CN107628610A - A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid - Google Patents
A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid Download PDFInfo
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- CN107628610A CN107628610A CN201711035685.3A CN201711035685A CN107628610A CN 107628610 A CN107628610 A CN 107628610A CN 201711035685 A CN201711035685 A CN 201711035685A CN 107628610 A CN107628610 A CN 107628610A
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Abstract
The invention belongs to technical field of graphene preparation technical field, and in particular to a kind of method that mechanical stripping method prepares graphene and graphene conductive liquid.Graphite is simply handled, you can obtain up-to-standard graphene and graphene conductive liquid.Raw material resources used in the present invention enriches, cost is relatively low, and preparation technology is simple, is easy to mass produce.
Description
Technical field
The invention belongs to technical field of graphene preparation, and in particular to a kind of mechanical stripping method prepares graphene and graphite
The method of alkene conduction liquid.
Background technology
The two-dimensional nano Carbon Materials that graphene is made up of the carbon atom of sp2 hydridization, it is considered to be build many other charcoals
The elementary cell of material.For example, graphene can be wrapped to form the fullerene of zero dimension；It can crimp as one-dimensional CNT,
The graphite of three-dimensional can be stacked as.It is therefore contemplated that graphene is the mother of all Carbon Materials.The preparation method of graphene has very
It is a variety of, there are chemical vapour deposition technique, epitaxial growth method, chemical synthesis and chemical oxidation stripping method using more at present.
Chemical vapour deposition technique is to be pyrolyzed small molecule hydro carbons at high temperature using metal substrate to obtain graphene.This method
It can obtain and be distributed the graphene homogeneous, area is larger and quality is higher；Shortcoming is price costly and yield is relatively low.
Epitaxial growth method is usually to be synthesized using silicon carbide substrate under conditions of high temperature high vacuum.Advantage is to prepare
Large scale, the graphene of high quality, but equipment used in it is general costly, and under graphene is shifted from substrate
Come also relatively difficult, yield is also than relatively low.
Chemical synthesis is mainly to be synthesized from bottom to top using organic compound presomas such as condensed-nuclei aromatics.This method
The advantages of be the size that can control graphene, it is low that shortcoming is still Yield comparison.
Chemical oxidation stripping method is by graphite oxidation, so as to increase graphite linings using the strong oxidizer such as sulfuric acid, potassium permanganate
Spacing, graphene oxide is obtained through ultrasound stripping, then through high temperature reduction, you can obtain graphene.The advantages of this method is production
Amount is higher, and price is relatively cheap, and shortcoming is that product defects is more, and environmental pollution is than more serious caused by preparation process.
Therefore, it is necessary to a kind of new method for preparing graphene and graphene conductive liquid.
The content of the invention
It is an object of the invention to for prior art cost it is high, yield poorly the problem of, there is provided a kind of mechanical stripping method
The method for preparing graphene and graphene conductive liquid.
Technical scheme is as follows：
A kind of method that mechanical stripping method prepares graphene, in turn includes the following steps：
Powdered graphite, solvent and dispersant are sufficiently mixed by step 1., obtain suspension；Described graphite and solvent
Ratio be 1:10-1:100, the ratio of graphite and dispersant is 100:1-1:1；1 μm~the 1mm of particle diameter of the powdered graphite；
In the suspension that step 2. obtains to step 1 carbon dioxide is passed through with the mode of pressurization；Described pressure is 5-
10MPa；
The mixed liquor that step 3. obtains step 2, which is placed in high pressure homogenizer, carries out homogenization, obtains graphene dispersion
Liquid；The pressure of high pressure homogenizer is set as 50~300MPa, repeats 3~5 homogenizations；
The graphene dispersing solution that step 4. obtains step 3, which is placed in ultrasonic machine, to be ultrasonically treated, after being handled
Graphene dispersing solution；Ultrasonic power is set as 100-3000W, time 1-10h；
Graphene dispersing solution after the processing that step 5. obtains step 4 is dried to obtain graphene powder.
The ratio of graphite and solvent described in the step 1 is 1:20~1:100.
The ratio of the graphite and dispersant is 20:1~5:1.
The graphite is native graphite, Delanium or expanded graphite.
1~10 μm of the particle diameter of the powdered graphite.
The solvent is using one or more mixing in deionized water, 1-METHYLPYRROLIDONE or ethanol
Liquid.
The dispersant is using dodecyl sodium sulfate, neopelex, polyvinyl alcohol, lignin sulfonic acid
One or more mixed liquors in sodium, cetyl trimethylammonium bromide or polyvinylpyrrolidone.
Described drying means is using lyophilized or drying.
A kind of method that graphene prepared using the above method prepares graphene conductive liquid, by the graphene powder of preparation
It is to obtain graphene conductive liquid afterwards with conductive auxiliary agent, compound solvent；Described graphene and the ratio of conductive auxiliary agent are 100:1-
1:100, the ratio of graphene and solvent is 1:10-1:100.
Described conductive auxiliary agent is CNT, carbon black, gas-phase growth of carbon fibre or amorphous carbon.
The solvent is using one or more mixing in deionized water, 1-METHYLPYRROLIDONE or ethanol
Liquid.
The beneficial effects of the present invention are：
Method provided by the present invention mainly has the characteristics of low cost, good dispersion, stability are good, production efficiency is high.This
The graphene number of plies that the preparation technology that invention provides obtains is about 10 layers or so；Conduct electricity very well；Good heat conductivity.In the present invention
Raw material resources used is abundant, cost is relatively low, and preparation technology is simple, is easy to mass produce.
Brief description of the drawings
Fig. 1 is the atomic force microscopy diagram of graphene prepared by the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail to the present invention.
Embodiment 1
A kind of preparation method of graphene and graphene conductive liquid is present embodiments provided, is in turn included the following steps：
Powdered graphite, solvent and dispersant are sufficiently mixed by step 1., obtain suspension；Described graphite and solvent
Ratio be 10:1-1:100, preferably 1:20~1:100, the ratio of graphite and dispersant is 100:1-1:1, preferably 20:1~
5:1；
Solvent and dispersant are sufficiently mixed first, powdered graphite is then poured into mixed liquor, obtains graphite suspension；
Powdery graphite, solvent and dispersant can be directly directly mixed to get suspension；
Described graphite can be native graphite, Delanium or expanded graphite；1 μm~the 1mm of particle diameter of powdered graphite,
Preferably 1~10 μm；
Described solvent is using one or more mixing in deionized water, 1-METHYLPYRROLIDONE or ethanol
Liquid；
Described dispersant is using dodecyl sodium sulfate, neopelex, polyvinyl alcohol, sulfomethylated lignin
One or more mixed liquors in sour sodium, cetyl trimethylammonium bromide or polyvinylpyrrolidone；
In the mixed liquor that step 2. obtains to step 1 carbon dioxide is passed through with the mode of pressurization；Described pressure position 5-
10MPa；The mixed liquor that step 3. obtains step 2, which is placed in high pressure homogenizer, carries out homogenization, obtains graphene dispersing solution
1；The pressure of high pressure homogenizer is set as 50~300MPa, repeats 3~5 homogenizations；
The graphene dispersing solution 1 that step 3 obtains is placed in ultrasonic machine and is ultrasonically treated by step 4., obtains graphene point
Dispersion liquid 2；Ultrasonic power is set as 100-3000W, time 1-10h；Step 5. dries the graphene dispersing solution 2 that step 4 obtains
Obtain graphene powder；Described drying means is using lyophilized or drying, 1~24 hour drying time；
Graphene conductive liquid is obtained after graphene powder that step 6. obtains step 5 and conductive auxiliary agent, solvent are compound；
Described conductive auxiliary agent is CNT, carbon black, gas-phase growth of carbon fibre or amorphous carbon；The solvent using go from
One or more mixed liquors in sub- water, 1-METHYLPYRROLIDONE or ethanol；Described graphene and the ratio of conductive auxiliary agent
Example is 100:1-1:100, preferably 20:1~5:1, the ratio of graphene and solvent is 1:10-1:100, preferably 1:20~1:
100。
The mechanical stripping method that the technical scheme of the present embodiment uses using the high speed shear of high pressure homogenizer, high frequency oscillation and
The mechanical forces such as convection current shock and corresponding fuel factor further peel off graphite, so as to obtain graphene dispersing solution, then pass through
Dry and can obtain graphene powder.The advantages of this method is that yield is higher, and price is relatively cheap, and preparation process green is without dirt
Dye.The graphene number of plies prepared using the technical program is about 10 layers or so；Conduct electricity very well；Good heat conductivity.In the present invention
Raw material resources used is abundant, cost is relatively low, and preparation technology is simple, is easy to mass produce.
Embodiment 2
The present embodiment provides a kind of preparation method of graphene and graphene conductive liquid on the basis of embodiment 1,
In turn include the following steps：
The preparation of step 1. graphene powder：By 1kg expanded graphites, 20kg deionized waters and 0.5kg polyvinylpyrrolidines
Ketone is well mixed to obtain suspension；
In the mixed liquor that step 2. obtains to step 1 carbon dioxide is passed through with the mode of pressurization；Described pressure position 8MPa；
The mixed liquor that step 3. obtains step 2, which is placed in high pressure homogenizer, carries out homogenization, obtains graphene dispersion
Liquid；The pressure of high pressure homogenizer is set as 200MPa, repeats 5 homogenizations；
The graphene dispersing solution that step 4. obtains step 3, which is placed in ultrasonic machine, to be ultrasonically treated, after being handled
Graphene dispersing solution；Ultrasonic power is set as 1000W, time 2h；Such as the atomic force microscopy analysis shows graphene of accompanying drawing 1
Thickness be 10 layers.
The graphene dispersing solution that step 5. obtains step 4 freezes and obtains graphene powder；Described drying time 2 is small
When；
Step 6. by the graphene powder 0.5kg that step 5 obtains with CNT 0.5kg and deionized water 50kg is compound
It can obtain graphene conductive liquid.
The step of embodiment 3-10, is same as Example 2, and design parameter see the table below.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.It is if these modifications and variations belong within the scope of the claims in the present invention and its equivalent technologies, then of the invention
It is also intended to comprising including these changes and modification.
Claims (10)
1. a kind of method that mechanical stripping method prepares graphene, it is characterised in that：In turn include the following steps：
Powdered graphite, solvent and dispersant are sufficiently mixed by step 1., obtain suspension；Described graphite and the ratio of solvent
Example is 1:10-1:100, the ratio of graphite and dispersant is 100:1-1:1；1 μm~the 1mm of particle diameter of the powdered graphite；
In the suspension that step 2. obtains to step 1 carbon dioxide is passed through with the mode of pressurization；Described pressure is 5-10MPa；
The mixed liquor that step 3. obtains step 2, which is placed in high pressure homogenizer, carries out homogenization, obtains graphene dispersing solution；If
The pressure for determining high pressure homogenizer is 50~300-MPa, repeats 3~5 homogenizations；
The graphene dispersing solution that step 4. obtains step 3, which is placed in ultrasonic machine, to be ultrasonically treated, the graphite after being handled
Alkene dispersion liquid；Ultrasonic power is set as 100-3000W, time 1-10h；
Graphene dispersing solution after the processing that step 5. obtains step 4 is dried to obtain graphene powder.
2. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：Described in step 1
Graphite and solvent ratio be 1:20~1:100.
3. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：The graphite is with dividing
The ratio of powder is 20:1~5:1.
4. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：The graphite is day
Right graphite, Delanium or expanded graphite.
5. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：The powdered graphite
1~10 μm of particle diameter.
6. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：The solvent uses
Be one or more mixed liquors in deionized water, 1-METHYLPYRROLIDONE or ethanol.
7. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：The dispersant is adopted
It is dodecyl sodium sulfate, neopelex, polyvinyl alcohol, sodium lignin sulfonate, cetyl trimethyl bromine
Change one or more mixed liquors in ammonium or polyvinylpyrrolidone.
8. the method that a kind of mechanical stripping method as claimed in claim 1 prepares graphene, it is characterised in that：Described drying side
Method is using lyophilized or drying.
9. a kind of method that graphene using described in claim 1 prepares graphene conductive liquid, it is characterised in that：By preparation
Graphene conductive liquid is obtained after graphene powder and conductive auxiliary agent, solvent are compound；Described graphene and the ratio of conductive auxiliary agent
Example is 100:1-1:100, the ratio of graphene and solvent is 1:10-1:100.
A kind of 10. method for preparing graphene conductive liquid as claimed in claim 1, it is characterised in that：Described conductive auxiliary agent
For CNT, carbon black, gas-phase growth of carbon fibre or amorphous carbon.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827102A (en) * | 2017-11-27 | 2018-03-23 | 内蒙古碳烯石墨新材料有限公司 | A kind of method for preparing graphene |
| CN108277483A (en) * | 2018-02-01 | 2018-07-13 | 中国科学院宁波材料技术与工程研究所 | Graphene is co-deposited chemical nickel-plating liquid and its coating method |
| CN108963255A (en) * | 2018-06-01 | 2018-12-07 | 湖南国盛石墨科技有限公司 | A kind of preparation method of the conduction liquid of containing graphene |
| CN109160507A (en) * | 2018-10-19 | 2019-01-08 | 上海纳米技术及应用国家工程研究中心有限公司 | The magnanimity preparation method of fluorinated graphene |
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN109915896A (en) * | 2019-03-05 | 2019-06-21 | 苏州暖开智能地暖科技有限公司 | A kind of energy conservation graphene floor heating device |
| CN110316730A (en) * | 2019-08-16 | 2019-10-11 | 西北大学 | A kind of preparation method of high concentration graphene concentration dispersion liquid |
| CN110808375A (en) * | 2019-11-07 | 2020-02-18 | 深圳市德方纳米科技股份有限公司 | Preparation method and device of graphene carbon nanotube composite conductive liquid and conductive liquid |
| CN111591982A (en) * | 2020-05-25 | 2020-08-28 | 杭州烯创科技有限公司 | Physical preparation method of graphene by using crystalline flake graphite as raw material |
| CN111732094A (en) * | 2020-07-07 | 2020-10-02 | 北京石墨烯研究院 | Method for preparing graphene through ultrasonic-assisted supercritical liquid phase stripping |
| CN112645314A (en) * | 2021-01-25 | 2021-04-13 | 唐山航天万源科技有限公司 | Graphene conductive liquid and preparation method and application thereof |
| CN114381129A (en) * | 2020-10-19 | 2022-04-22 | 中原大学 | Composite material and method for producing same |
| CN114477153A (en) * | 2022-01-27 | 2022-05-13 | 河南克莱威纳米碳材料有限公司 | Method for preparing graphene by using carbon nanofibers |
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| CN106672949A (en) * | 2016-11-29 | 2017-05-17 | 上海利物盛纳米科技有限公司 | Method for preparing graphene by assisting in stripping graphite based on gas solubilization |
| CN106986329A (en) * | 2016-01-18 | 2017-07-28 | 上海交通大学 | A kind of method for preparing graphene |
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| CN106986329A (en) * | 2016-01-18 | 2017-07-28 | 上海交通大学 | A kind of method for preparing graphene |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827102A (en) * | 2017-11-27 | 2018-03-23 | 内蒙古碳烯石墨新材料有限公司 | A kind of method for preparing graphene |
| CN108277483A (en) * | 2018-02-01 | 2018-07-13 | 中国科学院宁波材料技术与工程研究所 | Graphene is co-deposited chemical nickel-plating liquid and its coating method |
| CN108963255A (en) * | 2018-06-01 | 2018-12-07 | 湖南国盛石墨科技有限公司 | A kind of preparation method of the conduction liquid of containing graphene |
| CN109160507A (en) * | 2018-10-19 | 2019-01-08 | 上海纳米技术及应用国家工程研究中心有限公司 | The magnanimity preparation method of fluorinated graphene |
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN109915896A (en) * | 2019-03-05 | 2019-06-21 | 苏州暖开智能地暖科技有限公司 | A kind of energy conservation graphene floor heating device |
| CN110316730A (en) * | 2019-08-16 | 2019-10-11 | 西北大学 | A kind of preparation method of high concentration graphene concentration dispersion liquid |
| CN110808375A (en) * | 2019-11-07 | 2020-02-18 | 深圳市德方纳米科技股份有限公司 | Preparation method and device of graphene carbon nanotube composite conductive liquid and conductive liquid |
| CN111591982A (en) * | 2020-05-25 | 2020-08-28 | 杭州烯创科技有限公司 | Physical preparation method of graphene by using crystalline flake graphite as raw material |
| CN111732094A (en) * | 2020-07-07 | 2020-10-02 | 北京石墨烯研究院 | Method for preparing graphene through ultrasonic-assisted supercritical liquid phase stripping |
| CN114381129A (en) * | 2020-10-19 | 2022-04-22 | 中原大学 | Composite material and method for producing same |
| CN112645314A (en) * | 2021-01-25 | 2021-04-13 | 唐山航天万源科技有限公司 | Graphene conductive liquid and preparation method and application thereof |
| CN114477153A (en) * | 2022-01-27 | 2022-05-13 | 河南克莱威纳米碳材料有限公司 | Method for preparing graphene by using carbon nanofibers |
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