CN107445155A - A kind of graphene dispersing solution and preparation method thereof - Google Patents
A kind of graphene dispersing solution and preparation method thereof Download PDFInfo
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- CN107445155A CN107445155A CN201710680716.4A CN201710680716A CN107445155A CN 107445155 A CN107445155 A CN 107445155A CN 201710680716 A CN201710680716 A CN 201710680716A CN 107445155 A CN107445155 A CN 107445155A
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Abstract
The present invention relates to Material Field, specifically a kind of graphene dispersing solution and preparation method thereof.It is characterized in that every 100 parts of components by following number form：1 10 parts of graphene, 0.5 5 parts of dispersant, remaining is solvent；Its preparation method comprises the following steps：1）Graphene is prepared into powder；2）Graphene powder and dispersant are obtained into mixture；3）Mixed mixture is put into ball mill, mixture is ground；4）Mixture after grinding is put into solvent, uniformly mixed under conditions of magnetic field, ultrasonic wave, stirring；5）Graphene dispersing solution is obtained after mixing.The present invention compared with the existing technology, overcomes the shortcomings of traditional dispersion technology means, using physics and the coefficient method dispersed graphite alkene of chemistry；By the way of dry grinding and wet grinding combine, mixture is ground, wet-dry change grinding can make the granularity of graphene more uniform, and dispersiveness is more excellent.
Description
Technical field
The present invention relates to Material Field, specifically a kind of graphene dispersing solution and preparation method thereof.
Background technology
Graphene is the bi-dimensional cellular shape lattice structure that a kind of carbon atom by SP2 hydridization is formed with hexagon periodic arrangement
Inorganic nano sheet layer material, the unique monoatomic layer structure of graphene makes it be provided with many excellent performances, such as at room temperature
Electron mobility（2×105cm2·V·s）, intensity reaches 130GPa, and Young's modulus is about 1100GPa, and thermal conductivity factor is up to
5300W/ (mK), great specific surface area（Calculated value is 2630m2/g）.These excellent performances make it in the energy, micro-
The fields such as electronics, information, biological medicine and high-performance composite materials have broad application prospects.In ceramic composite field,
Material property is improved as strengthening mutually usually using one-dimensional carbon fiber, CNT and ceramic whisker, but these strengthen
Material such as CNT often disperses inequality in the base, is also easy to produce reunion.For CNT, graphene is more
With advantage, it preferably can be scattered in ceramic matrix, and equally has excellent mechanics, electrically and thermally performance.
The content of the invention
The present invention is overcome the deficiencies in the prior art, designs a kind of graphene dispersing solution and preparation method thereof, passes through dry method
The mode that grinding and wet grinding combine, is ground to the mixture of graphene powder and dispersant, makes granularity more equal
Even, dispersiveness is more excellent.
To achieve the above object, a kind of graphene dispersing solution and preparation method thereof is designed, it is characterised in that every 100 parts by such as
The component composition of lower number：Graphene 1-10 parts, dispersant 0.5-5 parts, remaining is solvent；
Its preparation method comprises the following steps：1）Graphene is taken, graphene is prepared into powder；2）By graphene powder with disperseing
Agent is mixed to get mixture；3）Mixed mixture is put into ball mill, combined using dry grinding and wet grinding
Mode, mixture is ground；4）Mixture after grinding is put into solvent, under conditions of magnetic field, ultrasonic wave, stirring
Uniformly mixed；5）Graphene dispersing solution is obtained after mixing.
The dispersant selects dimethyl carbonate（DMC）, N, N, N ', in N '-tetramethylethylenediamine, methyl formate or acetonitrile
One or more.
The one or more that the solvent is selected in absolute ethyl alcohol, ether or acetone.
Graphene powder is prepared in the step 1 can use mechanical stripping method, epitaxy method, heating SiC methods, chemistry
Any of reducing process, chemical cleavage method or CVD.
Graphene particles diameter in the step 3 after mixture grinding is less than 250nm.
Magnetic field intensity 0.5-5T in the step 4.
In the step 4 agitating mode be one minute clockwise, one minute counterclockwise, mixing speed 50-100r/min,
Mixing time 0.5-2h.
For the control mode of ultrasonic wave to open three seconds, Guan Sanmiao, the frequency of ultrasonic wave is 20-90KHz in the step 4, is surpassed
The power of sound wave is 1-5KW, and ultrasonic temperature is 25 DEG C.
The present invention compared with the existing technology, overcomes the shortcomings of traditional dispersion technology means, common using physics and chemistry
The method dispersed graphite alkene of effect；By the way of dry grinding and wet grinding combine, mixture is ground, wet-dry change
Grinding can make the granularity of graphene more uniform, and dispersiveness is more excellent.
Embodiment
Embodiment one：
2 parts of graphene is chosen, dispersant is dimethyl carbonate（DMC）, selection amount is 0.5 part, and solvent chooses absolute ethyl alcohol.First
By a small amount of dispersant dimethyl carbonate（DMC）It is well mixed with graphene, using ball mill grinding, first using dry grinding, turns
Speed is 20r/min, milling time 30min, adds dispersant and carries out wet grinding, rotating speed 50r/min, milling time is
60min, temperature are 25 DEG C, obtain the suspension of graphene and dispersant, then above-mentioned suspension is added into anhydrous ethanol solvent
In, it is stirred under the conditions of magnetic field intensity is 0.5T, mixing time 20min, agitating mode is one minute clockwise, the inverse time
Pin one minute, the solution after stirring is ultrasonically treated, supersonic frequency is 50 KHz, power 1KW, ultrasonic time 90min, is surpassed
Sound mode closes 3s, temperature is 25 DEG C, that is, obtains graphene dispersing solution to open 3s.The graphene dispersing solution of preparation is in three months
Agglomeration and sediment does not occur.
Embodiment two, 4 parts of graphene is chosen, dispersant is dimethyl carbonate（DMC）, selection amount is 1 part, and solvent chooses second
Ether.First by a small amount of dispersant dimethyl carbonate（DMC）It is well mixed with graphene, using ball mill grinding, first using dry method
Grinding, rotating speed 30r/min, milling time 30min, add dispersant and carry out wet grinding, rotating speed 80r/min, grind
It is 25 DEG C to consume time as 60min, temperature, obtains the suspension of graphene and dispersant, then above-mentioned suspension is added into ether
It is 2T in magnetic field intensity, mixing time 20min, agitating mode is one minute clockwise, one minute counterclockwise, will in solvent
Solution after stirring is ultrasonically treated, and supersonic frequency is 20 KHz, power 3KW, ultrasonic time 30min, and ultrasonic power is to open
3s, 3s is closed, temperature is 25 DEG C, that is, obtains graphene dispersing solution.The graphene dispersing solution of preparation was not reunited in three months
Phenomenon and sediment.
Embodiment three：
Choose 3 parts of graphene, dispersant N, N, N ', N '-tetramethylethylenediamine（TEMED）, selection amount is 1 part, and solvent is chosen
Absolute ethyl alcohol.First by a small amount of dispersant N, N, N ', N '-tetramethylethylenediamine（TEMED）It is well mixed with graphene, utilizes ball
Grinding machine is ground, and first using dry grinding, rotating speed 20r/min, milling time 30min, is added dispersant progress wet method and is ground
Mill, rotating speed 50r/min, milling time 60min, temperature are 25 DEG C, obtain the suspension of graphene and dispersant, then will be upper
State suspension to be added in anhydrous ethanol solvent, be 1T in magnetic field intensity, mixing time 20min, agitating mode is clockwise
One minute, one minute counterclockwise, the solution after stirring is ultrasonically treated, supersonic frequency is 70 KHz, power 3KW, when ultrasonic
Between be 60min, ultrasonic power closes 3s, temperature is 25 DEG C, that is, obtains graphene dispersing solution to open 3s.The graphene dispersion of preparation
Agglomeration and sediment did not occurred in three months for liquid.
Example IV：
Choose 5 parts of graphene, dispersant N, N, N ', N '-tetramethylethylenediamine（TEMED）, selection amount is 2 parts, and solvent is chosen
Acetone.First by a small amount of dispersant N, N, N ', N '-tetramethylethylenediamine（TEMED）It is well mixed with graphene, utilizes ball mill
Grinding, first using dry grinding, rotating speed 30r/min, milling time 30min, add dispersant and carry out wet grinding, turn
Speed is 80r/min, and milling time 60min, temperature is 25 DEG C, obtains the suspension of graphene and dispersant, then will be above-mentioned outstanding
Turbid is added in acetone solvent, is 5T in magnetic field intensity, mixing time 20min, agitating mode is one minute clockwise, inverse
Hour hands one minute, the solution after stirring being ultrasonically treated, supersonic frequency is 20 KHz, power 1KW, ultrasonic time 60min,
Ultrasonic power closes 3s, temperature is 25 DEG C, that is, obtains graphene dispersing solution to open 3s.The graphene dispersing solution of preparation was at three months
Agglomeration and sediment do not occur inside.
Embodiment five：
8 parts of graphene is chosen, dispersant is methyl formate（MF）, selection amount is 3 parts, and solvent chooses ether.It will divide on a small quantity first
Powder methyl formate（MF）It is well mixed with graphene, using ball mill grinding, first using dry grinding, rotating speed 20r/min,
Milling time is 30min, adds dispersant and carries out wet grinding, rotating speed 50r/min, milling time 60min, temperature is
25 DEG C, the suspension of graphene and dispersant is obtained, then above-mentioned suspension is added in ether solvent, is in magnetic field intensity
5T, mixing time 20min, agitating mode be one minute clockwise, one minute counterclockwise, by after stirring solution ultrasound at
Reason, supersonic frequency are 50 KHz, power 3KW, ultrasonic time 60min, and for ultrasonic power to open 3s, pass 3s, temperature is 25 DEG C,
Obtain graphene dispersing solution.Agglomeration and sediment did not occurred in three months for the graphene dispersing solution of preparation.
Embodiment six：
10 parts of graphene is chosen, dispersant is methyl formate（MF）, selection amount is 4 parts, and solvent chooses acetone.It will divide on a small quantity first
Powder methyl formate（MF）It is well mixed with graphene, using ball mill grinding, first using dry grinding, rotating speed 30r/min,
Milling time is 30min, adds dispersant and carries out wet grinding, rotating speed 80r/min, milling time 60min, temperature is
25 DEG C, the suspension of graphene and dispersant is obtained, then above-mentioned suspension is added in acetone solvent, is in magnetic field intensity
5T, mixing time 20min, agitating mode be one minute clockwise, one minute counterclockwise, by after stirring solution ultrasound at
Reason, supersonic frequency are 90 KHz, power 3KW, ultrasonic time 60min, and for ultrasonic power to open 3s, pass 3s, temperature is 25 DEG C,
Obtain graphene dispersing solution.Agglomeration and sediment did not occurred in three months for the graphene dispersing solution of preparation.
Embodiment seven：
8 parts of graphene is chosen, dispersant is acetonitrile, and selection amount is 3 parts, and solvent chooses absolute ethyl alcohol.First by a small amount of dispersant
Acetonitrile and graphene are well mixed, and using ball mill grinding, are using dry grinding, rotating speed 20r/min, milling time first
30min, add dispersant and carry out wet grinding, rotating speed 50r/min, milling time 60min, temperature is 25 DEG C, is obtained
The suspension of graphene and dispersant, then above-mentioned suspension is added in anhydrous ethanol solvent, it is 3T in magnetic field intensity, stirring
Time is 20min, and agitating mode is one minute clockwise, one minute counterclockwise, the solution after stirring is ultrasonically treated, supersonic frequency
Rate is 50 KHz, power 3KW, ultrasonic time 90min, and ultrasonic power closes 3s, temperature is 25 DEG C, that is, obtains stone to open 3s
Black alkene dispersion liquid.Agglomeration and sediment did not occurred in three months for the graphene dispersing solution of preparation.
Embodiment eight：
5 parts of graphene is chosen, dispersant is acetonitrile, and selection amount is 2 parts, and solvent chooses acetone.First by a small amount of dispersant acetonitrile
It is well mixed with graphene, using ball mill grinding, first using dry grinding, rotating speed 30r/min, milling time 30min,
Add dispersant and carry out wet grinding, rotating speed 80r/min, milling time 60min, temperature is 25 DEG C, obtains graphene
With the suspension of dispersant, then above-mentioned suspension is added in acetone solvent, is 2T in magnetic field intensity, mixing time is
20min, agitating mode are one minute clockwise, one minute counterclockwise, the solution after stirring are ultrasonically treated, supersonic frequency 30
KHz, power 5KW, ultrasonic time 60min, ultrasonic power close 3s, temperature is 25 DEG C, that is, obtains graphene dispersion to open 3s
Liquid.Agglomeration and sediment did not occurred in three months for the graphene dispersing solution of preparation.
Claims (8)
1. a kind of graphene dispersing solution and preparation method thereof, its feature forms in every 100 parts of components by following number：Graphene
1-10 parts, dispersant 0.5-5 parts, remaining is solvent；
Its preparation method comprises the following steps：1）Graphene is taken, graphene is prepared into powder；2）By graphene powder with disperseing
Agent is mixed to get mixture；3）Mixed mixture is put into ball mill, combined using dry grinding and wet grinding
Mode, mixture is ground；4）Mixture after grinding is put into solvent, under conditions of magnetic field, ultrasonic wave, stirring
Uniformly mixed；5）Graphene dispersing solution is obtained after mixing.
A kind of 2. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：The dispersant is selected
Dimethyl carbonate（DMC）, N, N, N ', the one or more in N '-tetramethylethylenediamine, methyl formate or acetonitrile.
A kind of 3. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：The solvent selects nothing
One or more in water-ethanol, ether or acetone.
A kind of 4. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：Made in the step 1
Standby graphene powder can use mechanical stripping method, epitaxy method, heating SiC methods, chemical reduction method, chemical cleavage method or
Any of CVD.
A kind of 5. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：Mixed in the step 3
Graphene particles diameter after compound grinding is less than 250nm.
A kind of 6. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：Magnetic in the step 4
Field intensity 0.5-5T.
A kind of 7. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：Stirred in the step 4
Mode is mixed as one minute clockwise, one minute counterclockwise, mixing speed 50-100r/min, mixing time 0.5-2h.
A kind of 8. graphene dispersing solution as claimed in claim 1 and preparation method thereof, it is characterised in that：Surpass in the step 4
The control mode of sound wave is opens three seconds, Guan Sanmiao, and the frequency of ultrasonic wave is 20-90KHz, and the power of ultrasonic wave is 1-5KW, ultrasound
Ripple temperature is 25 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516542A (en) * | 2018-06-27 | 2018-09-11 | 叶荣森 | A kind of preparation method of high fluorinated volume nanometer fluorinated graphene |
| CN108675289A (en) * | 2018-08-23 | 2018-10-19 | 中原工学院 | A kind of preparation method of graphene dispersing solution |
| CN113214606A (en) * | 2020-01-21 | 2021-08-06 | 常州第六元素材料科技股份有限公司 | Graphene-epoxy resin composite material and preparation method thereof |
| CN113429808A (en) * | 2021-06-28 | 2021-09-24 | 成都新柯力化工科技有限公司 | Isolation dispersant for preventing graphene agglomeration, preparation method and application method |
| CN113563595A (en) * | 2021-07-14 | 2021-10-29 | 南方电网科学研究院有限责任公司 | Bentonite grafting agent and preparation method and application thereof |
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| CN104857869A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | Graphene dispersion liquid and preparation method thereof |
| CN106430170A (en) * | 2016-10-18 | 2017-02-22 | 长沙理工大学 | Preparation method of graphene dispersion solution |
| CN107934949A (en) * | 2016-10-12 | 2018-04-20 | 上海大学 | A kind of preparation method of graphene dispersing solution for infused ceramic based composites |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104857869A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | Graphene dispersion liquid and preparation method thereof |
| CN107934949A (en) * | 2016-10-12 | 2018-04-20 | 上海大学 | A kind of preparation method of graphene dispersing solution for infused ceramic based composites |
| CN106430170A (en) * | 2016-10-18 | 2017-02-22 | 长沙理工大学 | Preparation method of graphene dispersion solution |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516542A (en) * | 2018-06-27 | 2018-09-11 | 叶荣森 | A kind of preparation method of high fluorinated volume nanometer fluorinated graphene |
| CN108675289A (en) * | 2018-08-23 | 2018-10-19 | 中原工学院 | A kind of preparation method of graphene dispersing solution |
| CN113214606A (en) * | 2020-01-21 | 2021-08-06 | 常州第六元素材料科技股份有限公司 | Graphene-epoxy resin composite material and preparation method thereof |
| CN113429808A (en) * | 2021-06-28 | 2021-09-24 | 成都新柯力化工科技有限公司 | Isolation dispersant for preventing graphene agglomeration, preparation method and application method |
| CN113563595A (en) * | 2021-07-14 | 2021-10-29 | 南方电网科学研究院有限责任公司 | Bentonite grafting agent and preparation method and application thereof |
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Effective date of registration: 20180709 Address after: 200241 room 4179, Wu Lou, 555 Dongchuan Road, Minhang District, Shanghai. Applicant after: New Mstar Technology Ltd (Shanghai) Address before: No. 9, No. 118, Xiudian Road, Pudong New Area, Shanghai Applicant before: Tian Wanhong Applicant before: Wang Libin |
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Application publication date: 20171208 |