CN111359449B - Electroactive film and method for preparing same - Google Patents
Electroactive film and method for preparing same Download PDFInfo
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- CN111359449B CN111359449B CN202010140410.1A CN202010140410A CN111359449B CN 111359449 B CN111359449 B CN 111359449B CN 202010140410 A CN202010140410 A CN 202010140410A CN 111359449 B CN111359449 B CN 111359449B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/26—Electrical properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses an electroactive film and a preparation method thereof, wherein the electroactive film comprises a base film, a graphene film, a conductive mesh material and a protective film; wherein the graphene film is formed on the base film; the conductive mesh material is adhered to the graphene film, and the protective film is covered on the conductive mesh material. The electrocatalysis membrane in the invention carries out electrocatalysis at the same time of membrane separation, thus, the problem of membrane pollution easily caused by membrane separation can be solved by decomposing organic matters through electrocatalysis, and the problems of poor decolorization effect, low mass transfer efficiency and the like of electrocatalysis also solved through the larger specific surface area of the membrane material.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to an electroactive membrane and a preparation method thereof.
Background
Because the water environment problem in China is severe, the water treatment requirement is increasingly improved, and the components of industrial wastewater and domestic sewage are complicated, the technical challenge on the advanced treatment of the wastewater and the sewage is continuously increased.
At present, two common advanced treatment processes are membrane separation and electrocatalysis, wherein the membrane separation has the problem of easy membrane pollution, and the electrocatalysis has the problems of poor decolorization effect, low mass transfer efficiency and the like, so that the application of the two advanced treatment processes is restricted.
Disclosure of Invention
The invention aims to overcome the defects of membrane separation and electrocatalysis, and provides an electroactive membrane capable of simultaneously realizing the functions of membrane separation and electrocatalysis and a preparation method thereof, so as to improve the advanced treatment effect of refractory organic matters in wastewater and sewage.
The technical scheme adopted by the invention for solving the technical problems is as follows: an electroactive film comprising a base film, a graphene film, a conductive mesh material, and a protective film;
wherein the graphene film is formed on the base film; the conductive mesh material is adhered to the graphene film, and the protective film is covered on the conductive mesh material.
Further, the base film is a ceramic film, a polytetrafluoroethylene film or a glass sand core film; and/or the conductive mesh material is a titanium mesh or a platinum mesh, the thickness of the conductive mesh material is not more than 0.2mm, and the density is not more than 100 meshes; and/or the protective film is a polytetrafluoroethylene film or a polyethylene film.
Further, the graphene film thickness is greater than 200 μm.
The invention also adopts the following technical scheme for solving the technical problems: a method of making an electroactive membrane, comprising:
s1, preparing graphite into oxidized expanded graphite powder by a chemical dispersion method;
s2, mixing the oxidized expanded graphite powder with water in proportion;
s3, dissolving the oxidized expanded graphite in water by using an ultrasonic or vibration method to obtain a graphene oxide dispersion liquid;
s4, reducing the graphene oxide dispersion liquid at a medium temperature to form stably dispersed graphene slurry;
s5, coating the graphene slurry on the base film by using a spraying, printing, suction pressing or spin coating method;
s6, forming a compact graphene film by coating an adhesive and rolling;
and S7, adhering the graphene film and the conductive mesh material, and covering a protective film to finally form the electroactive film.
Further, the S1 specifically includes:
s10, under an ice-water bath system, adding 1 part of 200-mesh-sieve graphite powder into 200-500 parts of 68% concentrated nitric acid by mass, stirring to a constant temperature, adding 5-10 parts of potassium chlorate into the mixture for 5 times under the stirring condition for not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s11, slowly heating to 20 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s12, slowly heating to 40 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s13, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying a filter cake at the temperature of 50 ℃ or less to obtain the oxidized expanded graphite powder.
Further, the S1 specifically includes:
s15, under an ice-water bath system, adding 1 part of graphite powder which is sieved by a 200-mesh sieve into 100-150 parts of 98% concentrated sulfuric acid by mass, stirring to a constant temperature, adding 2-3 parts of sodium nitrate in 2 times within not less than 5min under the stirring condition, adding 6-12 parts of potassium permanganate in 6 times within not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s16, slowly heating to 60 ℃ under the stirring condition, keeping the temperature for not less than 15min, and continuing stirring for 2-3 hours after keeping the temperature constant;
s17, adding 200 parts of ultrapure water under the stirring condition, and continuing stirring for 2-3 hours after keeping the temperature constant;
s18, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying the solid at 50 ℃ or less to obtain the oxidized expanded graphite powder.
Further, the mass ratio of the oxidized expanded graphite powder to water in the S2 is 1: 1000-2.5: 1000.
Further, the S4 specifically includes: adding the graphene oxide dispersion liquid into an organic dispersant to obtain a mixed solution; adding a reducing agent aqueous solution into the mixed solution, and adjusting the pH value to 8-10; and at the reduction temperature of not higher than 60 ℃, the reduction time is not less than 2h, so that the stably dispersed graphene slurry is formed.
Further, the organic dispersing agent is 40-70% of the graphene oxide dispersing liquid in percentage by volume, and the mass ratio of the reducing agent in the reducing agent aqueous solution to the graphene oxide is not less than 10: 1.
Further, the graphene film formed by adding the adhesive in the S6 and rolling is larger than 200 mu m in thickness, the adhesive is polytetrafluoroethylene dispersion, and the coating amount is not more than 1mL/dm2(ii) a S7 comprises, by weight, 70-85 parts of graphene slurry, 0.1 part of an adhesive and 15-30 parts of a conductive mesh material.
The invention has the following beneficial effects: the electrocatalysis membrane in the invention carries out electrocatalysis at the same time of membrane separation, thus, the problem of membrane pollution easily caused by membrane separation can be solved by decomposing organic matters through electrocatalysis, and the problems of poor decolorization effect, low mass transfer efficiency and the like of electrocatalysis also solved through the larger specific surface area of the membrane material.
Drawings
Fig. 1 is a schematic structural view of an electroactive membrane of the present invention;
FIG. 2 is a SEM image of a graphene film;
the notation in the figures means: 1-protective film; 2-a conductive mesh material; 3-a graphene film; 4-a base film; 5-conducting wire.
Detailed Description
The technical solution of the present invention is further described below with reference to the following embodiments and the accompanying drawings.
Example 1
The present embodiment provides an electroactive film comprising a base film 4, a graphene film 3, a conductive mesh material 2, and a protective film 1.
The base film 4 is a ceramic film, a polytetrafluoroethylene film or a glass sand core film, and the graphene film 3 is formed on the base film 4; the conductive mesh material 2 is adhered to the graphene film 3, and the protective film 1 is covered on the conductive mesh material 2, so as to form the electroactive film of the present embodiment, wherein the SEM image of the graphene film of the electroactive film is shown in fig. 2, wherein it can be obtained that the graphene film is very flat.
Preferably, the conductive mesh material 2 is connected to a wire to apply electric energy to the conductive mesh material 2 through the wire 5, so that the graphene film 3 can perform film separation and electrocatalytic separation.
The embodiment adopts a roughness higher, the intact reduction oxidation graphite alkene suppression of structure becomes the membrane to with electrically conductive network material bonding, form the graphite alkene electroactive membrane similar to three-dimensional electrode, the electroactive membrane of this embodiment realizes that membrane separation and electro-catalysis pollutant degradation go on simultaneously from this when using, has solved the respective shortcoming of membrane separation and electro-catalysis, the advanced treatment effect of difficult degradation organic matter in waste water and the sewage has been improved, and has extensive applicability, and the practicality is strong, and is high to difficult degradation organic matter treatment effeciency, characteristics such as electro-catalysis's current efficiency height.
Compare and go on in prior art's membrane separation and electro-catalysis separation, both do not combine together, and the electro-catalysis membrane in this embodiment carries out the electro-catalysis simultaneously at membrane separation, from this, both can rely on the electro-catalysis to decompose the organic matter and solve the problem that membrane separation has the membrane pollution of easily taking place, also can solve the decoloration effect that electro-catalysis exists poor and mass transfer efficiency low grade problem through the great specific surface area of membrane material.
In particular, in the embodiment, the electroactive film is formed by the graphene and the conductive mesh material, so that the electroactive film has good conductivity, a flat material structure, a huge specific surface area, a high young modulus, excellent electrical and thermal properties and a high-density electron cloud, and the graphene has a good technical effect in the application of the graphene in the field of water treatment.
Example 2
This example provides a method of preparing an electroactive film, in particular a method of preparing an electroactive film as described in example 1, comprising:
s1, preparing the graphite into the oxidized expanded graphite powder by a chemical dispersion method.
And S2, mixing the oxidized expanded graphite powder with water in proportion.
And S3, dissolving the oxidized expanded graphite in water by using an ultrasonic or vibration method to obtain the graphene oxide dispersion liquid.
And S4, reducing the graphene oxide dispersion liquid at medium temperature to form stably dispersed graphene slurry.
And S5, coating the graphene slurry on the base film by using a spraying, printing, drawing and pressing method or a spin coating method.
And S6, forming the dense graphene film by coating an adhesive and rolling.
And S7, adhering the graphene film and the conductive mesh material, and covering a protective film to finally form the electroactive film.
According to the preparation method of the electroactive film, the graphene oxide dispersion liquid is prepared by a chemical dispersion method, graphene oxide is reduced at medium temperature by an organic-hydrazine system, so that low-cost and high-quality graphene is obtained, and the graphene is suitable for film separation and electrocatalysis application; and a graphene film is formed on the base film, and the graphene film is bonded with a conductive mesh material, so that the graphene film can simultaneously have the effects of film separation and electrocatalysis, has a certain adsorption effect, and can be used for advanced treatment of difficultly-degraded organic matters in wastewater and sewage and purification of surface water.
In this embodiment, the chemical dispersion method in S1 includes:
s10, under an ice-water bath system, adding 1 part of 200-mesh-sieve graphite powder into 200-500 parts of 68% concentrated nitric acid by mass, stirring to a constant temperature, adding 5-10 parts of potassium chlorate into the mixture for 5 times under the stirring condition for not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s11, slowly heating to 20 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s12, slowly heating to 40 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s13, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying a filter cake at the temperature of 50 ℃ or less to obtain the oxidized expanded graphite powder.
Alternatively, the chemical dispersion method in S1 may also be implemented by the following steps:
s15, under an ice-water bath system, adding 1 part of graphite powder which is sieved by a 200-mesh sieve into 100-150 parts of 98% concentrated sulfuric acid by mass, stirring to a constant temperature, adding 2-3 parts of sodium nitrate in 2 times within not less than 5min under the stirring condition, adding 6-12 parts of potassium permanganate in 6 times within not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s16, slowly heating to 60 ℃ under the stirring condition, keeping the temperature for not less than 15min, and continuing stirring for 2-3 hours after keeping the temperature constant;
s17, adding 200 parts of ultrapure water under the stirring condition, and continuing stirring for 2-3 hours after keeping the temperature constant;
s18, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying the solid at 50 ℃ or less to obtain the oxidized expanded graphite powder.
Preferably, the mass ratio of the expanded graphite oxide powder to water in S2 is 1: 1000-2.5: 1000, and the water is secondary water meeting national Standard for Water for analytical laboratories (GB/T6682-2008).
Preferably, the oxidized expanded graphite is dissolved in water by ultrasonic or mechanical vibration in S3, so as to form a uniformly dispersed graphene oxide dispersion liquid.
Preferably, S4 is specifically: adding the graphene oxide dispersion liquid into an organic dispersant to obtain a mixed solution, wherein the organic dispersant can be ethylene glycol, glycerol or a mixed solution of ethylene glycol and glycerol; adding a reducing agent aqueous solution into the mixed solution, and adjusting the pH value to 8-10, wherein the reducing agent aqueous solution is preferably hydrazine hydrochloride solution or hydrazine sulfate solution; and at the reduction temperature of not higher than 60 ℃, the reduction time is not less than 2h, so that the stably dispersed graphene slurry is formed.
The organic dispersing agent is 40-70% of graphene oxide dispersing liquid in percentage by volume, and the mass ratio of a reducing agent (hydrazine hydrochloride or hydrazine sulfate) in a reducing agent aqueous solution to the graphene oxide is not less than 10: 1.
If the organic dispersant is ethylene glycol, the amount is 70%, if the organic dispersant is glycerin, the amount is 40%, and if the organic dispersant is a mixed solution thereof, the amount of the organic dispersant to be used is calculated from the volume ratio of ethylene glycol to glycerin.
When the reducing agent aqueous solution is hydrazine hydrochloride solution, the concentration of the hydrazine hydrochloride is not more than 1000 mg/L; when the reducing agent aqueous solution is a hydrazine sulfate solution, the concentration of the hydrazine sulfate solution is not more than 1000 mg/L.
And S5, completely and uniformly coating the graphene slurry on a base film, wherein the base film comprises a ceramic film, a polytetrafluoroethylene film, a glass sand core film and the like, and the aperture of the base film is less than 0.45 mu m.
The graphene film formed by adding the adhesive in S6 and rolling is more than 200 mu m in thickness, the adhesive is polytetrafluoroethylene dispersion (w/w 10%), and the coating amount is not more than 1mL/dm2。
The graphene film and the conductive mesh material in the S7 are bonded by means of adhesion, pressing and riveting, the conductive mesh material can be an inert metal mesh such as a titanium mesh or a platinum mesh, the thickness of the conductive mesh material is not more than 0.2mm, the density of the conductive mesh material is not more than 100 meshes, the protective film can be a polytetrafluoroethylene film or a polyethylene film, and the graphene slurry accounts for 70-85 parts, the adhesive accounts for 0.1 part, and the conductive mesh material accounts for 15-30 parts by weight.
Compared with the prior art, the preparation method of the electroactive film has the following advantages:
1. low production cost, low toxicity and safety: graphite powder, concentrated sulfuric acid, sodium nitrate and potassium permanganate used for preparing graphene oxide, dispersing agents and reducing agents used for reducing graphene and the like are conventional chemical products, so that the transportation is convenient, and a highly toxic reducing agent hydrazine or hydrazine hydrate of a traditional hydrazine reduction method is avoided; the preparation method does not have the working procedure of over 60 ℃, so high-temperature and high-pressure equipment is not needed, the volatilization of toxic and harmful gases such as nitrogen oxide, hydrazine and the like in the traditional chemical oxidation dispersion-hydrazine reduction method is avoided, and the method can be produced and applied in a large scale.
2. The obtained graphene film has a flat structure and good electrochemical performance: since the graphene is manufactured under the condition of medium temperature in the whole process, the structure of the graphene sheet layer can be stored to the maximum extent on the premise of large-scale production and application, and the manufactured graphene film structure is smoother than the graphene film manufactured by the traditional chemical oxidation dispersion-hydrazine reduction method. And the graphene film is flat in structure, so that the graphene film is good in electrochemical performance and meets the requirements of the graphene electroactive film.
3. The electroactive film has strong treatment capacity on refractory organics: the electroactive membrane has dual functions of membrane separation and electrocatalysis during operation, and the graphene membrane has high quality and strong membrane separation and electrocatalysis capabilities, so that the electroactive membrane has strong degradation capability on refractory organics. The invention has wide application range, strong practicability and higher current efficiency than the common electrocatalysis technology.
Example 3
This example provides a method for preparing an electroactive film, in which, after obtaining a graphene oxide dispersion liquid by the method for preparing an electroactive film of example 2, 10mL of the graphene oxide dispersion liquid 1g/L was added to 70mL of ethylene glycol, 10mL of a hydrazine sulfate solution 10g/L was then added, and finally, pH was adjusted to 9.2 with 20% sodium hydroxide to 100 mL. And then pouring the mixed solution into a 100mL beaker, putting the beaker into a constant-temperature magnetic stirrer, reacting for 2.0h at 60 ℃, pouring the reacted mixed solution into a suction filtration system, and pumping the mixed solution into a graphene membrane with the diameter of about 4.0cm by taking the polytetrafluoroethylene membrane as a base membrane. And then, attaching the graphene film to the titanium mesh, covering a layer of polytetrafluoroethylene film, and riveting the periphery to form the graphene electroactive film.
The electroactive film is used as an anode to treat the electroactive film with the concentration of 100mg/L, pH ═ m6.3 electrolyte K2SO4The conductivity of the solution is 7.8mS/cm, the transmembrane pressure difference in the treatment process is about 0.2-0.3 MPa, and the membrane flux is 66.32L/(m) of solution2h) The reaction residence time was 13.56min, and the current density was 4.42mA/cm2The cell voltage is about 4.6V. According to the implementation result, the methylene blue decolorization rate is as high as 98.4%. The embodiment shows that the electrocatalytic membrane comprising the graphene membrane has higher treatment efficiency on refractory organics.
Example 4
This example provides a method for preparing an electroactive film, in which, after obtaining a graphene oxide dispersion liquid by the method for preparing an electroactive film of example 2, 10mL of the graphene oxide dispersion liquid 1g/L was added to 50mL of glycerol, 10mL of a hydrazine sulfate solution 10g/L was then added, and finally, pH was adjusted to 8.8 with 20% sodium hydroxide to 100 mL. And then pouring the mixed solution into a 100mL beaker, putting the beaker into a constant-temperature magnetic stirrer, reacting for 2h at 60 ℃, pouring the reacted mixed solution into a suction filtration system, and pumping the mixed solution into a graphene membrane with the diameter of about 4.0cm by taking the polytetrafluoroethylene membrane as a base membrane. And then, attaching the graphene film to the titanium mesh, covering a layer of polytetrafluoroethylene film, and riveting the periphery to form the graphene electroactive film.
The electroactive film is used as an anode, the treatment is carried out on the electroactive film with the concentration of 100mg/L, pH-5.9 and the electrolyte K2SO4The conductivity of the bromamine acid solution is 7.4mS/cm, the transmembrane pressure difference in the treatment process is about 0.2-0.3 MPa, and the membrane flux is 66.32L/(m)2h) The reaction residence time was 13.56min, and the current density was 4.42mA/cm2The cell voltage is about 5.1V. According to the experimental result, the bromamine acid decolorization rate is as high as 98.8%, and the TOC removal rate is about 96.6%. The implementation case shows that the graphene electrocatalytic film has high treatment efficiency on refractory organics.
The sequence of the above embodiments is only for convenience of description and does not represent the advantages and disadvantages of the embodiments.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A method of making an electroactive membrane, comprising:
s1, preparing graphite into oxidized expanded graphite powder by a chemical dispersion method;
s2, mixing the oxidized expanded graphite powder with water in proportion;
s3, dissolving the oxidized expanded graphite in water by using an ultrasonic or vibration method to obtain a graphene oxide dispersion liquid;
s4, reducing the graphene oxide dispersion liquid at a medium temperature to form stably dispersed graphene slurry;
s5, coating the graphene slurry on the base film by using a spraying, printing, suction pressing or spin coating method;
s6, forming a compact graphene film by coating an adhesive and rolling;
s7, adhering the graphene film and the conductive mesh material, and covering a protective film to finally form an electroactive film;
wherein, S4 specifically is: adding the graphene oxide dispersion liquid into an organic dispersant to obtain a mixed solution; adding a reducing agent aqueous solution into the mixed solution, and adjusting the pH value to 8-10; and at the reduction temperature of not higher than 60 ℃, the reduction time is not less than 2h, so that the stably dispersed graphene slurry is formed.
2. The preparation method according to claim 1, wherein the S1 is specifically:
s10, under an ice-water bath system, adding 1 part of 200-mesh-sieve graphite powder into 200-500 parts of 68% concentrated nitric acid by mass, stirring to a constant temperature, adding 5-10 parts of potassium chlorate into the mixture for 5 times under the stirring condition for not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s11, slowly heating to 20 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s12, slowly heating to 40 ℃ under the stirring condition, keeping the heating time at no less than half an hour, and continuously stirring for 10-15 hours after keeping the temperature constant;
s13, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying a filter cake at the temperature of 50 ℃ or less to obtain the oxidized expanded graphite powder.
3. The preparation method according to claim 1, wherein the S1 is specifically:
s15, under an ice-water bath system, adding 1 part of graphite powder which is sieved by a 200-mesh sieve into 100-150 parts of 98% concentrated sulfuric acid by mass, stirring to a constant temperature, adding 2-3 parts of sodium nitrate in 2 times within not less than 5min under the stirring condition, adding 6-12 parts of potassium permanganate in 6 times within not less than half an hour, stirring to a constant temperature, and standing for half an hour;
s16, slowly heating to 60 ℃ under the stirring condition, keeping the temperature for not less than 15min, and continuing stirring for 2-3 hours after keeping the temperature constant;
s17, adding 200 parts of ultrapure water under the stirring condition, and continuing stirring for 2-3 hours after keeping the temperature constant;
s18, slowly adding 20-40 parts by mass of 30% hydrogen peroxide within half an hour or more, filtering, washing with 30 parts by mass of 5% diluted hydrochloric acid for three times, and drying the solid at 50 ℃ or less to obtain the oxidized expanded graphite powder.
4. The preparation method according to claim 1, wherein the mass ratio of the expanded graphite oxide powder to water in S2 is 1:1000 to 2.5: 1000.
5. The preparation method of claim 4, wherein the organic dispersant is 40-70% of the graphene oxide dispersion liquid by volume percentage, and the mass ratio of the reducing agent to the graphene oxide in the reducing agent aqueous solution is not less than 10: 1.
6. The preparation method of claim 1, wherein the graphene film formed by adding the binder in S6 and rolling has a thickness of more than 200 μm, the binder is polytetrafluoroethylene dispersion, and the coating amount is not more than 1mL/dm2(ii) a S7 comprises, by weight, 70-85 parts of graphene slurry, 0.1 part of an adhesive and 15-30 parts of a conductive mesh material.
7. An electroactive film produced by the method of producing an electroactive film according to any one of claims 1 to 6, comprising a base film, a graphene film, a conductive mesh material, and a protective film;
wherein the graphene film is formed on the base film; the conductive mesh material is adhered to the graphene film, and the protective film is covered on the conductive mesh material.
8. The electroactive membrane of claim 7 wherein the base membrane is a ceramic membrane, a polytetrafluoroethylene membrane, or a glass sand core membrane; and/or the conductive mesh material is a titanium mesh or a platinum mesh, the thickness of the conductive mesh material is not more than 0.2mm, and the density is not more than 100 meshes; and/or the protective film is a polytetrafluoroethylene film or a polyethylene film.
9. The electroactive film of claim 8 wherein the graphene film thickness is greater than 200 μ ι η.
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