CN111073443A - Super-amphiphobic coating and preparation method and application thereof - Google Patents
Super-amphiphobic coating and preparation method and application thereof Download PDFInfo
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- CN111073443A CN111073443A CN201811220728.XA CN201811220728A CN111073443A CN 111073443 A CN111073443 A CN 111073443A CN 201811220728 A CN201811220728 A CN 201811220728A CN 111073443 A CN111073443 A CN 111073443A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention provides a super-amphiphobic coating and a preparation method and application thereof, wherein the super-amphiphobic coating comprises a substrate resin layer; a coupling agent layer located over the base resin layer; and a particle layer located over the coupling agent layer. The super-amphiphobic coating prepared by the method has the advantages that the water contact angle and the hexadecane contact angle of the surface of the super-amphiphobic coating are both larger than 150 degrees, the rolling angles are both smaller than 3 degrees, the light transmittance is both larger than 92 percent, and the super-amphiphobic coating has good hydrophobic and oleophobic effects and simultaneously has good transmittance to visible light.
Description
Technical Field
The invention relates to a super-amphiphobic coating and a preparation method thereof, in particular to a super-amphiphobic coating with a water contact angle and an oil contact angle both larger than 150 degrees and a preparation method thereof.
Background
The existing super-hydrophobic coating can only realize super-hydrophobicity on water and has no oleophobic performance, which greatly limits the application scene of the coating. Since the components in the air contain a large amount of oil under natural use conditions, and adhere to the surface of the coating layer to cause the coating layer to fail, it is highly desirable to develop a superhydrophobic coating layer that is both hydrophobic and oleophobic. Moreover, in the methods for preparing the hydrophobic coating disclosed in the prior art, the average visible light transmittance is up to 75% at the highest, which is reduced by up to 25%, and the transparency of the substrate such as glass is affected, so the visible light transmittance of the hydrophobic coating needs to be improved.
Disclosure of Invention
Aiming at the problems, the invention provides the super-amphiphobic coating which is good in hydrophobic and oleophobic properties, high in transmittance and good in stability.
The invention provides a amphiphobic coating, which comprises the following components: a base resin layer; a coupling agent layer located over the base resin layer; and a particle layer located over the coupling agent layer.
In the aforementioned amphiphobic coating, the amphiphobic coating is a super-amphiphobic coating having both a water contact angle and an oil contact angle of greater than 150 °.
In the aforementioned amphiphobic coating, the base resin includes one or more of a silicone resin, an epoxy resin, a silicone-modified epoxy resin, and an acrylic resin.
In the aforementioned amphiphobic coating, the coupling agent comprises a silane coupling agent comprising one or more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane.
In the aforementioned amphiphobic coating, the particles comprise hydrophobic silica.
The invention also provides a method for preparing the amphiphobic coating, which is characterized by comprising the following steps:
adding a base resin and a curing agent into a first solvent to obtain a base resin solution;
adding a coupling agent into a second solvent to obtain a coupling agent solution;
adding the particles into a third solvent to obtain a particle solution; and
and sequentially coating the substrate resin solution, the coupling agent solution and the particle solution on a substrate to obtain the amphiphobic coating.
In the above method, the amphiphobic coating is a super-amphiphobic coating having both a water contact angle and an oil contact angle of greater than 150 °.
In the above method, the base resin comprises one or more of a silicone resin, an epoxy resin, a silicone-modified epoxy resin, and an acrylic resin; the curing agent comprises one or more of ethylenediamine, diethylenetriamine and m-phenylenediamine; and the first solvent comprises one or both of ethyl acetate and acetone.
In the above method, the coupling agent comprises a silane coupling agent comprising one or more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, and gamma- (methacryloyloxy) propyltrimethoxysilane; and the second solvent comprises one or more of ethanol, methanol, and isopropanol.
In the above method, the particles comprise hydrophobic silica; and the third solvent comprises one or more of ethanol, methanol, and isopropanol.
In the above method, the concentration of the base resin in the base resin solution is 10g/L to 30 g/L; the concentration of the coupling agent in the coupling agent solution is 10 g/L-30 g/L; and the concentration of the particles in the particle solution is 3g/L to 10 g/L.
In the above method, after the particles are added to the third solvent, the fluorosilane is added.
The invention also provides the application of the amphiphobic coating prepared by the method on a surface device.
According to the invention, by adopting the hydrophobic silicon oxide and combining the hydrophobic silicon oxide with the substrate resin and the coupling agent, the prepared super-amphiphobic coating can be hydrophobic and oleophobic, has high transmittance and good stability, can keep the surface free from dust for a long time, and greatly increases the practicability.
Drawings
FIG. 1 is a schematic view of a super-amphiphobic coating, wherein 1-substrate, 2-substrate resin layer, 3-coupling agent layer, 4-particle layer.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The application provides a super-amphiphobic coating with both water contact angle and oil contact angle larger than 150 degrees, which comprises a substrate resin layer; a coupling agent layer located over the base resin layer; and a particle layer over the coupling agent layer.
In some embodiments, the base resin includes one or more of silicone, epoxy, silicone modified epoxy, and acrylic resins, which may be used to enhance the adhesion of the particle layer to the base, such that the particle layer may be firmly adhered to the base.
In some embodiments, the coupling agent comprises a silane coupling agent, the silane coupling agent comprises one or more of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma- (methacryloyloxy) propyltrimethoxysilane (KH570), and the substrate resin contains hydroxyl and is a hydrophilic layer, and the particle layer is a hydrophobic layer, so that the particle layer cannot be effectively spread, the two layers can be effectively connected through the action of the coupling agent, the tight combination is realized, and the stability of the coating is improved.
In some embodiments, the particles are hydrophobic silica, wherein the hydrophobic silica is hydrophobic gas phase silica or hydrophobic silica prepared by a sol-gel method commonly used in the art, and the invention enables the prepared coating to provide better hydrophobic and oleophobic performances and simultaneously provide better permeability by combining with a substrate resin by using the hydrophobic silica.
The present application also provides a method of preparing a super-amphiphobic coating, the method comprising: adding base resin and a curing agent into ethyl acetate and/or acetone to obtain a base resin solution with the concentration of 10 g/L-30 g/L; adding a coupling agent into ethanol, methanol and/or isopropanol to obtain a coupling agent solution with the concentration of 10 g/L-30 g/L; adding the particles into ethanol, methanol and/or isopropanol at a concentration of 3-10 g/L, and adding fluorosilane (the mass ratio of fluorosilane to particles is 1-2: 8-10) to obtain a particle solution; and sequentially coating the substrate resin solution, the coupling agent solution and the particle solution on the substrate, wherein each layer is dried and then sprayed with the next layer, each layer is cured at the temperature of 80-120 ℃ for 20-40 min, and after all layers are cured, the super-amphiphobic coating is obtained.
In the method, the curing agent for the base resin (the mass ratio of the curing agent to the base resin is 0.5-1: 5-15) comprises one or more of ethylenediamine, diethylenetriamine and m-phenylenediamine, the solvent for the base resin uses ethyl acetate and/or acetone, and the concentration of the base resin solution is configured to be 10 g/L-30 g/L, so that the base resin can be better dissolved and cured, the base resin can be better combined with the base, the adhesion of the base resin is increased, and the adhesion of a subsequently formed particle layer to the base is further enhanced.
In the method, the coupling agent comprises a silane coupling agent, ethanol, methanol and/or isopropanol is used as a solution for the coupling agent, and the concentration of the coupling agent solution is configured to be 10 g/L-30 g/L, so that the coupling agent can be uniformly dispersed, the particle layer formed later can be effectively spread, and the base resin and the particle layer can be tightly combined.
In the method, the particles comprise hydrophobic gas phase silicon oxide (Shanghai Beijing industry development Co., Ltd.) or hydrophobic silicon oxide prepared by a sol-gel method commonly used in the field, so that the particle layer has better hydrophobic and oleophobic performances, and in addition, the concentration of the particle solution is configured to be 3 g/L-10 g/L and the particle solution is combined with the substrate resin, so that the prepared super-amphiphobic coating has better transmittance; in addition, the addition of the fluorosilane is used for further modifying the surface of the particle layer so as to further improve the hydrophobic and oleophobic performances of the particle layer.
Example 1
Adding epoxy resin and m-phenylenediamine into a corresponding solvent ethyl acetate, preparing the concentration of 10g/L, and performing ultrasonic dispersion for 30min to obtain a substrate resin solution; mixing a silane coupling agent KH560 with ethanol, preparing the mixture with the concentration of 20g/L, and performing ultrasonic dispersion for 30min to obtain a silane coupling agent solution; mixing hydrophobic gas-phase silicon oxide with an ethanol solution, preparing the concentration to be 3g/L, carrying out ultrasonic dispersion for 30min, then adding fluorosilane, and stirring for 30min to obtain a particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 0.5MPa each time, drying each layer, then spraying the next layer, curing each layer at 100 ℃ for 30min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
Example 2
Adding acrylic resin and diethylenetriamine into a corresponding solvent acetone, preparing the concentration of 20g/L, and performing ultrasonic dispersion for 50min to obtain a substrate resin solution; mixing a silane coupling agent KH550 with methanol, preparing the mixture with the concentration of 10g/L, and performing ultrasonic dispersion for 20min to obtain a silane coupling agent solution; mixing 10g of TEOS (tetraethyl orthosilicate), 4g of water and 8g of ammonia water by adopting a sol-gel method commonly used in the field to prepare hydrophobic silicon oxide, mixing the hydrophobic gas-phase silicon oxide with an ethanol solution, preparing the concentration of 5g/L, performing ultrasonic dispersion for 30min, adding fluorosilane, and stirring for 40min to obtain a particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 0.7MPa each time, drying each layer, then spraying the next layer, curing each layer at 800 ℃ for 20min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
Example 3
Adding the organic silicon modified epoxy resin and m-phenylenediamine into a corresponding solvent acetone, preparing the solution with the concentration of 10g/L, and performing ultrasonic dispersion for 30min to obtain a substrate resin solution; mixing a silane coupling agent KH570 with ethanol, preparing the mixture with the concentration of 20g/L, and performing ultrasonic dispersion for 30min to obtain a silane coupling agent solution; mixing hydrophobic gas-phase silicon oxide with an ethanol solution, preparing the concentration to be 3g/L, carrying out ultrasonic dispersion for 30min, then adding fluorosilane, and stirring for 30min to obtain a particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 0.5MPa each time, drying each layer, then spraying the next layer, curing each layer at 100 ℃ for 30min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
Example 4
Adding organic silicon resin and ethylenediamine into a corresponding solvent ethyl acetate, preparing the concentration of 10g/L, and performing ultrasonic dispersion for 20min to obtain a substrate resin solution; mixing a silane coupling agent KH560 with isopropanol, preparing the mixture with the concentration of 10g/L, and performing ultrasonic dispersion for 50min to obtain a silane coupling agent solution; mixing hydrophobic gas-phase silicon oxide with a methanol solution, preparing the concentration to be 3g/L, carrying out ultrasonic dispersion for 40min, then adding fluorosilane, and stirring for 40min to obtain a particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 1MPa each time, drying each layer, then spraying the next layer, curing each layer at 120 ℃ for 20min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
Example 5
Adding the organic silicon modified epoxy resin, acrylic resin and m-phenylenediamine into a mixed solution of corresponding solvents of ethyl acetate and acetone, preparing the concentration of 30g/L, and performing ultrasonic dispersion for 50min to obtain a substrate resin solution; mixing a silane coupling agent KH560 with methanol, preparing the mixture with the concentration of 30g/L, and performing ultrasonic dispersion for 20min to obtain a silane coupling agent solution; mixing hydrophobic gas-phase silicon oxide with isopropanol solution, preparing the concentration of 10g/L, performing ultrasonic dispersion for 30min, then adding fluorosilane, and stirring for 30min to obtain particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 0.5MPa each time, drying each layer, then spraying the next layer, curing each layer at 80 ℃ for 40min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
Example 6
Adding epoxy resin, m-phenylenediamine and ethylenediamine into corresponding ethyl acetate solvents, preparing the concentration of 20g/L, and performing ultrasonic dispersion for 30min to obtain a substrate resin solution; mixing silane coupling agents KH550 and KH560 with ethanol, preparing the mixture with the concentration of 20g/L, and performing ultrasonic dispersion for 30min to obtain a silane coupling agent solution; mixing hydrophobic gas-phase silicon oxide with an ethanol solution, preparing the concentration of 5g/L, performing ultrasonic dispersion for 30min, then adding fluorosilane, and stirring for 30min to obtain a particle solution.
And sequentially spraying the substrate resin solution, the silane coupling agent solution and the particle solution on the substrate by using a spray gun, wherein the spraying pressure is 0.5MPa each time, drying each layer, then spraying the next layer, curing each layer at 100 ℃ for 30min, and obtaining the transparent super-amphiphobic coating after the curing is finished.
The transparent super-amphiphobic coatings prepared in examples 1 and 6 were tested for light transmittance, contact angle and roll angle using a light transmittance meter (LH-206) and a contact angle meter (LAUDA, germany) using methods commonly used in the art, and the test results are as follows in table 1:
TABLE 1
| Examples | Light transmittance | Water contact angle/° c | Hexadecane contact Angle/° C | Roll angle/° |
| 1 | 95％ | 152 | 150 | 2 |
| 2 | 92％ | 160 | 152 | 3 |
| 3 | 93％ | 156 | 151 | 3 |
| 4 | 92％ | 158 | 150 | 2 |
| 5 | 94％ | 155 | 155 | 3 |
| 6 | 94％ | 157 | 153 | 2 |
As can be seen from the above table 1, the water contact angle and the hexadecane contact angle of the surface of the super-amphiphobic coating prepared by the method are both larger than 150 degrees, the rolling angles are both smaller than 3 degrees, the light transmittance is both larger than 92 percent, and the super-amphiphobic coating has good hydrophobic and oleophobic effects and simultaneously has good transmittance to visible light; the reason is that the hydrophobic silicon oxide enables the particle coating to have better hydrophobic and oleophobic performances, and the permeability of the super-amphiphobic coating is improved by combining the hydrophobic silicon oxide with the substrate resin.
In addition, the adhesion force of the particle layer and the substrate is enhanced by the substrate resin, the silane coupling agent can effectively connect the substrate resin and the particle layer, and the substrate resin and the particle layer are tightly combined, so that the stability of the coating is improved.
In addition, the amphiphobic coating prepared according to the above described method can be applied to surface devices, wherein the surface devices include surfaces of any object, such as glass surfaces, aircraft surfaces, automotive surfaces, and the like.
In conclusion, the super-amphiphobic coating prepared by the method can form a super-hydrophobic and super-oleophobic coating on various solid surfaces, does not change the air permeability and the appearance of the original surface, prevents the direct contact and adsorption of water, oil, dust and other dirt, plays roles in preventing dust, oil, dirt and moisture, reducing the coverage of rain, dew, frost, snow and ice and the like, and can be applied to the fields of glass, sanitary wares, aircraft skins, power grids and the like.
Those skilled in the art will appreciate that the above embodiments are merely exemplary embodiments and that various changes, substitutions, and alterations can be made without departing from the spirit and scope of the invention.
Claims (13)
1. An amphiphobic coating, comprising:
a base resin layer;
a coupling agent layer located over the base resin layer; and
a particle layer located over the coupling agent layer.
2. The amphiphobic coating of claim 1, wherein the amphiphobic coating is a super-amphiphobic coating having both a water contact angle and an oil contact angle of greater than 150 °.
3. The amphiphobic coating of claim 1, wherein the base resin in the base resin layer comprises one or more of a silicone resin, an epoxy resin, a silicone modified epoxy resin, and an acrylic resin.
4. The amphiphobic coating of claim 1, wherein the coupling agent in the coupling agent layer comprises a silane coupling agent comprising one or more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, and gamma- (methacryloyloxy) propyltrimethoxysilane.
5. The amphiphobic coating of claim 1, wherein the particles in the particle layer comprise hydrophobic silica.
6. A method of preparing a amphiphobic coating comprising:
adding a base resin and a curing agent into a first solvent to obtain a base resin solution;
adding a coupling agent into a second solvent to obtain a coupling agent solution;
adding the particles into a third solvent to obtain a particle solution; and
and sequentially coating the substrate resin solution, the coupling agent solution and the particle solution on a substrate to obtain the amphiphobic coating.
7. The method of claim 6, wherein the amphiphobic coating is a super-amphiphobic coating having both a water contact angle and an oil contact angle greater than 150 °.
8. The method of claim 6, wherein the base resin comprises one or more of a silicone resin, an epoxy resin, a silicone modified epoxy resin, and an acrylic resin; the curing agent comprises one or more of ethylenediamine, diethylenetriamine and m-phenylenediamine; and the first solvent comprises one or both of ethyl acetate and acetone.
9. The method of claim 6, wherein the coupling agent comprises a silane coupling agent comprising one or more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, and gamma- (methacryloyloxy) propyltrimethoxysilane; and the second solvent comprises one or more of ethanol, methanol, and isopropanol.
10. The method of claim 6, wherein the particles comprise hydrophobic silica; and the third solvent comprises one or more of ethanol, methanol, and isopropanol.
11. The method according to claim 6, wherein the concentration of the base resin in the base resin solution is 10g/L to 30 g/L; the concentration of the coupling agent in the coupling agent solution is 10 g/L-30 g/L; and the concentration of the particles in the particle solution is 3g/L to 10 g/L.
12. The method of claim 6, wherein a fluorosilane is added after the particles are added to the third solvent.
13. Use of a amphiphobic coating prepared according to the method of any of claims 6-12 on a surface device.
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Application publication date: 20200428 |