CN113185898A - Method for preparing super-hydrophobic dual-functional coating by adopting spraying method - Google Patents
Method for preparing super-hydrophobic dual-functional coating by adopting spraying method Download PDFInfo
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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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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention discloses a method for preparing MWCNTs-COOH (8-HQ)/ZnO super-hydrophobic dual-functional coating by adopting a spraying method, firstly loading 8-hydroxyquinoline on a carboxylated multi-wall carbon nanotube, then modifying nano zinc oxide by hexadecyl trimethoxy silane, and then mixing the two to obtain MWCNTs-COOH (8-HQ)/ZnO compound; spraying an epoxy resin thin layer on the surface of the substrate, and then spraying an MWCNTs-COOH (8-HQ)/ZnO composite layer on the surface of the epoxy resin layer. According to the invention, the carboxylated multi-walled carbon nanotube is used as a nano container load corrosion inhibitor, the modified nano zinc oxide can reduce the surface energy and provide a micro-nano coarse structure, and the combination of super-hydrophobicity and a corrosion inhibitor enables the coating to have a dual-function anticorrosion effect; the invention uses fluoride-free materials, is green and environment-friendly, has low production cost, simple preparation method, low requirement on reaction equipment and mild reaction condition, and can be produced in large scale.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of a MWCNTs-COOH (8-HQ)/ZnO super-hydrophobic dual-function coating.
Background
The development of the aviation manufacturing industry cannot be supported by the powerful aviation materials, and the emerging aviation materials are a solid foundation for continuous breakthrough and innovation of the aviation manufacturing industry. The aluminum alloy has the characteristics of high strength, low density, good ductility and the like, so that the aluminum alloy is widely applied to structures such as airplane frames, skins, fuel tanks, landing gear struts and the like, and is an important aviation material. However, in an environmental medium (e.g., corrosive element Cl in the atmosphere)-，SO2，NO2Etc.) the aluminum alloy is very sensitive to corrosion. Particularly, shipboard airplanes, seaplane airplanes and the like are often affected by water vapor, salt fog and other environments, which causes corrosion damages such as pitting corrosion, denudation and the like. With the increase of the service life of the airplane, the problem that the structure of the airplane is corroded by the environmental atmosphere becomes more and more prominent, and the problem becomes a serious problem for civil and military airplanes. At present, there are many measures for metal corrosion prevention, wherein it is more effective to cover a protective film on the metal surface, and the combination of super-hydrophobicity and corrosion inhibitor makes the coating have the dual-function corrosion prevention effect, so the research on the super-hydrophobic dual-function coating on the surface of the aluminum substrate has great significance.
Disclosure of Invention
In order to improve the super-hydrophobic performance of the substrate surface, the invention provides a method for preparing a MWCNTs-COOH (8-HQ)/ZnO super-hydrophobic dual-function coating on the substrate surface by adopting a spraying method.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme.
A method for preparing a super-hydrophobic dual-functional coating by adopting a spraying method is characterized by comprising the following steps: firstly loading 8-hydroxyquinoline (8-HQ) on a carboxylated multi-wall carbon nanotube (MWCNTs-COOH), then modifying nano zinc oxide by hexadecyl trimethoxy silane (HOTS), and mixing the two to obtain an MWCNTs-COOH (8-HQ)/ZnO compound; spraying an epoxy resin thin layer on the surface of a substrate, then spraying an MWCNTs-COOH (8-HQ)/ZnO composite layer on the surface of the epoxy resin layer, and testing the static contact angle and the rolling angle of the coating after the coating is completely cured.
Further, the method for preparing the super-hydrophobic bifunctional coating on the surface of the substrate by adopting the spraying method comprises the following specific steps:
(1) dispersing 8-hydroxyquinoline in deionized water, then adding a carboxylated multi-walled carbon nanotube, carrying out ultrasonic oscillation for 0.5 h, and carrying out magnetic stirring for 4 h under the water bath condition of 45 ℃ to form a uniformly dispersed suspension A;
(2) the suspension A was suction filtered 3 times to ensure maximum loading of 8-HQ on the MWCNTs-COOH, then dried in a vacuum oven at 60 ℃ for 12 h, ground to a powder for use.
(3) Dispersing nano ZnO in absolute ethyl alcohol, adding a hexadecyl trimethoxy silane modifier and a small amount of water, and performing ultrasonic oscillation for 0.5 h to form a solution B;
(4) adding the ground powder into the solution B, and magnetically stirring for 4 hours at the temperature of 45 ℃ in a water bath;
(5) epoxy resin and curing agent the ratio of 1: 1, diluting with absolute ethyl alcohol, uniformly stirring, spraying a thin layer on the surface of the treated aluminum substrate, and curing for 5 min at room temperature;
(6) then the MWCNTs-COOH (8-HQ)/ZnO compound solution is evenly sprayed on the surface of the epoxy resin film.
(7) Airing the prepared coating for 1 h at room temperature, and then drying in a vacuum drying oven at 60 ℃ for 12 h;
(8) after the coating is completely cured, a contact angle measuring instrument is used for testing the static contact angle and the rolling angle of the surface of the coating, and the static contact angle of the surface of the coating to water is 165 +/-1.6 degrees, and the rolling angle of the surface of the coating is 5 +/-0.7 degrees.
Furthermore, the carboxylated multi-walled carbon nanotubes in the step (1) are used as a nano container loaded corrosion inhibitor, so that the effect of the corrosion inhibitor is better.
Further, hexadecyl trimethoxy silane in the step (3) is used as a modifier, and is dehydrated and combined with hydroxyl on the surface of zinc oxide after hydrolysis, and a large amount of low surface groups reduce the surface energy of nano ZnO.
Further, the thickness of the epoxy resin coating in the step (5) can affect the embedding combination with the ZnO-MWCNTs compound layer, and a thin layer is preferably adopted for the epoxy resin coating, and the thickness is not preferably too large.
Further, the nano ZnO-MWCNTs compound solution is uniformly sprayed on the surface of the epoxy resin film by adopting a spraying method in the step (6), so that a micro/nano coarse structure is easily formed, and a super-hydrophobic effect is achieved.
The invention has the advantages that: (1) the carboxylated multi-walled carbon nano tube is used as a nano container load corrosion inhibitor, so that the efficiency of the corrosion inhibitor is improved; (2) the modifier adopts hexadecyl trimethoxy silane, uses a fluorine-free material, and is green and environment-friendly; (3) the aluminum substrate and the composite layer are combined by using the epoxy resin, the epoxy resin has strong adhesion to the base material, higher mechanical strength, simple construction and no pollution to the environment; (4) the coating is prepared by adopting a spraying method, so that the cost is low, the method is simple, the large-scale production can be realized, and the coating is not limited by a base material; (5) the nano zinc oxide, the modifier, the epoxy resin, the carboxylated multi-walled carbon nanotube and the like used in the invention are common raw materials, have low requirements on reaction equipment and have mild reaction conditions.
Drawings
FIG. 1 is an infrared spectrum of MWCNTs-COOH, 8-HQ, MWCNTs-COOH (8-HQ).
FIG. 2 is a thermogravimetric plot of MWCNTs-COOH, 8-HQ, MWCNTs-COOH (8-HQ).
FIG. 3 is an infrared spectrum of ZnO, Hexadecyltrimethoxysilane (HOTS), ZnO/HOTS.
FIG. 4 is an SEM image of a ZnO/HOTS-MWCNTs super-hydrophobic coating.
Fig. 5 is a schematic diagram of static contact angle and rolling angle of the super-hydrophobic coating.
Detailed Description
The present invention is illustrated by the examples given in conjunction with the examples given, but the examples given do not limit the invention in any way.
The first embodiment is as follows: weighing 2 g of 8-hydroxyquinoline, grinding the 8-hydroxyquinoline into powder, dispersing the powder in 20ml of deionized water, ultrasonically oscillating for 30 min, adding 0.1 g of carboxylated multi-walled carbon nanotube, magnetically stirring for 4 h at the temperature of 45 ℃ at 3000 r/s, performing suction filtration for 3 times to ensure that 8-HQ is loaded on MWCNTs-COOH to the maximum, drying for 12 h at the temperature of 60 ℃ in a vacuum drying oven, and grinding the powder for later use. 2 g of ZnO (30 nm grade) are weighed out and dispersed in 40 mL of absolute ethanol, and 0.2 mL of hexadecyltrimethoxysilane and 3 drops of H are added2O, performing ultrasonic oscillation for 30 min to obtain a solution A; adding the ground powder into the solution A, heating in a water bath at 45 ℃, and magnetically stirring for 4 hours; epoxy resin and curing agent the ratio of 1: 1, diluting with absolute ethyl alcohol, uniformly stirring, spraying a thin layer on the surface of the treated aluminum substrate, curing at room temperature for 5 min, and uniformly spraying the MWCNTs-COOH (8-HQ)/ZnO compound solution on the surface of the epoxy resin film. And (3) airing the prepared coating for 1 h at room temperature, and then drying the coating for 12 h in a vacuum drying oven at 60 ℃. And after the coating is completely cured, testing the static contact angle and the rolling angle of the surface of the coating by using a contact angle measuring instrument.
Example two: weighing 2 g of 8-hydroxyquinoline, grinding the 8-hydroxyquinoline into powder, dispersing the powder in 20ml of deionized water, ultrasonically oscillating for 30 min, adding 0.2 g of carboxylated multi-walled carbon nanotubes, magnetically stirring for 4 h at the temperature of 45 ℃ at 3000 r/s, performing suction filtration for 3 times to ensure that 8-HQ is loaded on MWCNTs-COOH to the maximum extent, then drying for 12 h at the temperature of 60 ℃ in a vacuum drying oven, and grinding the powder for later use. Weighing 2 g of ZnO (30 nm grade) and dispersing in 40 mL of absolute ethyl alcohol, adding 0.2 mL of hexadecyl trimethoxy silane and 3 drops of H2O, and performing ultrasonic oscillation for 30 min to obtain a solution A; adding the ground powder into the solution A, heating in a water bath at 45 ℃, and magnetically stirring for 4 hours; epoxy resin and curing agent the ratio of 1: 1, diluting with absolute ethyl alcohol, uniformly stirring, spraying a thin layer on the surface of the treated aluminum substrate, curing at room temperature for 5 min, and uniformly spraying the MWCNTs-COOH (8-HQ)/ZnO compound solution on the surface of the epoxy resin film. And (3) airing the prepared coating for 1 h at room temperature, and then drying the coating for 12 h in a vacuum drying oven at 60 ℃. And after the coating is completely cured, testing the static contact angle and the rolling angle of the surface of the coating by using a contact angle measuring instrument.
Example three: weighing 2 g of 8-hydroxyquinoline, grinding the 8-hydroxyquinoline into powder, dispersing the powder in 20ml of deionized water, ultrasonically oscillating for 30 min, adding 0.3 g of carboxylated multi-walled carbon nanotubes, magnetically stirring for 4 h at the temperature of 45 ℃ at 3000 r/s, performing suction filtration for 3 times to ensure that 8-HQ is loaded on MWCNTs-COOH to the maximum extent, then drying for 12 h at the temperature of 60 ℃ in a vacuum drying oven, and grinding the powder for later use. Weighing 2 g of ZnO (30 nm grade) and dispersing in 40 mL of absolute ethyl alcohol, adding 0.2 mL of hexadecyl trimethoxy silane and 3 drops of H2O, and performing ultrasonic oscillation for 30 min to obtain a solution A; adding the ground powder into the solution A, heating in a water bath at 45 ℃, and magnetically stirring for 4 hours; epoxy resin and curing agent the ratio of 1: 1, diluting with absolute ethyl alcohol, uniformly stirring, spraying a thin layer on the surface of the treated aluminum substrate, curing at room temperature for 5 min, and uniformly spraying the MWCNTs-COOH (8-HQ)/ZnO compound solution on the surface of the epoxy resin film. And (3) airing the prepared coating for 1 h at room temperature, and then drying the coating for 12 h in a vacuum drying oven at 60 ℃. And after the coating is completely cured, testing the static contact angle and the rolling angle of the surface of the coating by using a contact angle measuring instrument.
As shown in FIG. 1, MWCNTs-COOH (8-HQ) was at 2945-2926cm-1The absorption peak of (A) is attributed to the C-H stretching vibration on the benzene ring of 8-HQ, and the MWCNTs-COOH (8-HQ) is at 1089 cm-1The absorption peak of the method is attributed to the telescopic vibration of 8-HQC-N, and the successful loading of 8-HQ on MWCNTs-COOH can be obtained.
As shown in FIG. 2, there is a significant weight loss process from 70 to 180 ℃ due to the decomposition of 8-HQ in 8-HQ and MWCNTs-COOH (8-HQ). Accordingly, there is no weight loss between the same ranges of the MWCNTs-COOH curve. Therefore, the loading of 8-HQ in MWCNTs-COOH (8-HQ) was about 23%.
As shown in FIG. 3, ZnO/HOTS was used at 2926-2840cm-1The absorption peak of (A) is attributed to C-H stretching vibration of alkane in HOTS, and ZnO/HOTS is 1462cm-1The absorption peak of (a) is attributed to the flexural vibration of C-H of alkane in HOTS,ZnO/HOTS at 1099cm-1The absorption peak of (A) is attributed to the stretching vibration of Si-O-Si in HOTS, and the HOTS can be obtained to successfully modify ZnO.
As shown in the scanning electron microscope image of the surface of the MWCNTs-COOH (8-HQ)/ZnO coating shown in FIG. 4, it can be seen that the MWCNTs-COOH is wrapped by the nano ZnO to form a loose, porous and layered micron/nano coarse structure, which is the main reason for forming super-hydrophobicity of the coating.
Fig. 5 is a schematic diagram of static contact angle and rolling angle of the super-hydrophobic coating.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (6)
1. A method for preparing a super-hydrophobic dual-functional coating by adopting a spraying method is characterized by comprising the following steps: firstly loading 8-hydroxyquinoline (8-HQ) on a carboxylated multi-wall carbon nanotube (MWCNTs-COOH), then modifying nano zinc oxide by hexadecyl trimethoxy silane (HOTS), and mixing the two to obtain an MWCNTs-COOH (8-HQ)/ZnO compound; spraying an epoxy resin thin layer on the surface of a substrate, then spraying an MWCNTs-COOH (8-HQ)/ZnO composite layer on the surface of the epoxy resin layer, and testing the static contact angle and the rolling angle of the coating after the coating is completely cured.
2. The method for preparing the super-hydrophobic bifunctional coating by the spray coating method according to claim 1, which comprises the following steps:
(1) dispersing 8-hydroxyquinoline in deionized water, then adding a carboxylated multi-walled carbon nanotube, carrying out ultrasonic oscillation for 0.5 h, and carrying out magnetic stirring for 4 h under the water bath condition of 45 ℃ to form a uniformly dispersed suspension A;
(2) carrying out suction filtration on the suspension A for 3 times to ensure that 8-HQ is loaded on MWCNTs-COOH at the maximum, then drying for 12 h at 60 ℃ in a vacuum drying oven, and grinding into powder for later use;
(3) dispersing nano ZnO in absolute ethyl alcohol, adding a hexadecyl trimethoxy silane modifier and a small amount of water, and performing ultrasonic oscillation for 0.5 h to form a solution B;
(4) adding the ground powder into the solution B, and magnetically stirring for 4 hours at the temperature of 45 ℃ in a water bath;
(5) epoxy resin and curing agent the ratio of 1: 1, diluting with absolute ethyl alcohol, uniformly stirring, spraying a thin layer on the surface of the treated aluminum substrate, and curing for 5 min at room temperature;
(6) then evenly spraying the MWCNTs-COOH (8-HQ)/ZnO compound solution on the surface of the epoxy resin film;
(7) airing the prepared coating for 1 h at room temperature, and then drying in a vacuum drying oven at 60 ℃ for 12 h;
(8) after the coating is completely cured, a contact angle measuring instrument is used for testing the static contact angle and the rolling angle of the surface of the coating, and the static contact angle of the surface of the coating to water is 165 +/-1.6 degrees, and the rolling angle of the surface of the coating is 5 +/-0.7 degrees.
3. The method for preparing the super-hydrophobic bifunctional coating by the spray coating method according to claim 2, wherein the spray coating method comprises the following steps: the carboxylated multi-walled carbon nanotubes in the step (1) are used as a nano-container loading corrosion inhibitor.
4. The method for preparing the super-hydrophobic bifunctional coating by the spray coating method according to claim 2, wherein the spray coating method comprises the following steps: and (3) taking hexadecyl trimethoxy silane as a modifier, and dehydrating and combining with hydroxyl on the surface of zinc oxide after hydrolysis, wherein a large number of low-surface groups reduce the surface energy of the nano ZnO.
5. The method for preparing the super-hydrophobic bifunctional coating by the spray coating method according to claim 2, wherein the spray coating method comprises the following steps: the thickness of the epoxy resin coating in the step (5) can influence the embedding combination with the ZnO-MWCNTs compound layer, and a thin layer is preferably adopted for the epoxy resin coating.
6. The method for preparing the super-hydrophobic bifunctional coating by the spray coating method according to claim 2, wherein the spray coating method comprises the following steps: and (3) uniformly spraying the nano ZnO-MWCNTs compound solution on the surface of the epoxy resin film by adopting a spraying method in the step (6), so that a micro/nano coarse structure is easily formed.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113637391A (en) * | 2021-08-20 | 2021-11-12 | 西安石油大学 | Graphene self-repairing solvent-free epoxy anticorrosive paint and preparation method and use method thereof |
| CN113717556A (en) * | 2021-10-22 | 2021-11-30 | 西南交通大学 | Chromium-free zinc-aluminum coating containing nano filler and preparation method and application thereof |
| CN114085590A (en) * | 2021-11-15 | 2022-02-25 | 中北大学 | Method for forming organic-inorganic hybrid super-hydrophobic anticorrosive coating on surface of carbon steel |
| CN114656864A (en) * | 2022-04-05 | 2022-06-24 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
| CN114686103A (en) * | 2022-03-30 | 2022-07-01 | 陕西科技大学 | Super-hydrophobic composite anti-corrosion coating and construction method and application thereof |
| CN114988719A (en) * | 2022-06-22 | 2022-09-02 | 常州大学 | High-transparency hydrophobic-oleophobic self-cleaning coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113637391A (en) * | 2021-08-20 | 2021-11-12 | 西安石油大学 | Graphene self-repairing solvent-free epoxy anticorrosive paint and preparation method and use method thereof |
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| CN114656864A (en) * | 2022-04-05 | 2022-06-24 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
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| CN114988719A (en) * | 2022-06-22 | 2022-09-02 | 常州大学 | High-transparency hydrophobic-oleophobic self-cleaning coating and preparation method thereof |
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Application publication date: 20210730 |