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 PDF

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Publication number
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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China
Prior art keywords
graphene oxide
carbon fibre
resin
fibre composite
composite material
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CN201810403254.6A
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Chinese (zh)
Inventor
林育阳
陆千夏
王娟梅
赵志清
左鹏军
杨聪斌
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SHAANXI COUNTY MACHINERY RESEARCH INSTITUTE
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SHAANXI COUNTY MACHINERY RESEARCH INSTITUTE
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Priority to CN201810403254.6A priority Critical patent/CN108623989A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Reinforced Plastic Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

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

A kind of preparation method of graphene oxide resin carbon fibre composite material
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).
CN201810403254.6A 2018-04-28 2018-04-28 A kind of preparation method of graphene oxide resin carbon fibre composite material Pending CN108623989A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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
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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Publication number Priority date Publication date Assignee Title
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
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
CN107497404A (en) * 2017-10-18 2017-12-22 中南林业科技大学 A kind of preparation method of modified graphene oxide sorbing material

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
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
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
CN107497404A (en) * 2017-10-18 2017-12-22 中南林业科技大学 A kind of preparation method of modified graphene oxide sorbing material

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Cited By (5)

* Cited by examiner, † Cited by third party
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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