CN115304966A - Super-hydrophobic fluorine coating and preparation method thereof - Google Patents
Super-hydrophobic fluorine coating and preparation method thereof Download PDFInfo
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- CN115304966A CN115304966A CN202211144219.XA CN202211144219A CN115304966A CN 115304966 A CN115304966 A CN 115304966A CN 202211144219 A CN202211144219 A CN 202211144219A CN 115304966 A CN115304966 A CN 115304966A
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/506—Amines heterocyclic containing only nitrogen as a heteroatom having one nitrogen atom in the ring
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/16—Homopolymers or copolymers of vinylidene fluoride
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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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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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Abstract
The invention discloses a super-hydrophobic fluorine coating, which comprises a component A and a component B; the component A comprises polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a; the component B comprises a curing agent and an organic solvent B, wherein the curing agent is aminoethyl piperazine or methyl tetrahydrophthalic anhydride. The invention also discloses a preparation method of the super-hydrophobic fluorine coating. The super-hydrophobic fluorine coating not only has excellent super-hydrophobic performance, but also has better wear resistance, water flow impact resistance, corrosion resistance and adhesion performance, and can be widely used.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a fluorine coating and a preparation method thereof.
Background
The super-hydrophobic phenomenon is derived from the understanding of lotus leaf effect in nature and the like by human beings. The super-hydrophobic surface refers to a surface with a contact angle with water of more than 150 degrees and a rolling angle of less than 10 degrees. The phenomenon of superhydrophobicity has attracted extensive attention in recent years, and studies have shown that the preparation of superhydrophobic surfaces generally requires two conditions to be met: and (3) constructing a micro-nano secondary structure on the surface of the material by using a low-surface-energy substance.
The special surface wettability of the super-hydrophobic surface enables the super-hydrophobic surface to have wide application prospects in the aspects of water resistance, ice coating resistance, corrosion resistance and fluid transportation. The existing methods for preparing the super-hydrophobic surface comprise a sol-gel method, chemical vapor deposition, phase separation, electrodeposition, laser engraving and the like, and the methods have the defects of troublesome preparation, harsh conditions and the like.
In a large number of methods known at present, the prepared superhydrophobic surface cannot be used on a large scale due to poor resistance to hydraulic impact, abrasion resistance, corrosion resistance, and the like. Therefore, the development of the super-hydrophobic material with good hydrophobicity, better wear resistance, water impact resistance, corrosion resistance, strong adhesion and wide application range has important significance.
The fluorine coating is a high molecular material taking fluorine-containing polymer as a film forming substance, is coated on the surface of an object through a certain construction process, can be uniformly covered and well adhered on the surface of the object, and is cured to form a continuous paint film after a period of time under proper conditions. Compared with other coatings, the fluorine-containing coating has the advantages of good smoothness, strong hardness, large adhesive force, strong corrosion resistance, chemical resistance, non-adhesion, high and low temperature resistance, weather resistance, low friction and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a widely-used super-hydrophobic fluorine coating with good super-hydrophobic performance, better wear resistance, water flow impact resistance, corrosion resistance and adhesion performance and a preparation method thereof.
The coating obtained by the invention comprises two components, namely a component A and a component B;
the component A comprises polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a; wherein the mass ratio of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate and polyoxyethylene ether is 1: 0.5 to 3: 0.5 to 3: 0.1 to 0.8: 0.3 to 0.5; the mass ratio of the organic solvent a to the total mass of the polytetrafluoroethylene, the polyvinylidene fluoride, the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is (2-20): 1;
preferably, the mass ratio of the polytetrafluoroethylene to the polyvinylidene fluoride to the epoxy resin to the graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1:2:1.5:0.5:0.5;
preferably, the ratio of the mass of the organic solvent a to the total mass of the polytetrafluoroethylene, the polyvinylidene fluoride, the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is 10:1;
the component B comprises a curing agent and an organic solvent B, the curing agent is aminoethyl piperazine or methyl tetrahydrophthalic anhydride, and the mass ratio of the epoxy resin to the curing agent is 10: 2-4, the mass ratio of the organic solvent b to the curing agent is 5-10: 1;
preferably, the mass ratio of the epoxy resin to the curing agent is 10:3, the mass ratio of the organic solvent b to the curing agent is 8:1;
the organic solvent a and the organic solvent b are the same and are one or a mixture of more of ethanol, acetone, xylene, tetrahydrofuran and dichloromethane;
the polytetrafluoroethylene micro powder is DuPont MP1100 series, duPont MP1200 series, asahi glass gall FL1680 series, asahi glass gall L150J series or Dajin L5F;
preferably, the polytetrafluoroethylene micro powder is DuPont MP1100 series and DuPont MP1200 series F;
further, the epoxy resin is E-31 epoxy resin, E-44 epoxy resin or E-51 epoxy resin.
Further, the fluorine content of the graphite fluoride is 20-80%, and the average particle size is 50nm-10 μm.
The method for preparing the super-hydrophobic fluorine-containing coating comprises the following steps:
preparation of component A: placing polytetrafluoroethylene, polyvinylidene fluoride and epoxy resin in a reaction kettle, dissolving in part of organic solvent a, stirring for 10-100 minutes, and stopping stirring after the components are uniformly mixed to obtain a mixed solution;
dispersing graphite fluoride, polyoxyethylene ether and ammonium carbonate in the residual organic solvent a to obtain graphite fluoride emulsion; mixing the graphite fluoride emulsion with the epoxy resin solution, continuously stirring for 5-20 minutes, and stopping stirring after the components are uniformly mixed to obtain a component A;
preparation of component B: dissolving the aminoethyl piperazine or the methyl tetrahydrophthalic anhydride in the organic solvent B, stirring for 10 to 100 minutes, and stopping stirring after the components are uniformly mixed to obtain an aminoethyl piperazine solution, namely a component B.
The method for preparing the superhydrophobic fluorine-containing paint according to claim 5, comprising the steps of: and adding the component A into the component B, uniformly mixing, coating on the required surface, and curing, wherein the coating mode is spin coating, blade coating or spray coating.
The invention has the beneficial effects that:
1. the invention provides a super-hydrophobic fluorine coating, which comprises a component A and a component B, wherein the component A comprises polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate and polyoxyethylene ether, and the component B is prepared from a curing agent, namely aminoethyl piperazine. The super-hydrophobic fluorine coating has unique advantages in stability; the graphite fluoride is beneficial to improving the surface hydrophobic property and the corrosion resistance; the aminoethyl piperazine is a curing agent of the epoxy resin, and the epoxy resin has good mechanical property, chemical corrosion resistance and adhesion property with a substrate, so that a stable epoxy resin curing agent can be formed; the graphite fluoride can react with the aminoethyl piperazine, so that better bonding and the stability and combination of the whole system are facilitated; ammonium carbonate can play a role in buffering and maintain acid-base balance; the components play a role in synergy in the fluorine coating, so that the super-hydrophobic fluorine coating has excellent super-hydrophobic performance, and also has better wear resistance, water flow impact resistance, corrosion resistance and adhesion performance.
2. The raw materials of the super-hydrophobic fluorine coating are low-cost commercial products, the formula is simplified, the variety is few, the preparation method is simple and easy to implement, the use method is simple, convenient and quick, the super-hydrophobic fluorine coating is suitable for coating substrates made of different materials, and the super-hydrophobic fluorine coating can be widely used in a large area.
Detailed Description
The present invention is further illustrated by the following examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1
Preparation of component A: firstly, dissolving polytetrafluoroethylene (2 g), polyvinylidene fluoride (2 g) and E-51 epoxy resin (2 g) in ethanol (5 mL) to obtain a mixed solution; graphite fluoride (4 g) with a fluorine content of 50% and graphite fluoride particles with an average particle size of 100nm was dispersed in ethanol (25 mL) and dispersed with an electromagnetic stirrer at a rotation speed of 600r/min for 20min, ammonium carbonate (0.5 g) and polyoxyethylene ether (0.5 g) were added to the graphite fluoride dispersion, and the resulting dispersion was dispersed at a rotation speed of 600r/min for 20min to obtain a graphite fluoride emulsion. Then, the graphite fluoride emulsion was added to an ethanol solution of epoxy resin and stirred for 20min with an electromagnetic stirrer to ensure sufficient mixing to obtain component a (30.1 g).
Preparation of component B: aminoethylpiperazine (0.6 g) was added to ethanol (5 mL) for dilution and stirred to ensure dilution and dispersion, yielding an ethanolic aminoethylpiperazine solution, component B.
The coating method comprises the following steps: firstly, the prepared component B is added into the component A, and is dispersed for 20min at the rotating speed of 1000r/min, then is ultrasonically dispersed for 20min, and is dispersed for 10min at the rotating speed of 1000 r/min. And then coating the uniformly mixed coating on a glass plate by using a spraying or brushing mode, and curing for 1h at the high temperature of 100 ℃ to obtain a coating sample of the super-hydrophobic fluorine coating.
The obtained super-hydrophobic fluorine coating has higher water contact angle (153.1 +/-0.3 degrees) and lower rolling angle, reaches the standard of the super-hydrophobic coating, simultaneously has better wear resistance, water flow impact resistance and corrosion resistance than common coatings because of the fluorine-containing structure in the structure of the coating, and has good permeability to visible light,
example 2
Preparation of component A: first, polytetrafluoroethylene (2 g), polyvinylidene fluoride (1.8 g), and E-51 epoxy resin (2.5 g) were dissolved in acetone (5 mL) to obtain a mixed solution; graphite fluoride (4 g) containing 50% of fluorine and having an average particle size of 100nm was dispersed in acetone (25 mL) and dispersed at a rotation speed of 600r/min for 20min with an electromagnetic stirrer, and ammonium carbonate (0.5 g) and polyoxyethylene ether (0.5 g) were added to the graphite fluoride dispersion and dispersed at a rotation speed of 600r/min for 20min to obtain a graphite fluoride emulsion. Then, adding the graphite fluoride emulsion into an acetone solution of epoxy resin, and stirring for 20min by using an electromagnetic stirrer to ensure full mixing to obtain the component A.
Preparation of component B: aminoethylpiperazine (0.8 g) was added to acetone (5 mL) for dilution and stirred to ensure dilution and dispersion to give an acetone solution of aminoethylpiperazine, component B.
The coating method comprises the following steps: firstly, the prepared component B is added into the component A, and is dispersed for 20min at the rotating speed of 1000r/min, then is ultrasonically dispersed for 20min, and is dispersed for 10min at the rotating speed of 1000 r/min. And then the uniformly mixed coating is coated on a glass plate by using a spraying or brushing mode, and is cured for 2 hours at the temperature of 60 ℃ to obtain a coating sample of the super-hydrophobic fluorine coating.
The obtained super-hydrophobic fluorine coating has a higher water contact angle (152.8 +/-0.2 degrees) and a lower rolling angle, reaches the standard of the super-hydrophobic coating, and simultaneously has better wear resistance, water flow impact resistance and corrosion resistance than common coatings due to the fluorine-containing structure in the structure of the coating, and in addition, the coating can be cured at the temperature of 60 ℃, and the curing condition is simple and mild.
Example 3
Preparation of component A: firstly, dissolving polytetrafluoroethylene (2 g), polyvinylidene fluoride (2 g) and E-51 epoxy resin (2 g) in ethanol (5 mL) to obtain a mixed solution; graphite fluoride (4 g) with a fluorine content of 50% and graphite fluoride particles with an average particle size of 100nm was dispersed in ethanol (25 mL) and dispersed with an electromagnetic stirrer at a rotation speed of 600r/min for 20min, ammonium carbonate (0.5 g) and polyoxyethylene ether (0.5 g) were added to the graphite fluoride dispersion, and the resulting dispersion was dispersed at a rotation speed of 600r/min for 20min to obtain a graphite fluoride emulsion. Then, adding the graphite fluoride emulsion into an ethanol solution of epoxy resin, and stirring for 20min by using an electromagnetic stirrer to ensure full mixing to obtain the component A.
Preparation of component B: adding 0.6g of methyl tetrahydrophthalic anhydride into ethanol (5 mL) for dilution, and stirring to ensure dilution and dispersion to obtain an ethanol solution of the methyl tetrahydrophthalic anhydride, namely the component B.
The coating method comprises the following steps: firstly, the prepared component B is added into the component A, and is dispersed for 20min at the rotating speed of 1000r/min, then is ultrasonically dispersed for 20min, and is dispersed for 10min at the rotating speed of 1000 r/min. And then coating the uniformly mixed paint on an iron plate by using a spraying or brushing way, and curing for 1h at the high temperature of 100 ℃ to obtain a coating sample of the super-hydrophobic fluorine paint.
The obtained super-hydrophobic fluorine coating has a higher water contact angle (154.0 +/-0.3 degrees) and a lower rolling angle, reaches the standard of the super-hydrophobic coating, and simultaneously has better wear resistance, water flow impact resistance and corrosion resistance than common coatings due to the fluorine-containing structure in the structure of the coating, and in addition, the coating has good permeability to visible light.
Claims (5)
1. The super-hydrophobic fluorine-containing coating is characterized by comprising two components, namely a component A and a component B;
the component A comprises polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a; wherein the mass ratio of polytetrafluoroethylene, polyvinylidene fluoride, epoxy resin, graphite fluoride, ammonium carbonate and polyoxyethylene ether is 1: 0.5 to 3: 0.5 to 3: 0.1 to 0.8: 0.3 to 0.5; the mass ratio of the organic solvent a to the total mass of the polytetrafluoroethylene, the polyvinylidene fluoride, the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is (2-20): 1;
the component B comprises a curing agent and an organic solvent B, the curing agent is aminoethyl piperazine or methyl tetrahydrophthalic anhydride, and the mass ratio of the epoxy resin to the curing agent is 10: 2-4, the mass ratio of the organic solvent b to the curing agent is 5-10: 1;
the organic solvent a and the organic solvent b are the same and are one or a mixture of more of ethanol, acetone, xylene, tetrahydrofuran and dichloromethane.
2. The super-hydrophobic fluorine-containing coating according to claim 1, wherein the polytetrafluoroethylene micropowder is DuPont MP1100 series, duPont MP1200 series, asahi glass powder FL1680 series, asahi glass powder L150J series or Dajin L5F;
the epoxy resin is E-31 epoxy resin, E-44 epoxy resin or E-51 epoxy resin.
3. The super-hydrophobic fluorine-containing paint according to claim 1, wherein the fluorine content of the graphite fluoride is 20-80%, and the average particle size is 50nm-10 μm.
4. A method for preparing the superhydrophobic fluorine-containing coating material according to any one of claims 1 to 4, comprising:
preparation of component A: placing polytetrafluoroethylene, polyvinylidene fluoride and epoxy resin in a reaction kettle, dissolving in part of organic solvent a, stirring for 10-100 minutes, and stopping stirring after the components are uniformly mixed to obtain a mixed solution;
dispersing graphite fluoride, polyoxyethylene ether and ammonium carbonate in the residual organic solvent a to obtain graphite fluoride emulsion; and (3) mixing the graphite fluoride emulsion with the epoxy resin solution, continuously stirring for 5-20 minutes, and stopping stirring after the components are uniformly mixed to obtain the component A.
Preparation of component B: dissolving the aminoethyl piperazine or the methyl tetrahydrophthalic anhydride in the organic solvent B, stirring for 10 to 100 minutes, and stopping stirring after the components are uniformly mixed to obtain an aminoethyl piperazine solution, namely a component B.
5. The method for preparing the superhydrophobic fluorine-containing paint according to claim 4, comprising the steps of: and adding the component A into the component B, uniformly mixing, coating on the required surface, and curing, wherein the coating mode is spin coating, blade coating or spray coating.
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| CN116554761A (en) * | 2023-06-20 | 2023-08-08 | 湖北卓熙氟化股份有限公司 | Wear-resistant durable super-hydrophobic coating for windscreen wiper and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905816A (en) * | 2017-03-06 | 2017-06-30 | 华东理工大学 | Super-hydrophobic oleophobic coating and preparation method thereof and application method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106905816A (en) * | 2017-03-06 | 2017-06-30 | 华东理工大学 | Super-hydrophobic oleophobic coating and preparation method thereof and application method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116554761A (en) * | 2023-06-20 | 2023-08-08 | 湖北卓熙氟化股份有限公司 | Wear-resistant durable super-hydrophobic coating for windscreen wiper and preparation method thereof |
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