CN108275673A - A kind of preparation method of high-performance porous graphene film - Google Patents
A kind of preparation method of high-performance porous graphene film Download PDFInfo
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- CN108275673A CN108275673A CN201810303347.1A CN201810303347A CN108275673A CN 108275673 A CN108275673 A CN 108275673A CN 201810303347 A CN201810303347 A CN 201810303347A CN 108275673 A CN108275673 A CN 108275673A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention belongs to grapheme material technical fields, and in particular to a kind of preparation method of high-performance porous membrane includes the following steps：Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；Step 2, mixed liquor is put into progress 2 4h of ball-milling reaction in ball-milling device, graphene mixture is obtained after drying；Step 3, graphene mixture is added to the water stirring and forms viscous fluid, be then sprayed at substrate surface, graphene prefabricated membrane is obtained after drying；Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to being completely dissolved, obtain dispersion alcohol liquid；Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, 2 4h of micro-electrolysis reaction obtains graphene film.The preparation method of the present invention is simple and convenient, using ep-type material as raw material, and does not generate industrial wastewater, disclosure satisfy that the environmental requirement of industrialized production.
Description
Technical field
The invention belongs to grapheme material technical fields, and in particular to a kind of preparation method of high-performance porous membrane.
Background technology
Super capacitor material is the big key area that electrochemical capacitance is applied in real life, is also to restrict up to now
One big bottleneck of electrochemical capacitance application.Current electronics mainly develop toward the directions such as small, smart, and this requires the volume of electrochemical capacitance foots
Enough is small, to have higher requirement to energy density, the power density of super capacitor material.The electrochemical capacitance of Most current
Device is mainly based upon the cheap carbon material of electric double layer capacitance storing up electricity mechanism, but if expecting the larger possibility of energy density
It is too small.The development of capacitance material recent years is summarized, although carbon nano-tube material performance is preferable, its manufacturing cost is too high, does not have
It can be well used.Graphene is adequately studied, in capacitance material as emerging two-dimensional material in many fields
Material field has prodigious potential application.The research of grapheme material is also more, but most of is to concentrate on hydro-thermal method or graphite
In the compound research such as alkene and conducting polymer, metal oxide, it is difficult to realize the accurate preparation of graphene, this just constrains stone
Application of the black alkene in terms of precise electronic.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of high-performance porous graphene film,
Preparation method is simple and convenient, using ep-type material as raw material, and does not generate industrial wastewater, disclosure satisfy that industrialized production
Environmental requirement.
To realize the above technical purpose, the technical scheme is that：
A kind of preparation method of high-performance porous graphene film, includes the following steps：
Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；
Step 2, mixed liquor is put into progress ball-milling reaction 2-4h in ball-milling device, graphene mixture is obtained after drying；
Step 3, graphene mixture is added to the water stirring and forms viscous fluid, substrate surface is then sprayed at, after drying
Obtain graphene prefabricated membrane；
Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to completely molten
Solution obtains dispersion alcohol liquid；
Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, micro-electrolysis reaction 2-4h obtains graphene film.
A concentration of 30-70g/L of the graphene in absolute ethyl alcohol in the step 1, the addition of the dispersant are
The 20-40% of graphene quality, the dispersant use polyvinylpyrrolidone or polyethylene glycol 200, the stirring to stir
It is 2000-3000r/min to mix speed.
The temperature of ball-milling reaction in the step 2 is 60-70 DEG C, and drying temperature is 80-100 DEG C.
The mass ratio of graphene mixture and water in the step 3 is 3:The fountain height of 2-5, the sprinkling are 2-8g/
cm2, the temperature of the drying is 90-100 DEG C.
Base material in the step 3 uses substrate modified, the modification procedure of substrate modified as follows：
Base material is added in hydrochloric acid solution and stirs 2-4h by step a, is washed after taking-up and obtains acidification base material；
Step b, acidification base material is added in absolute ethyl alcohol and is stirred by ultrasonic, and is dried after removal and is obtained passivation base material；
Step c, alcohol-soluble resin is added and is stirred evenly into absolute ethyl alcohol, forms resinol liquid, then using spraying
Mode be evenly distributed on substrate surface, form substrate modified.
The addition of a concentration of 0.01-0.03mol/L of hydrochloric acid solution in the step a, the hydrochloric acid being capable of base materials
Covering, the mixing speed are 1000-2000r/min.
Absolute ethyl alcohol addition in the step b can be by acidification base material submergence, the supersonic frequency of the ultrasonic agitation
For 20-40kHz, temperature is 40-60 DEG C, and the drying temperature of the drying is 90-100 DEG C.
Alcohol-soluble resin in the step c uses Lauxite or polyvinyl butyral, the alcohol-soluble resin
The quantity for spray of a concentration of 30-180g/L, the substrate surface are 10-30g/L.
The volume ratio of ethyl alcohol and methanol in the step 4 is 3-7, and the tea polyphenols are a concentration of in mixed alcohol liquid
10-15g/L。
The tea polyphenols quality in dispersion alcohol liquid in the step 5 is the 20- of graphene quality in graphene prefabricated membrane
30%, the voltage of the micro-electrolysis reaction is 10-15V, current density 20-500mA/cm2, temperature is 50-60 DEG C.
Graphene is added into absolute ethyl alcohol step 1, and is aided with dispersant and stirs to form dispersed structure, prevents graphene
Reunite.
Mixed liquor is added into ball-milling device and carries out ball-milling reaction by step 2, and graphene particles are refined, and is formed more steady
Fixed fine powder structure, and during the drying process removing absolute ethyl alcohol obtains graphene particles and polyvinylpyrrolidone
Mixture；In mechanical milling process, not only graphene particles are further refined, but also polyvinylpyrrolidone is dispersed in
In graphene.
Step 3 stirs graphene mixture in water can form viscous fluid, and polyvinylpyrrolidone can be molten at this time
Solution in water, forms and has sticking liquid, graphene powder is bonded together；In base material table by the way of uniformly spraying
Face forms stable graphene film, bonds graphene using polyvinylpyrrolidone as adhesive, and as the water of solvent
It can remove during the drying process, form dry film.
Step 4 mixes ethyl alcohol and methanol, forms alcohol liquid that can be miscible, and can be dissolved in using tea polyphenols anhydrous
The characteristic of ethyl alcohol can ensure that tea polyphenols are dissolved in alcohol liquid, obtain dispersion alcohol liquid.
Graphene prefabricated membrane is added in dispersion alcohol liquid step 5, and carries out micro-electrolysis reaction, and ethyl alcohol is as dissolving at this time
Agent can dissolve polyvinylpyrrolidone, form relatively stable hole, while be reducing agent using tea polyphenols, with methanol
Good reduction effect can be played as electrolyte, the oxidized portion of graphene surface is removed, forms graphene-structured more
For close porous graphene film；It is simultaneously the dissolved efficiency of promotion polyvinylpyrrolidone.
From the above, it can be seen that the present invention has following advantages：
1. the preparation method of the present invention is simple and convenient, using ep-type material as raw material, and industrial wastewater is not generated, energy
Enough meet the environmental requirement of industrialized production.
2. the present invention uses ethyl alcohol and methanol as mixed alcohol liquid, can not only be using absolute ethyl alcohol as polyvinyl pyrrole
The dissolution solvent of alkanone binder, and using methanol as electrolyzer, tea polyphenols can form stable graphite as reducing agent
Alkene film porous structure.
Specific implementation mode
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of high-performance porous graphene film, includes the following steps：
Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；
Step 2, mixed liquor is put into progress ball-milling reaction 2h in ball-milling device, graphene mixture is obtained after drying；
Step 3, graphene mixture is added to the water stirring and forms viscous fluid, substrate surface is then sprayed at, after drying
Obtain graphene prefabricated membrane；
Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to completely molten
Solution obtains dispersion alcohol liquid；
Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, micro-electrolysis reaction 2h obtains graphene film.
A concentration of 30g/L of the graphene in absolute ethyl alcohol in the step 1, the addition of the dispersant is graphite
The 20% of alkene quality, the dispersant use polyvinylpyrrolidone, and the mixing speed of the stirring is 2000r/min.
The temperature of ball-milling reaction in the step 2 is 60 DEG C, and drying temperature is 80 DEG C.
The mass ratio of graphene mixture and water in the step 3 is 3:2, the fountain height of the sprinkling is 2g/cm2,
The temperature of the drying is 90 DEG C.
Base material in the step 3 uses substrate modified, the modification procedure of substrate modified as follows：
Base material is added in hydrochloric acid solution and stirs 2h by step a, is washed after taking-up and obtains acidification base material；
Step b, acidification base material is added in absolute ethyl alcohol and is stirred by ultrasonic, and is dried after removal and is obtained passivation base material；
Step c, alcohol-soluble resin is added and is stirred evenly into absolute ethyl alcohol, forms resinol liquid, then using spraying
Mode be evenly distributed on substrate surface, form substrate modified.
A concentration of 0.01mol/L of hydrochloric acid solution in the step a, the addition of the hydrochloric acid can base material covering,
The mixing speed is 1000r/min.
Absolute ethyl alcohol addition in the step b can be by acidification base material submergence, the supersonic frequency of the ultrasonic agitation
For 20kHz, temperature is 40 DEG C, and the drying temperature of the drying is 90 DEG C.
Alcohol-soluble resin in the step c uses Lauxite, a concentration of 30g/L of the alcohol-soluble resin described
The quantity for spray of substrate surface is 10g/L.
The volume ratio of ethyl alcohol and methanol in the step 4 is 3, a concentration of 10g/ of the tea polyphenols in mixed alcohol liquid
L。
The tea polyphenols quality in dispersion alcohol liquid in the step 5 is 20% of graphene quality in graphene prefabricated membrane,
The voltage of the micro-electrolysis reaction is 10V, current density 20mA/cm2, temperature is 50 DEG C.
Embodiment 2
A kind of preparation method of high-performance porous graphene film, includes the following steps：
Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；
Step 2, mixed liquor is put into progress ball-milling reaction 4h in ball-milling device, graphene mixture is obtained after drying；
Step 3, graphene mixture is added to the water stirring and forms viscous fluid, substrate surface is then sprayed at, after drying
Obtain graphene prefabricated membrane；
Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to completely molten
Solution obtains dispersion alcohol liquid；
Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, micro-electrolysis reaction 4h obtains graphene film.
A concentration of 70g/L of the graphene in absolute ethyl alcohol in the step 1, the addition of the dispersant is graphite
The 40% of alkene quality, the dispersant use polyethylene glycol 200, and the mixing speed of the stirring is 3000r/min.
The temperature of ball-milling reaction in the step 2 is 70 DEG C, and drying temperature is 100 DEG C.
The mass ratio of graphene mixture and water in the step 3 is 3:5, the fountain height of the sprinkling is 8g/cm2,
The temperature of the drying is 100 DEG C.
Base material in the step 3 uses substrate modified, the modification procedure of substrate modified as follows：
Base material is added in hydrochloric acid solution and stirs 4h by step a, is washed after taking-up and obtains acidification base material；
Step b, acidification base material is added in absolute ethyl alcohol and is stirred by ultrasonic, and is dried after removal and is obtained passivation base material；
Step c, alcohol-soluble resin is added and is stirred evenly into absolute ethyl alcohol, forms resinol liquid, then using spraying
Mode be evenly distributed on substrate surface, form substrate modified.
A concentration of 0.03mol/L of hydrochloric acid solution in the step a, the addition of the hydrochloric acid can base material covering,
The mixing speed is 2000r/min.
Absolute ethyl alcohol addition in the step b can be by acidification base material submergence, the supersonic frequency of the ultrasonic agitation
For 20-40kHz, temperature is 60 DEG C, and the drying temperature of the drying is 100 DEG C.
Alcohol-soluble resin in the step c uses Lauxite or polyvinyl butyral, the alcohol-soluble resin
The quantity for spray of a concentration of 180g/L, the substrate surface are 30g/L.
The volume ratio of ethyl alcohol and methanol in the step 4 is 7, a concentration of 15g/ of the tea polyphenols in mixed alcohol liquid
L。
The tea polyphenols quality in dispersion alcohol liquid in the step 5 is 30% of graphene quality in graphene prefabricated membrane,
The voltage of the micro-electrolysis reaction is 15V, current density 500mA/cm2, temperature is 60 DEG C.
Embodiment 3
A kind of preparation method of high-performance porous graphene film, includes the following steps：
Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；
Step 2, mixed liquor is put into progress ball-milling reaction 3h in ball-milling device, graphene mixture is obtained after drying；
Step 3, graphene mixture is added to the water stirring and forms viscous fluid, substrate surface is then sprayed at, after drying
Obtain graphene prefabricated membrane；
Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to completely molten
Solution obtains dispersion alcohol liquid；
Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, micro-electrolysis reaction 3h obtains graphene film.
A concentration of 50g/L of the graphene in absolute ethyl alcohol in the step 1, the addition of the dispersant is graphite
The 30% of alkene quality, the dispersant use polyvinylpyrrolidone, and the mixing speed of the stirring is 2500r/min.
The temperature of ball-milling reaction in the step 2 is 65 DEG C, and drying temperature is 90 DEG C.
The mass ratio of graphene mixture and water in the step 3 is 3:4, the fountain height of the sprinkling is 6g/cm2,
The temperature of the drying is 95 DEG C.
Base material in the step 3 uses substrate modified, the modification procedure of substrate modified as follows：
Base material is added in hydrochloric acid solution and stirs 3h by step a, is washed after taking-up and obtains acidification base material；
Step b, acidification base material is added in absolute ethyl alcohol and is stirred by ultrasonic, and is dried after removal and is obtained passivation base material；
Step c, alcohol-soluble resin is added and is stirred evenly into absolute ethyl alcohol, forms resinol liquid, then using spraying
Mode be evenly distributed on substrate surface, form substrate modified.
A concentration of 0.02mol/L of hydrochloric acid solution in the step a, the addition of the hydrochloric acid can base material covering,
The mixing speed is 1500r/min.
Absolute ethyl alcohol addition in the step b can be by acidification base material submergence, the supersonic frequency of the ultrasonic agitation
For 30kHz, temperature is 50 DEG C, and the drying temperature of the drying is 95 DEG C.
Alcohol-soluble resin in the step c uses Lauxite, a concentration of 100g/L of the alcohol-soluble resin described
The quantity for spray of substrate surface is 20g/L.
The volume ratio of ethyl alcohol and methanol in the step 4 is 5, a concentration of 13g/ of the tea polyphenols in mixed alcohol liquid
L。
The tea polyphenols quality in dispersion alcohol liquid in the step 5 is 25% of graphene quality in graphene prefabricated membrane,
The voltage of the micro-electrolysis reaction is 12V, current density 300mA/cm2, temperature is 55 DEG C.
Performance test
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Specific surface area m2/g | 367 | 381 | 423 |
In conclusion the present invention has the following advantages：
1. the preparation method of the present invention is simple and convenient, using ep-type material as raw material, and industrial wastewater is not generated, energy
Enough meet the environmental requirement of industrialized production.
2. the present invention uses ethyl alcohol and methanol as mixed alcohol liquid, can not only be using absolute ethyl alcohol as polyvinyl pyrrole
The dissolution solvent of alkanone binder, and using methanol as electrolyzer, tea polyphenols can form stable graphite as reducing agent
Alkene film porous structure.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical solution described in inventive embodiments.It will be understood by those of ordinary skill in the art that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of high-performance porous graphene film, it is characterised in that：Include the following steps：
Step 1, graphene is added into absolute ethyl alcohol, dispersant is then added and stirs to form mixed liquor；
Step 2, mixed liquor is put into progress ball-milling reaction 2-4h in ball-milling device, graphene mixture is obtained after drying；
Step 3, graphene mixture is added to the water stirring and forms viscous fluid, be then sprayed at substrate surface, obtained after drying
Graphene prefabricated membrane；
Step 4, ethyl alcohol and methanol are mixing uniformly to form mixed alcohol liquid, tea polyphenols is then added and stir to being completely dissolved, obtain
To dispersion alcohol liquid；
Step 5, graphene prefabricated membrane is added into dispersion alcohol liquid, micro-electrolysis reaction 2-4h obtains graphene film.
2. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：The step
A concentration of 30-70g/L of the graphene in absolute ethyl alcohol in rapid 1, the addition of the dispersant is the 20- of graphene quality
40%, the dispersant uses polyvinylpyrrolidone or polyethylene glycol 200, and the mixing speed of the stirring is 2000-
3000r/min。
3. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：The step
The temperature of ball-milling reaction in rapid 2 is 60-70 DEG C, and drying temperature is 80-100 DEG C.
4. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：The step
The mass ratio of graphene mixture and water in rapid 3 is 3:The fountain height of 2-5, the sprinkling are 2-8g/cm2, the drying
Temperature is 90-100 DEG C.
5. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：The step
Base material in rapid 3 uses substrate modified, the modification procedure of substrate modified as follows：
Base material is added in hydrochloric acid solution and stirs 2-4h by step a, is washed after taking-up and obtains acidification base material；
Step b, acidification base material is added in absolute ethyl alcohol and is stirred by ultrasonic, and is dried after removal and is obtained passivation base material；
Step c, alcohol-soluble resin is added and is stirred evenly into absolute ethyl alcohol, forms resinol liquid, then using the side of spraying
Formula is evenly distributed on substrate surface, forms substrate modified.
6. a kind of preparation method of high-performance porous graphene film according to claim 5, it is characterised in that：The step
A concentration of 0.01-0.03mol/L of hydrochloric acid solution in rapid a, the addition of the hydrochloric acid can base material covering, the stirring is fast
Degree is 1000-2000r/min.
7. a kind of preparation method of high-performance porous graphene film according to claim 5, it is characterised in that：The step
Absolute ethyl alcohol addition in rapid b can be by acidification base material submergence, and the supersonic frequency of the ultrasonic agitation is 20-40kHz, temperature
It it is 40-60 DEG C, the drying temperature of the drying is 90-100 DEG C.
8. a kind of preparation method of high-performance porous graphene film according to claim 5, it is characterised in that：The step
Alcohol-soluble resin in rapid c uses Lauxite or polyvinyl butyral, a concentration of 30-180g/ of the alcohol-soluble resin
The quantity for spray of L, the substrate surface are 10-30g/L.
9. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：The step
The volume ratio of ethyl alcohol and methanol in rapid 4 is 3-7, a concentration of 10-15g/L of the tea polyphenols in mixed alcohol liquid.
10. a kind of preparation method of high-performance porous graphene film according to claim 1, it is characterised in that：It is described
The tea polyphenols quality in dispersion alcohol liquid in step 5 is the 20-30% of graphene quality in graphene prefabricated membrane, the light electrolysis
The voltage of reaction is 10-15V, current density 20-500mA/cm2, temperature is 50-60 DEG C.
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Cited By (1)
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| CN109824041A (en) * | 2019-04-09 | 2019-05-31 | 广东墨睿科技有限公司 | A kind of lithium battery graphene conductive agent and preparation method thereof |
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