CN109401459A - A kind of high temperature scratch resistance non-sticking lining of carbon fiber modifying and preparation method thereof - Google Patents
A kind of high temperature scratch resistance non-sticking lining of carbon fiber modifying and preparation method thereof Download PDFInfo
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/04—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09D127/06—Homopolymers or copolymers of vinyl chloride
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- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses the high temperature scratch resistance non-sticking linings of carbon fiber modifying, it from bottom to top include priming coat, floating coat and finishing coat three parts, their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, floating coat includes fire resistant resin and fluororesin, finishing coat includes fluororesin, so that coating has excellent high temperature resistance, priming coat is modified fire resistant resin using carbon fiber, further enhances the heat-resisting quantity and scratch resistance of coating for the introducing of fire resistant resin.
Description
Technical field
The present invention relates to a kind of coatings, and in particular to a kind of high temperature scratch resistance non-sticking lining of carbon fiber modifying and its preparation side
Method belongs to technical field of coatings.
Background technique
With the development of the times, non-viscous paint is more and more widely used in kitchen tools, and the every aspects such as household electrical appliances, people are not to
The cognition and use of stick coating are also more and more deep, and the requirement to its performance also increases accordingly.Especially to currently on the market
Not viscous product such as decocts disk, frying pan, and coating is easy to be scratched or even fallen off when in use.So improving non-sticking lining in high temperature
Scratch resistance and hardness under (250~300 DEG C) state are the development trends of such product.
It is used for the cookers such as pot earliest from the seventies non-sticking lining, has more than 30 years history so far, scientific research personnel one
The various performances for the raising product directly made great efforts.Wearability is such as improved, a kind of fluoropolymer is disclosed in patent CN1500014A not
Adhesive coating layer is related to a kind of non-sticking lining that wearability is all good with food removing the two performance.The preferred silicon carbide of its inorganic filler or
The high rigidity substance such as boron nitride can reach 2000 Knoops although hardness is higher, since this particle is with the distribution of single body
In the bottom or middle part of coating, is combined by high temperature resistant binder with substrate, reach the characteristics of it improves wearability.But it is special
Property also only under normal temperature state when coating in use, especially high temperature (250~300 DEG C) when, binding resin is
Softened, high hardness particle then can have its prominent characteristic at normal temperature to external force resistance.
103465574 B of patent CN 105331260 A and CN is using PEEK resin as heat-resistant bonded resin, PEEK tree
Rouge is a kind of special engineering plastics haveing excellent performance.PEEK resin not only excellent heat resistance, but also there is high intensity, insulating properties
Stablize, hydrolysis, resistance to compression, high-fracture toughness is corrosion-resistant, and the machine components that composite material is fabricated to have self-lubricating effect.
Heatproof, thermal stability are good, superelevation is heat-resisting, and for HDT at 315 DEG C or more, it is 250 DEG C that temperature, which is used continuously, in UL.Mechanical property: PEEK is
Toughness and rigidity have both and obtain the plastics of balance.Especially it to the excellent endurance of alternate stress is most gone out in all plastics
Many, it can match in excellence or beauty with alloy material.Self-lubrication: PEEK has outstanding sliding properties in all plastics.Chemical-resistant resistance
Property (corrosion resistance): PEEK have excellent chemical resistance in common chemicals, can dissolve or destroy its
The only concentrated sulfuric acid, its corrosion resistance are close with nickel steel.Anti-flammability: PEEK is highly stable polymer, the sample of 1.45mm thickness
Product are not added any fire retardant just and can reach highest flame-retardant standard.Peel resistance: the peel resistance of PEEK is fine, therefore can be made into
Very thin or electromagnetic wire is coated, and can be used under severe conditions.Hydrolytic resistance: PEEK and its composite material be not by water and high pressure
The chemical affect of vapor, the product being made with this material is used continuously in high-temperature high pressure water can still keep excellent characteristics.
But its glass transition temperature (Tg=143 DEG C), hardness and scratch resistance when high temperature decline to a great extent, and can not meet cooker just
It is often used condition.And the glass transition temperature (Tg=250~300 DEG C) of polyamidoimide, polyether-ether-ketone glass transition temperature (Tg=
225 DEG C), by glass or fibre reinforced, certain performances are greatly improved, thus hardness and scratch resistance performance when enhancing high temperature.
Floating coat generally uses heat-resistant bonded resin and polytetrafluoroethylene (PTFE) (abbreviation 4F, PTFE) and perfluoroethylenepropylene total
Polymers (FEP), finishing coat are used in mixed way using PTFE and PFA, but its main component be polytetrafluoroethylene (PTFE) its be by tetrafluoroethene
Perfluorinated polymers made of copolymerization.There is polytetrafluoroethylene (PTFE) crystallinity height, molecular weight not to have branch, fluorine atom greatly, in molecule
It is closely arranged in around C-C skeleton, C-F bond energy height and fluorine atom play the design features such as shielding action to main chain, these are special
Point determines that it is small with coefficient of friction, do not absorb water, not viscous, non-ignitable, good weatherability, and use temperature range is wide excellent with dielectric properties
The features such as different, so that fluoro coatings have the good characteristic that other coating do not have, but its lower hardness determines that its is wear-resisting
It is poor with scratch resistance.
Summary of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of high temperature scratch resistance of carbon fiber modifying not
Adhesive coating layer and preparation method thereof.
To achieve the above object, the present invention adopts the following technical solutions:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat be 1:0.7~0.8:0.6~
0.7, in priming coat, the mass ratio of carbon fiber and fire resistant resin is 0.1~1:10；In floating coat, fire resistant resin with
The mass ratio of fluororesin is 100:1~2；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 60~70 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 40~50%, the reaction was continued to conversion ratio 85%, terminates poly-
Reaction is closed, unreacted monomer is recycled, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate are with mass ratio 1:0.2~0.3:0.1~0.2:0.08~0.1:0.02
The mixed machine of heat is added in~0.03:0.05~0.06, premixes under the conditions of 280~300 DEG C, is then fed into extruder extrusion molding, obtains
A kind of fire resistant resin.
Preferably, the carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
Preferably, the fire resistant resin of the carbon fiber modifying is melting extrusion after mixing carbon fiber with fire resistant resin
It is granulated and obtains.
Preferably, the priming coat further includes hammer agent, and weight accounting is 1~2%.
Preferably, the fluororesin is any one or more of selected from PTFE, FEP and PFA, in floating coat, into one
Step is preferably PTFE and the FEP mixing of mass ratio 3:1；In finishing coat, the further preferably PTFE and PFA of mass ratio 15:1
Mixing.
Preferably, the first dispersing agent is the mixing of hydroxypropyl methyl cellulose and the polyvinyl alcohol of 50~55mol% of alcoholysis degree
Object, the mass ratio of two components is 1:1.5~2 in the mixture；Second dispersing agent is the polyvinyl alcohol of 70~72mol% of alcoholysis degree.
It is further preferred that the hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1~0.2, content is 8~10%, first
Base degree of substitution is 1~2, and content is 20~25%.
Preferably, the quality of water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent
Than for 60~70:2~3:1~2:100:2~3:2~3:2~3.
Preferably, the coupling agent is silane resin acceptor kh-550.
Preferably, the crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, three's mass ratio
For 1:1~2.
Preferably, the initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3
~4:1.
Preferably, in step (D), 40~50 DEG C is cooled to and is re-fed into extruder progress extrusion molding.
Preferably, in step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: will be catalyzed
Agent, solvent and acrylic acid are added in reaction kettle together, stir evenly, and stand 10~20 minutes, then slowly drip isoprene
It adds in reaction kettle, stirs, control reactor temperature is 10~20 DEG C, is reacted 3~5 hours；Catalyst is recovered by filtration, distills
Recycling design and unreacted isoprene are to get acrylic acid modified isoprene rubber.
It is further preferred that isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.2~0.3:2~4:
0.1~0.3.
Still more preferably, the catalyst is alchlor, and solvent is dimethylbenzene.
It is further preferred that the time for adding of isoprene is 3~4 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
Preferably, in step (1), auxiliary agent is powdered polyacrylate surface modifier, and BYK-368P is purchased from Bi Kehua
It learns.The dosage of auxiliary agent is the 0.5~1% of micropowder weight.
Preferably, it in step (1), is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, so
After grind micro mist be made.
Preferably, in step (1), the size controlling of micro mist is at 20~30 μm.
Preferably, in step (1), the melt flow rate (MFR) (MFR) of micro mist is 9~80g/10min, the excessive then easy shape of MFR
It does not form a film at biggish graininess, the too low easy levelling of then coating.
Preferably, it in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, after the spraying of floating coat liquid
120 DEG C are sintered 10 minutes, are sintered 10 minutes for 400~410 DEG C after the spraying of finishing coat liquid.
Preferably, in step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol is added to the water, micro mist is added after mixing,
It stirs evenly, obtains liquid coating, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol,
Water quality ratio is 1:1.1:0.7:0.5.
Beneficial effects of the present invention:
The present invention from bottom to top includes priming coat, floating coat and finishing coat three parts, their raw material composition is as follows: priming coat packet
The fire resistant resin of carbon fiber modifying is included, floating coat includes fire resistant resin and fluororesin, and finishing coat includes fluororesin, high temperature resistant
So that coating has excellent high temperature resistance, priming coat is modified fire resistant resin using carbon fiber for the introducing of resin,
Further enhance the heat-resisting quantity and scratch resistance of coating.
The dosage of carbon fiber is very crucial, and the very few scratch resistance and heat-resisting quantity that product cannot be remarkably reinforced excessively understands shadow
Coating is rung to the adhesive force of substrate.
Fire resistant resin is with vinyl chloride monomer, acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate etc. are made of raw material, have been initially formed Corvic, have then introduced
The ingredients such as acrylic acid modified isoprene rubber, each component is synergistic, improves high temperature resistance.Isoprene rubber should carry out propylene
Otherwise instead sour modification can adversely affect the high temperature resistance of product.
When preparing Corvic, feeding sequence, the selection of dispersing agent and the opportunity that feeds intake, polymerization reaction terminate opportunity
Deng all extremely important, it is directly related to the high temperature resistance of final products obtained therefrom.
The present invention carries out coating preparation using the method for liquid spray, easy to operate, lower to equipment and technique requirement, right
The melt flow rate (MFR) of micro mist requires also not high, adaptation mass production.
Specific embodiment
Below with reference to embodiment, the present invention will be further elaborated, it should explanation, following the description merely to
It explains the present invention, its content is not defined.
Embodiment 1:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.7:0.6, in priming coat
In, the mass ratio of carbon fiber and fire resistant resin is 0.1:10；In floating coat, the mass ratio of fire resistant resin and fluororesin is
100:1；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 60 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 40%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), the mixed machine of heat is added with mass ratio 1:0.2:0.1:0.08:0.02:0.05 in silica aerogel powder, calcium stearate,
It is premixed under the conditions of 280 DEG C, is then fed into extruder extrusion molding, obtain a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 1%.
In floating coat, fluororesin PTFE；In finishing coat, the PTFE and PFA that fluororesin is mass ratio 15:1 are mixed
It forms.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 50mol%, the mixture
In two components mass ratio be 1:1.5；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 70mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1, content 8%, methyl substitution 1, content 20%.
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 60:
2:1:100:2:2:2.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:1.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3:1.
In step (D), it is cooled to 40 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 10 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 10 DEG C, is reacted 3 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.2:2:0.1.Catalyst is alchlor, molten
Agent is dimethylbenzene.The time for adding of isoprene is 3 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 1% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 20 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Embodiment 2:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.8:0.7, in primary coat
In layer, the mass ratio of carbon fiber and fire resistant resin is 1:10；In floating coat, the mass ratio of fire resistant resin and fluororesin is
100:2；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 70 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 50%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), heat is added with mass ratio 1:0.3:0.2:0.1:0.03:0.06 in silica aerogel powder, calcium stearate
Mixed machine premixes under the conditions of 300 DEG C, is then fed into extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 2%.
In floating coat, fluororesin FEP；In finishing coat, fluororesin PTFE.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 55mol%, the mixture
In two components mass ratio be 1:2；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 72mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.2, content 10%, methyl substitution 2, and content is
25%。
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 70:
3:2:100:3:3:3.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:2.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 4:1.
In step (D), it is cooled to 50 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 20 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 20 DEG C, is reacted 5 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.3:4:0.3.Catalyst is tri-chlorination
Aluminium, solvent are dimethylbenzene.The time for adding of isoprene is 4 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 0.5% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 30 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 410 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Embodiment 3:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.7:0.7, in priming coat
In, the mass ratio of carbon fiber and fire resistant resin is 0.1:10；In floating coat, the mass ratio of fire resistant resin and fluororesin is
100:2；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 60 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 50%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate are added heat with mass ratio 1:0.2:0.2:0.08:0.03:0.05 and mix
Machine premixes under the conditions of 300 DEG C, is then fed into extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 1%.
In floating coat, the PTFE and FEP that fluororesin is mass ratio 3:1 are mixed；In finishing coat, fluororesin is mass ratio
The PTFE and PFA of 15:1 is mixed.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 55mol%, the mixture
In two components mass ratio be 1:1.5；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 72mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1, content 10%, methyl substitution 1, and content is
25%。
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 60:
3:1:100:3:2:3.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:1.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 4:1.
In step (D), it is cooled to 40 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 20 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 10 DEG C, is reacted 5 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.2:4:0.1.Catalyst is alchlor,
Solvent is dimethylbenzene.The time for adding of isoprene is 4 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 0.5% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 30 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Embodiment 4:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.8:0.6, in priming coat
In, the mass ratio of carbon fiber and fire resistant resin is 1:10；In floating coat, the mass ratio of fire resistant resin and fluororesin is
100:1；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 70 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 40%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate are added heat with mass ratio 1:0.3:0.1:0.1:0.02:0.06 and mix
Machine premixes under the conditions of 280 DEG C, is then fed into extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 2%.
In floating coat, the PTFE and FEP that fluororesin is mass ratio 3:1 are mixed；In finishing coat, fluororesin is mass ratio
The PTFE and PFA of 15:1 is mixed.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 50mol%, the mixture
In two components mass ratio be 1:2；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 70mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.2, content 8%, methyl substitution 2, content 20%.
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 70:
2:2:100:2:3:2.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:2.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3:1.
In step (D), it is cooled to 50 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 10 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 20 DEG C, is reacted 3 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.3:2:0.3.Catalyst is alchlor,
Solvent is dimethylbenzene.The time for adding of isoprene is 3 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 1% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 20 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Embodiment 5:
A kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, from bottom to top include priming coat, floating coat and finishing coat three parts,
Their raw material composition is as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluorine
Resin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.75:0.65, in primary coat
In layer, the mass ratio of carbon fiber and fire resistant resin is 0.6:10；In floating coat, the mass ratio of fire resistant resin and fluororesin
For 100:1.5；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 65 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 45%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate are added heat with mass ratio 1:0.25:0.15:0.09:0.02:0.06 and mix
Machine premixes under the conditions of 290 DEG C, is then fed into extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 1.5%.
In floating coat, the PTFE and FEP that fluororesin is mass ratio 3:1 are mixed；In finishing coat, fluororesin is mass ratio
The PTFE and PFA of 15:1 is mixed.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 52mol%, the mixture
In two components mass ratio be 1:1.8；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 71mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1, content 9%, methyl substitution 2, content 22%.
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 65:
2.5:1.5:100:2.5:2.5:2.5.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:1.5.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3.5:1.
In step (D), it is cooled to 45 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 15 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 15 DEG C, is reacted 4 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.25:3:0.2.Catalyst is alchlor,
Solvent is dimethylbenzene.The time for adding of isoprene is 4 hours.
A kind of preparation method of the high temperature scratch resistance non-sticking lining of above-mentioned carbon fiber modifying, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 0.8% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 20 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Comparative example 1
A kind of non-sticky coating from bottom to top includes priming coat, floating coat and finishing coat three parts, their raw material composition is as follows:
Priming coat includes fire resistant resin, and floating coat includes fire resistant resin and fluororesin, and finishing coat includes fluororesin；Wherein, primary coat
The mass ratio of layer, floating coat and finishing coat is 1:0.75:0.65, in floating coat, the mass ratio of fire resistant resin and fluororesin
For 100:1.5；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 65 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 45%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide (PPS), polyether-ether-ketone
(PEEK), silica aerogel powder, calcium stearate are added heat with mass ratio 1:0.25:0.15:0.09:0.02:0.06 and mix
Machine premixes under the conditions of 290 DEG C, is then fed into extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, priming coat further includes hammer agent, and weight accounting is 1.5%.
In floating coat, the PTFE and FEP that fluororesin is mass ratio 3:1 are mixed；In finishing coat, fluororesin is mass ratio
The PTFE and PFA of 15:1 is mixed.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 52mol%, the mixture
In two components mass ratio be 1:1.8；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 71mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1, content 9%, methyl substitution 2, content 22%.
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 65:
2.5:1.5:100:2.5:2.5:2.5.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:1.5.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3.5:1.
In step (D), it is cooled to 45 DEG C and is re-fed into extruder progress extrusion molding.
In step (D), acrylic acid modified isoprene rubber is prepared by the following method to obtain: by catalyst, solvent
It is added in reaction kettle, stirs evenly together with acrylic acid, stand 15 minutes, then isoprene is slowly added dropwise to reaction kettle
Interior, stirring, control reactor temperature is 15 DEG C, is reacted 4 hours；It is recovered by filtration catalyst, is distilled to recover solvent and not anti-
The isoprene answered is to get acrylic acid modified isoprene rubber.
Isoprene, catalyst, solvent and acrylic acid mass ratio be 1:0.25:3:0.2.Catalyst is alchlor,
Solvent is dimethylbenzene.The time for adding of isoprene is 4 hours.
A kind of preparation method of above-mentioned non-sticking lining, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 0.8% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 20 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Comparative example 2
A kind of non-sticky coating from bottom to top includes priming coat, floating coat and finishing coat three parts, their raw material composition is as follows:
Priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes fire resistant resin and fluororesin, and finishing coat includes fluorine tree
Rouge；Wherein, the mass ratio of priming coat, floating coat and finishing coat is 1:0.75:0.65, in priming coat, carbon fiber and high temperature resistant
The mass ratio of resin is 0.6:10；In floating coat, the mass ratio of fire resistant resin and fluororesin is 100:1.5；The resistance to height
Warm resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 65 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 45%, the reaction was continued to conversion ratio 85%, and it is anti-to terminate polymerization
It answers, recycles unreacted monomer, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and polyphenylene sulfide (PPS), polyether-ether-ketone (PEEK), aerosil
The mixed machine of heat is added with mass ratio 1:0.15:0.09:0.02:0.06 in powder, calcium stearate, premixes under the conditions of 290 DEG C, then send
Enter extruder extrusion molding, obtains a kind of fire resistant resin.
Wherein, carbon fiber is the high-performance carbon fibers of modulus 300G pa or more (high model).
The fire resistant resin of carbon fiber modifying is that melting extrusion is granulated and obtains after mixing carbon fiber with fire resistant resin.
Priming coat further includes hammer agent, and weight accounting is 1.5%.
In floating coat, the PTFE and FEP that fluororesin is mass ratio 3:1 are mixed；In finishing coat, fluororesin is mass ratio
The PTFE and PFA of 15:1 is mixed.
First dispersing agent is the mixture of hydroxypropyl methyl cellulose and the polyvinyl alcohol of alcoholysis degree 52mol%, the mixture
In two components mass ratio be 1:1.8；Second dispersing agent is the polyvinyl alcohol of alcoholysis degree 71mol%.
The hydroxypropyl degree of substitution of hydroxypropyl methyl cellulose is 0.1, content 9%, methyl substitution 2, content 22%.
Water, the first dispersing agent, coupling agent, vinyl chloride monomer, crosslinking agent, initiator, the second dispersing agent mass ratio be 65:
2.5:1.5:100:2.5:2.5:2.5.
Coupling agent is silane resin acceptor kh-550.
Crosslinking agent is the mixture of polyethyleneglycol diacrylate and divinylbenzene, and three's mass ratio is 1:1.5.
Initiator is the mixture of isopropyl benzene hydroperoxide and benzoyl peroxide, and three's mass ratio is 3.5:1.
In step (D), it is cooled to 45 DEG C and is re-fed into extruder progress extrusion molding.
A kind of preparation method of above-mentioned non-sticking lining, the specific steps are as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
In step (1), auxiliary agent is powdered polyacrylate surface modifier, BYK-368P, purchased from Bi Ke chemistry.Auxiliary agent
Dosage is the 0.8% of micropowder weight.
In step (1), it is granulated after priming coat raw material is mixed with the auxiliary agent of corresponding amount by melting extrusion, then grounds travel
It is broken that micro mist is made.
In step (1), the size controlling of micro mist is at 20 μm.
It in step (2), is sintered 10 minutes for 400 DEG C after the spraying of priming coat micro mist liquid, 120 DEG C of burnings after the spraying of floating coat liquid
It knot 10 minutes, is sintered 10 minutes for 400 DEG C after the spraying of finishing coat liquid.
In step (2), N-Methyl pyrrolidone, ethyl alcohol, isopropanol are added to the water, micro mist is added after mixing, stirring is equal
It is even, liquid coating is obtained, liquid spraying can be carried out；Wherein, micro mist and N-Methyl pyrrolidone, ethyl alcohol, isopropanol, water quality
Than for 1:1.1:0.7:0.5.
Test example
The testing substrates that experimental method of the present invention is selected are die casting aluminium, surface roughness are as follows: 1.5~4 μm.
Laboratory apparatus:
High temperature scratch resistance tester (also known as tiger pawl tester), refill for ball-point pen (diameter 0.5mm tungsten carbide), Chinese pencil (1H-
9H): electromagnetic oven, sodium-chloride water solution, egg.
High temperature scratch resistance tester:
It is mainly formed by reciprocating section, rotating part and from transfer part, reciprocating part has heating function, and rotating part is logical to test piece
Cross the power that three refill for ball-point pens apply downward 400g.
1, high temperature scratch resistance is tested
Measured workpiece is fixed on the reciprocating part bracket, is heated to 200 DEG C, guarantees measured workpiece constant temperature 190~210
DEG C, three refill for ball-point pens are installed from transfer part, rotation section is adjusted to 150rpm, and reciprocating part is adjusted to 30 beats/min, start to test,
The coating damaged condition of observation measured workpiece is scratched with coating surface to fall off, and exposes the substrate time to judge benchmark.It is above-mentioned
It under the condition of high temperature, is delineated using Chinese pencil, the minimum hardness of scratch occurs in observation.
2, not viscoelastic test
Measured workpiece is placed on electromagnetic oven, guarantees that measured workpiece surface constant temperature at 150~170 DEG C, will be in 25 DEG C of room temperature
Egg squeeze into measured workpiece, when surface protein solidification, egg scooped up with wood shovel, egg is completely scooped up without being adhered, and is
Test passes through, in triplicate, evaluation result.
3, corrosion-resistant test
Detection reagent: the NaCl solution that mass fraction is 10%.
Testing process: measured workpiece is placed on electromagnetic oven or gas burner, pours into configured NaCl solution, lasting to boil
8 hours are boiled as a circulation, after testing, after cleaning up, specimen surface is flat and smooth, it is not blistering, do not fall off.Repeat N
It is secondary, up to coating foaming or fall off.
Dependence test is carried out to the coating of Examples 1 to 5 and comparative example 1~2, the results are shown in Table 1.
1. test result of table compares
| High temperature scratch resistance (minute) | Hot hardness | Non-sticky property | Corrosion resistance (hour) | |
| Embodiment 1 | ≥75 | 6H | Pass through | ≥96 |
| Embodiment 2 | ≥75 | 6H | Pass through | ≥96 |
| Embodiment 3 | ≥75 | 6H | Pass through | ≥96 |
| Embodiment 4 | ≥75 | 6H | Pass through | ≥96 |
| Embodiment 5 | ≥75 | 6H | Pass through | ≥96 |
| Comparative example 1 | 32 | 3H | Do not pass through | 48 |
| Comparative example 2 | 68 | 5H | Pass through | 72 |
As shown in Table 1, the coating of Examples 1 to 5 has excellent heat-resisting quantity and scratch resistance.Comparative example 1 omits carbon fiber, applies
The heat-resisting quantity and scratch resistance of layer are obviously deteriorated；Comparative example 2 omits acrylic acid modified isoprene rubber when preparing fire resistant resin,
Coating heat-resisting quantity is obviously deteriorated.
Above-mentioned, although specific embodiments of the present invention have been described, not to the limit of the scope of the present invention
System, based on the technical solutions of the present invention, those skilled in the art do not need to make the creative labor can make it is each
Kind modification or deformation are still within protection scope of the present invention.
Claims (10)
1. a kind of non-sticky coating of high temperature scratch resistance of carbon fiber modifying, which is characterized in that from bottom to top include priming coat, floating coat and
Finishing coat three parts, their raw material composition are as follows: priming coat includes the fire resistant resin of carbon fiber modifying, and floating coat includes resistance to
High-temperature resin and fluororesin, finishing coat include fluororesin；Wherein, the mass ratio of priming coat, floating coat and finishing coat be 1:0.7~
0.8:0.6~0.7, in priming coat, the mass ratio of carbon fiber and fire resistant resin is 0.1~1:10；In floating coat, resistance to height
The mass ratio of warm resin and fluororesin is 100:1~2；The fire resistant resin is manufactured by the following method:
(A) water, the first dispersing agent are added in polymeric kettle, vinyl chloride monomer is added after extracting vacuum, be uniformly mixed；
(B) coupling agent, crosslinking agent, initiator is added, carries out polymerization reaction under the conditions of being heated to 60~70 DEG C；
(C) the second dispersing agent is added when vinyl chloride monomer conversion ratio reaches 40~50%, the reaction was continued to conversion ratio 85%, terminates poly-
Reaction is closed, unreacted monomer is recycled, the centrifugation of gained slurries is dried to obtain Corvic；
(D) by Corvic obtained by step (C) and acrylic acid modified isoprene rubber, polyphenylene sulfide, polyether-ether-ketone, dioxy
SiClx aerogel powder, calcium stearate are with mass ratio 1:0.2~0.3:0.1~0.2:0.08~0.1:0.02~0.03:0.05
~0.06 is added the mixed machine of heat, premixes under the conditions of 280~300 DEG C, is then fed into extruder extrusion molding, obtains a kind of high temperature resistant tree
Rouge.
2. non-sticking lining according to claim 1, which is characterized in that the fire resistant resin of the carbon fiber modifying is by carbon
Melting extrusion is granulated and obtains after fiber is mixed with fire resistant resin.
3. non-sticking lining according to claim 1, which is characterized in that the priming coat further includes hammer agent, weight
Accounting is 1~2%.
4. non-sticking lining according to claim 1, which is characterized in that the fluororesin is in PTFE, FEP and PFA
It is any one or more.
5. non-sticking lining according to claim 1, which is characterized in that the first dispersing agent is hydroxypropyl methyl cellulose and alcohol
The mixture of the polyvinyl alcohol of 50~55mol% of solution degree, the mass ratio of two components is 1:1.5~2 in the mixture；Second dispersion
Agent is the polyvinyl alcohol of 70~72mol% of alcoholysis degree.
6. non-sticking lining according to claim 1, which is characterized in that water, the first dispersing agent, coupling agent, vinyl chloride monomer,
Crosslinking agent, initiator, the second dispersing agent mass ratio be 60~70:2~3:1~2:100:2~3:2~3:2~3.
7. non-sticking lining according to claim 1, which is characterized in that in step (D), acrylic acid modified isoprene rubber is
It is prepared by the following method: catalyst, solvent and acrylic acid being added in reaction kettle together, stirred evenly, stand 10
~20 minutes, then isoprene is slowly added dropwise to reaction kettle, is stirred, control reactor temperature is 10~20 DEG C, instead
It answers 3~5 hours；It is recovered by filtration catalyst, is distilled to recover solvent and unreacted isoprene to get acrylic acid modified different
Penta rubber.
8. the preparation method of non-sticking lining described in any one of claim 1~7, which is characterized in that specific step is as follows:
(1) auxiliary agent is added into priming coat raw material, and micro mist is made, obtains priming coat micro mist；
(2) liquid coating is made in priming coat micro mist obtained by step (1), the method sprayed using liquid, in the table of painted object
Face sprays to form priming coat；It sprays to form floating coat in base coating surface liquid after fire resistant resin and fluororesin physical mixed,
Fluororesin sprays to form finishing coat in floating coat surface liquid.
9. preparation method according to claim 8, which is characterized in that in step (1), by priming coat raw material and corresponding amount
It is granulated after auxiliary agent mixing by melting extrusion, then grinds and micro mist is made.
10. preparation method according to claim 8, which is characterized in that in step (1), the size controlling of micro mist 20~
30μm。
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| CN103465574A (en) * | 2013-07-01 | 2013-12-25 | 浙江鹏孚隆化工有限公司 | Scratch-resistant non-stick coating layer and coating method thereof |
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| CN102936412A (en) * | 2012-11-28 | 2013-02-20 | 广州聚赛龙新材料科技有限公司 | Carbon fiber reinforced polyetherimide/polyphenylene sulfide composite material and preparation method thereof |
| CN103465574A (en) * | 2013-07-01 | 2013-12-25 | 浙江鹏孚隆化工有限公司 | Scratch-resistant non-stick coating layer and coating method thereof |
| CN107964143A (en) * | 2017-12-07 | 2018-04-27 | 单动力 | A kind of isoamyl/fluorine silicon/fluorine ether compounded rubber and preparation method thereof |
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