CN108424618A - graphene/epoxy resin composite material and preparation method thereof - Google Patents
graphene/epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN108424618A CN108424618A CN201810225103.6A CN201810225103A CN108424618A CN 108424618 A CN108424618 A CN 108424618A CN 201810225103 A CN201810225103 A CN 201810225103A CN 108424618 A CN108424618 A CN 108424618A
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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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- Engineering & Computer Science (AREA)
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- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses graphene/epoxy resin composite materials, include the component of following parts by weight：300 parts of bisphenol A-type liquid epoxy resins, 0.3 43.5 parts of graphene microchips, 0.96 200.7 parts of bisphenol-As, 0.2 0.3 parts of catalyst, wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 171 244, and catalyst is triphenylphosphine and its derivative, the molecular weight ranges of graphene/epoxy resin composite material obtained are 345 20000, and graphene content is 0.1 8%.Preparation method is that graphene is scattered in advance in bisphenol A-type liquid epoxy resin, the graphene/bisphenol A-type liquid epoxy resin carries out polymerisation with bisphenol-A under the action of catalyst, the chemical energy generated using the polymerisation and the unlatching vacuum at 130 DEG C, redisperse and stripping are carried out to graphene under condition of negative pressure, to be made be uniformly dispersed, graphene/epoxy resin composite material that performance is splendid.
Description
Technical field
The present invention relates to epoxy resin composite material preparing technical field, specifically a kind of graphene/epoxy resin is compound
Material and preparation method thereof.
Background technology
Graphene is a kind of New Two Dimensional plane composite material, and it is abundant and new that special monoatomic layer determines that it has
Strange physical property.Studies have shown that graphene has excellent electrical properties, mechanical property and machinability.Its unique two
Structure and many excellent properties are tieed up, EP is being improved（Epoxy resin）Hot property, electromagnetic performance and mechanical property etc. have
Huge application potential.
It is easy between graphene due to dimensional effect but during preparing graphene/epoxy resin composite material
Agglomeration occurs, and the larger graphene dispersion that also easily leads to of epoxy resin-base viscosity is uneven, to a certain degree
On limit performance and the application of graphene/EP composite materials.
Invention content
To solve the above problems, a kind of graphene/epoxy resin composite material of present invention offer and preparation method thereof, graphite
Alkene disperses evenly in the base, and performance is more excellent.
The technical solution adopted by the present invention is：Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
0.3-43.5 parts of graphene microchip；
0.96-200.7 parts of bisphenol-A；
0.2-0.3 parts of catalyst；
Wherein, the catalyst is triphenylphosphine and its derivative, the molecular weight of graphene/epoxy resin composite material obtained
Range is 345-20000, and graphene content is 0.1-8%.
The epoxide equivalent of the bisphenol A-type liquid epoxy resin is 171-244.
Preferably, graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
0.32 part of graphene microchip；
1.0 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 171, and catalyst is triphenylphosphine and its derivative, is made
Graphene/epoxy resin composite material molecular weight 345, graphene content is 0.1%.
Preferably, graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
30 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184, and catalyst is triphenylphosphine and its derivative, is made
Graphene/epoxy resin composite material molecular weight 910, graphene content is 7%.
Preferably, graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
32 parts of graphene microchip；
151.2 parts of bisphenol-A；
0.25 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184, and catalyst is triphenylphosphine and its derivative, is made
The molecular weight of graphene/epoxy resin composite material be 3000, graphene content is 6.60%.
The preparation method of above-mentioned graphene/epoxy resin composite material, includes the following steps：
（1）In a kettle, the low molecular weight bisphenol A-type liquid epoxy resin of formula ratio is added, opens blender stirring, opens
Steam is warming up to 40 DEG C；
（2）The graphene microchip that formula ratio is put under 20-30 r/min stirring at low speed, finishes and is warming up to 80 DEG C, in this temperature
Lower height-regulating rotating speed quickly stirs 40min to 150 r/min；
（3）Speed of agitator is adjusted to 20-30 r/min, the bisphenol-A of formula ratio is added, the stirring fusing 30min at 80 DEG C, then add
Enter the catalyst of formula ratio, rotating speed is slowly turned up to 150 r/min, and be warming up to 120 DEG C, at this time steam off, it is allowed to rely on
Reaction heat voluntarily heats up；
（4）Vacuum pump is opened when temperature reaches 130 DEG C, so that vacuum degree is gradually raised to -0.095MP or more from 0, and keep temperature
60min is reacted between 130-200 DEG C, is closed vacuum pump, is filled with high-purity nitrogen, blowing sabot is cooled to room temperature to get stone
Black alkene/epoxy resin composite material.Vacuum is just opened since 130 DEG C carries out negative reaction, the graphene/epoxy produced in this way
Resin composite materials range of molecular weight distributions is narrower, and graphene disperses evenly in the composite, and dissolution filter removes graphite
Color of resin is also more shallow after alkene, and the graphene/epoxy resin composite material for the various contents produced is in various anticorrosive paints, powder
Dosage can reduce 10% or more in last coating, fireproof coating, conductive coating and casting glue, adhesive, and economic benefit significantly improves,
The performance shown is also better.
The beneficial effects of the invention are as follows：1, the stone that molecular weight ranges are 345-20000 can be made in method using the present invention
Black alkene/epoxy resin composite material.2, in preparation process, vacuum is just opened since 130 DEG C and carries out negative reaction, is produced in this way
Graphene/epoxy resin composite material range of molecular weight distributions it is narrower, graphene disperse in the composite evenly, dissolving
Color of resin is also more shallow after being filtered to remove graphene, and the graphene/epoxy resin composite material for the various contents produced is each
Dosage can reduce 10% or more in kind anticorrosive paint, powdery paints, fireproof coating, conductive coating and casting glue, adhesive, economy
Benefit significantly improves, and the performance shown is also better.
Specific implementation mode
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment
It is only used for explaining the present invention, be not intended to limit the scope of the present invention..
Embodiment 1
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
0.32 part of graphene microchip；
1.0 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 171.
The preparation method of above-mentioned graphene/epoxy resin composite material, includes the following steps：
（1）In a kettle, the bisphenol A-type liquid epoxy resin of 300 parts by weight is added, opens blender stirring, opens steam
It is warming up to 40 DEG C；
（2）The graphene microchip that 0.32 parts by weight are put under 20-30 r/min stirring at low speed, finishes and is warming up to 80 DEG C, herein
At a temperature of quickly stir 40min；
（3）Speed of agitator is adjusted to 20-30 r/min, the bisphenol-A of 1.0 parts by weight is added, the stirring fusing 30min at 80 DEG C,
The catalyst of 0.2 parts by weight is added, rotating speed is slowly turned up to 150 r/min, and be warming up to 120 DEG C, steam off, allows at this time
It voluntarily heats up by reaction heat；
（4）Vacuum pump is opened when temperature reaches 130 DEG C, so that negative pressure is gradually raised to 0.095MP or more from 0, and maintain the temperature at
60min is reacted between 130-200 DEG C, is closed vacuum pump, is filled with high-purity nitrogen, blowing obtains graphene epoxy resin composite wood
Material.Technical indicator：Graphene content 0.1% in graphene/epoxy resin, molecular weight 345, Electronic Speculum experiments have shown that, graphene dispersion
Uniformly.
Embodiment 2
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
30 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184.
Preparation process is the same as embodiment 1, technical indicator：Graphene content 7.0% in graphene/epoxy resin, molecular weight 910,
Electronic Speculum experiments have shown that, graphene dispersion is uniform.
Embodiment 3
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
30 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184.
The preparation process place different from embodiment 1 is that vacuum is opened since 160 DEG C carries out negative reaction.Technology refers to
Mark：Graphene content 7.0% in graphene/epoxy resin, molecular weight 940, Electronic Speculum contrast test show that graphene dispersion is uniform
For degree not as good as embodiment 2, the molecular weight of epoxy resin distribution tested with GPC method is obviously wider than embodiment 2.
Embodiment 4
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
32 parts of graphene microchip；
151.2 parts of bisphenol-A；
0.25 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184.
Preparation process is the same as embodiment 1, technical indicator：Graphene content 6.60%, molecular weight in graphene/epoxy resin
3000, Electronic Speculum experiments have shown that, graphene dispersion is uniform.
Embodiment 5
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
60 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184.
Preparation process is the same as embodiment 1, technical indicator：Graphene content 13.09%, molecular weight in graphene/epoxy resin
912, Electronic Speculum experiments have shown that, graphene is accumulated, dispersion it is uneven.
Embodiment 6
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
20 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 190.
The place that preparation process is different from embodiment 1 is：It does not open vacuum from 130 DEG C and carries out negative pressure dispersion stripping, skill
Art index：Graphene content 4.78% in graphene/epoxy resin, molecular weight 1000, Electronic Speculum experiments have shown that, graphene dispersion is not
Uniformly, there is accumulation agglomeration in part.
Embodiment 7
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
22 parts of graphene microchip；
58.5 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 260.
Preparation process is the same as embodiment 1, technical indicator：Graphene content 5.76%, molecular weight in graphene/epoxy resin
1120, Electronic Speculum experiments have shown that, graphene has slight agglomeration.
Embodiment 8
Graphene/epoxy resin composite material includes the component of following parts by weight：
300 parts of bisphenol A-type solid epoxy resin；
12 parts of graphene microchip；
10 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type solid epoxy resin is 500.
The preparation method of above-mentioned graphene/epoxy resin composite material, includes the following steps：
（1）In a kettle, the solid epoxy resin of 300 parts by weight is added, opens steam and is warming up to 40 DEG C and do not melt, after of continuing rising
Temperature starts to melt to 95 DEG C；
（2）Graphene is put under 20-30 r/min stirring at low speed, it is found that a large amount of graphenes overflow outside kettle, can not operate, test
Failure.
In order to which the graphene/EP composite materials for being uniformly dispersed, haveing excellent performance are made, people explore as in-situ inserted poly-
A variety of preparation methods of legal, solution intercalation method and melt intercalated method etc., but the present invention is different from above-mentioned preparation method, is by work(
The graphene of energyization is scattered in advance in the bisphenol A-type liquid epoxy resin of low molecular weight, under the action of catalyst the graphite
Alkene/bisphenol A-type liquid epoxy resin carries out polymerisation with bisphenol-A, and the chemical energy generated using the polymerisation is simultaneously being born
Redisperse and stripping are carried out to graphene under the conditions of pressure, (i.e. under condition of negative pressure, to graphene while polymerisation carries out
Carry out redisperse stripping）To be made be uniformly dispersed, various graphene/epoxy resin composite materials that performance is splendid.Wherein stone
Black alkene content is up to 2%, graphene/epoxy resin composite material of epoxide equivalent 800, the powder for 20% Zn content being used to prepare
Last coating, salt-fog resistant time ＞ 2000h or more.It is characterized by SEM etc., the result shows that, graphene is completely exfoliated, and
It is uniformly dispersed in the base, and the two interface compatibility is good, improves the thermal stability of composite material.The vitrifying of EB simultaneously
The thermal stability of temperature is improved.
Claims (6)
1. graphene/epoxy resin composite material, which is characterized in that include the component of following parts by weight：
300 parts of bisphenol A-type liquid epoxy resin；
0.3-43.5 parts of graphene microchip；
0.96-200.7 parts of bisphenol-A；
0.2-0.3 parts of catalyst；
Wherein, the catalyst is triphenylphosphine and its derivative, the molecular weight of graphene/epoxy resin composite material obtained
Range is 345-20000, and graphene content is 0.1-8%.
2. graphene/epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：The epoxide equivalent of the bisphenol A-type liquid epoxy resin is 171-244.
3. graphene/epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：
300 parts of bisphenol A-type liquid epoxy resin；
0.32 part of graphene microchip；
1.0 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 171, and catalyst is triphenylphosphine and its derivative, is made
The molecular weight of graphene/epoxy resin composite material be 345, graphene content is 0.1%.
4. graphene/epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：
300 parts of bisphenol A-type liquid epoxy resin；
30 parts of graphene microchip；
98 parts of bisphenol-A；
0.2 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184, and catalyst is triphenylphosphine and its derivative, is made
The molecular weight of graphene/epoxy resin composite material be 910, graphene content is 7%.
5. graphene/epoxy resin composite material according to claim 1, which is characterized in that including following parts by weight
Component：
300 parts of bisphenol A-type liquid epoxy resin；
32 parts of graphene microchip；
151.2 parts of bisphenol-A；
0.25 part of catalyst；
Wherein, the epoxide equivalent of bisphenol A-type liquid epoxy resin is 184, and catalyst is triphenylphosphine and its derivative, is made
The molecular weight of graphene/epoxy resin composite material be 3000, graphene content is 6.60%.
6. a kind of preparation method of graphene/epoxy resin composite material as described in claim 1, which is characterized in that including
Following steps：
（1）In a kettle, the low molecular weight bisphenol A-type liquid epoxy resin of formula ratio is added, opens blender stirring, opens
Steam is warming up to 40 DEG C；
（2）The graphene microchip that formula ratio is put under 20-30 r/min stirring at low speed, finishes and is warming up to 80 DEG C, in this temperature
Lower height-regulating rotating speed quickly stirs 40min to 150 r/min；
（3）Speed of agitator is adjusted to 20-30 r/min, the bisphenol-A of formula ratio is added, the stirring fusing 30min at 80 DEG C, then add
Enter the catalyst of formula ratio, rotating speed is slowly turned up to 150 r/min, and be warming up to 120 DEG C, at this time steam off, it is allowed to rely on
Reaction heat voluntarily heats up；
（4）Vacuum pump is opened when temperature reaches 130 DEG C, so that vacuum degree is gradually raised to -0.095MP or more from 0, and keep temperature
60min is reacted between 130-200 DEG C, is closed vacuum pump, is filled with high-purity nitrogen, blowing sabot is cooled to room temperature to get stone
Black alkene/epoxy resin composite material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110204868A (en) * | 2019-07-01 | 2019-09-06 | 常州第六元素材料科技股份有限公司 | A kind of graphene graft modification epoxy resin and preparation method thereof |
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| US20170100902A1 (en) * | 2014-05-07 | 2017-04-13 | Wichita State University | Nanocomposite microcapsules for self-healing of composite articles |
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| US20140299475A1 (en) * | 2011-10-27 | 2014-10-09 | Garmor, Inc. | Composite graphene structures |
| CN102516512A (en) * | 2011-11-23 | 2012-06-27 | 安徽神剑新材料股份有限公司 | Preparation method of 70/30 high-Tg mixed type polyester resin |
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| CN110204868A (en) * | 2019-07-01 | 2019-09-06 | 常州第六元素材料科技股份有限公司 | A kind of graphene graft modification epoxy resin and preparation method thereof |
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