CN108623989A - A kind of preparation method of graphene oxide resin carbon fibre composite material - Google Patents
A kind of preparation method of graphene oxide resin carbon fibre composite material Download PDFInfo
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- CN108623989A CN108623989A CN201810403254.6A CN201810403254A CN108623989A CN 108623989 A CN108623989 A CN 108623989A CN 201810403254 A CN201810403254 A CN 201810403254A CN 108623989 A CN108623989 A CN 108623989A
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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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
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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Abstract
A kind of preparation method of graphene oxide resin carbon fibre composite material, applied to preparing heavy-duty automotive speed changer synchronization device cone ring conical surface friction layer FB resin carbon fibre composite materials.Natural graphite prepares graphene oxide using Hummers methods, is modified processing by N dimethylformamides, isocyanates or derivatives thereof, then disperse by ultrasonic wave with acetone soln, obtains finely dispersed modified graphene oxide acetone dispersion liquor;Above-mentioned dispersion liquid and FB resin glues are subjected to configuration and homogenize process, the resin adhesive liquid containing modified graphene is evenly coated in carbon cloth is two-sided, and curing process obtains graphene oxide resin carbon fibre composite material.Carbon fibre composite prepared by the present invention, for interlaminar shear strength more than 55MPa, tensile strength is more than 800MPa at room temperature, and wear-resisting property (frictional testing machine) is less than 0.025g/cm2.The invention production process route is concise, graphene resin carbon fibre composite property is reliable and stable, is suitable for mass production.
Description
Technical field
The present invention relates to a kind of preparation method of carbon fibre composite, more particularly to a kind of graphene oxide resin carbon fiber
Tie up the preparation method of composite material.
Background technology
In heavy-duty automotive speed changer synchronizer mechanisms, the synchronization device cone ring for being bonded resin carbon fibre is that wherein core is closed
Key part, resin carbon fibre layer is that FB resin glues infiltrate the composite material being formed by curing with carbon cloth, worked in synchronizer
Cheng Zhong, resin carbon fibre layer have stable friction performance, friction coefficient height, high temperature resistant, it is wear-resistant, oil-containing heat dissipation, anti-lock, make
The advantages that with long lifespan.Due to raw material and curing process factor, often cause resin glue low with carbon-fiber-reinforced intensity, solid
Change process is easy the defects of forming internal fissure, bubble, and causing synchronization device cone ring, resin carbon fibre layer early stage is de- in use
It falls or wears, directly affect the service life of synchronizer.
Invention content
The graphene oxide resin carbon fibre that simple, performance that present invention aims at a kind of production process routes of offer is stablized
The preparation method of composite material.
In order to achieve the above objectives, the technical solution adopted by the present invention is:
1) preparation of graphene oxide
Graphene oxide is prepared using Hummers methods using natural graphite powder as raw material, then by the graphene oxide of preparation
It is placed in 60 DEG C of vacuum drying chamber fully dry;
2) graphene oxide is modified
Graphene oxide prepared by step 1), which is placed in solvent, enables solvent to flood graphene oxide, stirs 36h, most
It is fully washed by precipitation, filtering, with dichloroethylene, is dried in vacuo, obtains modified graphene oxide;
The solvent is the mixed solution of dinethylformamide and isocyanates or derivatives thereof, wherein N- dimethyl
The mass ratio of formamide and isocyanates or derivatives thereof is 40:1;
3) prepared by acetone dispersion liquor
(0.15-0.25) by weight percentage:1000, it weighs modified graphene oxide and is placed in acetone soln, ultrasonic wave
Disperse 2-4h, obtains finely dispersed modified graphene oxide acetone dispersion liquor;
4) prepared by graphene oxide FB resin matrixes glue
4 are pressed with modified graphene oxide acetone dispersion liquor and FB resin glues:(0.7-1.3) volume ratio configures, and is sufficiently stirred
It is uniform to obtain graphene oxide FB resin matrix glues;
5) prepared by composite material
Graphene oxide FB resin matrixes glue is applied into 600-1000ml by every 300 × 500cm and is evenly coated in carbon cloth
It is two-sided, cure 0.8-1.2 hours at 70 DEG C -80 DEG C, graphene oxide resin carbon fibre composite material is made in natural cooling.
The natural graphite powder of -30 μm of step 1) the natural graphite powder use.
Isocyanates described in the step 2) or derivatives thereof is aliphatic mono-isocyanate, aliphatic diisocyanate
Ester, hexylidene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, polyhexamethylene diisocyanate
Ester, cyclohexane diisocyanate;Aromatic monoisocyanate, aromatic diisocyanate, aromatic poly-isocyanate, diphenyl
Methane diisocyanate, diphenyl methane polymeric isocyanate or toluene di-isocyanate(TDI).
To overcome and reducing the defect generated in resin carbon fibre layer preparation process, it is compound to further increase resin carbon fibre
The comprehensive performance and service life of material.The present invention starts with from FB resin glues, adds the graphite oxide olefinic carbon nanometer haveing excellent performance
Material, can not only reinforced resin carbon fiber interfacial combined function, and solidification process internal fissure and bubble can be overcome etc.
Defect effectively promotes the comprehensive mechanical performance index of the composite material.
The present invention solves the problems, such as that graphene oxide is easy to reunite, and improves the dispersion of graphene oxide in acetone
Property, and the interfacial bond strength of FB resins and carbon fiber is improved using the excellent toughness of graphene oxide and intensity, it improves
The comprehensive mechanical performance of graphene oxide resin carbon fibre composite material:Interlaminar shear strength is more than 55MPa at room temperature, and tension is strong
Degree is more than 800MPa, and wear-resisting property (frictional testing machine) is less than 0.025g/cm2.Graphene oxide resin carbon prepared by the present invention
Fibrous composite frictional layer is bonded in by high temperature and pressure curing process on synchronization device cone ring matrix, in 150 DEG C of operating conditions
Under, service life reaches 130,000 times or more.
Specific implementation mode
Embodiment 1:
1) preparation of graphene oxide
Graphene oxide is prepared using Hummers methods for raw material for (- 30 μm) with natural graphite powder, then by the oxidation of preparation
Graphene is placed in 60 DEG C of vacuum drying chamber fully dry;
2) graphene oxide is modified
Graphene oxide prepared by step 1), which is placed in solvent, enables solvent to flood graphene oxide, stirs 36h, most
It is fully washed by precipitation, filtering, with dichloroethylene, is dried in vacuo, obtains modified graphene oxide;
The solvent is that the mass ratio of dinethylformamide and aromatic monoisocyanate is 40:1;
3) prepared by acetone dispersion liquor
By weight percentage 0.15:1000, it weighs modified graphene oxide and is placed in acetone soln, ultrasonic wave disperses 2h,
Obtain finely dispersed modified graphene oxide acetone dispersion liquor;
4) prepared by graphene oxide FB resin matrixes glue
4 are pressed with modified graphene oxide acetone dispersion liquor and FB resin glues:0.7 volume ratio configures, and stirs
Graphene oxide FB resin matrix glues;
5) prepared by composite material
Graphene oxide FB resin matrixes glue by every 300 × 500cm is applied 600ml, and to be evenly coated in carbon cloth two-sided,
Cure 0.8 hour at 70 DEG C, graphene oxide resin carbon fibre composite material is made in natural cooling.
The result of test evaluation the present embodiment:Interlaminar shear strength is 57MPa, tensile strength 800MPa at room temperature, resistance to
Grind performance (frictional testing machine) 0.025g/cm2.By the graphene oxide resin carbon fibre composite material frictional layer of preparation, pass through
High temperature and pressure curing process is bonded on synchronization device cone ring matrix, and under 150 DEG C of operating conditions, service life reaches 130,000 times.
Embodiment 2:
1) preparation of graphene oxide
Graphene oxide is prepared using Hummers methods for raw material for (- 30 μm) with natural graphite powder, then by the oxidation of preparation
Graphene is placed in 60 DEG C of vacuum drying chamber fully dry;
2) graphene oxide is modified
Graphene oxide prepared by step 1), which is placed in solvent, enables solvent to flood graphene oxide, stirs 36h, most
It is fully washed by precipitation, filtering, with dichloroethylene, is dried in vacuo, obtains modified graphene oxide;
The solvent is that the mass ratio of dinethylformamide and aromatic diisocyanate is 40:1;
3) prepared by acetone dispersion liquor
By weight percentage 0.20:1000, it weighs modified graphene oxide and is placed in acetone soln, ultrasonic wave disperses 3h,
Obtain finely dispersed modified graphene oxide acetone dispersion liquor;
4) prepared by graphene oxide FB resin matrixes glue
4 are pressed with modified graphene oxide acetone dispersion liquor and FB resin glues:1.0 volume ratios configure, and stir
Graphene oxide FB resin matrix glues;
5) prepared by composite material
Graphene oxide FB resin matrixes glue by every 300 × 500cm is applied 800ml, and to be evenly coated in carbon cloth two-sided,
Cure 1 hour at 75 DEG C, graphene oxide resin carbon fibre composite material is made in natural cooling.
The result of test evaluation the present embodiment:Interlaminar shear strength is 59MPa, tensile strength 830MPa at room temperature, resistance to
Grind performance (frictional testing machine) 0.023g/cm2.By the graphene oxide resin carbon fibre composite material frictional layer of preparation, pass through
High temperature and pressure curing process is bonded on synchronization device cone ring matrix, and under 150 DEG C of operating conditions, service life reaches 13.7 ten thousand
It is secondary.
Embodiment 3:
1) preparation of graphene oxide
Graphene oxide is prepared using Hummers methods for raw material for (- 30 μm) with natural graphite powder, then by the oxidation of preparation
Graphene is placed in 60 DEG C of vacuum drying chamber fully dry;
2) graphene oxide is modified
Graphene oxide prepared by step 1), which is placed in solvent, enables solvent to flood graphene oxide, stirs 36h, most
It is fully washed by precipitation, filtering, with dichloroethylene, is dried in vacuo, obtains modified graphene oxide;
The solvent is that the mass ratio of dinethylformamide and aromatic poly-isocyanate is 40:1;
3) prepared by acetone dispersion liquor
By weight percentage 0.25:1000, it weighs modified graphene oxide and is placed in acetone soln, ultrasonic wave disperses 4h,
Obtain finely dispersed modified graphene oxide acetone dispersion liquor;
4) prepared by graphene oxide FB resin matrixes glue
4 are pressed with modified graphene oxide acetone dispersion liquor and FB resin glues:1.3 volume ratios configure, and stir
Graphene oxide FB resin matrix glues;
5) prepared by composite material
Graphene oxide FB resin matrixes glue by every 300 × 500cm is applied 1000ml, and to be evenly coated in carbon cloth two-sided,
Cure 1.2 hours at 80 DEG C, graphene oxide resin carbon fibre composite material is made in natural cooling.
The result of test evaluation the present embodiment:Interlaminar shear strength is 61MPa, tensile strength 890MPa at room temperature, resistance to
Grind performance (frictional testing machine) 0.020g/cm2.By the graphene oxide resin carbon fibre composite material frictional layer of preparation, pass through
High temperature and pressure curing process is bonded on synchronization device cone ring matrix, and under 150 DEG C of operating conditions, service life reaches 13.5 ten thousand
It is secondary.
Claims (3)
1. a kind of preparation method of graphene oxide resin carbon fibre composite material, it is characterised in that:
1) preparation of graphene oxide
Graphene oxide is prepared using Hummers methods using natural graphite powder as raw material, is then placed in the graphene oxide of preparation
It is fully dry in 60 DEG C of vacuum drying chamber;
2) graphene oxide is modified
Graphene oxide prepared by step 1), which is placed in solvent, enables solvent to flood graphene oxide, stirs 36h, most passes through afterwards
Precipitation, filtering are fully washed with dichloroethylene, are dried in vacuo, are obtained modified graphene oxide;
The solvent is the mixed solution of dinethylformamide and isocyanates or derivatives thereof, wherein N- dimethyl formyl
The mass ratio of amine and isocyanates or derivatives thereof is 40:1;
3) prepared by acetone dispersion liquor
(0.15-0.25) by weight percentage:1000, it weighs modified graphene oxide and is placed in acetone soln, ultrasonic wave dispersion
2-4h obtains finely dispersed modified graphene oxide acetone dispersion liquor;
4) prepared by graphene oxide FB resin matrixes glue
With modified graphene oxide acetone dispersion liquor and FB resin glues example 4 by volume:(0.7-1.3) is configured, and is sufficiently stirred
The uniform mixing of 0.5-1h;
5) prepared by composite material
Graphene oxide FB resin matrixes glue by every 300 × 500cm is applied 600-1000ml, and to be evenly coated in carbon cloth two-sided,
Cure 0.8-1.2 hours at 70 DEG C -80 DEG C, graphene oxide resin carbon fibre composite material is made in natural cooling.
2. the preparation method of graphene oxide resin carbon fibre composite material according to claim 1, it is characterised in that:Institute
State the natural graphite powder of -30 μm of step 1) natural graphite powder use.
3. the preparation method of graphene oxide resin carbon fibre composite material according to claim 1, it is characterised in that:Institute
It is aliphatic mono-isocyanate, aliphatic diisocyanate, hexylidene two to state isocyanates described in step 2) or derivatives thereof
Isocyanates, isophorone diisocyanate, hexamethylene diisocyanate, polyhexamethylene diisocyanate, hexamethylene two
Isocyanates;Aromatic monoisocyanate, aromatic diisocyanate, aromatic poly-isocyanate, two isocyanide of diphenyl methane
Acid esters, diphenyl methane polymeric isocyanate or toluene di-isocyanate(TDI).
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Cited By (3)
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CN110524532A (en) * | 2019-08-31 | 2019-12-03 | 三体次元信息科技(宁波)有限公司 | Electron type artificial-muscle electric actuator and preparation method thereof and the application in finger actuation device |
CN110863346A (en) * | 2019-11-26 | 2020-03-06 | 陕西华夏粉末冶金有限责任公司 | Preparation method of carbon-carbon fiber composite material for conical surface friction layer of heavy-duty automobile transmission synchronizer cone ring |
CN115595037A (en) * | 2022-10-13 | 2023-01-13 | 江阴润方机械制造有限公司(Cn) | High-strength stainless steel retainer ring for filling machine and preparation process thereof |
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CN104910333A (en) * | 2015-06-24 | 2015-09-16 | 深圳职业技术学院 | Modified graphene oxide polymer composite material and preparation method thereof |
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CN102795873A (en) * | 2012-07-30 | 2012-11-28 | 哈尔滨工业大学 | Method for interface modification of carbon/carbon composite material by graphene/polymer coating |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110524532A (en) * | 2019-08-31 | 2019-12-03 | 三体次元信息科技(宁波)有限公司 | Electron type artificial-muscle electric actuator and preparation method thereof and the application in finger actuation device |
CN110524532B (en) * | 2019-08-31 | 2020-12-11 | 三体次元信息科技(宁波)有限公司 | Electronic artificial muscle electric actuator, preparation method thereof and application thereof in finger driving device |
CN110863346A (en) * | 2019-11-26 | 2020-03-06 | 陕西华夏粉末冶金有限责任公司 | Preparation method of carbon-carbon fiber composite material for conical surface friction layer of heavy-duty automobile transmission synchronizer cone ring |
CN115595037A (en) * | 2022-10-13 | 2023-01-13 | 江阴润方机械制造有限公司(Cn) | High-strength stainless steel retainer ring for filling machine and preparation process thereof |
CN115595037B (en) * | 2022-10-13 | 2024-03-08 | 江阴润方机械制造有限公司 | High-strength stainless steel clamping ring for filling machine and preparation process thereof |
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