CN106752806B - The preparation method of polyether ketone ketone electrostatic spraying powder coating with cross-linking properties - Google Patents
The preparation method of polyether ketone ketone electrostatic spraying powder coating with cross-linking properties Download PDFInfo
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- CN106752806B CN106752806B CN201710062805.2A CN201710062805A CN106752806B CN 106752806 B CN106752806 B CN 106752806B CN 201710062805 A CN201710062805 A CN 201710062805A CN 106752806 B CN106752806 B CN 106752806B
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- polyether ketone
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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
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
- C09D5/038—Anticorrosion agents
Abstract
The invention belongs to polymer powder processing technique fields, and in particular to a kind of preparation method of the polyether ketone ketone electrostatic spraying powder coating with cross-linking properties.This method is by polyether ketone ketone after the completion of polymerization through being mechanically pulverized, polyether ketone ketone coarse powder is obtained after washing, drying, coarse powder is after stablizing processing, modifying agent is added and obtains modified coarse powder, it will be modified coarse powder afterwards through air-flow crushing, polyether ketone ketone fine powder is obtained, then screened obtains polyether ketone ketone electrostatic spraying powder coating.Present invention process is easy, crush efficiency is high, impurity content is low, polyether ketone ketone electrostatic spraying powder coating is made to be uniformly dispersed, centralized particle diameter, and granule-morphology almost spherical, it can get polyether ketone ketone coating by electrostatic spraying, it can be obviously improved the binding force of polyether ketone ketone and metallic matrix after modified, while its high temperature resistant and chemical corrosion resistance are correspondinglyd increase, can be used as coating and be widely used in corrosion-resistant field.
Description
Technical field
The invention belongs to polymer powder processing technique fields, and in particular to a kind of polyether ketone ketone with cross-linking properties is quiet
The preparation method of electrospray powdery paints.
Background technique
Polyether ketone ketone (PEKK) resin is a kind of semicrystalline thermoplastic special engineering plastic, is after polyether-ether-ketone (PEEK)
The another special construction type thermoplastic resin developed later, have outstanding high temperature resistance, mechanical performance, corrosion resistance and
Tribological property etc., simultaneously because its unique chemical structure can form high adhesion force coating with metal, compared to polytetrafluoroethyl-ne
Alkene (PTFE) coating and polyphenylene sulfide (PPS) coating have better heat resisting temperature, impact resistance and scraping and wiping resistance performance, are coated
It can be obtained in metal surface and have excellent performance widely used PEKK coated article.
Electrostatic powder coating technology is most environmentally friendly one of the application techniques of paint industry, the object of spraying be by pure solid at
The powdery paints being grouped as does not contain any volatile organic solvent, has fundamentally prevented organic volatile pollution, electrostatic
Waste pollution will not be also generated during applying.Powder shape and partial size are very big on electrostatic spraying efficiency and coating layer thickness influence,
Powder particle is ideal in spherical obtained spray efficiency.If powder diameter is too small to be unfavorable for electrostatic spraying operation, can lead
Cause cover light；And powder diameter will lead to greatly very much between powder there are gap, when solidification, generates defect, also has blocking spray gun
Possibility.
Powdery paints even compact is applied on the metal surface, shielding action can effectively prevent corrosive medium with
The direct contact of metal surface, and then slow down the generation of corrosion.Although there are certain shielding actions for powdery paints, in height
Under warm condition of high voltage, the permeability of strong corrosive media is extremely strong, as time went on, still has a small amount of medium and passes through coating, from
And corrosion is generated to metal, corrosion product volume gradually expands, and final coating blistering falls off, and loses antiseptic property.For high temperature,
High vacuum, high corrosion extreme environment, existing corrosion-inhibiting coating are difficult to meet the requirements, and PEKK has ketone group more higher than PEEK content,
The promotion of ketone group ratio, which increases main chain rigidity, glass transition temperature Tg and fusing point Tm, has different degrees of mention compared with PEEK
Height, while the presence of C=O bond increases its active site combined with metal (carbon steel, stainless steel, aluminium alloy).However
For PEKK compared with PEEK, crystallinity is lower, and crystallization rate is slow, is weaker than PEEK so as to cause its chemical corrosion resistance, by changing
Property can further promote its binding force with metal, while improving its ability for resisting chemical attack, it is steady to obtain more preferably size
It is qualitative.
Summary of the invention
The object of the present invention is to provide a kind of polyether ketone ketone electrostatic spraying powder paintings with cross-linking properties of simple process
The preparation method of material, centralized particle diameter, the granule-morphology almost spherical of the powdery paints of preparation, the polyether ketone ketone sprayed
The chemical corrosion resistance and dimensional stability of coating are effectively promoted, and the binding force of polyether ketone ketone coating and matrix is strong.
The preparation method of polyether ketone ketone electrostatic spraying powder coating of the present invention with cross-linking properties is: will first gather
Polyether ketone ketone after the completion of conjunction obtains polyether ketone ketone coarse powder after mechanical crushing, washing, drying, after stablizing processing, with modification
Agent, which is uniformly mixed, obtains modified coarse powder, then will be modified coarse powder through air-flow crushing, obtains polyether ketone ketone fine powder, finally screened to obtain
Polyether ketone ketone electrostatic spraying powder coating.
Wherein, the modifying agent is xanthene, xanthenes alcohol, 9- phenylxanthen or bis- [4- (9- xanthenes hydrogen-based) phenyl] ethers
One or more of.In electrostatic spray process, above-mentioned substance heats in high temperature air can produce phenyl ring free radical and makes to gather
Ether ketone ketone polymer crosslinks, and about 200 DEG C to 400 DEG C of the temperature of cross-linking process, preferably from about 250 DEG C to 350 DEG C, crosslinking
The binding force that can be obviously improved polyether ketone ketone coating and metal occurs, while promoting the size under its chemical corrosion resistance and high temperature
Stability.By forcing the interface of removing to may determine that its binding force from metal base polyether ketone ketone coating, and polyether ketone ketone
Coating crosslinking degree can be judged by observing it whether 100 DEG C dissolve for the concentrated sulfuric acid 1 hour.
The processing of stablizing is to keep polyether ketone ketone coarse powder 1~4 hour under 180~260 DEG C of vacuum.At stablizing
It after reason, is shunk in cellular polyether ketone ketone, voidage reduces, and can remove unstable small point for causing hot setting to generate defect
Son, meanwhile, crystallinity is further promoted, and is conducive to crush efficiency promotion and postorder electrostatic spraying film forming.
The mechanical milling processes use pipe line type high-shearing emulsifier.
Terephthaloyl groups and the ratio of isophthalic diformyl are 50:50~60:40 in the polyether ketone ketone.
The particle size range of the polyether ketone ketone coarse powder is 0.1~3mm, the inherent viscosity of polyether ketone ketone coarse powder is 0.5~
0.7dl/g。
The amount of modifier is the 0.5~1% of polyether ketone ketone meal quality.
The partial size of the polyether ketone ketone electrostatic spraying powder coating is 100~300 mesh.
Beneficial effects of the present invention are as follows:
The present invention successively passes through high-shear emulsion machine and airslide disintegrating mill two-stage using polyether ketone ketone polymer as starting material
Polyether ketone ketone fine powder is made in crushing system.Before carrying out air-flow crushing, polyether ketone ketone coarse powder need to be handled through stablizing, so that in porous
Shape polyether ketone ketone is shunk, and voidage reduces, meanwhile, crystallinity is further promoted, and crush efficiency is helped to improve, when shortening crushing
Between, grain corner is eliminated, granule-morphology is improved.Be added modifying agent, can be obviously improved after the completion of electrostatic spraying polyether ketone ketone with
The binding force of metal base, while promoting its chemical corrosion resistance and high temperature dimensional stability.
Detailed description of the invention
Fig. 1 is the process flow chart for preparing polyether ketone ketone electrostatic spraying powder coating.
Fig. 2 is the stereoscan photograph of 1 polyether ketone ketone fine powder of embodiment.
Fig. 3 is 1 appearance of coat photo of embodiment.
Fig. 4 is that 1 coating of embodiment draws lattice experiment test chart.
Fig. 5 is 1 appearance of coat photo of comparative example.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
By diphenyl ether, paraphthaloyl chloride (T) and m-phthaloyl chloride (I) pass through Friedel-Crafts reaction synthesizing polyether ketone ketone,
The molar ratio of T:I is 50:50 in middle product, and polyether ketone ketone is slowly added to crush in pipe line type high-shearing emulsifier, with
By washing, being dried to obtain the polyether ketone ketone coarse powder that inherent viscosity is 0.6dl/g, the particle size of coarse powder is 0.1~1mm.
It takes polyether ketone ketone coarse powder 100kg to be kept for 4 hours at 180 DEG C, 0.5kg xanthene modifying agent is added, through air-flow powder
The broken D50 that obtains is 50 μm of polyether ketone ketone fine powders, screened that 200 mesh polyether ketone ketone electrostatic spraying powder coatings, scanning electron microscope are shone
Piece is as shown in Figure 2.Above-mentioned polyether ketone ketone powder paint is passed through on 340 DEG C of carbon steel base material using electrostatic spraying mode
Hot setting obtains polyether ketone ketone coating, the smooth zero defect in surface, as shown in Figure 3.Pass through GB/T 9286-1998 cross cut test
Test, reaches 0 grade, coating binding force is excellent, as shown in Figure 4.A small amount of coating is taken to immerse insoluble, chemically-resistant corruption in 1 hour in the concentrated sulfuric acid
Corrosion is excellent.
Comparative example 1
By diphenyl ether, paraphthaloyl chloride (T) and m-phthaloyl chloride (I) pass through Friedel-Crafts reaction synthesizing polyether ketone ketone,
The molar ratio of T:I is 50:50 in middle product, and polyether ketone ketone is slowly added to crush in pipe line type high-shearing emulsifier, with
By washing, being dried to obtain the polyether ketone ketone coarse powder that inherent viscosity is 0.6dl/g, the particle size of coarse powder is 0.1~1mm.
0.5kg xanthene modifying agent is added in 100kg polyether ketone ketone coarse powder, obtaining D50 through air-flow crushing is 50 μm poly-
Ether ketone ketone fine powder, it is screened to obtain 200 mesh polyether ketone ketone electrostatic spraying powder coatings.Using electrostatic spraying mode by above-mentioned polyether-ketone
Ketone powder coating is sprayed on 340 DEG C of carbon steel base material, obtains polyether ketone ketone coating through hot setting, coating surface is matt and
The defects of there are shrinkage cavities, as shown in Figure 5.It is tested by GB/T 9286-1998 cross cut test, reaches 0 grade, coating binding force is excellent.
Take a small amount of coating immerse in the concentrated sulfuric acid 1 hour it is insoluble, chemical corrosion resistance is excellent.
Comparative example 2
By diphenyl ether, paraphthaloyl chloride (T) and m-phthaloyl chloride (I) pass through Friedel-Crafts reaction synthesizing polyether ketone ketone,
The molar ratio of T:I is 50:50 in middle product, and polyether ketone ketone is slowly added to crush in pipe line type high-shearing emulsifier, with
By washing, being dried to obtain the polyether ketone ketone coarse powder that inherent viscosity is 0.6dl/g, the particle size of coarse powder is 0.1~1mm.
100kg polyether ketone ketone coarse powder is taken to be kept for 4 hours at 180 DEG C, obtaining D50 through air-flow crushing is 50 μm of polyether ketone ketone
Fine powder, it is screened to obtain 200 mesh polyether ketone ketone electrostatic spraying powder coatings.Using electrostatic spraying mode by above-mentioned polyether ketone ketone powder
Coating is sprayed on 350 DEG C of carbon steel base material, obtains polyether ketone ketone coating, the smooth zero defect of coating surface through hot setting.It is logical
GB/T 9286-1998 cross cut test test is crossed, reaches 1 grade, coating binding force is preferable.A small amount of coating is taken to immerse in the concentrated sulfuric acid 1 small
When all dissolve, chemical corrosion resistance is poor.
Embodiment 2
By diphenyl ether, paraphthaloyl chloride (T) and m-phthaloyl chloride (I) pass through Friedel-Crafts reaction synthesizing polyether ketone ketone,
The molar ratio of T:I is 55:45 in middle product, and polyether ketone ketone is slowly added to crush in pipe line type high-shearing emulsifier, with
By washing, being dried to obtain the polyether ketone ketone coarse powder that inherent viscosity is 0.55dl/g, the particle size of coarse powder is 0.1~2mm.
It takes polyether ketone ketone coarse powder 100kg to be kept for 3 hours at 230 DEG C, 0.8kg xanthenes alcohol modifying agent is added, through air-flow powder
The broken D50 that obtains is 49.5 μm of polyether ketone ketone fine powders, screened to obtain 100 mesh polyether ketone ketone electrostatic spraying powder coatings.Using electrostatic
Above-mentioned polyether ketone ketone powder paint on 345 DEG C of stainless steel substrate, is obtained polyether-ketone through hot setting by spraying method
Ketone coating, the smooth zero defect in surface.It is tested by GB/T 9286-1998 cross cut test, reaches 0 grade, coating binding force is excellent.It takes
A small amount of coating immerse in the concentrated sulfuric acid 1 hour it is insoluble, chemical corrosion resistance is excellent.
Embodiment 3
By diphenyl ether, paraphthaloyl chloride (T) and m-phthaloyl chloride (I) pass through Friedel-Crafts reaction synthesizing polyether ketone ketone,
The molar ratio of T:I is 60:40 in middle product, and polyether ketone ketone is slowly added to crush in pipe line type high-shearing emulsifier, with
By washing, being dried to obtain the polyether ketone ketone coarse powder that inherent viscosity is 0.68dl/g, the particle size of coarse powder is 0.1~3mm.
It takes polyether ketone ketone coarse powder 100kg to be kept for 1 hour at 250 DEG C, 1kg 9- phenylxanthen modifying agent is added, through gas
It is 50.5 μm of polyether ketone ketone fine powders that stream, which crushes and obtains D50, screened to obtain 300 mesh polyether ketone ketone electrostatic spraying powder coatings.Using
Electrostatic spraying mode on 350 DEG C of aluminum alloy base material, is gathered above-mentioned polyether ketone ketone powder paint through hot setting
Ether ketone ketone coating, the smooth zero defect in surface.It is tested by GB/T 9286-1998 cross cut test, reaches 0 grade, coating binding force
It is excellent.Take a small amount of coating immerse in the concentrated sulfuric acid 1 hour it is insoluble, chemical corrosion resistance is excellent.
Embodiment and comparative example coating performance is tested, as a result such as table 1.
The performance test results table of 1 powdery paints film of table
Claims (5)
1. a kind of preparation method of the polyether ketone ketone electrostatic spraying powder coating with cross-linking properties, it is characterised in that: will first gather
Polyether ketone ketone after the completion of conjunction obtains polyether ketone ketone coarse powder after mechanical crushing, washing, drying, after stablizing processing, with modification
Agent, which is uniformly mixed, obtains modified coarse powder, then will be modified coarse powder through air-flow crushing, obtains polyether ketone ketone fine powder, finally screened to obtain
Polyether ketone ketone electrostatic spraying powder coating；The modifying agent is xanthene, xanthenes alcohol, 9- phenylxanthen or bis- [4- (9- xanthenes
One or more of hydrogen-based) phenyl] ether；
The processing of stablizing is to keep polyether ketone ketone coarse powder 1~4 hour under 180~260 DEG C of vacuum；
The amount of modifier is the 0.5~1% of polyether ketone ketone meal quality.
2. preparation method according to claim 1, it is characterised in that: the mechanical milling processes are cut using pipeline height
Cut mulser.
3. preparation method according to claim 1, it is characterised in that: in the polyether ketone ketone terephthaloyl groups and
The ratio of phenyl-diformyl base is 50:50~60:40.
4. preparation method according to claim 1, it is characterised in that: the particle size range of the polyether ketone ketone coarse powder is
0.1~3mm, the inherent viscosity of polyether ketone ketone coarse powder are 0.5~0.7dl/g.
5. preparation method according to claim 1, it is characterised in that: the polyether ketone ketone electrostatic spraying powder coating
Partial size is 100~300 mesh.
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| CN108948940A (en) * | 2018-06-19 | 2018-12-07 | 界首市创新门窗有限公司 | A method of avoiding aluminum alloy doors and windows Surface of profile dusty spray coating shrinkage cavity |
| CN112852249A (en) * | 2021-01-22 | 2021-05-28 | 江苏江南烯元石墨烯科技有限公司 | Preparation and use methods of graphene polyether-ether-ketone anticorrosive high-temperature-resistant powder coating |
| CN113473320B (en) * | 2021-07-16 | 2023-05-02 | 辽宁弗佰克高新材料有限公司 | Loudspeaker vibrating diaphragm and loudspeaker |
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| US5175218A (en) * | 1990-09-28 | 1992-12-29 | E. I. Du Pont De Nemours And Company | Crosslinking polymers with compounds containing xanthene groups |
| JP6041806B2 (en) * | 2010-09-27 | 2016-12-14 | アーケマ・インコーポレイテッド | Heat-treated polymer powder |
| CN102653584B (en) * | 2012-04-25 | 2014-06-25 | 金发科技股份有限公司 | Polyether-ether-ketone resin as well as preparation method and application thereof |
| CN104497240A (en) * | 2014-12-17 | 2015-04-08 | 江门市优巨新材料有限公司 | Industrial synthesis method and application of high-fluidity polyether ether ketone resin |
| CN104974633B (en) * | 2015-03-11 | 2017-03-08 | 浙江鹏孚隆化工有限公司 | Ultra-fine powder, preparation method thereof for the polyether-ether-ketone resin of water paint |
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