CN109021286A - A kind of dispersion and dispersing method of graphene - Google Patents
A kind of dispersion and dispersing method of graphene Download PDFInfo
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- CN109021286A CN109021286A CN201810898875.6A CN201810898875A CN109021286A CN 109021286 A CN109021286 A CN 109021286A CN 201810898875 A CN201810898875 A CN 201810898875A CN 109021286 A CN109021286 A CN 109021286A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of dispersion of graphene and dispersing method, the dispersion of graphene includes: 0.1 ~ 0.5 part of graphene；1 ~ 3 part, 1 ~ 5 part of polyvinyl alcohol, 90 ~ 120 parts of alcohol diluent, 30 ~ 50 parts of ethers diluent of -4 methylcoumarin of 7- hydroxyl.The embodiment of the present invention obtains graphene dispersion system and improves the dispersibility of graphene in organic solvent, also improves the dispersibility of graphene in the epoxy, improves the compatibility of graphene in the epoxy.
Description
Technical field
The present invention relates to the dispersions of graphene, more particularly it relates to a kind of dispersion of graphene and dispersion
Method.
Background technique
Graphene have good electric conductivity, mechanical performance and physical and chemical performance and be widely used in electronics industry,
The fields such as composite material, sensor device.As a kind of inorganic filler, graphene, which is added in epoxy resin, to be significantly improved
The mechanical property of epoxy resin, and opposite conventional inorganic fillers, graphene dosage is less, and modified effect is more preferable.However, at present
The poor dispersion of graphene in the epoxy, agglomeration is more apparent, and the performance of composite material needs to be further increased.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of dispersion of graphene and dispersing methods.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The embodiment of the invention provides a kind of dispersions of graphene, according to parts by weight, the dispersion of the graphene
It include: 0.1 ~ 0.5 part of graphene；1 ~ 3 part of -4 methylcoumarin of 7- hydroxyl, 1 ~ 5 part of polyvinyl alcohol, alcohol diluent 90 ~ 120
Part, 30 ~ 50 parts of ethers diluent.
In above scheme, the alcohol diluent selection: in methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol or benzyl alcohol
It is at least one.
In above scheme, the ethers diluent is glycidol ether.
In above scheme, the graphene selects times of non-oxidized graphite alkene, redox graphene, graphene oxide
It is a kind of.
The embodiment of the invention also provides the methods of its dispersion for preparing above-mentioned graphene, and the method includes steps
It is rapid:
S10, graphene is added in the alcohol diluent of part, ultrasonic agitation uniformly, obtains graphene dispersing solution；
S20, remaining the alcohol diluent and the ethers diluent are mixed evenly, the 7- hydroxyl is then added
- 4 methylcoumarin of base and the polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, the graphene dispersing solution is instilled into the diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
30min or more.
In above scheme, the part alcohol diluent accounts for the 1/3 ~ 1/2 of whole alcohol diluents in step S10.
In above scheme, in step S20, ultrasonic agitation temperature is 30 ~ 60 DEG C, in step S30, the temperature stirred in drop
No more than 40 DEG C.
The embodiment of the invention provides a kind of dispersion of graphene and dispersing methods, improve graphene organic molten
Dispersibility in agent also improves the dispersibility of graphene in the epoxy, improves the phase of graphene in the epoxy
Capacitive, the epoxy resin composite material mechanical property for being added to graphene dispersion system improve a lot.
Specific embodiment
The invention will be further described combined with specific embodiments below.Following embodiment is only used for clearly illustrating
Technical solution of the present invention, and not intended to limit the protection scope of the present invention.
First aspect present invention embodiment provides a kind of dispersion of graphene, according to parts by weight, the graphite
The dispersion of alkene includes: 0.1 ~ 0.5 part of graphene；1 ~ 3 part of -4 methylcoumarin of 7- hydroxyl, 1 ~ 5 part of polyvinyl alcohol, alcohols is dilute
Release 90 ~ 120 parts of agent, 30 ~ 50 parts of ethers diluent.
In an optional implementation of the invention, alcohol diluent selection: methanol, ethyl alcohol, propyl alcohol, butanol, second two
At least one of alcohol or benzyl alcohol.
In an optional implementation of the invention, ethers diluent is glycidol ether.Preferably, ethers diluent
Including but not limited to butyl glycidyl ether, neopentylglycol diglycidyl ether, phenyl glycidyl ether, ethylene glycol two shrink sweet
Oily ether etc..
In an optional implementation of the invention, graphene select non-oxidized graphite alkene, redox graphene,
Graphene oxide it is any.
The method that second aspect of the present invention embodiment additionally provided prepare the dispersion of above-mentioned graphene, the method
Comprising steps of
S10, graphene is added in the alcohol diluent of part, ultrasonic agitation uniformly, obtains graphene dispersing solution；
S20, remaining the alcohol diluent and the ethers diluent are mixed evenly, the 7- hydroxyl is then added
- 4 methylcoumarin of base and the polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, the graphene dispersing solution is instilled into the diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
30min or more.
In an optional implementation of the invention, it is dilute to account for whole alcohols for the part alcohol diluent in step S10
Release the 1/3 ~ 1/2 of agent.
In another optional implementation of the invention, in step S20, ultrasonic agitation temperature is 30 ~ 60 DEG C, step
In S30, the temperature stirred in drop is no more than 40 DEG C.
The present invention will be further described combined with specific embodiments below, it is to be understood that the present invention is not limited to
Lower embodiment.
Embodiment one
Prepare the dispersion of graphene:
S10,0.1g graphene oxide is added in 30g ethyl alcohol, ultrasonic agitation uniformly, obtains graphene dispersing solution；The part alcohol
Class diluent accounts for the 1/3 ~ 1/2 of whole alcohol diluents.
S20,60g ethyl alcohol and 30f butyl glycidyl ether are mixed evenly, it is fragrant that -4 methyl of 1g7- hydroxyl is then added
Legumin and 1g polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, above-mentioned graphene dispersing solution is instilled into diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
35min obtains the dispersion of graphene.
Prepare graphene-epoxy resin composite material:
The dispersion of above-mentioned graphene is mixed with the epoxy resin of 35g, then epoxy resin is added in mechanical stirring 15min
Curing agent obtains graphene-epoxy resin composite material after solidification.
Performance test:
1, graphene dispersion system obtains stability: at -2 ~ 120 DEG C, graphene resulting dispersion system 60 days nothings of uniform and stable preservation
Agglomeration；
2, graphene-epoxy resin composite material obtains stability: through scanning electron microscopic observation, graphene-ring manufactured in the present embodiment
Graphene dispersion is uniform in epoxy resin composite material, and the tensile property ratio of graphene-epoxy resin composite material is not added with graphite
The epoxide resin material of alkene improves 90%.
Embodiment two
Prepare the dispersion of graphene:
S10,0.2g graphene oxide is added in 40g methanol, ultrasonic agitation uniformly, obtains graphene dispersing solution；
S20,50g alcohol diluent and 35g phenyl glycidyl ether are mixed evenly, -4 first of 1.5g7- hydroxyl is then added
Butylcoumariii and 1g polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, the graphene dispersing solution is instilled into the diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
40min。
Prepare graphene-epoxy resin composite material:
The dispersion of above-mentioned graphene is mixed with the epoxy resin of 60g, then epoxy resin is added in mechanical stirring 30min
Curing agent obtains graphene-epoxy resin composite material after solidification.
Performance test:
1, graphene dispersion system obtains stability: at -2 ~ 120 DEG C, graphene resulting dispersion system 60 days nothings of uniform and stable preservation
Agglomeration；
2, graphene-epoxy resin composite material obtains stability: through scanning electron microscopic observation, graphene-ring manufactured in the present embodiment
Graphene dispersion is uniform in epoxy resin composite material, and the tensile property ratio of graphene-epoxy resin composite material is not added with graphite
The epoxide resin material of alkene improves 110%.
Embodiment three
Prepare the dispersion of graphene:
S10,0.45g graphene is added in 50g ethyl alcohol, ultrasonic agitation uniformly, obtains graphene dispersing solution；
S20,50g ethyl alcohol and 50g butyl glycidyl ether are mixed evenly, -4 methylcoumarin of 2.5g7- hydroxyl is then added
Element and 3.5g polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, the graphene dispersing solution is instilled into the diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
45min。
Prepare graphene-epoxy resin composite material:
The dispersion of above-mentioned graphene is mixed with the epoxy resin of 60g, then epoxy resin is added in mechanical stirring 25min
Curing agent obtains graphene-epoxy resin composite material after solidification.
Performance test:
1, graphene dispersion system obtains stability: at -2 ~ 120 DEG C, graphene resulting dispersion system 60 days nothings of uniform and stable preservation
Agglomeration；
2, graphene-epoxy resin composite material obtains stability: through scanning electron microscopic observation, graphene-ring manufactured in the present embodiment
Graphene dispersion is uniform in epoxy resin composite material, and the tensile property ratio of graphene-epoxy resin composite material is not added with graphite
The epoxide resin material of alkene improves 102%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of dispersion of graphene, which is characterized in that according to parts by weight, the dispersion of the graphene includes:
0.1 ~ 0.5 part of graphene；1 ~ 3 part of -4 methylcoumarin of 7- hydroxyl, 1 ~ 5 part of polyvinyl alcohol, 90 ~ 120 parts of alcohol diluent, ethers
30 ~ 50 parts of diluent.
2. the dispersion of graphene according to claim 1, which is characterized in that the alcohol diluent selection: methanol,
At least one of ethyl alcohol, propyl alcohol, butanol, ethylene glycol or benzyl alcohol.
3. the dispersion of graphene according to claim 1, which is characterized in that the ethers diluent is glycidol
Ether.
4. the dispersion of graphene according to claim 1, which is characterized in that the graphene selects non-oxygen fossil
Black alkene, redox graphene, graphene oxide it is any.
5. a kind of method for preparing any one of Claims 1-4 graphene dispersion system, which is characterized in that the method
Comprising steps of
S10, graphene is added in the alcohol diluent of part, ultrasonic agitation uniformly, obtains graphene dispersing solution；
S20, remaining the alcohol diluent and the ethers diluent are mixed evenly, the 7- hydroxyl is then added
- 4 methylcoumarin of base and the polyvinyl alcohol, ultrasonic agitation uniformly, obtain diluent mixed liquor；
S30, the graphene dispersing solution is instilled into the diluent mixed liquor, is stirred in drop, after being added dropwise to complete, ultrasonic disperse
30min or more.
6. according to the method described in claim 5, it is characterized in that, the part alcohol diluent accounts for whole alcohol in step S10
The 1/3 ~ 1/2 of class diluent.
7. according to the method described in claim 5, it is characterized in that, ultrasonic agitation temperature is 30 ~ 60 DEG C, step in step S20
In S30, the temperature stirred in drop is no more than 40 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810898875.6A CN109021286A (en) | 2018-08-08 | 2018-08-08 | A kind of dispersion and dispersing method of graphene |
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| CN201810898875.6A CN109021286A (en) | 2018-08-08 | 2018-08-08 | A kind of dispersion and dispersing method of graphene |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104627985A (en) * | 2013-11-07 | 2015-05-20 | 中国科学院上海有机化学研究所 | Graphene capable of being dispersed in organic solvent and water-phase synthesis method thereof |
| CN104772064A (en) * | 2015-03-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Method for preparing grapheme dispersion liquid |
| CN105315476A (en) * | 2015-11-17 | 2016-02-10 | 重庆理工大学 | Method for preparing modified graphene-polyvinyl alcohol composite film |
| KR20170040449A (en) * | 2015-10-02 | 2017-04-13 | 인하대학교 산학협력단 | Gas Barrier Film using graphene which is grafted with PVA and Method for Preparing the Same |
-
2018
- 2018-08-08 CN CN201810898875.6A patent/CN109021286A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104627985A (en) * | 2013-11-07 | 2015-05-20 | 中国科学院上海有机化学研究所 | Graphene capable of being dispersed in organic solvent and water-phase synthesis method thereof |
| CN104772064A (en) * | 2015-03-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Method for preparing grapheme dispersion liquid |
| KR20170040449A (en) * | 2015-10-02 | 2017-04-13 | 인하대학교 산학협력단 | Gas Barrier Film using graphene which is grafted with PVA and Method for Preparing the Same |
| CN105315476A (en) * | 2015-11-17 | 2016-02-10 | 重庆理工大学 | Method for preparing modified graphene-polyvinyl alcohol composite film |
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