CN110862756A - Wear-resistant super-hydrophobic coating and preparation method thereof - Google Patents
Wear-resistant super-hydrophobic coating and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a wear-resistant super-hydrophobic coating and a preparation method thereof. Uniformly mixing the absolute ethyl alcohol dispersion liquid of the hydrophobic silicon dioxide nano particles and the single-component aqueous polyurethane solution to obtain the hydrophobic silicon dioxide nano particles/single-component aqueous polyurethane dispersion liquid, then brushing or spraying the dispersion liquid on a substrate, and curing at room temperature for 5 hours to obtain the wear-resistant super-hydrophobic coating. The prepared super-hydrophobic solution can be stored in a sealed way for a long time, can be coated at any time, can be cured at room temperature, and is very convenient. The substrate may be any one of glass, metal, plastic, ceramic, and stone. The static water contact angle of the surface of the wear-resistant super-hydrophobic coating is 151-153 degrees, the rolling angle is 4-6 degrees, and the wear-resistant super-hydrophobic coating can rub 1800cm on 320-mesh sand paper along a straight line under the pressure of 2500 Pa. The preparation method has the advantages of simple preparation process, convenience in operation, environmental friendliness, low cost and the like, has higher practical value and application prospect, and can be applied to various fields.
Description
Technical Field
The invention belongs to the technical field of super-hydrophobic materials, and particularly relates to a preparation method of a wear-resistant super-hydrophobic coating.
Background
Superhydrophobic surfaces having high water contact angles greater than 150 ° and low sliding angles less than 10 ° are of great interest in a number of applications. At present, there are many methods for successfully and artificially preparing the super-hydrophobic coating, but in order to really make the super-hydrophobic coating widely used in practice, a fatal defect of the super-hydrophobic coating, namely, the super-hydrophobic coating has very limited mechanical stability and cannot resist mechanical touch, needs to be overcome.
In order to solve the problem of mechanical strength of the super-hydrophobic coating, many methods for preparing the wear-resistant super-hydrophobic coating are available at present, for example, patent CN106675339A discloses a simple preparation method of a low-cost high-strength super-hydrophobic coating, in which epoxy resin (E51) is used as an adhesive, and is added into acetone together with metal powder, a low-surface-energy modifier and a curing agent, and the acetone is uniformly dispersed and then coated. Patent CN107189656A discloses a preparation method of a wear-resistant super-hydrophobic coating based on polycarbonate, which comprises the steps of firstly coating a layer of polycarbonate glue on a substrate, then coating a solution for an intermediate layer on the glue, further coating a surface layer solution on the intermediate layer after the solution for the intermediate layer is dried, and drying to obtain the wear-resistant super-hydrophobic coating. The method needs to use toxic acetone as a solvent, is complex to operate, needs to coat multiple layers, and is not beneficial to practical application. Patent CN106118422A discloses a nano SiO2The composite polysiloxane modified waterborne terpene EP/PU super-hydrophobic self-cleaning polymer and the preparation method thereof have high requirements on curing temperature, the curing is required to be carried out at 120 ℃, and the curing conditions are not favorable for large-scale production.
Most of the known methods for preparing the wear-resistant super-hydrophobic coating have the problems of harsh preparation conditions, complex preparation method, toxicity, harm and the like, so the method for preparing the wear-resistant super-hydrophobic coating by adopting the method which has simple preparation process, mild conditions, environmental protection and low cost and can preserve the dispersion liquid for a long time is about the development and application prospect of the super-hydrophobic technology.
Disclosure of Invention
The invention aims to provide a preparation method of an abrasion-resistant super-hydrophobic coating, which is environment-friendly, easy to operate and low in cost. The single-component waterborne polyurethane takes water as a solvent, has the characteristics of low price and environmental protection, but the hydrophobic nano silicon dioxide can not be dispersed in the water. According to the invention, a water-absolute ethanol solution is used as a solvent, a hydrophobic silicon dioxide nanoparticle/waterborne polyurethane uniform mixed solution is obtained at a proper proportion, and the prepared coating has excellent super-hydrophobic property and wear resistance. The coating liquid can be stored for a long time in a sealed way, can be solidified at room temperature, can be coated at any time, is very convenient, and can be used for mass production and application.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a wear-resistant super-hydrophobic coating specifically comprises the following steps: uniformly mixing the hydrophobic silicon dioxide ethanol dispersion liquid and the single-component aqueous polyurethane solution, then coating the mixture on the surface of a substrate, and drying the substrate at room temperature for 5 hours to obtain the hydrophobic silicon dioxide/aqueous polyurethane wear-resistant super-hydrophobic composite coating. The hydrophobic coating has excellent hydrophobic property, and the static water contact angle of the surface of the coating is 151-153 degrees, and the rolling angle is 4-6 degrees. The abrasion resistance is shown in that the coating still maintains superhydrophobicity (contact angle >150 °) after rubbing the coating on 320 mesh sandpaper along a straight line at a pressure of 2500Pa for a distance of 1800 cm.
The preparation method of the wear-resistant super-hydrophobic coating specifically comprises the following steps:
(1) uniformly mixing single-component waterborne polyurethane with a proper amount of water to prepare a single-component waterborne polyurethane aqueous solution;
(2) adding the hydrophobic silicon dioxide nano particles into absolute ethyl alcohol, and strongly stirring for 1h at the temperature of 60 ℃ to uniformly disperse the hydrophobic silicon dioxide nano particles in the absolute ethyl alcohol to obtain a hydrophobic silicon dioxide nano particle dispersion liquid;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (1) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid;
(4) coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid in the step (3) on the surface of a base material in a brush coating or spraying manner, wherein the coating times are 1-2 times, the coating interval of each time is 30min, and completely curing after standing at room temperature for 5 h;
in the step (1), the mass ratio of the single-component waterborne polyurethane to water is 1: 1-2;
in the step (2), the mass ratio of the hydrophobic nano-silica to the absolute ethyl alcohol is (0.20-0.28): 1.0;
in the step (3), the mass ratio of the single-component waterborne polyurethane to the hydrophobic silicon dioxide is 1: 0.8 to 1.0 parts by weight,
the synthesis of the hydrophobic silica nanoparticles in the step (2) comprises the following steps:
the synthesis raw material molar ratio of the nano silicon dioxide with the hydrophobic modified surface is as follows: tetraethoxysilane, absolute ethyl alcohol, ammonia water, distilled water, methyl triethoxysilane = 1: 30: x: 1: y, wherein x is more than or equal to 4.5 and less than or equal to 5.3, and y is more than or equal to 0.5 and less than or equal to 0.75;
b, mixing and stirring tetraethoxysilane and absolute ethyl alcohol at the temperature of 60 ℃ for 10min according to the proportion, then dropwise adding a mixed solution of deionized water and ammonia water, strongly stirring for 2h at the temperature of 60 ℃, dropwise adding triethoxymethylsilane, continuously stirring for 1h at the temperature of 60 ℃, aging for 24h at room temperature, then placing in a drying oven at the temperature of 60 ℃ for 2-3 days, and completely evaporating the solvent to obtain the hydrophobic silicon dioxide nanoparticles.
The invention has the beneficial effects that:
the hydrophobic silicon dioxide nano-particles/single-component waterborne polyurethane dispersion prepared by the wear-resistant super-hydrophobic coating can be stored for a long time, can be cured at room temperature, can be coated at any time, and is very convenient. The preparation method has the advantages of simple preparation process, mild conditions, environmental protection, low cost and wide applicability; the prepared wear-resistant super-hydrophobic coating has excellent super-hydrophobicity and wear resistance, and the static water contact angle of the surface of the coating is 151-153 degrees, and the rolling angle is 4-6 degrees. The abrasion resistance is shown in that the coating still maintains superhydrophobicity (contact angle >150 °) after rubbing the coating on 320 mesh sandpaper along a straight line at a pressure of 2500Pa for a distance of 1800 cm.
Drawings
FIG. 1 is a surface water contact angle state diagram of the abrasion-resistant super-hydrophobic coating obtained in example 1.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the abrasion resistant superhydrophobic coating obtained in example 1.
FIG. 3 is an infrared spectrum of the hydrophobic silica nanoparticles of example 1.
FIG. 4 is a graph of contact angle of the abrasion-resistant superhydrophobic coating obtained in example 1 as a function of rubbing distance.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) Mixing 12.4mL of tetraethyl orthosilicate and 97.2mL of absolute ethyl alcohol, carrying out reflux stirring at 60 ℃ for 10min, then dropwise adding a mixed solution of 11.8mL of ammonia water and 1mL of deionized water, carrying out reflux stirring at 60 ℃ for 2h, then dropwise adding 5.5mL of triethoxymethylsilane, continuing to carry out reflux stirring at 60 ℃ for 1h, ageing at room temperature for 24h, then placing in a 60 ℃ oven for 2 days, and completely evaporating the solvent to obtain hydrophobic silica nanoparticles;
(2) adding 1g of hydrophobic silica nanoparticles into 3.95g of absolute ethyl alcohol, and strongly stirring for 1h at 60 ℃ to uniformly disperse the hydrophobic silica nanoparticles in the absolute ethyl alcohol to obtain a hydrophobic silica nanoparticle dispersion liquid; uniformly mixing 1g of single-component waterborne polyurethane with 1g of water to prepare a single-component waterborne polyurethane aqueous solution;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (2) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid; coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid on a glass substrate for 2 times, wherein the coating interval of each time is 30min, standing at room temperature for 5h, and then completely curing to obtain a durable super-hydrophobic coating;
the product obtained in example 1 was characterized by taking 5 points on the surface of the coating and measuring the average contact angle value of 151.2 °, the rolling angle of 4.4 °, and fig. 1 is a state diagram of the contact angle at a certain point on the coating. FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the coating surface, from which it can be seen that the microstructure of the coating is a micro-nano porous coarse structure, and the size of the silica particles is 70-90 nm. FIG. 3 is an infrared spectrum of hydrophobic silica nanoparticles, in which the groups corresponding to the respective peaks have been indicated, and from which it can be seen that methyl groups have been grafted to the surface of the silica particles after surface modification. The coated glass is placed on 320-mesh sand paper in a downward mode, the coated glass is slightly pushed to rub in the linear direction under the pressure of 2500Pa, after the coated glass is pushed for 10cm, the rectangular coated glass is rotated for 90 degrees clockwise, then the coated glass is pushed for 10cm forward, and the operation is continued sequentially. The contact angle of the coating after rubbing was measured at 50cm per rubbing. The results show that the coating remains superhydrophobic after being rubbed for 1800 cm. Fig. 4 is a graph of contact angle of a superhydrophobic coating as a function of rubbing distance.
Example 2
(1) Mixing 37.2mL of tetraethyl orthosilicate and 291.6mL of anhydrous ethanol, carrying out reflux stirring at 60 ℃ for 10min, then dropwise adding a mixed solution of 35.4mL of ammonia water and 3mL of deionized water, carrying out reflux stirring at 60 ℃ for 2h, then dropwise adding 16.5mL of triethoxymethylsilane, continuing to carry out reflux stirring at 60 ℃ for 1h, ageing at room temperature for 24h, then placing in a 60 ℃ oven for 3 days, and completely evaporating the solvent to obtain hydrophobic silica nanoparticles;
(2) adding 5g of hydrophobic silica nanoparticles into 19.75g of absolute ethyl alcohol, and strongly stirring for 1h at 60 ℃ to uniformly disperse the hydrophobic silica nanoparticles in the absolute ethyl alcohol to obtain a hydrophobic silica nanoparticle dispersion liquid; uniformly mixing 5g of single-component waterborne polyurethane with 5g of water to prepare a single-component waterborne polyurethane aqueous solution;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (2) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid; coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid on a glass substrate for 2 times, wherein the coating interval of each time is 30min, standing at room temperature for 5h, and then completely curing to obtain a durable super-hydrophobic coating;
the coating prepared in this example had an average water contact angle of 151.3 deg., a rolling angle of 4.6 deg., and a measured abrasion resistance distance of 1800 cm.
Example 3
(1) Mixing 12.4mL of tetraethyl orthosilicate and 97.2mL of absolute ethyl alcohol, carrying out reflux stirring at 60 ℃ for 10min, then dropwise adding a mixed solution of 11.8mL of ammonia water and 1mL of deionized water, carrying out reflux stirring at 60 ℃ for 2h, then dropwise adding 5.5mL of triethoxymethylsilane, continuing to carry out reflux stirring at 60 ℃ for 1h, ageing at room temperature for 24h, then placing in a 60 ℃ oven for 2 days, and completely evaporating the solvent to obtain hydrophobic silica nanoparticles;
(2) adding 0.8g of hydrophobic silica nanoparticles into 3.95g of absolute ethyl alcohol, and strongly stirring for 1h at 60 ℃ to uniformly disperse the hydrophobic silica nanoparticles in the absolute ethyl alcohol to obtain a hydrophobic silica nanoparticle dispersion liquid; uniformly mixing 1g of single-component waterborne polyurethane with 1g of water to prepare a single-component waterborne polyurethane aqueous solution;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (2) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid; coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid on a glass substrate for 2 times, wherein the coating interval of each time is 30min, standing at room temperature for 5h, and then completely curing to obtain a durable super-hydrophobic coating;
the coatings prepared in this example had an average water contact angle of 152.1 deg., a roll angle of 4.0 deg., and a measured abrasion resistance distance of 1500 cm.
Comparative example 1
(1) Mixing 12.4mL of tetraethyl orthosilicate and 97.2mL of absolute ethyl alcohol, carrying out reflux stirring at 60 ℃ for 10min, then dropwise adding a mixed solution of 11.8mL of ammonia water and 1mL of deionized water, carrying out reflux stirring at 60 ℃ for 2h, then dropwise adding 5.5mL of triethoxymethylsilane, continuing to carry out reflux stirring at 60 ℃ for 1h, ageing at room temperature for 24h, then placing in a 60 ℃ oven for 2 days, and completely evaporating the solvent to obtain hydrophobic silica nanoparticles;
(2) adding 1g of hydrophobic silica nanoparticles into 3.95g of absolute ethyl alcohol, and strongly stirring for 1h at 60 ℃ to uniformly disperse the hydrophobic silica nanoparticles in the absolute ethyl alcohol to obtain a hydrophobic silica nanoparticle dispersion liquid; 1g of single-component waterborne polyurethane is uniformly mixed with 0.5g of water to prepare a single-component waterborne polyurethane aqueous solution;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (2) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid; coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid on a glass substrate for 2 times, wherein the coating interval of each time is 30min, standing at room temperature for 5h, and then completely curing to obtain a durable super-hydrophobic coating;
the coating prepared in this example had an average water contact angle of 142.7 ° and was not superhydrophobic.
Comparative example 2
(1) Mixing 12.4mL of tetraethyl orthosilicate and 97.2mL of absolute ethyl alcohol, carrying out reflux stirring at 60 ℃ for 10min, then dropwise adding a mixed solution of 11.8mL of ammonia water and 1mL of deionized water, carrying out reflux stirring at 60 ℃ for 2h, then dropwise adding 5.5mL of triethoxymethylsilane, continuing to carry out reflux stirring at 60 ℃ for 1h, ageing at room temperature for 24h, then placing in a 60 ℃ oven for 2 days, and completely evaporating the solvent to obtain hydrophobic silica nanoparticles;
(2) adding 1g of hydrophobic silica nanoparticles into 7.9g of absolute ethyl alcohol, and strongly stirring for 1h at 60 ℃ to uniformly disperse the hydrophobic silica nanoparticles in the absolute ethyl alcohol to obtain a hydrophobic silica nanoparticle dispersion liquid; uniformly mixing 1g of single-component waterborne polyurethane with 1g of water to prepare a single-component waterborne polyurethane aqueous solution;
(3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step (2) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step (2), stirring vigorously at 60 ℃ for 1h, and performing ultrasonic treatment for 30min to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid; coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid on a glass substrate for 2 times, wherein the coating interval of each time is 30min, standing at room temperature for 5h, and then completely curing to obtain a durable super-hydrophobic coating;
the coatings prepared in this example had an average water contact angle of 153.5 deg., were superhydrophobic, but measured a wear distance of 600 cm.
Claims (8)
1. A preparation method of a wear-resistant super-hydrophobic coating is characterized by comprising the following steps: uniformly mixing the ethanol dispersion liquid of the hydrophobic nano-silica and the aqueous solution of the single-component waterborne polyurethane, then coating the mixture on the surface of a substrate, and curing the mixture at room temperature to obtain the silica/waterborne polyurethane wear-resistant super-hydrophobic composite coating.
2. The method for preparing the abrasion-resistant super-hydrophobic coating according to claim 1, wherein: the base material is any one of glass, metal, plastic, ceramic and stone.
3. The method for preparing the abrasion-resistant super-hydrophobic coating according to claim 1, wherein: the method comprises the following specific steps:
1) uniformly mixing single-component waterborne polyurethane with a proper amount of water to prepare a single-component waterborne polyurethane aqueous solution;
2) adding the hydrophobic silicon dioxide nano particles into absolute ethyl alcohol, and strongly stirring for 1h at the temperature of 60 ℃ to uniformly disperse the hydrophobic silicon dioxide nano particles in the absolute ethyl alcohol to obtain a hydrophobic silicon dioxide nano particle dispersion liquid;
3) mixing 1 part of the single-component aqueous polyurethane solution obtained in the step 1) with 1 part of the hydrophobic silica nanoparticle dispersion liquid obtained in the step 2), stirring vigorously, and performing ultrasonic treatment to obtain a hydrophobic silica/aqueous polyurethane dispersion liquid;
4) coating the hydrophobic silicon dioxide/waterborne polyurethane dispersion liquid obtained in the step 3) on the surface of a base material in a brush coating or spraying manner, wherein the coating times are 1-2 times, the coating interval of each time is 30min, and completely curing after standing at room temperature for 5 h.
4. The method for preparing an abrasion-resistant superhydrophobic coating according to claim 3, characterized in that: the mass ratio of the single-component waterborne polyurethane to water in the step 1) is 1: 1.
5. the method for preparing the abrasion-resistant super-hydrophobic coating according to claim 3, wherein: the mass ratio of the hydrophobic nano silicon dioxide to the absolute ethyl alcohol in the step 2) is 0.20-0.28: 1.0.
6. the method for preparing the abrasion-resistant super-hydrophobic coating according to claim 3, wherein: the violent stirring in the step 3) is carried out for 1h at the temperature of 60 ℃; the ultrasonic treatment time is 30 min.
7. The method for preparing the abrasion-resistant super-hydrophobic coating according to claim 3, wherein: the mass ratio of the single-component waterborne polyurethane to the hydrophobic nano silicon dioxide in the step 3) is 1: 0.8 to 1.0.
8. The method for preparing an abrasion-resistant superhydrophobic coating according to claim 3, characterized in that: the synthesis of the hydrophobic silica nanoparticles in the step 2) comprises the following steps:
(1) the synthesis raw material molar ratio of the surface hydrophobic modified nano silicon dioxide is as follows: tetraethoxysilane, absolute ethyl alcohol, ammonia water, distilled water, methyl triethoxysilane = 1: 30: x: 1: y, wherein x is more than or equal to 4.5 and less than or equal to 5.3, and y is more than or equal to 0.5 and less than or equal to 0.75;
(2) mixing and stirring tetraethoxysilane and absolute ethyl alcohol at the temperature of 60 ℃ for 10min according to the proportion, then dropwise adding a mixed solution of deionized water and ammonia water, strongly stirring for 2h at the temperature of 60 ℃, dropwise adding triethoxymethylsilane, continuously stirring for 1h at the temperature of 60 ℃, aging for 24h at room temperature, and then placing in an oven at the temperature of 60 ℃ for 2-3 days to completely evaporate the solvent to obtain the hydrophobic silicon dioxide nano-particles.
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