CN105419450A - Highly-wear-resistant super-hydrophobic composite coating and preparation method thereof - Google Patents
Highly-wear-resistant super-hydrophobic composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a highly-wear-resistant super-hydrophobic composite coating and a preparation method thereof. The preparation method includes the steps that the surface of a base is coated with hydrophobic resin primer containing compound micropowder through a brush coating or spray coating method, the surface of the resin primer is sprayed with hydrophobic organic/inorganic hybrid nano-paint after semi-curing, and the highly-wear-resistant super-hydrophobic composite coating is obtained after complete curing. The highly-wear-resistant super-hydrophobic composite coating and the preparation method thereof have the advantages that equipment and the process are simple, operation is easy and cost is low, and have the industrial mass production prospect. The prepared super-hydrophobic composite coating can be applied to various hard/soft bases such as glass, copper, aluminum, stainless steel, exterior wall tiles, wood, paper and cloth and can bear damage of external force such as sanding.
Description
Technical field
The invention belongs to coating preparation field, particularly a kind of high abrasion super hydrophobic composite coating and preparation method thereof.
Background technology
The function such as self-cleaning, drag reduction, waterproof that the distinctive super infiltration feature of super hydrophobic surface makes super hydrophobic material have, antifog, anti-ice, heat transfer, the micro-/ nano coarse structures such as bionical lotus leaf surface, water skipper leg, insect wing prepare the focus that super hydrophobic material becomes current thin-film material preparation research, all have broad application prospects in fields such as aviation, navigation, the energy, building, electronics, anticorrosion, sensor, heat transfers.Super-hydrophobic characteristic is jointly determined by the hydrophobicity of material and roughness, and low surface free energy and suitable roughness prepare the indispensable factor of two of super hydrophobic surface.
At present, the technology of preparing of super hydrophobic surface comprises top-down wet etching, reactive ion etching, impression, mechanical workout, laser ablation etc., also comprises chemical oxidation from bottom to top, electrochemical oxidation, electrochemical deposition, sol-gel, Hydrothermal Synthesis, spraying etc.But the super-hydrophobic coat/film prepared by these technology, except needing expensive plant and instrument and harsh processing condition, is difficult to carry out large-scale industrial production, all there is comparatively easily destroyed risk.As [Science such as Deng, 2012,335:67] report and be attached to substrate surface by vapour deposition process candle ash, after heat treatment obtain super-hydrophobic/super oleophobic films again, although the film obtained by the method can have certain intensity (sand washing), but still there is no the destructive force level that can reach in practical application, and the method complex process, be difficult to realize industrial applications.
By sprayed coating film method the super-hydrophobic spray coating liquor of preparation uniformly sprayed that to form super-hydrophobic coat in substrate be a kind of at present comparatively common method.Ge etc. [Part.Part.Syst.Charact.2014,31:763] report super-hydrophobic/super oleophobic SiO by sprayed coating film method
2nanoparticle is sprayed at the substrates such as polyester, resin, aluminium foil, cotton, obtains super-hydrophobic/super oleophobic coating on its surface, but this coating to be washed away or after the outside destroy such as sand washing at water, all can its hydrophobic ability of reduction in various degree until lose hydrophobicity.
Find according to existing document, mainly there is following problem in various super-hydrophobic coats synthesized at present: first, by preparing the super hydrophobic material of higher-strength in the material surface structure micro/nano structure that there is intrinsic hydrophobic, complex process, scope is narrower, greatly retrains with regard to this its Working environment; The second, the super-hydrophobic coat obtained by sprayed coating film method of existing report, although it is simple to have instrument and supplies, operates the advantages such as simple and easy and with low cost, all there is the features such as intensity is weak, fragile, limits its range of application greatly.Therefore, how retaining device and technique simple, operate on the basis of the advantage such as simple and easy and with low cost, strengthening the wear resistance of hydrophobic coating, is realize hydrophobic coating moves towards application committed step and important channel from laboratory.
Summary of the invention
The object of the invention is the problem that super-hydrophobic coat intensity is low, fragile, application conditions is harsh etc. existed to overcome above-mentioned prior art, provide a kind of high abrasion super hydrophobic composite coating and preparation method thereof, to obtain the compound coating of the outside destroy such as preparation can bear sand papering, water washes away on hard/flexible subserate.This technical equipment and technique is simple, it is simple and easy, with low cost to operate, and is easy to commercial scale production.
Technical scheme of the present invention is: a kind of high abrasion super hydrophobic composite coating, comprises stratum basale, is provided with the priming paint that thickness is 20 ~ 200 μm on the base layer, surface coverage finish paint, and thickness is the 10-50% of base coat thickness; Described priming paint is hydrophobic resin, micro powder granule, tensio-active agent and resin curing agent are dispersed in semicure in the solvent that mixes and form, and described micro powder granule is tetrafluoroethylene, diamond, aluminum oxide, titanium oxide, silicon oxide or its fluorinated modified particle; Described finish paint adds isopyknic hydrophobicity sheet micro mist again after the ethanolic soln of hydrophobic nano-silica particle and hydrophobic polymer binding agent acetone soln equal-volume mix and the solidification of wilkinite mixing solutions obtains, described hydrophobicity sheet micro mist is that the length of silicon fluoride process is at glass flake, oyster shell whiting, the mica powder of 50 ~ 800 μm, concentration is 0.1-10mg/mL, and described bentonite content is 1.2-2.5wt.%; Described stratum basale comprises soft or hard substrate.
Described stratum basale comprise in glass, copper, aluminium, stainless steel, exterior wall tile, timber, paper, cloth any one.
Described hydrophobic resin is any one in fluorocarbon resin, silicone resin or fluorinated modified urethane, fluorinated modified epoxy resin.
The described solvent that mixes comprises butylacetate, acetone, toluene, dimethyl formamide, hydrogen fluorine ether.
Described tensio-active agent is that one or more in described tensio-active agent polyoxygenated ethylamine, sodium lauryl sulphate, Tween20, Span80 or fluorine carbon are used in combination.
Described micro powder granule is mixed the weight such as 100-500 object coarse particles and 1500-2500 object fine particle, and addition accounts for the 0.1-0.6% of resin quality.
Described hydrophobic polymer binding agent is the mixture of the weight proportions such as one or both polymkeric substance in PMMA (polymethylmethacrylate), PDMS (polydimethylsiloxane), PVDF (polyvinylidene difluoride (PVDF)) or POSS (caged silsesquioxane), adds the 20-50% that weight accounts for silica dioxide granule.
Described dewatering nano silica dioxide granule is any one in aerosil, monodisperse silica or beading silicon-dioxide, and concentration is 1-20mg/mL.
Described silicon fluoride end group is oxyethyl group, methoxyl group or chloro, and concentration is 0.01-0.1mg/mL.
The method of the high abrasion super hydrophobic composite coating described in preparation, comprises the following steps:
(1) priming paint preparation and preparation: hydrophobic resin is added the solvent that mixes, ultrasonic with under mechanical stirring compound condition, be dispersed to resin to dissolve completely, obtain resin solution, add micro powder granule, tensio-active agent and resin curing agent subsequently, continue composite stirring and obtain finely dispersed hydridization priming paint suspension, after standing, gas removal, directly uniform coating is formed at substrate surface by brushing or spraying method, by brushing and spraying passage, adjustment coat-thickness is 20-200 μm, and solidification obtains semicure priming paint;
(2) finish paint preparation and preparation: hydrophobic nano-silica particle is added ethanol, ultrasonic disperse, hydrophobic polymer binding agent is added acetone, room temperature mechanical stirs, the nano particle of equal-volume mixing subsequently and binder solution, continue to stir, add hydrophobicity sheet micro mist and the wilkinite mixing solutions of isopyknic silicon fluoride process again, stir and obtain the finish paint suspension of micro-nano granules hydridization, be sprayed at primed surface solidification after last supersound process and obtain high abrasion super hydrophobic composite coating.
Beneficial effect:
(1) interpolation of micro mist and compounded technology in priming paint, significantly improve the wear resistance of priming paint, simultaneously for finish paint provides more coarse substrate, further enhancing super-hydrophobicity and the wear resistance of topcoat;
(2) add tensio-active agent in priming paint, and use ultrasonic and mechanical stirring composite diffusion technology, improve dispersiveness and the homogeneity of hydridization priming paint suspension;
(3) add polymeric binder in topcoat paint, topcoat paint self bonding strength can be significantly improved;
(4) add hydrophobicity sheet micro mist in topcoat paint, by spraying air-flow, vertically can insert priming paint, during with extraneous contact, can available protecting nano particle, thus improve the wear resistance of finish paint;
(5) add wilkinite in topcoat paint, play dispersion and thickening power, avoid the sedimentation of sheet micro mist;
(6) add silicon fluoride in topcoat paint, can fluoridize further the unmodified micro mist of sheet completely and nano particle, and form fluorinated film when spraying at substrate surface, this is all conducive to the super-hydrophobicity and the wear resistance that improve coating;
(7) the high abrasion super hydrophobic composite coating wear resistance prepared of the inventive method is good, after the extra large sand of 100kPa high pressure water impact 1h, 1kg washes away, rete super-hydrophobicity is unchanged, and the finger of certain pressure scratches, sand papering, can not destroy the ultra-hydrophobicity of rete;
(8) coating is ageing-resistant good with resistance to acids and bases, and after physical environment places 1 year, rete outward appearance, color have no significant change, and after various acid-base solution soaks 3 days, still has excellent super-hydrophobicity;
(9) the inventive method equipment used and technique simply, operate simple and easy and with low cost, and reaction conditions is gentle, and energy consumption is little, and cost is low, reproducible, is suitable for scale operation.
Accompanying drawing illustrates:
Fig. 1. high abrasion super hydrophobic composite coating preparation flow figure.
Fig. 2. the water contact angle of compound coating and roll angle in substrate of glass.
Fig. 3. the water contact angle of high abrasion super hydrophobic composite coating and roll angle in metal base.
Fig. 4. the water contact angle of high abrasion super hydrophobic composite coating and roll angle in material of construction substrate.
Fig. 5. the water contact angle of high abrasion super hydrophobic composite coating and roll angle on flexible subserate.
Fig. 6. the water contact angle of high abrasion super hydrophobic composite coating after different number of times sand papering.
Fig. 7. high abrasion super hydrophobic composite coating soaks the water contact angle after different time through different pH value.
Embodiment:
A preparation method for high abrasion super hydrophobic composite coating, step is:
(1) priming paint preparation and preparation: hydrophobic resin is added the solvent that mixes by a certain percentage, ultrasonic with under 500-1500rpm mechanical stirring compound condition, dispersion 5-30min dissolves completely to resin, obtain resin solution, add the composite micro powder granule of certain proportion subsequently, tensio-active agent and resin curing agent, continue composite stirring 5-30min, obtain finely dispersed hydridization priming paint suspension, after leaving standstill 3-10min degasification, by brushing or spraying technology, directly form uniform coating at substrate surface, by brushing and spraying passage, adjustment coat-thickness is 20-200 μm, under 30-80 DEG C of condition, solidification 1-48h, obtain required semicure priming paint, according to resin properties, also normal temperature or photocuring can be carried out, described resin can be fluorocarbon resin, silicone resin or fluorinated modified urethane, fluorinated modified epoxy resin etc., the solvent that mixes comprises butylacetate, acetone, toluene, dimethyl formamide, hydrogen fluorine ether etc., weight ratio 1:1 ~ the 3:1 of resin and solvent.Described solidifying agent addition is 0.05 ~ 20% relative to resin, and described solidifying agent comprises N3390, TPA-100,593,703.Described micro powder granule is tetrafluoroethylene, diamond, aluminum oxide, titanium oxide, silicon oxide or its fluorinated modified particle, composite is the weight such as 100-500 object coarse particles and 1500-2500 object fine particle mixed, addition is 0.1-0.6% relative to resin, described tensio-active agent can use nonionogenic tenside (as polyoxygenated ethylamine) or anion surfactant (as sodium lauryl sulphate), also can be Tween20, Span80 or fluorocarbon surfactant, can also two or more be used in combination, adding weight is 0.01-0.1% relative to micro powder granule,
(2) finish paint preparation and preparation: hydrophobic nano-silica particle is added ethanol, ultrasonic disperse 5-60min, hydrophobic polymer binding agent is added acetone, room temperature mechanical stirs 12h, the nano particle of equal-volume mixing subsequently and binder solution, continue magnetic force or mechanical stirring 1h, add hydrophobicity sheet micro mist and the wilkinite mixing solutions of isopyknic silicon fluoride process again, magnetic force or mechanical stirring 24h, obtain the finish paint suspension of micro-nano granules hydridization, described hydrophobic nanoparticles can be aerosil, monodisperse silica or beading silicon-dioxide, concentration is 1-20mg/mL, described polymeric binder can be PMMA, PDMS, the mixture of the weight proportions such as one or both polymkeric substance of PVDF or POSS etc., adding weight is 20-50% relative to silica dioxide granule, described sheet micro mist is length at the glass flake of 50-800 μm, oyster shell whiting, mica powder etc., concentration is 0.1-10mg/mL, described wilkinite concentration is 1.2-2.5%, the end group of described silicon fluoride can be oxyethyl group, methoxyl group, sec.-propyl or chloro, concentration is 0.01-0.1mg/mL, last supersound process 10-30min, be sprayed at primed surface, again under 20-80 DEG C or UV-irradiation, solidification 1-48h, high abrasion super hydrophobic composite coating can be obtained.
Embodiment 1
Fluorocarbon resin is added in butyl acetate solvent by weight 3:1, dissolve completely to resin with composite diffusion 5min under 500rpm mechanical stirring ultrasonic, by the weight ratio relative to resin, add 100 composite orders of the quality such as 0.1% and 1500 order tetrafluoroethylene and 0.05% solidifying agent, add the polyoxygenated ethylamine that weight relative to micro powder granule is 0.01% again, continue composite stirring 5min, obtain finely dispersed hydridization priming paint suspension, after leaving standstill 3min degasification, spray 20 μm of thick coatings in glass basic surface, after solidifying 48h under 30 DEG C of conditions, obtain required priming paint.
Hydrophobic nano-silica particle is added ethanol, ultrasonic disperse 5min, preparation 1mg/mL suspension, again polyvinylidene difluoride (PVDF) (PVDF) is dissolved in acetone, room temperature mechanical stirs 12h, obtain 0.4mg/mL solution, after equal-volume mixing, continue mechanical stirring 1h, add 50 μm of long glass flakes that isopyknic methoxyl group silicon fluoride soaks 24h again, bentonite suspension, silicon fluoride concentration is 0.01mg/mL, glass flake concentration is 0.1mg/mL, wilkinite concentration is 1.2%, finally mixing solutions is continued ultrasonic 10min, be sprayed at primed surface again, can obtain and wear-resistingly super-hydrophobicly meet coating, its water contact angle is 157.2 °, roll angle is 2.7 ° (Fig. 2).
Embodiment 2
Hydrophobic silicones resin 2:1 is added in acetone solvent, dissolve completely to resin with composite diffusion 20min under 1000rpm mechanical stirring ultrasonic, 250 orders that the quality such as interpolation 0.3% are composite and 2000 order diamonds, 0.05% sodium lauryl sulphate and 10% solidifying agent, continue composite stirring 20min, obtain finely dispersed hydridization priming paint suspension, after leaving standstill 5min degasification, brush 10 μm of thick coatings in metal (copper, aluminium, stainless steel) substrate surface, to place in air after 4min again by the hydrophobic nano-silica particle spray coating of 10mg/mL in primed surface, wear-resisting super hydrophobic composite coating is obtained after baking-curing 24h at 50 DEG C, its water contact angle is 158.5 °, roll angle is 5.4 ° (Fig. 3).
Embodiment 3
Fluorinated modified epoxy resin 1:1 is added in toluene solvant, dissolve completely to resin with composite diffusion 30min under 1500rpm mechanical stirring ultrasonic, add 500 composite orders of the quality such as 0.6wt.% and 2500 order aluminum oxide, 0.1% polyoxygenated ethylamine and 20% solidifying agent, continue composite stirring 30min, obtain finely dispersed hydridization priming paint suspension, after leaving standstill 10min degasification, brush 20 μm of thick coatings in material of construction (exterior wall tile, plank) substrate surface, to place in air after 5min again by the hydrophobic nano-silica particle spray coating of 20mg/mL in primed surface, wear-resisting super hydrophobic composite coating is obtained after baking-curing 48h at 80 DEG C, its water contact angle is 158.0 °, roll angle is 4.7 ° (Fig. 4).
Embodiment 4
Hydrophobicity fluorocarbon resin 3:1 is added in butyl acetate solvent, dissolve completely to resin with composite diffusion 10min under 1000rpm mechanical stirring ultrasonic, 250 orders that the quality such as interpolation 0.3% are composite and 2500 order tetrafluoroethylene, 0.05% nonionogenic tenside and 10% solidifying agent, continue composite stirring 10min, obtain finely dispersed hydridization priming paint suspension.In order to measure water contact angle on flexible subserate and roll angle, in advance with a kind of double faced adhesive tape by untapped, clean filter paper and cloth on the glass sheet bonding respectively.After above-mentioned hydridization priming paint suspension is left standstill 10min degasification, spray 1 μm of thick coating in flexible subserate (filter paper, cloth) surface, to 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 of baking 24h, its water contact angle is respectively 157.4 °, and roll angle is 4.0 ° (Fig. 5).
Embodiment 5
Glass is selected to characterize the wear resistance of high abrasion super hydrophobic composite coating as substrate, glass-based egative film is prepared the high abrasion super hydrophobic composite coating of above-described embodiment 4, be put on 240 order sand paper again, under 100g pressure, take 10cm as conduct distance, polish for one-period for twice in length and breadth, wherein often polish and change a sand paper 5 times.Fig. 6 is the water contact angle after its different polishing number of times, and result shows that it still possesses ultra-hydrophobicity through sand papering 70 all after dates.
Embodiment 6
Select glass to characterize the resistance to acids and bases of high abrasion super hydrophobic composite coating as substrate, glass-based egative film is prepared the high abrasion super hydrophobic composite coating of above-described embodiment 4, then be put in pH value and be respectively in the solution of 4,7,10 and soak.Fig. 7 is the water contact angle after its different soak time, and result shows that it still possesses ultra-hydrophobicity after different pH value soaks 3 days.
Claims (10)
1. a high abrasion super hydrophobic composite coating, comprises stratum basale, it is characterized in that, is provided with the priming paint that thickness is 20 ~ 200 μm on the base layer, surface coverage finish paint, and thickness is the 10-50% of base coat thickness; Described priming paint is hydrophobic resin, micro powder granule, tensio-active agent and resin curing agent are dispersed in semicure in the solvent that mixes and form, and described micro powder granule is tetrafluoroethylene, diamond, aluminum oxide, titanium oxide, silicon oxide or its fluorinated modified particle; Described finish paint adds isopyknic hydrophobicity sheet micro mist again after the ethanolic soln of hydrophobic nano-silica particle and hydrophobic polymer binding agent acetone soln equal-volume mix and the solidification of wilkinite mixing solutions obtains, described hydrophobicity sheet micro mist is that the length of silicon fluoride process is at glass flake, oyster shell whiting, the mica powder of 50 ~ 800 μm, concentration is 0.1-10mg/mL, and described bentonite content is 1.2-2.5wt.%; Described stratum basale comprises soft or hard substrate.
2. high abrasion super hydrophobic composite coating as claimed in claim 1, is characterized in that, described stratum basale comprise in glass, copper, aluminium, stainless steel, exterior wall tile, timber, paper, cloth any one.
3. high abrasion super hydrophobic composite coating as claimed in claim 1, is characterized in that, described hydrophobic resin is any one in fluorocarbon resin, silicone resin or fluorinated modified urethane, fluorinated modified epoxy resin.
4. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, the described solvent that mixes comprises butylacetate, acetone, toluene, dimethyl formamide, hydrogen fluorine ether.
5. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, described tensio-active agent is that one or more in described tensio-active agent polyoxygenated ethylamine, sodium lauryl sulphate, Tween20, Span80 or fluorine carbon are used in combination.
6. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, described micro powder granule is mixed the weight such as 100-500 object coarse particles and 1500-2500 object fine particle, and addition accounts for the 0.1-0.6% of resin quality.
7. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, described hydrophobic polymer binding agent is the mixture of the weight proportions such as one or both polymkeric substance in PMMA, PDMS, PVDF or POSS, adds the 20-50% that weight accounts for silica dioxide granule.
8. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, described dewatering nano silica dioxide granule is any one in aerosil, monodisperse silica or beading silicon-dioxide, and concentration is 1-20mg/mL.
9. high abrasion super hydrophobic composite coating as claimed in claim 1, it is characterized in that, described silicon fluoride end group is oxyethyl group, methoxyl group or chloro, and concentration is 0.01-0.1mg/mL.
10. prepare the method for the arbitrary described high abrasion super hydrophobic composite coating of claim 1 ~ 9, it is characterized in that, comprise the following steps:
(1) priming paint preparation and preparation: hydrophobic resin is added the solvent that mixes, ultrasonic with under mechanical stirring compound condition, be dispersed to resin to dissolve completely, obtain resin solution, add micro powder granule, tensio-active agent and resin curing agent subsequently, continue composite stirring and obtain finely dispersed hydridization priming paint suspension, after standing, gas removal, directly uniform coating is formed at substrate surface by brushing or spraying method, by brushing and spraying passage, adjustment coat-thickness is 20-200 μm, and solidification obtains semicure priming paint;
(2) finish paint preparation and preparation: hydrophobic nano-silica particle is added ethanol, ultrasonic disperse, hydrophobic polymer binding agent is added acetone, room temperature mechanical stirs, the nano particle of equal-volume mixing subsequently and binder solution, continue to stir, add hydrophobicity sheet micro mist and the wilkinite mixing solutions of isopyknic silicon fluoride process again, stir and obtain the finish paint suspension of micro-nano granules hydridization, be sprayed at primed surface solidification after last supersound process and obtain high abrasion super hydrophobic composite coating.
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| CN117160824A (en) * | 2023-11-02 | 2023-12-05 | 中国科学院宁波材料技术与工程研究所 | Composite elastic drag reduction coating with multilayer structure, and preparation method and application thereof |
| CN117160824B (en) * | 2023-11-02 | 2024-02-23 | 中国科学院宁波材料技术与工程研究所 | Composite elastic drag reduction coating with multilayer structure, and preparation method and application thereof |
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