtains the solution that mass concentration is 12% in dimethyl acetamide, it is molten toward this
Phosphotungstic acid hydrate is added in liquid, mass concentration of the phosphotungstic acid hydrate in the solution is 8%, is heated to 90~95 DEG C simultaneously
Mechanical stirring 2.5~3.5 hours, obtain mixed solution；
(3) above-mentioned mixed solution is cast on clean glass plate, is heated to solvent and evaporates to obtain uniformly to be covered by film
The glass plate of uniform fold is first dried 10h at 80 DEG C, is then warming up to 100 DEG C of dry 10h, is cooled to by the glass plate of lid
After room temperature, glass immersion is made into thin film separation in deionized water, the film after separation is rinsed, drying, obtains full vanadium liquid
Galvanic battery amberplex S0.6T0.4(SxTyIn, S represents sulfonated polyether sulfone, and T represents phosphotungstic acid, and X is above-mentioned steps multiplied by 2
(2) in mixed solution sulfonated polyether sulfone mass concentration, y multiplied by 2 be above-mentioned steps (2) mixed solution in phosphotungstic acid matter
Measure concentration).
Embodiment 2
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), by the polyether sulfone after sulfonation
It is dissolved in and obtains the solution that mass concentration is 8% in dimethyl acetamide, and final product is all-vanadium flow battery ion exchange
Film S0.4T0.4。
Comparative example 1
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), phosphotungstic acid hydration is not added
Object, and final product is all-vanadium flow battery amberplex S1.0T0.0。
Comparative example 2
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), by the polyether sulfone after sulfonation
It is dissolved in and obtains the solution that mass concentration is 18% in dimethyl acetamide, phosphotungstic acid hydrate, phosphotungstic acid are added into the solution
Mass concentration of the hydrate in the solution is 2%, and final product is all-vanadium flow battery amberplex S0.9T0.1。
Comparative example 3
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), by the polyether sulfone after sulfonation
It is dissolved in and obtains the solution that mass concentration is 16% in dimethyl acetamide, phosphotungstic acid hydrate, phosphotungstic acid are added into the solution
Mass concentration of the hydrate in the solution is 4%, and final product is all-vanadium flow battery amberplex S0.8T0.2。
Comparative example 4
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), by the polyether sulfone after sulfonation
It is dissolved in and obtains the solution that mass concentration is 14% in dimethyl acetamide, phosphotungstic acid hydrate, phosphotungstic acid are added into the solution
Mass concentration of the hydrate in the solution is 6%, and final product is all-vanadium flow battery amberplex S0.7T0.3。
Comparative example 5
The embodiment is identical as above-described embodiment 1, the difference is that, in step (2), by the polyether sulfone after sulfonation
It is dissolved in and obtains the solution that mass concentration is 10% in dimethyl acetamide, phosphotungstic acid hydrate, phosphotungstic acid are added into the solution
Mass concentration of the hydrate in the solution is 10%, and final product is all-vanadium flow battery amberplex S0.5T0.5。
Effect example
1, to all-vanadium flow battery amberplex S obtained in above-described embodiment1.0T0.0、S0.9T0.1、S0.8T0.2、
S0.7T0.3、S0.6T0.4、S0.5T0.5And the pattern and battery performance of existing Nafion112 carries out test experiments, specific test side
Method is as follows：
(1) film thickness is tested：Film thickness is one of important parameter of amberplex, take dry membrane sample 2cm ×
The rectangle micrometer of 2cm size respectively to four angles of membrane sample rectangle and quadrangle and center thickness detect and ask flat
Mean value, measurement error is at ± 20 μm.
(2) test of water absorption rate：Water absorption rate is also one of important parameter of amberplex, can calculate film by following formula
Water absorption rate：
WsAnd WdryWeight respectively after water suction with dry film.
(3) ion exchange capacity (IEC) test of film
It is measured using conventional acid-base titration, specially：Film is immersed in 1M NaCl solution 24 hours, proton
By sodium ion exchange, acid is converted into sodium salt, the NaOH drop that the proton exchanged in solution (hydrogen ion) is titrated as 0.05mol/L
It is fixed.The calculation formula of ion exchange capacity is：
In formula, VNaOHAnd CNaOHIt is the volume and concentration of the NaOH standard solution of consumption, WdIt is the matter of membrane sample after drying
Amount.
According to document sulfonation degree DS can be calculated with following formula：
(4) proton conductivity is tested
(electrochemical workstation CHI760C) proton conductivity is measured with electrochemistry AC impedence method.Perturbation voltage AC is
5.0mV frequency range 1.0Hz to 100kHz. proton conductivity (σ) can be calculated with following formula：
σ=L/AR
L is two interelectrode distances, and A is the real contact area of sample film, and R is the impedance of film.
(5) vanadium performance test is hindered
The permeability of vanadium ion (IV) by with the diffusion battery measuring device of UF membrane as shown in Figure 1, device mainly has
Two and half electrolytic cells, centre are separated by diaphragm.1.5M VOSO is housed in the electrolytic cell of right side4/3M H2SO4In solution, in order to reduce
Left side is equipped with 1.5M MgSO because osmotic pressure caused by concentration difference changes in the electrolytic cell on the left side4/3M H2SO4, each half electricity
Liquor capacity is 45ml in solution slot, and the area of film is 3.14cm2.Both ends electrolytic cell is constantly carried out with magnetic agitation pump
It recycles in order to avoid there is concentration polarization.Left side Adlerika is taken to measure by ultraviolet-visible spectrophotometer at regular intervals
Its absorbance (λmax=765nm), VO2+Permeability P can be fitted to obtain by Fick's law of diffusion, be shown below：
In formula, VLFor left side electrolyte volume, cm3；L is the thickness of sample film, μm；A is effective product of sample film, cm2；
P is the permeability of V (IV)；CRFor the concentration of V (IV) in the solution of right side, mol/L；CLIt (t) is V (IV) in solution on the left of t moment
Ion concentration.The ion selectivity of film is determined by the ratio of conductivity and permeability.
(6) pattern test
The surface texture of the polymer film of preparation is investigated with SEM.All-vanadium flow battery amberplex is dried at 80 DEG C
It is 2 hours dry, except the moisture content on striping surface layer, then it is covered in golden watch layer and is allowed to conductive.Observe SEM's under different magnifying powers
Microscope figure, as shown in Figure 2.Film surface micrograph shown in Fig. 2 a shows the form of polymeric blends.Pure sulfonated polyether
Sulfone film SPES (Fig. 2 a) shows smooth and uniform surface.With the addition (Fig. 2 b and Fig. 2 c) of phosphotungstic acid TPA, in film table
Face detects the particle less than 1um.This may be the aggregation of phosphotungstic acid TPA and knot due in sulfonated polyether sulfone SPES structure
It is brilliant.With the increase of the mass fraction of phosphotungstic acid TPA, more molecules are detected.But in these mixed with polymers
It is difficult to observe miscible sex differernce in object, this shows that sulfonated polyether sulfone SPES and phosphotungstic acid TPA are highly compatibles.
(7) battery performance test
The vanadium redox flow battery charge-discharge test of application is by two carbon felt electrodes, by sulfonated polyether sulfone (PES)/phosphoric acid tungsten
(TPA) composite membrane is sandwiched in assembles between two combination electrodes, is clamped with two graphite electrode plates.All these components are all
It is fixed between two stainless steel plates.2.0M V (II)/V (III) is in 3.0M H2SO4In solution, 2.0M V (IV)/V (V) exists
3.0M H2SO4In solution, respectively as the electrolyte of cathode and anode, magnetic drive pump carries out recycling corresponding electrolytic cell of entering to enter
In.It is 75 milliliters in the volume of each cell bath, the effective area of film is 30cm2.The electric current of VRB monocell test
Density is 40mAcm-2In order to avoid the corrosion of graphite plate, the maximum charging voltage of battery is 1.6V, and minimum discharge voltage is
0.8V。
Anode electrolyte is 1.5mol/LVO2+/VO2+With the H of 3mol/L2SO4Solution, electrolyte liquid are 1.5mol/L
VO+/V2+With the H of 3mol/L2SO4Solution.Positive and negative anodes electrolyte passes through, and the effective area of film is 9cm2, in each half-cell
The volume of solution is 20mL, carries out the charge-discharge test of battery, by LAND CT2001A for the corruption for preventing electrode and collector
Erosion, test condition are 20 DEG C of room temperature, humidity 40%.
2, test result
The main performance of above-mentioned the surveyed film of test method is as shown in table 1 below：
The main performance of 1 film of table
Table 1 summarizes sulfonated polyether sulfone (SPES)/thickness of phosphoric acid tungsten (TPA) composite membrane, ion exchange capacity, sulfonation
Degree, tensile strength and water absorption rate.From Table 2, it can be seen that the ion exchange capacity of composite membrane is in every gram of composite membrane
SO3The reduction of H and reduce, the water absorption rate of composite membrane increases with the increase of phosphotungstic acid.
In view of the high-crystallinity of phosphotungstic acid, the increase of phosphotungstic acid is reasonably that it can extend the crystal region of polymer
Domain inhibits the absorption of its water.Therefore, compared with simple sulfonated polyether sulfone film and Nafion112 film, hybrid films are less likely
It expands in water.The behavior of expansion and the mechanical stability of film are closely related.With Nafion112 and pure sulfonated polyether sulfone film phase
Than composite membrane has higher tensile strength, shows that mechanical stability can be enhanced in phosphotungstic acid.This is because the suction of hydrone
It echos diffusion and occurs mainly in hydrophilic area, caused by sulfonic group, and film is then provided by the crystal region that hydrophobic main chain is formed
Mechanical stability.Phosphotungstic acid, which is added, can be improved the crystallinity of polymeric blends, further increase its mechanical stability.
(2) vanadium ion is unfavorable factor for vanadium redox flow battery VRB by ion exchange film transfer, because it will lead to
The self discharge of battery and lower coulombic efficiency.The vanadium ion permeability (P) of film is listed in table 2：
Conductivity, permeability, the selectivity test result of 2 film of table
The S from table 20.6T0.4Film and S1.0T0.0The comparison of film can be seen that, infiltration of the increase of phosphotungstic acid TPA to vanadium ion
Rate has a great impact：As discussed in document, the crystallization of phosphotungstic acid TPA can limit the expansion behavior of film, this and it
Ion selectivity it is closely related.Table 2 shows the good proton conductivity due to phosphotungstic acid TPA, sulfonated polyether sulfone (SPES)/
The proton conductivity of phosphoric acid tungsten (TPA) composite membrane is higher.The performance of vanadium redox flow battery VRB amberplex is usually according to proton
What conductivity was evaluated with the infiltrative ratio of vanadium ion.Higher selectivity is necessary to realizing better performance.
In addition, being clearly demonstrated in battery in Fig. 3, the linear approximate relationship between time and vanadium (IV) ion concentration.
Rise the result shows that ion exchange capacity represents permeability (P) with the increase of sulfonation degree DS, this is because in film
SO3The increase and enrichment of H group can the more and more transport channels of cation offer.
(3) battery performance is tested, as a result as shown in the following table 3 and Fig. 4, wherein table 3 and Fig. 4 show that sulfonation is poly-
Ether sulfone (SPES)/phosphoric acid tungsten (TPA) composite membrane ion selectivity is apparently higher than Nafion112 film.
3 battery performance test (37mAcm of table-2, cycle-index 150 times)
| Sample | Coulombic efficiency CE (%) | Voltage efficiency VE (%) | Energy efficiency EE (%) |
| Nafion112 | 85.7 | 92.5 | 79.3 |
| S1.0T0.0 | 88.5 | 84.2 | 74.5 |
| S0.9T0.1 | 95.3 | 84.3 | 80.3 |
| S0.8T0.2 | 96.2 | 85.7 | 82.4 |
| S0.7T0.3 | 97.8 | 86 | 84.1 |
| S0.6T0.4 | 98.4 | 86.7 | 85.3 |
| S0.5T0.5 | 97.5 | 87.1 | 84.9 |
The coulombic efficiency (CE) of vanadium redox flow battery and the charge-discharge performance of energy efficiency (EE) are listed in table 3, it be by
What pure sulfonated polyether sulfone film (SPES), sulfonated polyether sulfone (SPES)/phosphoric acid tungsten (TPA) composite membrane and Nafion112 film formed.
It is 37mAcm in current density-2, under conditions of 150 periods of loop test, it can be seen that phosphotungstic acid TPA is added on film
Facilitate the coulombic efficiency CE of improvement vanadium redox flow battery VRB.
Charge-discharge performance is determined by the overpotential of oxidation-reduction pair potential and battery in each half-cell.In vanadium redox flow battery
In VRB system, caused by overpotential is partly due to film resistance.Therefore, higher film resistance will lead to higher charging voltage
With lower discharge voltage, as shown in Figure 5.Compared with Nafion112 film, the cell with S 0.6T0.4 film has obviously more
High voltage efficiency (VE).This result matches very much with lower resistance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (4)
1. a kind of preparation method of all-vanadium flow battery amberplex, which is characterized in that this approach includes the following steps：
(1) polyether sulfone after sulfonation is dissolved in and obtains the solution that mass concentration is 8~12% in dimethyl acetamide, toward the solution
Middle addition phosphotungstic acid hydrate, mass concentration of the phosphotungstic acid hydrate in the solution are 8%, are heated to 90~95 DEG C and machinery
Stirring 2.5~3.5 hours, obtains mixed solution；
(2) above-mentioned mixed solution is cast on clean glass plate, is heated to solvent and evaporates to obtain by film uniform fold
The glass plate of uniform fold is first dried 10h at 80 DEG C, is then warming up to 100 DEG C of dry 10h, is cooled to room temperature by glass plate
Afterwards, film is separated from glass plate.
2. the preparation method of all-vanadium flow battery amberplex as described in claim 1, which is characterized in that in step (1)
In, the sulfonation process of the polyether sulfone is specially：
A, 10 grams of polyether sulfone powder are slowly added to the H that 100ml mass concentration is 98%2SO4In solution；
B, 20ml camphorsulfonic acid at room temperature, is added dropwise to H by the speed of 2~4 seconds/drop2SO4In solution, after completion of dropwise addition
Reaction solution is poured into ice water, mechanical stirring terminates reaction；
C, will terminate the product after reacting is wash with distilled water 7 to pH value, after dry 12 hours at 80 DEG C obtain sulfonation
Polyether sulfone.
3. the preparation method of all-vanadium flow battery amberplex as described in claim 1, which is characterized in that in step (1)
In, the mass concentration of sulfonated polyether sulfone is 10% in the solution.
4. the preparation method of all-vanadium flow battery amberplex as described in claim 1, which is characterized in that in step (2)
In, the process that the film is separated from glass plate is：Glass immersion is made into thin film separation in deionized water, after separation
Film rinse, drying.
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Cited By (1)
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| CN112825359A (en) * | 2019-11-21 | 2021-05-21 | 重庆神华薄膜太阳能科技有限公司 | Composite ion exchange membrane and preparation method and application thereof |
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