CN105419450B - A kind of high abrasion super hydrophobic composite coating and preparation method thereof - Google Patents
A kind of high abrasion super hydrophobic composite coating and preparation method thereof Download PDFInfo
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- CN105419450B CN105419450B CN201510855358.7A CN201510855358A CN105419450B CN 105419450 B CN105419450 B CN 105419450B CN 201510855358 A CN201510855358 A CN 201510855358A CN 105419450 B CN105419450 B CN 105419450B
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Abstract
The invention discloses a kind of high abrasion super hydrophobic composite coating and preparation method thereof, using brushing or spraying process, hydrophobic resin priming paint containing compounding micro mist is coated on substrate surface, hydrophobicity hybrid nano paint is sprayed at resin primer surface again after semi-solid preparation, is obtained after being fully cured.It is simple with equipment and technique, the advantages that simple and of low cost is operated, and there is industrial-scale production prospect.The super hydrophobic composite coating that the present invention prepares can be applied to various hard/flexible subserates, such as glass, copper, aluminium, stainless steel, exterior wall tile, timber, paper, cloth, and can bear the destruction of the external force such as sand paper polishing.
Description
Technical field
The invention belongs to coating preparation field, more particularly to a kind of high abrasion super hydrophobic composite coating and preparation method thereof.
Background technology
It is self-cleaning, drag reduction that the distinctive super infiltration feature of super hydrophobic surface make it that super hydrophobic material has, waterproof, antifog, anti-
The micro-/ nano coarse structure such as the functions such as ice, heat transfer, bionical lotus leaf surface, water skipper leg, insect wing prepare super hydrophobic material into
For a hot spot of current thin-film material preparation research, in aviation, navigation, the energy, building, electronics, anti-corrosion, sensor, heat transfer
Wide application prospect is respectively provided with Deng field.Super-hydrophobic characteristic is together decided on by the hydrophobicity and roughness of material, low
Surface free energy and suitable roughness be to prepare two indispensable factors of super hydrophobic surface.
At present, the technology of preparing of super hydrophobic surface includes top-down wet etching, reactive ion etching, coining, machine
Tool processing, laser ablation etc., also include chemical oxidation, electrochemical oxidation, electrochemical deposition, sol-gel, water from bottom to top
Thermal synthesis, spraying etc..However, by super-hydrophobic coat/film prepared by these technologies except need expensive instrument and equipment and
Harsh process conditions, it is difficult to carry out scale industrial production, exist and be easier to destroyed risk.Such as Deng
【Science,2012,335:67】Report and substrate surface is attached to candle ash by vapour deposition process, then after heat treatment
Super-hydrophobic/superoleophobic film is obtained, although can have certain intensity (sand washing) by the film that this method obtains, according to
The old destructive power that can not reach in practical application is horizontal, and this method complex process, it is difficult to realizes industrial applications.
It is mesh to be uniformly sprayed the super-hydrophobic spray coating liquor of preparation in substrate formation super-hydrophobic coat by sprayed coating film method
Preceding a kind of relatively conventional method.Ge etc.【Part.Part.Syst.Charact.2014,31:763】Report and applied by spraying
Embrane method is by super-hydrophobic/superoleophobic SiO2Nano-particle is sprayed at the substrates such as polyester, resin, aluminium foil, cotton, is surpassed on its surface
Hydrophobic/super oleophobic coating, still, the coating after water washes away or the external force such as sand washing is destroyed, reduction that can be different degrees of its dredge
Outlet capacity is until lose hydrophobicity.
Found according to existing document, synthesized various super-hydrophobic coats are primarily present problems with present：First, lead to
Cross and preparing the super hydrophobic material of higher-strength with intrinsic hydrophobic material surface construction micro/nano structure, complex process,
Scope is relatively narrow, its working environment is greatly constrained with regard to this；Second, being obtained by sprayed coating film method for existing report is super thin
Water coating, although simple with equipment and technique, operates the advantages that simple and of low cost, weak, fragile there are intensity
The features such as, greatly limit its application range.Therefore, how simple in retaining device and technique, operation is simple and cost is low
On the basis of the advantages that honest and clean, strengthen the wearability of hydrophobic coating, be to realize that hydrophobic coating moves towards the key step of application from laboratory
Rapid and important channel.
The content of the invention
The purpose of the invention is to overcome above-mentioned super-hydrophobic coat intensity existing in the prior art it is low, it is fragile, application
The problem of condition harshness etc., there is provided a kind of high abrasion super hydrophobic composite coating and preparation method thereof, to obtain in hard/flexible subserate
The composite coating that the external force such as upper preparation can bear sand paper polishing, water washes away are destroyed.The technical equipment and technique are simple, operate letter
Easily, it is of low cost, it is easy to industrial-scale production.
The technical scheme is that：A kind of high abrasion super hydrophobic composite coating, including basalis, are equipped with the base layer
Thickness is 20~200 μm of priming paint, and surface covering finishing coat, thickness is the 10-50% of base coat thickness；The priming paint is hydrophobicity
Resin, micro powder granule, surfactant and resin curing agent are dispersed in semi-solid preparation in the solvent that mixes and form, the micro mist
Particle is polytetrafluoroethylene (PTFE), diamond, aluminium oxide, titanium oxide, silica or its fluorinated modified particle；The finishing coat is hydrophobic
Property nanometer silicon dioxide particle ethanol solution and hydrophobic polymer binding agent acetone soln in equal volume after mixing again plus
Enter isometric hydrophobicity sheet micro mist and bentonite mixed solution cures to obtain, the hydrophobicity sheet micro mist is silicon fluoride
Glass flake, oyster shell whiting, mica powder of the processed length at 50~800 μm, concentration 0.1-10mg/mL, the swelling
Native content is 1.2-2.5wt.%；The basalis includes soft or hard substrate.
The basalis includes any one in glass, copper, aluminium, stainless steel, exterior wall tile, timber, paper, cloth.
The hydrophobic resin is fluorocarbon resin, organic siliconresin or fluorinated modified polyurethane, fluorinated modified asphalt mixtures modified by epoxy resin
Any one in fat.
The solvent that mixes includes butyl acetate, acetone, toluene, dimethylformamide, hydrofluoroether.
The surfactant is the surfactant polyoxygenated ethylamine, lauryl sodium sulfate, Tween
20th, the one or more in Span 80 or fluorine carbon are used in mixed way.
The micro powder granule is to mix the weight such as the fine grained of the coarse granule of 100-500 mesh and 1500-2500 mesh
Even, additive amount accounts for the 0.1-0.6% of resin quality.
The hydrophobic polymer binding agent is PMMA (polymethyl methacrylate), PDMS (polydimethylsiloxanes
Alkane), the weight proportion such as one or both of PVDF (Kynoar) or POSS (caged silsesquioxane) polymer it is mixed
Compound, addition weight account for the 20-50% of silica dioxide granule.
The dewatering nano silica dioxide granule is aerosil, monodisperse silica or beading titanium dioxide
Any of silicon, concentration 1-20mg/mL.
The silicon fluoride end group is ethyoxyl, methoxyl group or chloro, concentration 0.01-0.1mg/mL.
The method for preparing the high abrasion super hydrophobic composite coating, comprises the following steps：
(1) priming paint is prepared and prepared：Hydrophobic resin is added into the solvent that mixes, in ultrasound and mechanical agitation compound condition
Under, it is dispersed to resin and is completely dissolved, obtain resin solution, then adds micro powder granule, surfactant and resin curing agent, after
Continuous composite stirring obtains finely dispersed hydridization priming paint suspension, after standing, gas removal, by brushing or spraying process is directly in base material
Surface forms uniform coating, and by brushing and spraying passage, adjustment coating layer thickness is 20-200 μm, cures and obtains semi-solid preparation bottom
Paint；
(2) finishing coat is prepared and prepared：Hydrophobic nano-silica particle is added into ethanol, ultrasonic disperse, by hydrophobicity
Polymeric binder adds acetone, and room temperature mechanical stirring, then isometric mixing nano particle and binder solution, continue to stir
Uniformly, the hydrophobicity sheet micro mist and bentonite mixed solution of isometric silicon fluoride processing are added, it is micro- to stir evenly acquisition
The finishing coat suspension of nano particle hydridization, it is super-hydrophobic compound to be sprayed at primed surface curing acquisition high abrasion after being finally ultrasonically treated
Coating.
Beneficial effect：
(1) addition of micro mist and compounded technology in priming paint, have been obviously improved the wearability of priming paint, while are provided for finishing coat
Rougher substrate, further enhancing the super-hydrophobicity and wearability of topcoat；
(2) surfactant is added in priming paint, and using ultrasound and mechanical agitation composite diffusion technology, improves hydridization bottom
Paint the dispersiveness and uniformity of suspension；
(3) polymeric binder is added in topcoat paint, topcoat paint itself bond strength can be significantly improved；
(4) hydrophobicity sheet micro mist is added in topcoat paint, by spraying air-flow, priming paint can be inserted vertically into, connect with the external world
When touching, can effectively protect nano particle, so as to improve the wearability of finishing coat；
(5) bentonite is added in topcoat paint, plays scattered and thickening power, avoid the sedimentation of sheet micro mist；
(6) silicon fluoride is added in topcoat paint, unmodified complete sheet micro mist and nano particle can be further fluorinated,
And fluorinated film is formed in substrate surface in spraying, this is all conducive to the super-hydrophobicity and wearability that improve coating；
(7) the high abrasion super hydrophobic composite coating wearability that prepared by the method for the present invention is good, 100kPa high pressure water impacts 1h,
After the sea sand of 1kg is washed away, film layer super-hydrophobicity is unchanged, and the finger of certain pressure scratches, sand paper polishing, can not destroy film layer
Ultra-hydrophobicity；
(8) coating is ageing-resistant and resistance to acid and alkali is good, and after natural environment is placed 1 year, film layer appearance, color become without obvious
Change, after various acid-base solutions soak 3 days, still with excellent super-hydrophobicity；
(9) the method for the present invention device therefor and technique are simple, and operation is simply and of low cost, and reaction condition is gentle, energy consumption
Small, cost is low, reproducible, is suitable for mass producing.
Brief description of the drawings：
Fig. 1 high abrasion super hydrophobic composite coating preparation flow figures.
The water contact angle and roll angle of composite coating in Fig. 2 substrate of glass.
The water contact angle and roll angle of high abrasion super hydrophobic composite coating in Fig. 3 metallic substrates.
The water contact angle and roll angle of high abrasion super hydrophobic composite coating in Fig. 4 construction material substrates.
The water contact angle and roll angle of high abrasion super hydrophobic composite coating on Fig. 5 flexible subserates.
Water contact angle of Fig. 6 high abrasions super hydrophobic composite coatings after the polishing of different number sand paper.
Water contact angle of Fig. 7 high abrasions super hydrophobic composite coatings after different pH value soaks different time.
Embodiment：
A kind of preparation method of high abrasion super hydrophobic composite coating, step are：
(1) priming paint is prepared and prepared：Hydrophobic resin is added into the solvent that mixes by a certain percentage, in ultrasound and 500-
Under 1500rpm mechanical agitation compound conditions, scattered 5-30min to resin is completely dissolved, and obtains resin solution, then addition is certain
Micro powder granule, surfactant and the resin curing agent of ratio compounding, continue composite stirring 5-30min, obtain finely dispersed
Hydridization priming paint suspension, after standing 3-10min degasification, by brushing or spraying technology, directly forms uniformly in substrate surface
Coating, by brushing and spraying passage, under the conditions of adjustment coating layer thickness is 20-200 μm, 30-80 DEG C, cures 1-48h, obtains institute
Semi-solid preparation priming paint is needed, according to resin properties, can also carry out room temperature or photocuring, the resin can be fluorocarbon resin, organosilicon
Resin or fluorinated modified polyurethane, fluorinated modified epoxy resin etc., the solvent that mixes include butyl acetate, acetone, toluene, dimethyl
The weight ratio 1 of formamide, hydrofluoroether etc., resin and solvent:1~3:1.The curing agent additive amount is 0.05 relative to resin
~20%, the curing agent includes N3390, TPA-100,593,703.The micro powder granule is polytetrafluoroethylene (PTFE), Buddha's warrior attendant
Stone, aluminium oxide, titanium oxide, silica or its fluorinated modified particle, compounding are by the coarse granule and 1500-2500 of 100-500 mesh
The weight such as purpose fine grained are uniformly mixed, and additive amount is 0.1-0.6% relative to resin, and the surfactant can use
Nonionic surfactant (such as polyoxygenated ethylamine) or anion surfactant (such as lauryl sodium sulfate) or
Tween 20, Span 80 or fluorocarbon surfactant, can be used in mixed way with two or more, and addition weight is relative to micro mist
Particle is 0.01-0.1%；
(2) finishing coat is prepared and prepared：Hydrophobic nano-silica particle is added into ethanol, ultrasonic disperse 5-60min will
Hydrophobic polymer binding agent adds acetone, and room temperature mechanical stirring 12h, then isometric mixing nano particle and binding agent are molten
Liquid, continues magnetic force or mechanical agitation 1h, adds hydrophobicity sheet micro mist and the bentonite mixing of isometric silicon fluoride processing
Solution, magnetic force or mechanical agitation 24h, obtain the finishing coat suspension of micro-nano granules hydridization, and the hydrophobic nanoparticles can be with
It is aerosil, monodisperse silica or beading silica, concentration 1-20mg/mL, the polymer glues
Knot agent can be the mixture of the weight proportions such as one or two kinds of polymer of PMMA, PDMS, PVDF or POSS etc., add weight
20-50% relative to silica dioxide granule, the sheet micro mist be length 50-800 μm of glass flake, oyster shell whiting,
Mica powder etc., concentration 0.1-10mg/mL, the bentonite concentration are 1.2-2.5%, and the end group of the silicon fluoride can be
Ethyoxyl, methoxyl group, isopropyl or chloro, concentration 0.01-0.1mg/mL, are finally ultrasonically treated 10-30min, are sprayed at bottom
Surface is painted, then under 20-80 DEG C or ultraviolet light, cures 1-48h, you can obtains high abrasion super hydrophobic composite coating.
Embodiment 1
By fluorocarbon resin by weight 3:1 adds in butyl acetate solvent, compound under ultrasound and 500rpm mechanical agitations
Scattered 5min is completely dissolved to resin, by the weight ratio relative to resin, adds 100 mesh and 1500 that the quality such as 0.1% compounds
Mesh polytetrafluoroethylene (PTFE) and 0.05% curing agent, then add weight relative to micro powder granule be 0.01% polyoxygenated ethylamine, after
Continuous composite stirring 5min, obtains finely dispersed hydridization priming paint suspension, and after standing 3min degasification, 20 μ m-thick coatings of spraying are in glass
Glass substrate surface, after curing 48h under the conditions of 30 DEG C, priming paint needed for acquisition.
Hydrophobic nano-silica particle is added into ethanol, ultrasonic disperse 5min, prepares 1mg/mL suspension, then will be poly-
Vinylidene (PVDF) dissolves in acetone, and room temperature mechanical stirring 12h, obtains 0.4mg/mL solution, after isometric mixing, continue machinery
1h is stirred, adds 50 μm of long glass flakes, bentonite suspensions of isometric methoxyl group silicon fluoride immersion 24h, silicon fluoride
Concentration is 0.01mg/mL, and glass flake concentration is 0.1mg/mL, and bentonite concentration is 1.2%, finally continues to surpass by mixed solution
Sound 10min, then be sprayed at primed surface, you can obtain it is wear-resisting it is super-hydrophobic meet coating, its water contact angle is 157.2 °, roll angle
For 2.7 ° (Fig. 2).
Embodiment 2
By hydrophobic silicones resin 2:1 adds in acetone solvent, the composite diffusion under ultrasound and 1000rpm mechanical agitations
20min is completely dissolved to resin, adds 250 mesh and 2000 mesh diamonds, 0.05% dodecyl sulphur of the compounding of the quality such as 0.3%
Sour sodium and 10% curing agent, continue composite stirring 20min, obtain finely dispersed hydridization priming paint suspension, stand 5min degasification
Afterwards, 10 μ m-thick coatings are brushed to place in metal (copper, aluminium, stainless steel) substrate surface, air after 4min again by the thin of 10mg/mL
Water-based nano silicon dioxide particle spray coating obtains wear-resisting super-hydrophobic compound painting in primed surface after baking-curing 24h at 50 DEG C
Layer, its water contact angle are 158.5 °, and roll angle is 5.4 ° (Fig. 3).
Embodiment 3
By fluorinated modified epoxy resin 1:1 adds in toluene solvant, the composite diffusion under ultrasound and 1500rpm mechanical agitations
30min is completely dissolved to resin, adds 500 mesh and 2500 mesh aluminium oxide, 0.1% polyoxyethylene of the quality such as 0.6wt.% compounding
Base amine and 20% curing agent, continue composite stirring 30min, obtain finely dispersed hydridization priming paint suspension, stand 10min degasification
Afterwards, 20 μ m-thick coatings are brushed to place in construction material (exterior wall tile, plank) substrate surface, air after 5min again by 20mg/mL
Hydrophobic nano-silica particle spray coating in primed surface, obtained after baking-curing 48h at 80 DEG C wear-resisting super-hydrophobic multiple
Coating is closed, its water contact angle is 158.0 °, and roll angle is 4.7 ° (Fig. 4).
Embodiment 4
By hydrophobicity fluorocarbon resin 3:1 adds in butyl acetate solvent, compound point under ultrasound and 1000rpm mechanical agitations
10min is dissipated to be completely dissolved to resin, 250 mesh and 2500 mesh polytetrafluoroethylene (PTFE) of the addition compounding of the quality such as 0.3%, 0.05% it is non-from
Sub- surfactant and 10% curing agent, continue composite stirring 10min, obtain finely dispersed hydridization priming paint suspension.In order to
The water contact angle and roll angle on flexible subserate are measured, is in advance distinguished untapped, clean filter paper and cloth with a kind of double faced adhesive tape
Bonding is on the glass sheet.After above-mentioned hydridization priming paint suspension is stood 10min degasification, 1 μ m-thick coating of spraying is in flexible subserate (filter
Paper, cloth) surface, place in air after 5min again by the hydrophobic nano-silica particle spray coating of 10mg/mL in primed surface,
High abrasion super hydrophobic composite coating is obtained after 40 DEG C are toasted 24h, its water contact angle is respectively 157.4 °, and roll angle is 4.0 °
(Fig. 5).
Embodiment 5
Wearability of the glass as substrate characterization high abrasion super hydrophobic composite coating is selected, in the preparation of substrate of glass on piece
The high abrasion super hydrophobic composite coating of embodiment 4 is stated, then is put on 240 mesh sand paper, under 100g pressure, using 10cm as row
Footpath distance, polishes for a cycle twice in length and breadth, wherein 5 replacements, one sand paper of often polishing.Fig. 6 is its difference polishing time
Water contact angle after number, the results showed that after sand paper polishes 70 cycles, it still possesses ultra-hydrophobicity.
Embodiment 6
Resistance to acid and alkali of the glass as substrate characterization high abrasion super hydrophobic composite coating is selected, is prepared in substrate of glass on piece
The high abrasion super hydrophobic composite coating of above-described embodiment 4, then it is respectively to be soaked in 4,7,10 solution to be put in pH value.Fig. 7
For the water contact angle after its different soaking time, the results showed that after different pH value is soaked 3 days, it still possesses super-hydrophobic
Performance.
Claims (10)
1. a kind of high abrasion super hydrophobic composite coating, including basalis, it is characterised in that on the base layer equipped with thickness for 20 ~
200 μm of priming paint, surface covering finishing coat, thickness is the 10-50 % of base coat thickness；The priming paint is hydrophobic resin, micro mist
Particle, surfactant and resin curing agent are dispersed in semi-solid preparation in the solvent that mixes and form, and the micro powder granule is poly-
Tetrafluoroethene, diamond, aluminium oxide, titanium oxide, silica or its fluorinated modified particle；The finishing coat is hydrophobic nano two
The ethanol solution and hydrophobic polymer binding agent acetone soln of silicon oxide particle add in equal volume after mixing in equal volume
Hydrophobicity sheet micro mist and bentonite mixed solution cure to obtain, the hydrophobicity sheet micro mist is that silicon fluoride is processed
Glass flake, oyster shell whiting, mica powder of the length at 50 ~ 800 μm, concentration are 0.1-10 mg/mL, and the bentonite content is
1.2-2.5 wt.%；The basalis includes soft or hard substrate.
2. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the basalis include glass,
Any one in copper, aluminium, stainless steel, exterior wall tile, timber, paper, cloth.
3. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the hydrophobic resin is fluorine carbon
Any one in resin, organic siliconresin or fluorinated modified polyurethane, fluorinated modified epoxy resin.
4. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the solvent that mixes includes acetic acid
Butyl ester, acetone, toluene, dimethylformamide, hydrofluoroether.
5. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the surfactant is polyoxy
The one or more changed in ethylamine, lauryl sodium sulfate, Tween 20, Span 80 or fluorine carbon are used in mixed way.
6. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the micro powder granule is by 100-
The weight such as the coarse granule of 500 mesh and the fine grained of 1500-2500 mesh is uniformly mixed, and additive amount accounts for the 0.1-0.6 % of resin quality.
7. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the hydrophobic polymer bonds
Agent is the mixture of the weight proportions such as one or both of PMMA, PDMS, PVDF or POSS polymer, and addition weight accounts for dioxy
The 20-50 % of silicon carbide particle.
8. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the dewatering nano silica
Particle is any of aerosil, monodisperse silica or beading silica, and concentration is 1-20 mg/mL.
9. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterised in that the silicon fluoride end group is ethoxy
Base, methoxyl group or chloro, concentration are 0.01-0.1 mg/mL.
10. prepare the method for any high abrasion super hydrophobic composite coating of claim 1 ~ 9, it is characterised in that including under
Row step：
（1）Priming paint is prepared and prepared：Hydrophobic resin is added into the solvent that mixes, under ultrasound and mechanical agitation compound condition, point
It is dissipated to resin to be completely dissolved, obtains resin solution, then add micro powder granule, surfactant and resin curing agent, continues multiple
The finely dispersed hydridization priming paint suspension of stirring to obtain is closed, after standing, gas removal, by brushing or spraying process is directly in substrate surface
Uniform coating is formed, by brushing and spraying passage, adjustment coating layer thickness is 20-200 μm, cures and obtains semi-solid preparation priming paint；
（2）Finishing coat is prepared and prepared：Hydrophobic nano-silica particle is added into ethanol, ultrasonic disperse, by hydrophobic polymerizable
Thing binding agent adds acetone, and room temperature mechanical stirring, then isometric mixing nano particle and binder solution, it is equal to continue stirring
It is even, the hydrophobicity sheet micro mist and bentonite mixed solution of isometric silicon fluoride processing are added, stirs evenly acquisition micro-nano
The finishing coat suspension of rice grain hydridization, is sprayed at primed surface and cures the acquisition super-hydrophobic compound painting of high abrasion after being finally ultrasonically treated
Layer.
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| JP2012020248A (en) * | 2010-07-15 | 2012-02-02 | Nicca Chemical Co Ltd | Water repellent coating film, method for manufacturing this film and functional material with water repellent coating film |
| JP6213320B2 (en) * | 2014-03-17 | 2017-10-18 | 三菱電機株式会社 | Outdoor blower |
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