CN106905816B - Super-hydrophobic oleophobic coating and preparation method and use method thereof - Google Patents

Super-hydrophobic oleophobic coating and preparation method and use method thereof Download PDF

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CN106905816B
CN106905816B CN201710127998.5A CN201710127998A CN106905816B CN 106905816 B CN106905816 B CN 106905816B CN 201710127998 A CN201710127998 A CN 201710127998A CN 106905816 B CN106905816 B CN 106905816B
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epoxy resin
organic solvent
graphite fluoride
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CN106905816A (en
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杨先金
张富龙
蒋盼盼
桑晴晴
赵兴
牛文利
张帅
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East China University of Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • 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
    • 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
    • C09D7/65—Additives macromolecular
    • 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
    • C09D7/66—Additives characterised by particle size
    • C09D7/68—Particle size between 100-1000 nm

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  • Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
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  • Health & Medical Sciences (AREA)
  • Nanotechnology (AREA)
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  • Paints Or Removers (AREA)

Abstract

The invention discloses a super-hydrophobic oleophobic fluorocarbon coating, which comprises a component A and a component B; the component A comprises epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a; the mass ratio of the epoxy resin to the graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1: 0.5-3: 0.25-0.5: 0.25 to 0.5; the component B comprises a curing agent and an organic solvent B, the curing agent is aminoethyl piperazine, and the mass ratio of the epoxy resin to the curing agent is 10: 2 to 4. The invention also discloses a preparation method and a use method of the super-hydrophobic oleophobic fluorocarbon coating. The super-hydrophobic oleophobic fluorocarbon coating not only has excellent super-hydrophobic oleophobic performance, but also has better wear resistance, water flow impact resistance, corrosion resistance and adhesion performance, and can be widely used.

Description

Super-hydrophobic oleophobic coating and preparation method and use method thereof
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a super-hydrophobic oleophobic fluorocarbon coating as well as a preparation method and a use method thereof.
Background
The super-hydrophobic phenomenon comes from the understanding of lotus leaf effect in nature and the like by human beings. The super-hydrophobic and oleophobic 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 research has shown that the preparation of superhydrophobic and oleophobic 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 and oleophobic surface enables the super-hydrophobic and oleophobic surface to have wide application prospects in the aspects of water resistance, ice coating resistance, oil resistance, corrosion resistance and fluid transportation. The existing methods for preparing the super-hydrophobic and oleophobic surface comprise a sol-gel method, chemical vapor deposition, phase separation, electrodeposition, laser engraving and the like, and the methods often have the defects of troublesome preparation, harsh conditions and the like.
In a large number of methods known at present, the prepared super-hydrophobic and oleophobic surface cannot be used on a large scale due to poor water pressure impact resistance, wear resistance, corrosion resistance and the like. Therefore, the development of the super-hydrophobic material with good hydrophobicity, super-oleophobic property, good wear resistance, water flow impact resistance, corrosion resistance, strong adhesion and wide application range has important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a widely-used super-hydrophobic and oleophobic fluorocarbon coating which has good super-hydrophobic and oleophobic properties, better wear resistance, water flow impact resistance, corrosion resistance and adhesion properties, and a preparation method and a use method thereof.
The super-hydrophobic oleophobic fluorocarbon coating comprises a component A and a component B;
the component A comprises epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a; the mass ratio of the epoxy resin to the graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1: 0.5-3: 0.25-0.5: 0.25 to 0.5; the mass ratio of the organic solvent a to the total mass of the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is 1.5-10: 1;
the component B comprises a curing agent and an organic solvent B, the curing agent is aminoethyl piperazine, and the mass ratio of the epoxy resin to the curing agent is 10: 2-4, wherein 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 graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1: 1-2: 0.25-0.5: 0.25 to 0.5.
Further, the mass ratio of the epoxy resin to the graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1: 1-2: 0.25: 0.25. wherein the mass of the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is 1: 2: 0.25: the embodiment of 0.25 is particularly effective.
Preferably, the epoxy resin is E-51 epoxy resin, E-44 epoxy resin or E-31 epoxy resin. The E-51 epoxy resin, the E-44 epoxy resin and the E-31 epoxy resin are two-part type A epoxy resins, wherein E-51, E-44 and E-31 respectively represent average epoxy values of 0.51, 0.44 and 0.31. High epoxy value, low viscosity, high viscosity after solidification and high brittleness.
Further, the epoxy resin is E-51 epoxy resin, and the mass ratio of the epoxy resin to the curing agent is 10: 3.
preferably, the fluorine content of the graphite fluoride is 30-60%, and the fluorine content is more preferably 50%.
Preferably, the graphite fluoride fine particles have an average particle diameter of 100nm to 10 μm, and a smaller particle diameter of 100nm is more preferable.
Preferably, the organic solvent a and the organic solvent b are the same and are one or a mixture of more of solvents such as acetone, ethanol, dichloromethane and the like, and ethanol with low cost and toxicity is preferred.
The method for preparing the super-hydrophobic oleophobic fluorocarbon coating comprises the following steps:
preparation of component A: dissolving epoxy resin in a part of organic solvent a to obtain an epoxy resin 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 an epoxy resin solution, and stirring to obtain a component A;
preparation of component B: dissolving the aminoethylpiperazine in an organic solvent B to obtain an aminoethylpiperazine solution, namely a component B.
The application method of the super-hydrophobic oleophobic fluorocarbon coating comprises the following steps: and adding the component A into the component B, uniformly mixing, coating on the required surface and curing.
The required surface is a board surface such as a wood board, a paperboard, an epoxy resin board, an iron board and the like which can be coated with the coating.
The curing is performed at 100 ℃ for 1 hour, but is not limited thereto.
When the component A and the component B are mixed, a diluent can be added, wherein the diluent is one or a mixture of more of solvents such as acetone, ethanol, dichloromethane and the like, and is preferably consistent with the organic solvents a and B.
The invention has the beneficial effects that:
1. the invention provides a super-hydrophobic oleophobic fluorocarbon coating which comprises a component A and a component B, wherein the component A comprises epoxy resin, graphite fluoride, ammonium carbonate and polyoxyethylene ether, and the component B is prepared from a curing agent of aminoethyl piperazine. The super-hydrophobic oleophobic fluorocarbon coating has unique advantages in stability; the graphite fluoride is beneficial to the improvement of the hydrophobic and oleophobic performance of the surface 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; the ammonium carbonate can play a role in buffering and maintain acid-base balance; the components play a role in synergy in the fluorocarbon coating, so that the super-hydrophobic oleophobic fluorocarbon coating disclosed by the invention not only has excellent super-hydrophobic oleophobic performance, but also has better wear resistance, water flow impact resistance, corrosion resistance and adhesion performance.
2. The raw materials of the super-hydrophobic oleophobic fluorocarbon coating are low-cost commercial products, the formula is simplified, the variety is few, the preparation method is simple and easy, the use method is simple, convenient and quick, the super-hydrophobic oleophobic fluorocarbon coating is suitable for coating substrates made of different materials, and the super-hydrophobic oleophobic fluorocarbon coating can be widely used in a large area.
Detailed Description
The present invention will be further described with reference to 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.
The materials and equipment used in the following examples are commercially available.
Example 1
The super-hydrophobic oleophobic fluorocarbon coating
1. Composition of
And (2) component A: 2g of E-51 epoxy resin, 4g of graphite fluoride, 0.5g of ammonium carbonate, 0.5g of polyoxyethylene ether and 30mL of ethanol; wherein the fluorine content of the graphite fluoride is 50%, and the average particle diameter of the graphite fluoride particles is 100 nm.
And (B) component: 0.6g of aminoethylpiperazine and 5mL of ethanol.
2. Preparation method
Preparation of component A: firstly, dissolving E-51 epoxy resin (2g) in ethanol (5mL) to obtain an ethanol solution of the epoxy resin; dispersing graphite fluoride (4g) in ethanol (25mL), dispersing for 20min at the rotating speed of 600r/min by using an electromagnetic stirrer, adding ammonium carbonate (0.5g) and polyoxyethylene ether (0.5g) into the graphite fluoride dispersion, and dispersing for 20min at the rotating speed of 600r/min by using the electromagnetic stirrer to obtain the 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 (0.6g) was added to ethanol (5mL) for dilution and stirred to ensure dilution and dispersion, to obtain an ethanol solution of aminoethylpiperazine, component B.
3. Coating method and performance effects thereof
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 substrate plate (comprising a wood plate, a paperboard, an epoxy resin plate and an iron plate) with the size of A4 by using a spraying or brushing mode, and the substrate plate is cured for 1 hour at the high temperature of 100 ℃ to obtain a coating sample of the super-hydrophobic and oleophobic fluorocarbon coating. The coating samples were tested for properties and the results are shown in table 1.
Example 2
The superhydrophobic oleophobic fluorocarbon coating of example 2 differs from example 1 only in that: the content of graphite fluoride in the component A is 2g, and the rest components and the preparation method are the same.
Referring to example 1, the component A and the component B were uniformly mixed and coated on a wood board, and the cured coating sample was subjected to a performance test, the test results of which are shown in Table 1.
Example 3
The superhydrophobic oleophobic fluorocarbon coating of example 3 differs from example 1 only in that: the fluorine content of the graphite fluoride in the component A is 30 percent, and the rest components and the preparation method are the same.
Referring to example 1, the component A and the component B were uniformly mixed and coated on a wood board, and the cured coating sample was subjected to a performance test, the test results of which are shown in Table 1.
Comparative example 1
The fluorocarbon coating of comparative example 1 is different from that of example 1 only in that the content of graphite fluoride in component a is 0.25g, and the remaining composition and preparation method are the same.
Referring to example 1, the component A and the component B were uniformly mixed and coated on a wood board, and the cured coating sample was subjected to a performance test, the test results of which are shown in Table 1.
Comparative example 2
The fluorocarbon coating of comparative example 2 differs from example 1 only in that: the content of the epoxy resin in the component A is 0.5g, and the rest components and the preparation method are the same.
Referring to example 1, the component A and the component B were uniformly mixed and coated on a wood board, and the cured coating sample was subjected to a performance test, the test results of which are shown in Table 1.
TABLE 1 Performance test results of examples 1-4 and comparative examples 1-2
Figure BDA0001239076910000041
The test results in table 1 show that, in comparative examples 1 and 2, because the mixture ratio of the raw materials is not within the range disclosed by the present invention, each component cannot exert its own action and synergistic action, and the superhydrophobic and oleophobic properties do not meet the requirements, in the superhydrophobic and oleophobic fluorocarbon coatings of embodiments 1 to 3 of the present invention, each component can exert a better synergistic action, so that the superhydrophobic and oleophobic fluorocarbon coatings have excellent superhydrophobic and oleophobic properties, the contact angles of the coating surface and water are both greater than 150 °, and the rolling angles are both less than 6 °.
In addition, the super-hydrophobic oleophobic fluorocarbon coating also has good wear resistance, water flow impact resistance, corrosion resistance and adhesion performance. The test result shows that the water flow impact resistance can bear the water flow speed of 30m/s (the Weber number is 38000), and the water flow impact resistance can meet the indoor and outdoor use to a certain extent. In the aspect of corrosion resistance, after 1mol/L hydrochloric acid is soaked for 1 hour and 1mol/L NaOH is soaked for 1 hour, the hydrophobic and oleophobic performance can still be maintained. In the aspect of adhesion performance, the water and oil repellent performance can be still maintained after 2 hours under the condition that the wind speed is 20m/s (8-level wind power).
The above embodiment also shows that the raw materials of the super-hydrophobic oleophobic fluorocarbon coating are low-cost commercial products, the formula is simplified, the types are few, the preparation method is simple and feasible, the use method is simple, convenient and quick, the coating is suitable for coating substrates made of different materials, and the coating can be widely used in a large area.
The above description is a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the present invention may be made by those skilled in the art without departing from the principle of the present invention, and such modifications and embellishments should also be considered as within the scope of the present invention.

Claims (6)

1. A super hydrophobic and oleophobic fluorine-containing coating is composed of a component A and a component B;
the component A consists of epoxy resin, graphite fluoride, ammonium carbonate, polyoxyethylene ether and an organic solvent a;
wherein the mass ratio of the epoxy resin to the graphite fluoride to the ammonium carbonate to the polyoxyethylene ether is 1: 1-2: 0.25-0.5: 0.25 to 0.5; the mass ratio of the organic solvent a to the total mass of the epoxy resin, the graphite fluoride, the ammonium carbonate and the polyoxyethylene ether is 1.5-10: 1;
the component B consists of a curing agent and an organic solvent B;
wherein the curing agent is aminoethyl piperazine, and the mass ratio of the epoxy resin to the curing agent is 10: 2-4, wherein the mass ratio of the organic solvent b to the curing agent is (5-10): 1;
the epoxy resin is E-51 epoxy resin, and the fluorine content of the graphite fluoride is 30-50%.
2. The fluorine-containing paint according to claim 1, wherein the mass ratio of the epoxy resin to the curing agent is 10: 3.
3. the fluorine-containing coating material according to claim 1, wherein the graphite fluoride fine particles have an average particle diameter of 100nm to 10 μm.
4. The fluorine-containing paint according to claim 1, wherein the organic solvent a and the organic solvent b are the same and are one or a mixture of acetone, ethanol and dichloromethane.
5. A method for producing the fluorine-containing coating material according to any one of claims 1 to 4, characterized by comprising:
preparation of component A: dissolving epoxy resin in a part of organic solvent a to obtain an epoxy resin 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 an epoxy resin solution, and stirring to obtain a component A;
preparation of component B: dissolving the aminoethylpiperazine in an organic solvent B to obtain an aminoethylpiperazine solution, namely a component B.
6. The method of using the fluorine-containing coating material according to any one of claims 1 to 4, comprising the steps of: and adding the component A into the component B, uniformly mixing, coating on the required surface and curing.
CN201710127998.5A 2017-03-06 2017-03-06 Super-hydrophobic oleophobic coating and preparation method and use method thereof Expired - Fee Related CN106905816B (en)

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EP3569629B1 (en) 2018-05-17 2022-07-06 Evonik Operations GmbH Fast curing epoxy systems
US11286335B2 (en) 2018-05-17 2022-03-29 Evonik Operations Gmbh Fast-curing epoxy systems
EP3569630B1 (en) 2018-05-17 2022-08-03 Evonik Operations GmbH Fast curing epoxy systems
US11359048B2 (en) 2018-05-17 2022-06-14 Evonik Operations Gmbh Fast-curing epoxy systems
CN108646927A (en) * 2018-07-18 2018-10-12 杨程飞扬 A kind of portable computer keyboard
CN109321081A (en) * 2018-08-20 2019-02-12 南方科技大学 A kind of anti-corrosion of metal erosion resisting coating and preparation method thereof
EP3660069B1 (en) 2018-11-29 2024-01-03 Evonik Operations GmbH Fast curing epoxy systems
CN115304966A (en) * 2022-09-20 2022-11-08 安徽徽邦漆业有限公司 Super-hydrophobic fluorine coating and preparation method thereof

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