CN108383111A - A kind of graphene slurry and preparation method thereof - Google Patents
A kind of graphene slurry and preparation method thereof Download PDFInfo
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- CN108383111A CN108383111A CN201810446500.6A CN201810446500A CN108383111A CN 108383111 A CN108383111 A CN 108383111A CN 201810446500 A CN201810446500 A CN 201810446500A CN 108383111 A CN108383111 A CN 108383111A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The present invention discloses a kind of graphene slurry and preparation method thereof, wherein the preparation method of the graphene slurry includes the following steps：Graphene powder is prepared by liquid phase synthesizing method in oligoacrylonitrile；The graphene powder is subjected to mechanical ball mill processing；Dispersant is dissolved into solvent and obtains mixed solvent；Graphene powder after ball-milling treatment is added in the mixed solvent, ultrasonic wave added obtains graphene slurry after being uniformly dispersed.Preparation method of the present invention has the advantages of simple for process, there are no pollution to the environment, and good dispersion, stability height, highly concentrated graphene slurry can be prepared, and obtained graphene slurry can be used for the field of new materials such as conduction, heat conduction.
Description
Technical field
The present invention relates to field of graphene more particularly to a kind of graphene slurry and preparation method thereof.
Background technology
From 2004 by Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao loves
Since it was found that, graphene is always the research hotspot of people.Graphene is made of single layer of carbon atom, has excellent electricity, machine
Tool, characteristic optically and thermally etc., in necks such as composite material, energy storage material, battery material, electronic device, biomaterials
Domain is with a wide range of applications.
So far, grapheme material be in the world it is known it is most thin be also most hard material, it has very excellent
The resistivity ratio copper of electric conductivity and heat conductivility, graphene is also low, and thermal coefficient is also far above diamond.But due to
The large specific surface area of graphene is easy to happen reunion, thus has seriously affected its performance, how application when keep graphene
Efficient dispersion is current urgent need to solve the problem.
Currently, preparing high concentration, high-stability graphene dispersing solution is an important skill for solving graphene downstream application
Art.At this stage the preparation method of graphene dispersing solution be typically in preparation process add coupling agent, modifying agent to graphene into
Row modification, but the operation of this process is more complicated, obtained graphene dispersing solution performance is unsatisfactory, and concentration is relatively low,
And the coupling agent etc. added belongs to impurity can also influence its subsequent applications to a certain extent.
Therefore, the existing technology needs to be improved and developed.
Invention content
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene slurry and its preparation sides
Method, it is intended to solve existing graphene dispersing solution process is complicated for operation and the graphene dispersing solution stability that is prepared
Problem low, concentration is relatively low.
Technical scheme is as follows：
A kind of preparation method of graphene slurry, wherein include the following steps：
Graphene powder is prepared by liquid phase synthesizing method in oligoacrylonitrile；
The graphene powder is subjected to ball-milling treatment；
Dispersant is dissolved into solvent and obtains mixed solvent；
Graphene powder after ball-milling treatment is added in the mixed solvent, graphene slurry is obtained after being uniformly dispersed.
The preparation method of the graphene slurry, wherein described to prepare oligoacrylonitrile by liquid phase synthesizing method
Graphene powder is obtained, following steps are specifically included：
Oligoacrylonitrile is pre-processed at a temperature of inert atmosphere, 220-300 DEG C to obtain graphene presoma；
The graphene presoma is subjected to crosslinking sintering at a temperature of inert atmosphere, 1000-1500 DEG C；
Sintered product will be crosslinked and carry out graphitization sintering at a temperature of inert atmosphere, 2400-3000 DEG C, obtain graphene
Powder.
The preparation method of the graphene slurry, wherein the time of the ball-milling treatment is 1-6 hours.
The preparation method of the graphene slurry, wherein the mass ratio of the dispersant and the solvent is 1：1~10.
The preparation method of the graphene slurry, wherein the dispersant is polyvinylpyrrolidone, carboxymethyl cellulose
One kind in element, acetate ethylene copolymer.
The preparation method of the graphene slurry, wherein the solvent is N-Methyl pyrrolidone, ethyl alcohol, formamide
It is one or more in acetone, ethyl acetate, dichloromethane.
The preparation method of the graphene slurry, wherein described to be separated into ultrasonic disperse.
The preparation method of the graphene slurry, wherein the power of the ultrasonic disperse is 50-100Hz.
The preparation method of the graphene slurry, wherein the mass concentration of the graphene slurry is 0.01-20mg/
mL。
A kind of graphene slurry, wherein be prepared using preparation method as described above.
Advantageous effect：The present invention provides a kind of preparation method of graphene slurry, by liquid phase synthesis thermal chemical reaction with
The method that solid-phase sintering is combined is prepared graphene powder, graphene carbon atomic plane structural integrity, the defect of formation be few,
The number of plies is low, has the characteristics that high conductivity, high thermal conductivity.Preparation method of the present invention without being modified to graphene or
Modification, is handled by simple process, and good dispersion, stability height, highly concentrated graphene slurry can be prepared.
Description of the drawings
Fig. 1 is the Raman spectrogram of the graphene slurry prepared by the embodiment of the present invention 3.
Fig. 2 is the scanning electron microscope (SEM) photograph of the graphene slurry prepared by the embodiment of the present invention 3.
Specific implementation mode
A kind of graphene slurry of present invention offer and preparation method thereof, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
The preparation method of a kind of graphene slurry of the present invention, wherein include the following steps：
S100, by oligoacrylonitrile by liquid phase synthesizing method, graphene powder is prepared；
S200, the graphene powder is subjected to ball-milling treatment；
S300, it dispersant is dissolved into solvent obtains mixed solvent；
S400, the graphene powder after ball-milling treatment is added in the mixed solvent, graphene slurry is obtained after being uniformly dispersed.
The graphene powder of high quality is prepared by liquid phase synthesizing method using homemade LPAN as raw material by the present invention,
The graphene powder is configured to graphene slurry after ball-milling treatment with the solvent containing dispersant.Graphite of the present invention
The preparation method of alkene slurry has the following advantages：
1, it uses unique liquid phase synthesizing method and prepares graphene powder raw material；
2, mechanical milling process can be with further such that detach between graphene sheet layer；
3, dispersant is added, can effectively improve the dispersibility of graphene, it is made to be uniformly dispersed, improves dispersion concentration；
4, method and process used in the present invention is simple, is safe from harm to environment.
The step S100 specifically includes following steps：
S101, by oligoacrylonitrile in inert atmosphere（Such as nitrogen atmosphere）, pre-processed to obtain at a temperature of 220-300 DEG C
Graphene presoma；
S102, by the graphene presoma in inert atmosphere（Such as nitrogen atmosphere）, be crosslinked at a temperature of 1000-1500 DEG C
Sintering；
Graphene presoma is carried out crosslinking sintering by the present invention under the atmosphere of nitrogen, and crosslinking sintering temperature is 1000-1500 DEG C,
Graphene presoma can be made to be cross-linked to form two-dimension plane structure under the sintering temperature；
S103, sintered product will be crosslinked in inert atmosphere（Such as argon gas atmosphere）, carry out graphite at a temperature of 2400-3000 DEG C
Change sintering, obtains graphene powder.
The present invention is crosslinked sintered product and is graphitized formation under the graphitization sintering temperature with purity height, granularity
The graphene powder of uniform feature.
The step S200 is specifically included：Obtained graphene powder is put into ball grinder and carries out ball-milling treatment.Ball
Honed journey can be further such that detach, to be conducive to improve the dispersibility of graphene slurry between graphene sheet layer.Wherein,
Ball mill used by mechanical milling process can be planetary ball mill, the multiclass ball mill such as high energy ball mill.
Preferably, the time of the ball-milling treatment is 1-6 hours, to ensure that graphene film layer separation is complete.It needs to illustrate
, those skilled in the art can be according to the needs of practical application, to the progress of ball-milling treatment time suitable for adjustment.
In the step S300, it is preferred that the mass ratio of the dispersant and the solvent is 1：1 ~ 10, the mass ratio
Mixed solvent can effectively improve the dispersion concentration of graphene.
Preferably, the dispersant is one in polyvinylpyrrolidone, hydroxymethyl cellulose, acetate ethylene copolymer
Kind.The dispersant can effectively avoid agglomeration of the graphene powder in graphene slurry, improve graphene slurry
Stability.
Preferably, the solvent is in N-Methyl pyrrolidone, ethyl alcohol, formamide acetone, ethyl acetate, dichloromethane
It is one or more.Graphene powder of the present invention after ball-milling treatment with most of common solvents needed for it can be configured to
The graphene slurry wanted, used solvent are not limited to the above-mentioned solvent enumerated.Graphene slurry of the present invention is used
Solvent range it is wide, be conducive to expand graphene slurry application range.
In the step S400, it is preferred that described to be separated into ultrasonic disperse, the power of the ultrasonic disperse is 50-
100Hz.The present invention is disperseed by ultrasonic wave added, further promotes the dispersibility of graphene powder in graphene slurry.
The mass concentration of graphene slurry of the present invention is 0.01-20mg/mL.Graphene slurry prepared by the present invention
It is not susceptible to reunite, the concentration of graphene slurry has good dispersibility and stability up to 20mg/mL.
The preparation method of graphene slurry of the present invention is in preparation process without adding coupling agent, modifying agent to graphite
Alkene is modified, and with simple, the environmental-friendly feature of process, promotes the application range of graphene slurry.
The present invention provides a kind of graphene slurry, wherein is prepared using preparation method as described above.System of the present invention
Standby graphene slurry is conducive to its subsequent application without impurity such as coupling agent, modifying agent.Graphene slurry prepared by the present invention
Material has the characteristics that good dispersion, stability are good.
Technical scheme of the present invention is illustrated below by specific embodiment.
Embodiment 1
It is prepared via a method which the graphene slurry of 4mg/mL：
(1) oligoacrylonitrile is pre-processed to obtain stone at a temperature of 260 DEG C first in a nitrogen atmosphere for raw material
Black alkene presoma；
(2) in a nitrogen atmosphere by graphene presoma, crosslinking sintering is carried out at a temperature of 1400 DEG C；
(3) and then under an argon atmosphere it, is graphitized sintering at a temperature of 3000 DEG C, obtains graphene powder；
(4) by obtained graphene powder in high energy ball mill ball milling 1 hour；
(5) 4g dispersants PVP is dissolved into the nmp solvent of 100mL and arrives mixed solvent；
(6) graphene powder of 400mg is added in the mixed solvent, is disperseed by ultrasonic wave added, is configured to the graphite of 4mg/mL
Alkene slurry.
Embodiment 2
It is prepared via a method which the graphene slurry of 6mg/mL：
(1) oligoacrylonitrile is pre-processed to obtain stone at a temperature of 260 DEG C first in a nitrogen atmosphere for raw material
Black alkene presoma；
(2) in a nitrogen atmosphere by graphene presoma, crosslinking sintering is carried out at a temperature of 1400 DEG C；
(3) and then under an argon atmosphere it, is graphitized sintering at a temperature of 3000 DEG C, obtains graphene powder；
(4) by obtained graphene powder in high energy ball mill ball milling 1 hour；
(5) 4g dispersants PVP is dissolved into the nmp solvent of 100mL and arrives mixed solvent；
(6) graphene powder of 600mg is added in the mixed solvent, is disperseed by ultrasonic wave added, is configured to the graphite of 6mg/mL
Alkene slurry.
Embodiment 3
It is prepared via a method which the graphene slurry of 10mg/mL：
(1) oligoacrylonitrile is pre-processed to obtain stone at a temperature of 260 DEG C first in a nitrogen atmosphere for raw material
Black alkene presoma；
(2) in a nitrogen atmosphere by graphene presoma, crosslinking sintering is carried out at a temperature of 1400 DEG C；
(3) and then under an argon atmosphere it, is graphitized sintering at a temperature of 3000 DEG C, obtains graphene powder；
(4) by obtained graphene powder in high energy ball mill ball milling 1 hour；
(5) 4g dispersants PVP is dissolved into the nmp solvent of 100mL and arrives mixed solvent；
(6) graphene powder of 1000mg is added in the mixed solvent, is disperseed by ultrasonic wave added, is configured to the stone of 10mg/mL
Black alkene slurry.
Fig. 1 is the Raman spectrogram of graphene slurry prepared by the present embodiment.As can be seen from Figure 1 the present embodiment is made
Graphene purity in standby graphene slurry is high, and impurity content is few.Fig. 2 is graphene slurry prepared by the embodiment of the present invention
Scanning electron microscope (SEM) photograph.As can be seen from Figure 2 the graphene sheet layer in the graphene slurry prepared by the present embodiment is effectively divided
From, and have the characteristics that homogeneous grain diameter.
Embodiment 4
It is prepared via a method which the graphene slurry of 15mg/mL：
(1) oligoacrylonitrile is pre-processed to obtain stone at a temperature of 260 DEG C first in a nitrogen atmosphere for raw material
Black alkene presoma；
(2) in a nitrogen atmosphere by graphene presoma, crosslinking sintering is carried out at a temperature of 1400 DEG C；
(3) and then under an argon atmosphere it, is graphitized sintering at a temperature of 3000 DEG C, obtains graphene powder；
(4) by obtained graphene powder in high energy ball mill ball milling 1 hour；
(5) 4g dispersants PVP is dissolved into the nmp solvent of 100mL and arrives mixed solvent；
(6) graphene powder of 1500mg is added in the mixed solvent, is disperseed by ultrasonic wave added, is configured to the stone of 15mg/mL
Black alkene slurry.
The stability of the embodiment 1-4 graphene slurries prepared is tested.Graphene slurry prepared by embodiment 1-4
Material is poured into the vial that number is 1,2,3,4 and is stood respectively, observes whether graphite slurry has layering, reunites now week about
As.It is found by test in one month, the graphite slurry prepared by embodiment 1-4 is generated without layering, agglomeration.
In conclusion the present invention provides a kind of preparation method of graphene slurry, oligoacrylonitrile is closed by liquid phase
Graphene powder is obtained at method；The graphene powder is subjected to ball milling stripping；Dispersant is dissolved into solvent and is mixed
Solvent；Graphene powder after ball milling is removed is added in the mixed solvent, and graphene slurry is obtained after dispersion.It is of the present invention
Preparation method there is simple for process, the advantages of there are no pollution to the environment, can prepare that good dispersion, stability are high, concentration is high
Graphene slurry.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of graphene slurry, which is characterized in that include the following steps：
Graphene powder is prepared by liquid phase synthesizing method in oligoacrylonitrile；
The graphene powder is subjected to ball-milling treatment；
Dispersant is dissolved into solvent and obtains mixed solvent；
Graphene powder after ball-milling treatment is added in the mixed solvent, graphene slurry is obtained after being uniformly dispersed.
2. the preparation method of graphene slurry according to claim 1, which is characterized in that described to lead to oligoacrylonitrile
It crosses liquid phase synthesizing method and graphene powder is prepared, specifically include following steps：
Oligoacrylonitrile is pre-processed at a temperature of inert atmosphere, 220-300 DEG C to obtain graphene presoma；
The graphene presoma is subjected to crosslinking sintering at a temperature of inert atmosphere, 1000-1500 DEG C；
Sintered product will be crosslinked and carry out graphitization sintering at a temperature of inert atmosphere, 2400-3000 DEG C, obtain graphene
Powder.
3. the preparation method of graphene slurry according to claim 1, which is characterized in that the time of the ball-milling treatment is
1-6 hours.
4. the preparation method of graphene slurry according to claim 1, which is characterized in that the dispersant and the solvent
Mass ratio be 1：1~10.
5. the preparation method of graphene slurry according to claim 1, which is characterized in that the dispersant is polyethylene pyrrole
One kind in pyrrolidone, carboxymethyl cellulose, acetate ethylene copolymer.
6. the preparation method of graphene slurry according to claim 1, which is characterized in that the solvent is N- methylpyrroles
It is one or more in alkanone, ethyl alcohol, formamide acetone, ethyl acetate, dichloromethane.
7. the preparation method of graphene slurry according to claim 1, which is characterized in that described to be separated into ultrasonic disperse.
8. the preparation method of graphene slurry according to claim 7, which is characterized in that the power of the ultrasonic disperse is
50-100Hz。
9. the preparation method of graphene slurry according to claim 1, which is characterized in that the quality of the graphene slurry
A concentration of 0.01-20mg/mL.
10. a kind of graphene slurry, which is characterized in that be prepared using the preparation method as described in claim 1-9 is any.
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Cited By (6)
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| CN109888244A (en) * | 2019-03-15 | 2019-06-14 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene coated graphitization coal negative electrode material, battery and preparation method thereof |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
| CN114671429A (en) * | 2022-04-27 | 2022-06-28 | 深圳材启新材料有限公司 | Preparation method of high-quality graphene dispersion liquid |
| CN114744159A (en) * | 2022-05-07 | 2022-07-12 | 中国人民解放军陆军工程大学 | Battery cathode slurry manufacturing method and battery |
| CN114792585A (en) * | 2022-01-20 | 2022-07-26 | 马国庆 | Preparation treatment process of graphene slurry with strong magnetic and electric properties |
| CN115093692A (en) * | 2022-06-27 | 2022-09-23 | 中国石油大学(北京) | Graphene composite electromagnetic shielding film and preparation method thereof |
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| CN115093692A (en) * | 2022-06-27 | 2022-09-23 | 中国石油大学(北京) | Graphene composite electromagnetic shielding film and preparation method thereof |
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