CN108134096A - A kind of method of modifying of carbon felt for vanadium redox battery electrode - Google Patents
A kind of method of modifying of carbon felt for vanadium redox battery electrode Download PDFInfo
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- CN108134096A CN108134096A CN201711301735.8A CN201711301735A CN108134096A CN 108134096 A CN108134096 A CN 108134096A CN 201711301735 A CN201711301735 A CN 201711301735A CN 108134096 A CN108134096 A CN 108134096A
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
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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
- H01M4/00—Electrodes
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- H01M4/96—Carbon-based electrodes
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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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- 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
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Abstract
The invention discloses a kind of method of modifying of carbon felt for vanadium redox battery electrode, which includes the following steps：PAN based carbon felt is immersed in treatment fluid A, impregnates completely, obtains mixed system B；Polyallylamine hydrochloride, vanadium trioxide and treatment fluid C, mixing are taken, obtains mixed system D；Mixed system D is added in mixed system B, mixing, obtain mixed system E；Treatment fluid F is added dropwise into mixed system E, fully after reaction, takes out PAN based carbon felt, washes, it is dry；HNO in treatment fluid A3、H2SO4For 150~170 and 230~260mg/g；HNO in treatment fluid C3For 150~170mg/g；Peracetic acid is 180~200mg/g in treatment fluid F；The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.2~0.5：1：15~18, have the advantages that improve electrochemical reversibility.
Description
Technical field
The present invention relates to a kind of method of modifying of carbon felt for vanadium redox battery electrode.
Background technology
Vanadium redox battery (TheAll-vanadiumRedoxFlowBattery, hereinafter referred to as vanadium cell)
It is by propositions such as the MKazacos of Australian NewSouthWales universities.It using vanadium ion different valence state between it is mutual
Convert the charge and discharge process to complete vanadium cell.Vanadium cell has a clear superiority compared with traditional storage battery：Vanadium cell can be according to need
Electrolyte is added, charge capacity is big, strong operability；It can theoretically realize unlimited charge and discharge, charge and discharge are reachable in practice
10000 times or more, long lifespan；It can realize and instantaneously recharge；Super-charge super-discharge does not damage power supply；Green non-pollution etc..Vanadium cell
Anode with V4+/V5+Right as electricity, cathode is with V2+/V3+It is right as electricity.Its principle of electrochemical reaction can be used to lower reaction table
Show：
Charging process：
Anode：VO2++H2O→VO2 ++2H++ e, E0=1.00V；
Cathode：V3++e→V2+, E0=-0.26V；
Discharge process：
Anode：VO2 ++2H++e→VO2++H2O, E0=1.00V；
Cathode：V2+→V3++ e, E0=-0.26V；
Electrode standard electric potential difference is about 1.26V.
It is extensive since carbon class electrode has the characteristics that big very low cost, surface area, good conductivity, stability are high
In the electrode material of vanadium cell.Although carbon class electrode have other class electrodes without advantage, as electrode
For material, it must also have good electrochemical reversibility.
Invention content
The object of the present invention is to provide a kind of method of modifying of carbon felt for vanadium redox battery electrode, have and improve electrochemistry
Reversible advantage.
The present invention above-mentioned technical purpose technical scheme is that：
A kind of method of modifying of carbon felt for vanadium redox battery electrode, includes the following steps：
PAN based carbon felt is immersed in treatment fluid A, impregnates completely, obtains mixed system B；
Polyallylamine hydrochloride, vanadium trioxide and treatment fluid C, mixing are taken, obtains mixed system D；
Mixed system D is added in mixed system B, mixing, obtain mixed system E；
Treatment fluid F is added dropwise into mixed system E, fully after reaction, takes out PAN based carbon felt, washes, it is dry；
Wherein, treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 150~
170 and 230~260mg/g；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 150~170mg/g in treatment fluid C；
Treatment fluid F includes Peracetic acid and water, a concentration of 180~200mg/g of the Peracetic acid in treatment fluid F；
The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.2~0.5：1：15~18.
Further preferably：The PAN based carbon felt that the PAN based carbon felt selection is prepared at 2000 DEG C.
Further preferably：The method of modifying carries out at 20~32 DEG C.
Further preferably：In treatment fluid A, HNO3、H2SO4Concentration be respectively 162 and 246mg/g；
In treatment fluid C, HNO3A concentration of 157mg/g；
In treatment fluid F, a concentration of 185mg/g of Peracetic acid；
The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.4：1：16.
Further preferably：The drying carries out under nitrogen protection, and drying temperature is 40~60 DEG C.
Further preferably：Also added with polyallylamine hydrochloride in treatment fluid F, polyallylamine hydrochloride is in treatment fluid F
In a concentration of 3mg/g.Individual polyallylamine hydrochloride has Peracetic acid stabilization, but when polypropylene amine hydrochloric acid
Salt, vanadium trioxide and Peracetic acid mixing then promote the decomposition of Peracetic acid.
Further preferably：The pretreatment added before above-mentioned steps is additionally included in, the pretreatment is first clear using treatment fluid G
It washes and is washed with water, the treatment fluid G includes SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15~
18 and 10~12mg/g.
Further preferably：The pretreatment carries out under ultrasound, and ultrasonic temperature is 20~32 DEG C.
In conclusion the invention has the advantages that：
Active group is introduced on the surface of PAN based carbon felt to be modified, and greatly improves electro-chemical activity and electricity
Chemical invertibity；
Modified process is the synergistic effect in sulfuric acid, nitric acid, polyallylamine hydrochloride, vanadium trioxide and Peracetic acid
Lower realization.In acid condition, Peracetic acid has certain oxidisability, can be to stone incomplete on PAN based carbon felt
It the carbonnitrogen bond of inkization, the heterocycle containing carbonnitrogen bond and is not aoxidized completely into the carbonnitrogen bond of hexatomic ring；In addition in polypropylene amine
Under the conditions of hydrochloride is existing, vanadium trioxide react with Peracetic acid generate the substance with more strong oxidizing property (high-valence state
Vanadium such as V5+) with further chlorinated polypropylene itrile group carbon felt, while it can also promote decomposition (point of Peracetic acid of Peracetic acid
Solution is reversible reaction, adds in the ability that vanadium trioxide can be used as catalyst degradation positive reaction to carry out, so that driving a reaction is to mistake
The positive reaction that fluoroacetic acid decomposes carries out), greatly accelerate reaction rate, the oxidation journey of maximum PAN based carbon felt
Degree；
The concentration of each treatment fluid is strictly controlled in modifying process, reduces excess processes and concentration mistake caused by concentration overrich
It is low and handle possibility not to the utmost, it can be solved the above problems using the concentration of the application, suitable for large-scale production.
Description of the drawings
It is poly- that Fig. 1 is that commercially available PAN based carbon felt (reference substance), the embodiment 1-2 prepared at 2000 DEG C is modified
The cyclic voltammetry curve of acrylonitrile group carbon felt；Wherein, ● be modified obtained PAN based carbon felt for embodiment 1, ■ is implements
Example 2 is modified obtained PAN based carbon felt, ▲ it is reference substance；
Fig. 2 is the cyclic voltammetry curve for the PAN based carbon felt that embodiment 3-5 is modified；Wherein, ▲ it is embodiment 3
Modified obtained PAN based carbon felt, ■ are that embodiment 4 is modified obtained PAN based carbon felt, ● it is modified for embodiment 5
Obtained PAN based carbon felt；
Fig. 3 is the cyclic voltammetry curve for the PAN based carbon felt that embodiment 6-8 is modified；Wherein, ▲ it is embodiment 6
Modified obtained PAN based carbon felt, ■ are that embodiment 7 is modified obtained PAN based carbon felt, ● it is modified for embodiment 8
Obtained PAN based carbon felt.
Specific embodiment
This specific embodiment is only explanation of the invention, is not limitation of the present invention, people in the art
Member can as needed make the present embodiment the modification of no creative contribution after this specification is read, but as long as at this
It is all protected in the protection domain of invention by Patent Law.
Embodiment 1：A kind of method of modifying of carbon felt for vanadium redox battery electrode, includes the following steps：
(1) it pre-processes：
The PAN based carbon felt prepared at commercially available 2000 DEG C is taken, is cut into 8cm × 8cm specifications, is first surpassed with treatment fluid G
It cleans under sound, then is cleaned under water ultrasound, forced air drying at 30 DEG C；
G includes SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15 and 10mg/g；
(2) pretreated PAN based carbon felt is immersed in 50ml treatment fluids A, impregnates and extremely impregnate within 28 hours completely,
Obtain mixed system B；
Treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 162 Hes
246mg/g；
(3) 703mg polyallylamine hydrochlorides, 5g vanadium trioxides and 20ml treatment fluid C, mixing is taken to obtain mixed system
D；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 157mg/g in treatment fluid C；
(4) mixed system D is added in mixed system B, mixing, obtains mixed system E；
(5) 432g treatment fluid F are added dropwise into mixed system E, reaction takes out polyacrylonitrile-based carbon in 2 hours to abundant reaction
Felt, washing are dry at lower 40 DEG C of nitrogen protection；
Treatment fluid F includes polyallylamine hydrochloride, Peracetic acid and water, and polyallylamine hydrochloride, Peracetic acid are being handled
Concentration in liquid F is respectively 3mg/g, 185mg/g；
Except drying process, the equal temperature control of other processes is 20~32 DEG C；
The dosage of vanadium trioxide is 5g, the dosage of polyallylamine hydrochloride for (432 × 3/1000)+(703/1000)=
1.296+0.703=1.999g the dosage of Peracetic acid is 432 × 185/1000=79.92g；Polyallylamine hydrochloride, three oxygen
The mass ratio for changing two vanadium and Peracetic acid is 0.4:1:16.
Embodiment 2：A kind of method of modifying of carbon felt for vanadium redox battery electrode, with embodiment 1 the difference lies in,
In treatment fluid G, SDS, H2SO4Concentration in treatment fluid G is respectively 18 and 12mg/g.
Embodiment 3：A kind of method of modifying of carbon felt for vanadium redox battery electrode, includes the following steps：
(1) it pre-processes：
The PAN based carbon felt prepared at commercially available 2000 DEG C is taken, is cut into 8cm × 8cm specifications, is first surpassed with treatment fluid G
It cleans under sound, then is cleaned under water ultrasound, forced air drying at 30 DEG C；
G includes SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15 and 10mg/g；
(2) pretreated PAN based carbon felt is immersed in 50ml treatment fluids A, impregnates and extremely impregnate within 28 hours completely,
Obtain mixed system B；
Treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 162 Hes
246mg/g；
(3) 2g polyallylamine hydrochlorides, 5g vanadium trioxides and 20ml treatment fluid C, mixing is taken to obtain mixed system D；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 157mg/g in treatment fluid C；
(4) mixed system D is added in mixed system B, mixing, obtains mixed system E；
(5) 432g treatment fluid F are added dropwise into mixed system E, reaction takes out polyacrylonitrile-based carbon in 2 hours to abundant reaction
Felt, washing are dry at lower 40 DEG C of nitrogen protection；
Treatment fluid F includes Peracetic acid and water, a concentration of 185mg/g of the Peracetic acid in treatment fluid F；
Except drying process, the equal temperature control of other processes is 20~32 DEG C；
The dosage of vanadium trioxide is 5g, and the dosage of polyallylamine hydrochloride is 2g, the dosage of Peracetic acid for 432 ×
185/1000=79.92g；The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.4:1:16.
Embodiment 4：A kind of method of modifying of carbon felt for vanadium redox battery electrode, includes the following steps：
(1) it pre-processes：
The PAN based carbon felt prepared at commercially available 2000 DEG C is taken, is cut into 8cm × 8cm specifications, is first surpassed with treatment fluid G
It cleans under sound, then is cleaned under water ultrasound, forced air drying at 30 DEG C；
G includes SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15 and 10mg/g；
(2) pretreated PAN based carbon felt is immersed in 50ml treatment fluids A, impregnates and extremely impregnate within 28 hours completely,
Obtain mixed system B；
Treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 150 Hes
230mg/g；
(3) 1g polyallylamine hydrochlorides, 5g vanadium trioxides and 20ml treatment fluid C, mixing is taken to obtain mixed system D；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 170mg/g in treatment fluid C；
(4) mixed system D is added in mixed system B, mixing, obtains mixed system E；
(5) 417g treatment fluid F are added dropwise into mixed system E, reaction takes out polyacrylonitrile-based carbon in 2 hours to abundant reaction
Felt, washing are dry at lower 40 DEG C of nitrogen protection；
Treatment fluid F includes Peracetic acid and water, a concentration of 180mg/g of the Peracetic acid in treatment fluid F；
Except drying process, the equal temperature control of other processes is 20~32 DEG C；
The dosage of vanadium trioxide is 5g, and the dosage of polyallylamine hydrochloride is 1g, the dosage of Peracetic acid for 417 ×
180/1000=75.06g；The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.2:1:15.
Embodiment 5：A kind of method of modifying of carbon felt for vanadium redox battery electrode, includes the following steps：
(1) it pre-processes：
The PAN based carbon felt prepared at commercially available 2000 DEG C is taken, is cut into 8cm × 8cm specifications, is first surpassed with treatment fluid G
It cleans under sound, then is cleaned under water ultrasound, forced air drying at 30 DEG C；
G includes SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15 and 10mg/g；
(2) pretreated PAN based carbon felt is immersed in 50ml treatment fluids A, impregnates and extremely impregnate within 28 hours completely,
Obtain mixed system B；
Treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 170 Hes
260mg/g；
(3) 2.5g polyallylamine hydrochlorides, 5g vanadium trioxides and 20ml treatment fluid C, mixing is taken to obtain mixed system D；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 150mg/g in treatment fluid C；
(4) mixed system D is added in mixed system B, mixing, obtains mixed system E；
(5) 451g treatment fluid F are added dropwise into mixed system E, reaction takes out polyacrylonitrile-based carbon in 2 hours to abundant reaction
Felt, washing are dry at lower 40 DEG C of nitrogen protection；
Treatment fluid F includes Peracetic acid and water, a concentration of 200mg/g of the Peracetic acid in treatment fluid F；
Except drying process, the equal temperature control of other processes is 20~32 DEG C；
The dosage of vanadium trioxide is 5g, and the dosage of polyallylamine hydrochloride is 2.5g, the dosage of Peracetic acid for 451 ×
200/1000=90.2g；The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.5:1:18.
Embodiment 6：A kind of method of modifying of carbon felt for vanadium redox battery electrode, with embodiment 3 the difference lies in,
It is not pre-processed.
Embodiment 7：A kind of method of modifying of carbon felt for vanadium redox battery electrode, with embodiment 3 the difference lies in,
The commercially available PAN based carbon felt that PAN based carbon felt selection is prepared at 1400 DEG C.
Embodiment 8：A kind of method of modifying of carbon felt for vanadium redox battery electrode, with embodiment 3 the difference lies in,
Method of modifying carries out at 50 DEG C.
Cyclic voltammetry
The polyacrylonitrile being modified respectively with the commercially available PAN based carbon felt, the embodiment 1-8 that prepare at 2000 DEG C
Base carbon felt is test object, is work pole by test object, work area 1.5cm2, platinum electrode is as auxiliary electrode, saturation
Calomel electrode is reference electrode, forms three-electrode system, carries out cyclic voltammetry.Sweep speed is 20mVs-1。
Test result is as shown in Figs. 1-3.It is shown in figure, the peak value of reference substance is respectively -0.8V/-0.8mAcm2With-
0.3V/0.7mA·cm2, the peak value of embodiment 1 is respectively -0.6V/-1.5mAcm2With -0.5V/1.5mAcm2, embodiment 2
Peak value be respectively -0.6V/-1.4mAcm2With -0.5V/1.5mAcm2, the peak value of embodiment 3 is respectively -0.7V/-
1.2mA·cm2With -0.5V/1.2mAcm2, the peak value of embodiment 4 is respectively -0.7V/-1.1mAcm2With -0.4V/
1.1mA·cm2, the peak value of embodiment 5 is respectively -0.7V/-1.1mAcm2With -0.4V/1.0mAcm2, the peak of embodiment 6
Value is respectively -0.6V/-0.7mAcm2With -0.4V/0.7mAcm2, the peak value of embodiment 7 is respectively -0.7V/-0.8mA
cm2With -0.4V/0.8mAcm2, the peak value of embodiment 8 is respectively -0.7V/-0.9mAcm2With -0.5V/0.8mAcm2。
There are a pair of apparent redox peaks respectively in the range of -1.0V~0V in electrode, corresponding to V2+/V3+Electricity is right
Oxidation reaction and reduction reaction, treated that the electro-chemical activity of electrode on it significantly carries for the method for modifying through the application
Height, peak value greatly improve；Spike potential difference also greatly reduces, and invertibity significantly improves.
The specific implementation of the invention is not to be limited to these illustrations for more than content, and technology belonging to the present invention is led
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, several simple deduction or replace can also be made,
Present invention scope of patent protection determined by the appended claims should be all considered as belonging to.
Claims (8)
1. a kind of method of modifying of carbon felt for vanadium redox battery electrode, which is characterized in that include the following steps：
PAN based carbon felt is immersed in treatment fluid A, impregnates completely, obtains mixed system B；
Polyallylamine hydrochloride, vanadium trioxide and treatment fluid C, mixing are taken, obtains mixed system D；
Mixed system D is added in mixed system B, mixing, obtain mixed system E；
Treatment fluid F is added dropwise into mixed system E, fully after reaction, takes out PAN based carbon felt, washes, it is dry；
Wherein, treatment fluid A includes HNO3、H2SO4And water, and HNO3、H2SO4Concentration in treatment fluid A is respectively 150~170
With 230~260mg/g；
Treatment fluid C includes HNO3And water, and HNO3A concentration of 150~170mg/g in treatment fluid C；
Treatment fluid F includes Peracetic acid and water, a concentration of 180~200mg/g of the Peracetic acid in treatment fluid F；
The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.2~0.5：1：15~18.
2. the method for modifying of a kind of carbon felt for vanadium redox battery electrode according to claim 1, which is characterized in that described
The PAN based carbon felt that PAN based carbon felt selection is prepared at 2000 DEG C.
3. the method for modifying of a kind of carbon felt for vanadium redox battery electrode according to claim 2, which is characterized in that described
Method of modifying carries out at 20~32 DEG C.
4. a kind of method of modifying of carbon felt for vanadium redox battery electrode according to claim 3, which is characterized in that
In treatment fluid A, HNO3、H2SO4Concentration be respectively 162 and 246mg/g；
In treatment fluid C, HNO3A concentration of 157mg/g；
In treatment fluid F, a concentration of 185mg/g of Peracetic acid；
The mass ratio of polyallylamine hydrochloride, vanadium trioxide and Peracetic acid is 0.4：1：16.
5. the method for modifying of a kind of carbon felt for vanadium redox battery electrode according to claim 4, which is characterized in that described
Drying carries out under nitrogen protection, and drying temperature is 40~60 DEG C.
A kind of 6. method of modifying of carbon felt for vanadium redox battery electrode according to claim 5, which is characterized in that processing
Also added with polyallylamine hydrochloride, a concentration of 3mg/g of the polyallylamine hydrochloride in treatment fluid F in liquid F.
7. the method for modifying of a kind of carbon felt for vanadium redox battery electrode according to claim 6, which is characterized in that also wrap
The pretreatment added before above-mentioned steps is included, the pretreatment is first washed with water using treatment fluid G cleanings, the treatment fluid G packets
Include SDS, H2SO4And water, and SDS, H2SO4Concentration in treatment fluid G is respectively 15~18 and 10~12mg/g.
8. the method for modifying of a kind of carbon felt for vanadium redox battery electrode according to claim 7, which is characterized in that described
Pretreatment carries out under ultrasound, and ultrasonic temperature is 20~32 DEG C.
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| CN110456118A (en) * | 2019-08-13 | 2019-11-15 | 大同新成新材料股份有限公司 | A kind of preparation method for adsorbing fused salt mixt carbon felt electrode |
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