CN113698850A - Wear-resistant corrosion-resistant super-hydrophobic composite coating and preparation method thereof - Google Patents
Wear-resistant corrosion-resistant super-hydrophobic composite coating and preparation method thereof Download PDFInfo
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- 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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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a wear-resistant corrosion-resistant super-hydrophobic composite coating and a preparation method thereof. Uniformly mixing the mica-silica composite powder functionally modified by the silane coupling agent KH-560 with epoxy resin and ethyl acetate to obtain epoxy resin/mica-silica sol, then spraying the epoxy resin/mica-silica sol on a substrate, and curing for 2 hours at 80 ℃ to obtain the wear-resistant corrosion-resistant super-hydrophobic composite coating. The water contact angle of the surface of the coating is 155-160 degrees, the rolling angle is 2-4 degrees, the contact angle after the coating is rubbed on 320-mesh SiC sand paper for 2000cm along a straight line under the pressure of 2000Pa is 148.3 degrees, the surface is kept hydrophobic after the coating is soaked in 3.5wt% NaCl solution for 30 days, and the contact angle can reach 146.0 degrees. The preparation method is simple, environment-friendly and low in cost, is suitable for the surfaces of different substrates such as glass, metal, wood, ceramic, stone and the like, and has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of super-hydrophobic materials, and particularly relates to a wear-resistant corrosion-resistant super-hydrophobic composite coating and a preparation method thereof.
Background
The super-hydrophobic coating is a wetting phenomenon that a contact angle of a water drop on the surface of a solid is larger than 150 degrees and a rolling angle is smaller than 10 degrees, and the super-hydrophobic coating draws great attention in recent years due to wide application prospects, but the problems of poor mechanical stability, complex preparation process and poor corrosion resistance generally exist in the super-hydrophobic coating.
CN111117384A discloses a preparation method of a high-mechanical-strength wear-resistant corrosion-resistant super-hydrophobic coating material, wherein the prepared coating has both wear resistance and corrosion resistance, but the operation is complicated, and fluorine element and acetone are introduced during the preparation of the coating, so that the toxicity is not environment-friendly. CN111171648A discloses a preparation method of a wear-resistant super-hydrophobic coating, which is characterized in that super-hydrophobic silicon dioxide, acrylate copolymer and alcohol solvent are uniformly mixed and then sprayed on a substrate, the process is simple and easy to control, the coating substrate has good adaptability, friction resistance, strong adhesive force and long service life, and is environment-friendly, but the corrosion resistance of the coating is not evaluated.
Disclosure of Invention
The invention aims to provide a high-wear-resistance corrosion-resistance super-hydrophobic composite coating and a preparation method thereof. The spraying coating process is adopted, the operation is simple, and the large-scale production and application are easy to realize.
In order to achieve the purpose, the invention adopts the following technical scheme:
uniformly mixing hydrophobic mica-silica composite powder functionally modified by a silane coupling agent KH-560, epoxy resin and ethyl acetate to obtain epoxy resin/mica-silica sol, spraying the epoxy resin/mica-silica sol on a substrate, and curing at 80 ℃ for 2 hours to obtain the wear-resistant corrosion-resistant super-hydrophobic composite coating. The water contact angle of the surface of the coating is 155-160 degrees, the rolling angle is 2-4 degrees, the contact angle after the coating is rubbed on 320-mesh SiC paper for 2000cm along a straight line under the pressure of 2000Pa is 148.3 degrees, the surface is kept hydrophobic after the coating is soaked in 3.5wt% NaCl solution for 30 days, and the contact angle is 146.0 degrees.
The preparation method of the wear-resistant corrosion-resistant super-hydrophobic composite coating comprises the following steps:
1) dispersing hydrophobic nano-silica and hydrophobically modified mica powder in an ethanol solution of a silane coupling agent KH-560, performing ultrasonic treatment for 10min, stirring for 1h, and drying to obtain mica-silica composite powder functionally modified by the silane coupling agent KH-560;
2) adding the KH-560 functionalized modified mica-silica composite powder prepared in the step 1) into a mixed solution of epoxy resin E-51 and ethyl acetate, performing ultrasonic treatment for 10min, and stirring at 25 ℃ for 1h to obtain epoxy resin/mica-silica sol;
3) adding a curing agent T31 into the epoxy resin/mica-silica sol prepared in the step 2), stirring for 10min, spraying on a substrate, and curing at 80 ℃ for 2h to obtain the mica-silica/epoxy resin wear-resistant corrosion-resistant super-hydrophobic composite coating.
The hydrophobic nano silicon dioxide in the step 1) is synthesized by the following steps: the molar ratio of the synthetic raw materials is as follows: tetraethoxysilane, absolute ethyl alcohol, ammonia water, deionized water, methyltriethoxysilane = 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; and (2) refluxing and stirring tetraethoxysilane and absolute ethyl alcohol at 60 ℃ for 10min, dropwise adding a mixed solution of deionized water and ammonia water, refluxing and stirring at 60 ℃ for 10min, dropwise adding methyl triethoxysilane, refluxing and stirring at 60 ℃ for 2h, aging at room temperature for 24h, and drying at 60 ℃ for 2 days to obtain the hydrophobic nano-silicon dioxide.
The synthesis of the hydrophobically modified mica powder in the step 1) comprises the following steps: putting 150-mesh mica powder, methyltrimethoxysilane and ammonia water in a closed container, and performing vapor deposition for 1h at 70 ℃ to obtain hydrophobically modified mica powder; the mass ratio of the mica powder to the methyltrimethoxysilane to the ammonia water is 4: 1: 2.
in the step 1), the mass ratio of the hydrophobic nano-silica to the hydrophobically modified mica powder is 3: 1; the mass ratio of the silane coupling agent KH-560 to the ethanol is 5: 100, respectively; the mass ratio of the powder to the solvent is 1: 1.
the mass ratio of the epoxy resin E-51 to the ethyl acetate is 5: 18, the mass ratio of the epoxy resin E-51 to the curing agent T-31 is 2: 1.
the invention has the beneficial effects that: the method is simple, environment-friendly, low in cost and easy to realize large-scale production and application. The prepared super-hydrophobic coating has excellent super-hydrophobicity, wear resistance and corrosion resistance, the water contact angle of the surface of the coating is 155-160 degrees, the rolling angle is 2-4 degrees, the contact angle after the coating is rubbed on 320-mesh SiC paper along a straight line under the pressure of 2000Pa is 148 degrees, the surface is kept hydrophobic after the coating is soaked in 3.5wt% NaCl solution for 30 days, and the contact angle can reach 146 degrees.
Drawings
FIG. 1 is a surface water contact angle state diagram of the wear-resistant corrosion-resistant super-hydrophobic composite coating obtained in example 1.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the wear-resistant and corrosion-resistant superhydrophobic composite coating obtained in example 1.
FIG. 3 is an infrared spectrum of the mica powder, the hydrophobically modified mica powder and the KH-560 functionalized modified mica-silica composite powder of example 1.
Fig. 4 is a graph of the contact angle of the wear-resistant and corrosion-resistant super-hydrophobic composite coating obtained in example 1 as a function of the friction distance.
FIG. 5 is a surface water contact angle state diagram of the wear-resistant and corrosion-resistant super-hydrophobic composite coating obtained in example 1 after being soaked in 3.5wt% NaCl solution for 30 days.
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) 12.4ml of tetraethyl orthosilicate and 97.2ml of absolute ethyl alcohol are placed in a three-neck flask and are stirred under reflux at 60 ℃ for 10min, then 1ml of water and 11.8ml of ammonia water are uniformly mixed, the mixed solution is dropwise added into the three-neck flask at the speed of 1 second and a drop, 9.5 ml of methyltriethoxysilane is dropwise added into the three-neck flask after the dropwise addition is finished and is stirred under reflux at 60 ℃ for 10min, and the reflux is further stirred at 60 ℃ for 2 h. And after stirring, sealing the solution, standing for 24 hours at room temperature, and then drying the obtained solution in an oven at 60 ℃ for 2 days to obtain the nano silicon dioxide powder with the surface subjected to hydrophobic modification.
(2) 2g of mica powder, 0.5g of methyltrimethoxysilane and 0.1g of ammonia water are placed in a closed container and put in a 70 ℃ oven for vapor deposition to obtain the hydrophobically modified mica powder.
(3) Dispersing 0.75g of hydrophobic silica and 0.25g of hydrophobic mica powder in 5 mass percent KH-560 ethanol solution, carrying out ultrasonic agitation for 10min, stirring for 1h, and drying to obtain the silane coupling agent KH-560 functionalized modified mica-silica composite powder.
(4) And (3) adding the KH-560 functionalized modified mica-silica composite powder prepared in the step (3) into a mixed solution of 0.25g of epoxy resin E-51 and 1ml of ethyl acetate, performing ultrasonic treatment for 10min, and stirring at 25 ℃ for 1h to obtain epoxy resin/mica-silica sol.
(5) And (4) adding 0.125g of curing agent T31 into the epoxy resin/mica-silica sol in the step (4), stirring for 10min, spraying on a glass substrate, and curing at 80 ℃ for 2h to obtain the wear-resistant corrosion-resistant super-hydrophobic composite coating.
The powder obtained in example 1 and the coating are characterized, fig. 1 is a contact angle state diagram of a certain point on the surface of the coating, the static contact angle at the point is 154.5 degrees, and the rolling angle of the coating is 3.5 degrees. Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the surface of the coating from which it can be seen that the epoxy resin bonds the hydrophobic silica and mica particles together well and forms a denser coating on the surface of the substrate. The surface of the coating has a micro-nano coarse structure, partial nano silicon dioxide in the glue solution is agglomerated by airflow in the spraying process to form approximately spherical micro aggregates, and meanwhile, the surface of the substrate is observed to be completely covered by the coating, so that the wear resistance and the corrosion resistance of the coating are improved. FIG. 3 is an infrared spectrum of mica powder, hydrophobically modified mica powder and KH-560 functionalized modified mica-silica composite powder, wherein the hydrophobically modified mica powder has a sample size of 1274cm-1Si-CH of (A)3And the absorption peak formed by C-H absorption vibration proves that the methyl group is successfully grafted to the surface of the mica powder. The KH-560 modified hydrophobic mica powder-silicon dioxide is 1274cm-1The intensity of the peak is much larger than that of the modified mica powder, which indicates that KH-560 successfully carries out functional modification on the mica powder. KH-560 modified mica-silica sample at 2980 cm-1Has a correspondence to-CH3Absorption peak of antisymmetric stretching vibration, furtherIndicating that KH-560 has successfully functionally modified hydrophobic mica-silica particles. FIG. 4 is a graph showing the relationship between the contact angle of the surface of the wear-resistant corrosion-resistant super-hydrophobic composite coating and the friction distance, a glass slide (2.5 cm × 6 cm) coated with the super-hydrophobic coating is placed on 320-mesh SiC abrasive paper, the coating faces downwards, a weight of 200g is placed on the glass slide, then the glass slide is linearly pushed forwards by 10cm by using tweezers, the glass slide is rotated clockwise by 90 degrees and then linearly pushed forwards by 10cm, and the contact angle of the coating is measured every 100cm of friction. As a result, as shown in the figure, the contact angle of the coating surface was 150 ℃ when the abrasion distance was 1900cm, and the superhydrophobicity was maintained. The surface contact angle of the coating after soaking in 3.5wt% NaCl solution for 30 days was 146.0 DEG, and the coating still remained hydrophobic.
Example 2 (without using KH-560 functional modifier)
(1) The preparation methods of the hydrophobically modified nano-silica powder and the mica powder are the same as those in example 1.
(2) 0.15g of hydrophobic silica and 0.05g of hydrophobic mica powder were added to a mixed solution of 0.25g of epoxy resin E-51 and 1ml of ethyl acetate, and the mixture was stirred at 25 ℃ for 1 hour after ultrasonic treatment for 10min to obtain an epoxy resin/mica-silica sol.
(3) And (3) adding 0.125g of curing agent T31 into the epoxy resin/mica-silica sol in the step (2), stirring for 10min, spraying on a glass substrate, and curing at 80 ℃ for 2h to obtain the wear-resistant corrosion-resistant super-hydrophobic coating.
The coatings prepared in this example had an average water contact angle of 155 deg. and a roll angle of 3.8 deg.. The abrasion resistance distance of the coating was 1400cm as measured by a sandpaper abrasion test, and the surface remained hydrophobic after soaking in a 3.5wt% NaCl solution for 15 days. Compared with example 1, the abrasion resistance and salt water corrosion resistance of the coating functionally modified by using the silane coupling agent KH-560 are obviously improved.
Example 3
(1) The preparation method of the hydrophobically modified nano silica powder is the same as that of example 1.
(2) 0.25g of epoxy resin E-51 and 1ml of ethyl acetate are mixed uniformly, 0.20g of hydrophobic silica powder is added, ultrasonic treatment is carried out for 10min, and then stirring is carried out for 1h at 25 ℃ to obtain the epoxy resin/silica sol.
(3) And (3) adding 0.125g of curing agent T31 into the epoxy resin/silicon dioxide sol in the step (2), stirring for 10min, spraying on a glass substrate, and curing at 80 ℃ for 2h to obtain the super-hydrophobic coating.
The coatings prepared in this example had an average water contact angle of 152.29 ° and a roll angle of 3.5 °. The abrasion resistance distance of the coating was 300cm as measured by a sandpaper abrasion test, and the surface was wetted to lose superhydrophobicity after soaking in a 3.5wt% NaCl solution for 5 days.
Compared with the examples 2 and 3, the super-hydrophobic coating prepared from the silicon dioxide has poor wear resistance and salt water corrosion resistance, and the super-hydrophobic coating of the composite layer sheet mica powder has obviously improved wear resistance and salt water corrosion resistance.
Example 4
(1) The preparation method of the hydrophobically modified nano silica powder is the same as that of example 1.
(2) Dispersing 1g of hydrophobic silica powder into 5 mass percent KH-560 ethanol solution, carrying out ultrasonic treatment for 10min, stirring for 1h, and drying to obtain the silane coupling agent KH-560 modified silica powder.
(3) 0.25g of epoxy resin E-51 and 1ml of ethyl acetate are mixed uniformly, 0.20g of KH-560 modified silica powder is added, ultrasonic treatment is carried out for 10min, and then stirring is carried out for 1h at 25 ℃ to obtain epoxy resin/silica sol.
(4) And (4) adding 0.125g of curing agent T31 into the epoxy resin/silicon dioxide sol in the step (3), stirring for 10min, spraying on a glass substrate, and curing at 80 ℃ for 2h to obtain the wear-resistant corrosion-resistant super-hydrophobic coating.
The coatings prepared in this example had an average water contact angle of 151.45 ° and a roll angle of 4.0 °. The abrasion resistance was measured to be 1000cm and the surface remained wet after 30 days of immersion in 3.5wt% NaCl solution.
In comparison with examples 3 and 4, the coating functionally modified with silane coupling agent KH-560 has significantly improved abrasion resistance and salt water corrosion resistance compared to the coating not functionally modified.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. The wear-resistant corrosion-resistant super-hydrophobic composite coating is characterized in that: the composition is mica-silica/epoxy resin.
2. A method for preparing the wear-resistant corrosion-resistant superhydrophobic composite coating of claim 1, characterized in that: the mica-silica/epoxy resin wear-resistant corrosion-resistant super-hydrophobic composite coating is prepared by taking hydrophobic nano-silica, hydrophobically modified mica powder, epoxy resin and ethyl acetate as main components, uniformly mixing, spraying the mixture on the surface of a base material, and curing at 80 ℃.
3. The method of claim 2, wherein: the base material is glass, metal, plastic, ceramic or stone.
4. The method of claim 2, wherein: the method comprises the following specific steps:
1) dispersing hydrophobic nano-silica and hydrophobically modified mica powder in an ethanol solution of a silane coupling agent KH-560, performing ultrasonic treatment for 10min, stirring for 1h, and drying to obtain mica-silica composite powder functionally modified by the silane coupling agent KH-560;
2) adding the KH-560 functionalized modified mica-silica composite powder prepared in the step 1) into a mixed solution of epoxy resin E-51 and ethyl acetate, performing ultrasonic treatment for 10min, and stirring at 25 ℃ for 1h to obtain epoxy resin/mica-silica sol;
3) adding a curing agent T31 into the epoxy resin/mica-silica sol prepared in the step 2), stirring for 10min, spraying on a substrate, and curing at 80 ℃ for 2h to obtain the mica-silica/epoxy resin wear-resistant corrosion-resistant super-hydrophobic composite coating.
5. The method of claim 4, wherein: the hydrophobic nano silicon dioxide in the step 1) is synthesized by the following steps:
the molar ratio of the synthetic raw materials is as follows: tetraethoxysilane, absolute ethyl alcohol, ammonia water, deionized water, methyltriethoxysilane = 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;
and (2) refluxing and stirring tetraethoxysilane and absolute ethyl alcohol at 60 ℃ for 10min, dropwise adding a mixed solution of deionized water and ammonia water, refluxing and stirring at 60 ℃ for 10min, dropwise adding methyl triethoxysilane, refluxing and stirring at 60 ℃ for 2h, aging at room temperature for 24h, and drying at 60 ℃ for 2 days to obtain the hydrophobic nano-silicon dioxide.
6. The method of claim 4, wherein: the synthesis of the hydrophobically modified mica powder in the step 1) comprises the following steps: putting 150-mesh mica powder, methyltrimethoxysilane and ammonia water in a closed container, and performing vapor deposition for 1h at 70 ℃ to obtain hydrophobically modified mica powder; the mass ratio of the mica powder to the methyltrimethoxysilane to the ammonia water is 4: 1: 2.
7. the method of claim 4, wherein: in the step 1), the mass ratio of the hydrophobic nano-silica to the hydrophobically modified mica powder is 3: 1; the mass ratio of the silane coupling agent KH-560 to the ethanol is 5: 100, respectively; the mass ratio of the powder to the solvent is 1: 1.
8. the method of claim 4, wherein: the mass ratio of the epoxy resin E-51 to the ethyl acetate is 5: 18, the mass ratio of the epoxy resin E-51 to the curing agent T-31 is 2: 1.
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CN115198516A (en) * | 2022-03-11 | 2022-10-18 | 天津仁爱学院 | Modified epoxy resin solution and super-hydrophobic fiber felt prepared by applying modified epoxy resin solution |
CN116589878A (en) * | 2023-07-19 | 2023-08-15 | 北京碧海云智新材料技术有限公司 | Long-acting self-cleaning graphene ceramic water paint and preparation method and application thereof |
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CN116589878A (en) * | 2023-07-19 | 2023-08-15 | 北京碧海云智新材料技术有限公司 | Long-acting self-cleaning graphene ceramic water paint and preparation method and application thereof |
CN116589878B (en) * | 2023-07-19 | 2023-10-24 | 北京碧海云智新材料技术有限公司 | Long-acting self-cleaning graphene ceramic water paint and preparation method and application thereof |
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