CN114985234A - Super-hydrophobic coating and preparation method thereof - Google Patents

Super-hydrophobic coating and preparation method thereof Download PDF

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CN114985234A
CN114985234A CN202210479549.8A CN202210479549A CN114985234A CN 114985234 A CN114985234 A CN 114985234A CN 202210479549 A CN202210479549 A CN 202210479549A CN 114985234 A CN114985234 A CN 114985234A
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coating
cyanoacrylate
silicone oil
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龙宇华
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Beijing Xiaomi Mobile Software Co Ltd
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    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
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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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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
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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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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
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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
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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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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    • B05D2502/00—Acrylic polymers
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    • B05D2518/00—Other type of polymers
    • B05D2518/10—Silicon-containing polymers
    • B05D2518/12—Ceramic precursors (polysiloxanes, polysilazanes)
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    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2601/00—Inorganic fillers
    • B05D2601/20—Inorganic fillers used for non-pigmentation effect
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2601/00—Inorganic fillers
    • B05D2601/20—Inorganic fillers used for non-pigmentation effect
    • B05D2601/22—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2601/00—Inorganic fillers
    • B05D2601/20—Inorganic fillers used for non-pigmentation effect
    • B05D2601/24—Titanium dioxide, e.g. rutile

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Abstract

The application discloses a super-hydrophobic coating and a preparation method thereof. The super-hydrophobic coating comprises a first coating and a second coating; the first coating is disposed on a substrate, the first coating comprising a polymer of an alpha-cyanoacrylate and inorganic nanoparticles; the second coating is disposed on the first coating, the second coating comprising silicone oil; the silicone oil includes a liquid-state polysiloxane having an organic side chain and being free of an active hydrogen group. The super-hydrophobic coating has the characteristics of good hydrophobicity, high mechanical strength, good wear resistance, good stability, good oil stain resistance, wide application range and the like.

Description

Super-hydrophobic coating and preparation method thereof
Technical Field
The application belongs to the technical field of coatings, and particularly relates to a super-hydrophobic coating and a preparation method thereof.
Background
The super-hydrophobic material has special non-hydrophilic and self-cleaning properties, has many characteristic properties such as dust prevention, drag reduction, ice prevention and the like, arouses development interests of scientists and engineers in a plurality of application fields, and has wide application in daily life and various industrial fields in the aspects of self-cleaning coatings, impermeable textiles, microfluids, laboratory chip equipment, biotechnology, fluid drag reduction equipment, ice-covering-preventing materials and the like.
The surface of the super-hydrophobic material has a larger contact angle and a smaller sliding angle, and the structure of the surface and the specific substance of the surface influence the wetting performance. Two methods are mainly used for preparing the surface of the super-hydrophobic material in the current research: firstly, preparing a proper micro-nano structure on the surface of a hydrophobic material, wherein the structure can be prepared by methods such as chemical etching, electrochemical deposition, a sol-gel method, chemical vapor deposition, a template method, photoetching, a phase separation and self-assembly method, chemical deposition, a nano silicon dioxide method and the like; the second is to modify the surface of a solid material with a suitable roughness so that it has a low surface energy, whereas decorations are typically chemical agents and are mostly fluorides. To obtain high contact angles, many superhydrophobic surfaces are processed with fluorosurfactants. While very high contact angles can be obtained by surface modification using fluorosurfactants, the cost of these chemicals is generally high.
In recent years, with the research of the super-hydrophobic material, researchers regulate and control the microstructure of the surface of the super-hydrophobic material through various methods to obtain a micro rough structure, so that the super-hydrophobic performance of the surface is realized. However, most of these methods suffer from various drawbacks and disadvantages; in particular, the micro-rough structure prepared by a chemical method generally has the problems of low mechanical strength, poor wear resistance, poor stability and the like, and is easily damaged by external force, so that the super-hydrophobicity is lost; the surface thereof is also easily contaminated with oily substances, resulting in deterioration of hydrophobicity.
Therefore, the development of a superhydrophobic surface material with convenient preparation, high mechanical strength, good wear resistance and good stability is a problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the application provides a super-hydrophobic coating and a preparation method thereof. The super-hydrophobic coating has the characteristics of good hydrophobicity, high mechanical strength, good wear resistance, good stability, good oil stain resistance, wide application range and the like.
In order to achieve the technical effects, the technical scheme adopted by the application is as follows:
in a first aspect of exemplary embodiments of the present application, there is provided a method of preparing a superhydrophobic coating, including:
coating a first coating liquid on a substrate, wherein the first coating liquid comprises the following raw materials in parts by mass: 1-30 parts by mass of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles and 90-110 parts by mass of a first organic solvent;
evaporating the first organic solvent under a first preset condition, and carrying out in-situ spontaneous polymerization on the alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, wherein the polymer of the alpha-cyanoacrylate bonds the inorganic nanoparticles on the surface of the substrate to form the first coating;
coating the second coating liquid on the first coating, wherein the second coating liquid comprises the following raw materials in parts by mass: 0.01-10 parts by mass of silicone oil and 90-110 parts by mass of a second organic solvent; the silicone oil comprises a liquid polysiloxane having an organic side chain and no active hydrogen group;
and under a second preset condition, evaporating the second organic solvent to form a silicon oil layer, wherein the silicon oil layer is the second coating.
In some embodiments, the inorganic nanoparticles comprise one or more of silica nanoparticles, titania nanoparticles, zinc oxide nanoparticles, alumina nanoparticles, ferric oxide nanoparticles, zirconia nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles, cobalt oxide nanoparticles.
In some embodiments, the α -cyanoacrylate comprises one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate, and octyl 2-cyanoacrylate.
In some embodiments, the silicone oil comprises one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methylphenyl silicone oil, methyl ethoxy silicone oil, and methyl trifluoropropyl silicone oil.
In some embodiments, the first organic solvent comprises one or more of an ester organic solvent, a ketone organic solvent, a haloalkane organic solvent, and an aprotic polar solvent.
In some embodiments, the second organic solvent comprises one or more of halogenated alkanes, halogenated alkenes, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol, butanol.
In some embodiments, the mass ratio of the alpha-cyanoacrylate to the inorganic nanoparticles, C1, is 1:1 to 15: 1.
In some embodiments, the mass ratio C2 of the inorganic nanoparticles in the first coating liquid to the silicone oil in the second coating liquid is 10:1 to 100: 1.
In a second aspect of exemplary embodiments of the present application, there is provided a superhydrophobic coating prepared using the above preparation method, including a first coating layer and a second coating layer;
the first coating disposed on the substrate, the first coating comprising: 1-30 parts by mass of a polymer of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles;
the second coating disposed on the first coating, the second coating comprising: 0.01 to 10 parts by mass of a silicone oil; the silicone oil includes a liquid-state polymerized siloxane having an organic side chain and containing no active hydrogen group.
In a third aspect of the exemplary embodiments herein, there is provided a use of a superhydrophobic coating in the preparation of an electronic device.
Benefits of the present application include, but are not limited to: the super-hydrophobic coating prepared by the preparation method of the super-hydrophobic coating comprises a first coating and a second coating, wherein the second coating is coated on the first coating; the first coating comprises polymers of alpha-cyanoacrylate and inorganic nanoparticles, and can form firm micro-nano coarse structures; the super-hydrophobic coating has good adhesive force, mechanical strength, wear resistance and stability; the second coating comprises a silicon oil layer positioned on the micro-nano-scale protruding structure, so that the super-hydrophobic coating has good oil stain resistance.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the application and together with the description, serve to explain the principles of the embodiments of the application. In the drawings, like reference numerals are used to indicate like elements. The drawings in the following description are directed to some, but not all embodiments of the application. For a person skilled in the art, other figures can be derived from these figures without inventive effort.
FIG. 1 is a schematic diagram illustrating the structure of a superhydrophobic coating, according to an exemplary embodiment.
Reference numerals:
100-superhydrophobic coating, 1-first coating, 11-inorganic nanoparticles, polymer of 12-alpha-cyanoacrylate, 2-second coating, 3-substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the present application will be clearly and completely described below with reference to the embodiments of the present application, and it is obvious that the described embodiments are some, but not all embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The application provides a super-hydrophobic coating and a preparation method thereof.
A method of preparing a superhydrophobic coating of an exemplary embodiment of the present application includes:
coating a first coating liquid on a substrate, wherein the first coating liquid comprises the following raw materials in parts by mass: 1-30 parts by mass of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles and 90-110 parts by mass of a first organic solvent;
evaporating the first organic solvent under a first preset condition, carrying out in-situ spontaneous polymerization on the alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, and bonding the inorganic nanoparticles on the surface of the substrate by the polymer of the alpha-cyanoacrylate to form a first coating;
coating a second coating liquid on the first coating, wherein the second coating liquid comprises the following raw materials in parts by mass: 0.01-10 parts by mass of silicone oil and 90-110 parts by mass of a second organic solvent; the silicone oil comprises a liquid polysiloxane having an organic side chain and no active hydrogen group;
and under a second preset condition, evaporating the second organic solvent to form a silicon oil layer, wherein the silicon oil layer is a second coating.
In the process of preparing the super-hydrophobic coating, the first coating is prepared from alpha-cyanoacrylate, inorganic nano-particles and a first organic solvent, the inorganic nano-particles form a micro-nano-scale convex structure, the first organic solvent is evaporated, the alpha-cyanoacrylate is subjected to polymerization reaction to generate a polymer of the alpha-cyanoacrylate, and the inorganic nano-particles can be bonded on a substrate to form a firm micro-nano-scale rough structure to prepare the first coating; the second coating is prepared from silicone oil and a second organic solvent, the second organic solvent is evaporated, the silicone oil forms a very thin coating on the micro-nano-scale protruding structure, and the silicone oil has very low surface energy and oil stain resistance. Therefore, the prepared super-hydrophobic coating has good hydrophobic property, mechanical strength, wear resistance, stability and anti-contamination property.
In this application, inorganic nano-particle size is small, and the particle diameter is nanometer level, can coat the protruding structure that forms nanometer level on the substrate surface for the water droplet is held up, can only contact the top portion of protruding structure, has one deck air film between water droplet and protruding structure surface. Therefore, the actual contact area of the water droplets with the surface is small, and the water droplets easily roll off the surface.
In exemplary embodiments provided herein, the inorganic nanoparticles include one or more of silica nanoparticles, titania nanoparticles, zinc oxide nanoparticles, alumina nanoparticles, iron trioxide nanoparticles, zirconium dioxide nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles, cobalt oxide nanoparticles. Wherein, the particle size of the inorganic nano-particles can be 20-800nm, also can be 30-250nm, also can be 50-200 nm. The inorganic nano-particles with reasonable particle size range are beneficial to forming a micro-nano-level convex structure, so that the hydrophobic effect of the super-hydrophobic coating is improved.
In the present application, the polymer of α -cyanoacrylate is polymerized from α -cyanoacrylate, which is a binder for binding inorganic nanoparticles to a substrate to form a first coating layer. The structural general formula of the alpha-cyanoacrylate is shown in chemical formula 1:
Figure BDA0003627176600000061
wherein R is alkyl, or alkoxyalkyl.
The alpha-cyanoacrylate contains cyano group and ester bond with strong polarity, has strong adhesion to polar adherends, shows high adhesion strength, and forms polymer molecular chains with good adhesion on the surfaces of various materials.
In the exemplary embodiments provided herein, the α -cyanoacrylate includes one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate, and octyl 2-cyanoacrylate. Alpha-cyanoacrylate is subjected to in-situ spontaneous polymerization reaction under the condition of meeting moisture (or water vapor) in the air at normal temperature without ultraviolet irradiation to generate a polymer of the alpha-cyanoacrylate, and the polymer is crosslinked into a film; the first coating can be rapidly cured at normal temperature by conventional coating means.
In exemplary embodiments provided herein, the silicone oil comprises a liquid polymeric siloxane having organic side chains and free of active hydrogen groups; the silicone oil can be one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl ethoxy silicone oil and methyl trifluoro propyl silicone oil.
The silicone oil comprises liquid polysiloxane which has organic side chain and does not contain active hydrogen group, and the surface energy of the silicone oil is lower due to the organic side chain, so that the interaction force between the surface of the formed coating and water drops is small, and the water drops can easily roll off from the surface. In addition, the silicone oil does not contain active hydrogen groups, so that the silicone oil has strong chemical inertia and is difficult to generate polymerization reaction, and the silicone oil has good dustproof and oil-proof performance and can improve the oil stain resistance of the coating. In order to form a uniform and smooth second coating, a silicone oil having a low viscosity, such as a silicone oil having a viscosity of 50 to 400 mPas, may be selected.
In exemplary embodiments provided herein, the first organic solvent includes one or more of an ester organic solvent, a ketone organic solvent, a halogenated alkane organic solvent, and an aprotic polar solvent. The ester organic solvent, the ketone organic solvent, the halogenated alkane organic solvent and the aprotic polar solvent have high solubility to the inorganic nanoparticles and the alpha-cyanoacrylate, so that the inorganic nanoparticles and the alpha-cyanoacrylate can be uniformly mixed, and the first coating is conveniently formed. The first organic solvent may include one or more of ethyl acetate, butyl acetate, isobutyl acetate, acetone, butanone, pentanone, dichloromethane, dimethylformamide.
In exemplary embodiments provided herein, the second organic solvent comprises one or more of halogenated alkanes, halogenated alkenes, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol, butanol. These second organic solvents can better dissolve the silicone oil, facilitating the formation of a thin, uniform layer of silicone oil, i.e., the second coating, on the surface of the first coating.
In exemplary embodiments provided herein, the haloalkane comprises one or more of trifluorotrichloroethane, monofluorodichloroethane, dichloropentafluoropropane, pentafluorobutane, 1-dichloro-1-fluoroethane. The halogenated olefin may be trans-1, 2-dichloroethylene.
In the exemplary embodiments provided herein, the mass ratio of alpha-cyanoacrylate to inorganic nanoparticles, C1, is from 1:1 to 15: 1.
In order to give consideration to both hydrophobicity and adhesive force of the super-hydrophobic coating, the mass ratio of the alpha-cyanoacrylate to the inorganic nanoparticles needs to be reasonably controlled, and the mass ratio is too small, so that the adhesive force of the super-hydrophobic coating is poor, and the stability and the wear resistance of the super-hydrophobic coating are influenced; the mass ratio is too large, the content of inorganic nano particles is too small, and the hydrophobicity of the super-hydrophobic coating is poor; wherein the mass ratio of the alpha-cyanoacrylate to the inorganic nano-particles is 1:1-15:1, or 2:1-10:1, or 2:1-5: 1.
In the exemplary embodiment provided herein, in the superhydrophobic coating, the mass ratio C2 of the inorganic nanoparticles in the first coating liquid to the silicone oil in the second coating liquid is 10:1 to 100: 1.
The super-hydrophobic coating has good hydrophobicity, the inorganic nano-particles of the first layer are stuck on the substrate by cyanoacrylate polymer, and a micro-nano coarse structure of the first element of the super-hydrophobic coating is provided; the silicone oil coating of the second layer has a "low surface energy", providing the second element of the superhydrophobic coating. The micro-nano coarse structure and the low surface energy act together to enable the super-hydrophobic coating to have good hydrophobicity, so that the mass ratio of the inorganic nanoparticles in the first coating liquid to the silicone oil in the second coating liquid needs to be reasonably controlled, and the mass ratio is 10:1-100:1, or 30:1-80: 1.
In an exemplary embodiment provided herein, a method of preparing a first coating liquid includes: adding inorganic nanoparticles into a part of the first organic solvent, and performing ultrasonic dispersion to obtain an inorganic nanoparticle dispersion liquid; adding alpha-cyanoacrylate into the rest of the first organic solvent, mixing and dissolving to obtain an alpha-cyanoacrylate solution; and adding the inorganic nanoparticle dispersion liquid into the alpha-cyanoacrylate solution, and uniformly mixing to obtain a first coating liquid.
In an exemplary embodiment provided herein, a method of preparing a second coating liquid includes: and adding the silicone oil into a second organic solvent, and mixing and dissolving to obtain a second coating liquid.
In the exemplary embodiment provided herein, the first preset condition is a dry curing process, wherein the temperature T1 of the dry curing process may be 15-100 ℃, and the time T1 of the dry curing process may be 0.5-5 h. The second preset condition is a drying treatment, wherein the temperature T2 of the drying treatment can be 15-90 ℃, and the time T2 of the drying treatment can be 0.5-3 h.
In the application, a first coating liquid is coated on the surface of a substrate in a spraying, dip-coating, roll-coating or brush-coating mode, and under a first preset condition, a first organic solvent is evaporated, alpha-cyanoacrylate performs in-situ spontaneous polymerization to generate a polymer of alpha-cyanoacrylate, and inorganic nanoparticles are bonded on the substrate, so that a first coating is obtained. At room temperature with relative humidity, the alpha-cyanoacrylate can carry out in-situ spontaneous polymerization reaction through water vapor induction to generate alpha-cyanoacrylate polymer, the alpha-cyanoacrylate polymer has good cohesiveness and strength on the surfaces of various materials such as high molecular materials, metal materials, inorganic non-metal materials and the like, and inorganic nano particles can be firmly adhered to the surfaces of the materials, so that a firm micro-nano coarse structure is formed, and the coating has a first element of a super-hydrophobic coating, namely a micro-nano convex structure.
And coating the second coating liquid on the first coating by spraying or dip-coating, evaporating the second organic solvent under a second preset condition, and attaching a layer of very thin silicone oil on the micro-nano-scale convex structure to obtain a second coating. Wherein, the silicone oil has very low surface energy, so that the coating has the second element of the super-hydrophobic coating, namely low surface energy; and the silicone oil has good anti-contamination performance, so the super-hydrophobic coating also has good anti-contamination performance.
In exemplary embodiments provided herein, the material of the substrate is a polymer material, a metal material, or an inorganic non-metal material.
The superhydrophobic coating 100 according to the exemplary embodiment of the present application is prepared by the method for preparing the superhydrophobic coating according to the exemplary embodiment of the present application, and as shown in fig. 1, includes a first coating 1 and a second coating 2;
a first coating 1 is provided on a substrate 3, the first coating comprising: 1-30 parts by mass of a polymer of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles;
a second coating layer 2 is disposed on the first coating layer 1, the second coating layer including: 0.01 to 10 parts by mass of a silicone oil; the silicone oil includes a liquid-state polymerized siloxane having an organic side chain and containing no active hydrogen group.
The superhydrophobic coating 100 of the present application includes two layers, as shown in fig. 1, a first coating layer 1 coated on a surface of a substrate 3, and a second coating layer 2 coated on a surface of the first coating layer 1. The first coating 1 comprises a polymer 12 of alpha-cyanoacrylate and inorganic nano particles 11, the inorganic nano particles 11 form a micro-nano convex structure, the polymer 12 of the alpha-cyanoacrylate bonds the inorganic nano particles 11 on the substrate 3, so that a firm micro-nano coarse structure is formed, the super-hydrophobic coating has good adhesive force, and the super-hydrophobic coating is suitable for products prepared from materials such as high molecular materials, metal materials, inorganic non-metal materials and the like, and has wide application range, good hydrophobic performance, high mechanical strength, good wear resistance and good stability. The second coating 2 comprises silicone oil, the silicone oil forms a very thin coating on the micro-nano level convex structure, the silicone oil has very low surface energy, so that the hydrophobic performance of the super-hydrophobic coating is enhanced, and the silicone oil has good anti-contamination performance, so that the super-hydrophobic coating also has good anti-contamination performance. The hydrophobic property of the superhydrophobic coating of the present application is determined by both surface roughness and surface energy; if a micro-nano raised structure is not constructed, a super-hydrophobic surface is difficult to prepare by simply using a substance with low surface energy; if only a micro-nano convex structure is constructed, the outermost layer is not coated with low-surface-energy silicone oil, and the hydrophobic effect and the oil stain resistance effect of the super-hydrophobic coating can not be realized.
The super-hydrophobic coating liquid of the present exemplary embodiment includes a first coating liquid and a second coating liquid;
the first coating liquid comprises the following raw materials in parts by mass: 1-30 parts by mass of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles and 90-110 parts by mass of a first organic solvent;
the second coating liquid comprises the following raw materials in parts by mass: 0.01-10 parts by mass of silicone oil and 90-110 parts by mass of a second organic solvent; the silicone oil includes a liquid-state polymerized siloxane having an organic side chain and containing no active hydrogen group.
In the present application, the first coating liquid includes α -cyanoacrylate, inorganic nanoparticles, and a first organic solvent. Wherein the alpha-cyanoacrylate is 1-30 parts by mass, 3-15 parts by mass or 5-10 parts by mass. The inorganic nano-particles are 1 to 6 parts by mass, 1.5 to 5 parts by mass and 2 to 4 parts by mass. The first organic solvent is 90-110 parts by mass, 95-105 parts by mass, and 98-102 parts by mass.
In the present application, the second coating liquid includes silicone oil and a second organic solvent. Wherein the silicone oil is 0.01-10 parts by mass, and can also be 0.05-2 parts by mass. The second organic solvent is 90-110 parts by mass, and may be 90-105 parts by mass.
The first coating liquid and the second coating liquid are stored separately and are uniformly mixed when in use, and the mass ratio of the first coating liquid to the second coating liquid is 1:1 when in mixing.
The super-hydrophobic coating of the exemplary embodiment of the application is applied to the preparation of electronic equipment, so that the electronic equipment has good hydrophobic property, high mechanical strength, good wear resistance, good stability and good oil stain resistance.
In order to more clearly explain the technical scheme of the present application, preferred examples one-preferred example three of the superhydrophobic coating are listed herein, wherein the raw material components and the preparation method of the superhydrophobic coating of the preferred examples one-preferred example three of the present application are shown as follows. It should be noted that the raw material components and contents of the super-hydrophobic coating layers of examples 1 to 16 and the parameters of the preparation method do not limit the protection scope of the present application
Preferred example 1
Formulation of the first coating liquid
90-110 parts by mass of first organic solvent
1-30 parts by mass of alpha-cyanoacrylate
1-6 parts by mass of inorganic nano-particles,
formulation of the second coating liquid
90-110 parts by mass of second organic solvent
0.01 to 10 parts by mass of a silicone oil,
wherein the inorganic nanoparticles comprise one or more of silicon dioxide nanoparticles, titanium dioxide nanoparticles, zinc oxide nanoparticles, aluminum oxide nanoparticles, ferric oxide nanoparticles, zirconium dioxide nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles and cobalt oxide nanoparticles; the alpha-cyanoacrylate comprises one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate and 2-octyl cyanoacrylate; the silicone oil comprises one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl ethoxy silicone oil and methyl trifluoro propyl silicone oil; the first organic solvent comprises one or more of ester organic solvent, ketone organic solvent, halogenated alkane organic solvent and aprotic polar solvent; the second organic solvent comprises one or more of halogenated alkane, halogenated alkene, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol and butanol.
The preparation method of the first coating liquid comprises the following steps: adding inorganic nanoparticles into a part of the first organic solvent, and performing ultrasonic dispersion to obtain an inorganic nanoparticle dispersion liquid; adding alpha-cyanoacrylate into the rest of the first organic solvent, and mixing and dissolving to obtain an alpha-cyanoacrylate solution; adding the inorganic nanoparticle dispersion liquid into the alpha-cyanoacrylate solution, and uniformly mixing to obtain a first coating liquid;
the preparation method of the second coating liquid comprises the following steps: adding silicone oil into a second organic solvent, and mixing and dissolving to obtain a second coating liquid;
the preparation method of the super-hydrophobic coating comprises the following steps: dip-coating a substrate (an aluminum alloy plate, a PET film or a ceramic sheet) with the first coating solution, then placing the substrate in an environment of 15-100 ℃ for drying and curing for 0.5-5h, evaporating the first organic solvent, carrying out in-situ spontaneous polymerization on alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, and bonding inorganic nanoparticles on the surface of the substrate by the polymer of the alpha-cyanoacrylate to form a first coating; and dip-coating the substrate coated with the first coating with a second coating liquid, then placing the substrate in an environment of 15-90 ℃ for evaporation and drying for 0.5-3h, completely evaporating the second organic solution, forming a silicon oil layer on the first coating, wherein the silicon oil layer is the second coating, and the first coating and the second coating jointly form a super-hydrophobic coating. The water contact angle of the obtained super-hydrophobic coating is measured to be 150-160 degrees, the rolling angle is measured to be 2-8 degrees, and the super-hydrophobic coating has super-hydrophobic performance.
Preferred example two
Formulation of the first coating liquid
90-110 parts by mass of first organic solvent
1-30 parts by mass of alpha-cyanoacrylate
1-6 parts by mass of inorganic nano-particles,
formulation of the second coating liquid
90-110 parts by mass of second organic solvent
0.01 to 10 parts by mass of a silicone oil,
wherein the inorganic nanoparticles comprise one or more of silicon dioxide nanoparticles, titanium dioxide nanoparticles, zinc oxide nanoparticles, aluminum oxide nanoparticles, ferric oxide nanoparticles, zirconium dioxide nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles and cobalt oxide nanoparticles; the alpha-cyanoacrylate comprises one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate and 2-octyl cyanoacrylate; the silicone oil comprises one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl ethoxy silicone oil and methyl trifluoro propyl silicone oil; the first organic solvent comprises one or more of ester organic solvent, ketone organic solvent, halogenated alkane organic solvent and aprotic polar solvent; the second organic solvent comprises one or more of halogenated alkane, halogenated olefin, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol and butanol; the mass ratio of the alpha-cyanoacrylate to the inorganic nano-particles C1 is 1:1-15: 1; the mass ratio C2 of the inorganic nano particles in the first coating liquid to the silicone oil in the second coating liquid is 10:1-100: 1.
The preparation method of the first coating liquid comprises the following steps: adding inorganic nanoparticles into a part of the first organic solvent, and performing ultrasonic dispersion to obtain an inorganic nanoparticle dispersion liquid; adding alpha-cyanoacrylate into the rest of the first organic solvent, and mixing and dissolving to obtain an alpha-cyanoacrylate solution; adding the inorganic nanoparticle dispersion liquid into the alpha-cyanoacrylate solution, and uniformly mixing to obtain a first coating liquid;
the preparation method of the second coating liquid comprises the following steps: adding silicone oil into a second organic solvent, and mixing and dissolving to obtain a second coating solution;
the preparation method of the super-hydrophobic coating comprises the following steps: dip-coating a substrate (an aluminum alloy plate, a PET film or a ceramic sheet) with the first coating solution, then placing the substrate in an environment of 15-100 ℃ for drying and curing for 0.5-5h, evaporating the first organic solvent, carrying out in-situ spontaneous polymerization on alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, and bonding inorganic nanoparticles on the surface of the substrate by the polymer of the alpha-cyanoacrylate to form a first coating; and dip-coating the substrate coated with the first coating with a second coating solution, then placing the substrate in an environment of 15-90 ℃ for evaporation and drying for 0.5-3h, completely evaporating the second organic solution, forming a silicon oil layer on the first coating, wherein the silicon oil layer is the second coating, and the first coating and the second coating jointly form a super-hydrophobic coating. The water contact angle of the obtained super-hydrophobic coating is measured to be 150-160 degrees, the rolling angle is measured to be 2-8 degrees, and the super-hydrophobic coating has super-hydrophobic performance.
Preferred example three
Formulation of the first coating liquid
90-110 parts by mass of first organic solvent
1-30 parts by mass of alpha-cyanoacrylate
1-6 parts by mass of inorganic nano-particles,
formulation of the second coating liquid
90-110 parts by mass of second organic solvent
0.01 to 10 parts by mass of a silicone oil,
wherein the inorganic nanoparticles comprise one or more of silicon dioxide nanoparticles, titanium dioxide nanoparticles, zinc oxide nanoparticles, aluminum oxide nanoparticles, ferric oxide nanoparticles, zirconium dioxide nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles and cobalt oxide nanoparticles; the alpha-cyanoacrylate comprises one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate and 2-octyl cyanoacrylate; the silicone oil comprises one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl ethoxy silicone oil and methyl trifluoro propyl silicone oil; the first organic solvent comprises one or more of ethyl acetate, butyl acetate, isobutyl acetate, acetone, butanone, pentanone, dichloromethane and dimethylformamide; the second organic solvent comprises one or more of trifluorotrichloroethane, fluorodichloroethane, dichloropentafluoropropane, pentafluorobutane, 1-dichloro-1-fluoroethane, trans-1, 2-dichloroethylene, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol and butanol.
The preparation method of the first coating liquid comprises the following steps: adding inorganic nanoparticles into a part of the first organic solvent, and performing ultrasonic dispersion to obtain an inorganic nanoparticle dispersion liquid; adding alpha-cyanoacrylate into the rest of the first organic solvent, and mixing and dissolving to obtain an alpha-cyanoacrylate solution; adding the inorganic nanoparticle dispersion liquid into the alpha-cyanoacrylate solution, and uniformly mixing to obtain a first coating liquid;
the preparation method of the second coating liquid comprises the following steps: adding silicone oil into a second organic solvent, and mixing and dissolving to obtain a second coating liquid;
the preparation method of the super-hydrophobic coating comprises the following steps: dip-coating a substrate (an aluminum alloy plate, a PET film or a ceramic sheet) with the first coating solution, then placing the substrate in an environment of 15-100 ℃ for drying and curing for 0.5-5h, evaporating the first organic solvent, carrying out in-situ spontaneous polymerization on alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, and bonding inorganic nanoparticles on the surface of the substrate by the polymer of the alpha-cyanoacrylate to form a first coating; and dip-coating the substrate coated with the first coating with a second coating solution, then placing the substrate in an environment of 15-90 ℃ for evaporation and drying for 0.5-3h, completely evaporating the second organic solution, forming a silicon oil layer on the first coating, wherein the silicon oil layer is the second coating, and the first coating and the second coating jointly form a super-hydrophobic coating. The water contact angle of the obtained super-hydrophobic coating is measured to be 150-160 degrees, the rolling angle is measured to be 2-8 degrees, and the super-hydrophobic coating has super-hydrophobic performance.
The raw material formulation ingredients and amounts of the superhydrophobic coatings of examples 1-16 are also listed in table 1 herein. It should be noted that the raw material components and contents of the superhydrophobic coatings of examples 1-16 of the present application do not limit the scope of protection of the present application.
Table 1 raw material components and contents of the superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000141
TABLE 1 (subsequent) raw Material Components and amounts of the Superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000142
Figure BDA0003627176600000151
TABLE 1 (subsequent) raw Material Components and amounts of the Superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000152
TABLE 1 (subsequent) raw Material Components and amounts of the Superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000161
The superhydrophobic coatings of examples 1-16 were prepared according to the following method, and the water contact angle and the rolling angle of the superhydrophobic coatings of examples 1-16 were measured, and the results of the property measurement are shown in table 2.
The preparation method of the first coating liquid comprises the following steps: adding inorganic nanoparticles into a part of the first organic solvent, and performing ultrasonic dispersion to obtain an inorganic nanoparticle dispersion liquid; adding alpha-cyanoacrylate into the rest of the first organic solvent, mixing and dissolving to obtain an alpha-cyanoacrylate solution; adding the inorganic nanoparticle dispersion liquid into the alpha-cyanoacrylate solution, and uniformly mixing to obtain a first coating liquid;
the preparation method of the second coating liquid comprises the following steps: adding silicone oil into a second organic solvent, and mixing and dissolving to obtain a second coating liquid;
the preparation method of the super-hydrophobic coating comprises the following steps: dip-coating an aluminum alloy plate (substrate) with a first coating solution, then placing the aluminum alloy plate (substrate) in an environment of 15-100 ℃ for drying and curing for 0.5-5h, evaporating a first organic solvent, carrying out in-situ spontaneous polymerization on alpha-cyanoacrylate to generate an alpha-cyanoacrylate polymer, and bonding inorganic nanoparticles on the surface of the substrate by the alpha-cyanoacrylate polymer to form a first coating; and dip-coating the substrate coated with the first coating with a second coating liquid, then placing the substrate in an environment of 15-90 ℃ for evaporation and drying for 0.5-3h, completely evaporating the second organic solution, forming a silicon oil layer on the first coating, wherein the silicon oil layer is the second coating, and the first coating and the second coating jointly form a super-hydrophobic coating.
Table 2 results of performance tests of the superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000171
TABLE 2 (continuation) results of the measurements of the properties of the superhydrophobic coatings of examples 1-16
Figure BDA0003627176600000172
As can be seen from the data of the performance test results recorded in Table 2, the superhydrophobic coatings of examples 1-16 have water contact angles of 153 ° to 158 ° and rolling angles of 3 ° to 8 °, indicating that the superhydrophobic coatings of examples 1-16 of the present application have superhydrophobic performance.
The super-hydrophobic coating prepared by the preparation method comprises two layers, wherein the first layer is a first coating coated on the surface of a substrate, and the second layer is a second coating coated on the surface of the first coating. The first coating is prepared from alpha-cyanoacrylate, inorganic nano-particles and a first organic solvent, the inorganic nano-particles form a micro-nano-scale convex structure, the first organic solvent is evaporated, alpha-cyanoacrylate is subjected to polymerization reaction to generate a polymer of the alpha-cyanoacrylate, and the inorganic nano-particles can be bonded on a substrate to form a firm micro-nano-scale rough structure; the super-hydrophobic coating not only has good hydrophobic performance, but also has high mechanical strength, good wear resistance and good stability. The second coating is prepared from silicone oil and a second organic solvent, the second organic solvent is evaporated, the silicone oil forms a very thin coating on the micro-nano-scale raised structure, the silicone oil has very low surface energy, so that the hydrophobic performance of the super-hydrophobic coating is enhanced, and the silicone oil has good anti-contamination performance, so that the super-hydrophobic coating also has good anti-contamination performance. When the super-hydrophobic coating is applied to the surfaces of materials such as high polymer materials, metal materials, inorganic non-metal materials and the like, the materials not only have good hydrophobic performance, but also have good mechanical strength, wear resistance, stability and oil stain resistance.
Finally, it should be noted that: the above examples are only for illustrating the technical solutions of the present application, and are not limited thereto. Although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.

Claims (10)

1. A method for preparing a super-hydrophobic coating is characterized by comprising the following steps:
coating a first coating liquid on a substrate, wherein the first coating liquid comprises the following raw materials in parts by mass: 1-30 parts by mass of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles and 90-110 parts by mass of a first organic solvent;
evaporating the first organic solvent under a first preset condition, and carrying out in-situ spontaneous polymerization on the alpha-cyanoacrylate to generate a polymer of the alpha-cyanoacrylate, wherein the polymer of the alpha-cyanoacrylate bonds the inorganic nanoparticles on the surface of the substrate to form the first coating;
coating the second coating liquid on the first coating, wherein the second coating liquid comprises the following raw materials in parts by mass: 0.01-10 parts by mass of silicone oil and 90-110 parts by mass of a second organic solvent; the silicone oil comprises a liquid polysiloxane having an organic side chain and no active hydrogen group;
and under a second preset condition, evaporating the second organic solvent to form a silicon oil layer, wherein the silicon oil layer is the second coating.
2. The method of claim 1, wherein the inorganic nanoparticles comprise one or more of silica nanoparticles, titania nanoparticles, zinc oxide nanoparticles, alumina nanoparticles, ferric oxide nanoparticles, zirconia nanoparticles, copper oxide nanoparticles, cerium oxide nanoparticles, nickel oxide nanoparticles, and cobalt oxide nanoparticles.
3. The method of claim 1, wherein the alpha-cyanoacrylate comprises one or more of methyl 2-cyanoacrylate, ethyl 2-cyanoacrylate, propyl 2-cyanoacrylate, isopropyl 2-cyanoacrylate, n-butyl 2-cyanoacrylate, octyl 2-cyanoacrylate, and octyl 2-cyanoacrylate.
4. The method for preparing the superhydrophobic coating according to claim 1, wherein the silicone oil comprises one or more of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methylphenyl silicone oil, methyl ethoxy silicone oil and methyl trifluoro propyl silicone oil.
5. The method for preparing the superhydrophobic coating according to claim 1, wherein the first organic solvent comprises one or more of ester organic solvent, ketone organic solvent, halogenated alkane organic solvent, and aprotic polar solvent.
6. The method of claim 1, wherein the second organic solvent comprises one or more of halogenated alkane, halogenated alkene, hexamethyldisiloxane, benzene, dimethyl ether, methyl ethyl ketone, carbon tetrachloride, acetone, dioxane, ethanol, butanol.
7. The preparation method of the superhydrophobic coating of claim 1, wherein the mass ratio of the α -cyanoacrylate to the inorganic nanoparticles C1 is 1:1-15: 1.
8. The method for preparing the superhydrophobic coating of claim 1, wherein a mass ratio C2 of the inorganic nanoparticles in the first coating liquid to the silicone oil in the second coating liquid is 10:1-100: 1.
9. A superhydrophobic coating prepared by the preparation method of any one of claims 1-8, comprising a first coating layer and a second coating layer;
the first coating disposed on the substrate, the first coating comprising: 1-30 parts by mass of a polymer of alpha-cyanoacrylate, 1-6 parts by mass of inorganic nanoparticles;
the second coating disposed on the first coating, the second coating comprising: 0.01 to 10 parts by mass of a silicone oil; the silicone oil includes a liquid-state polymerized siloxane having an organic side chain and containing no active hydrogen group.
10. Use of the superhydrophobic coating of claim 9 in the preparation of an electronic device.
CN202210479549.8A 2022-05-05 2022-05-05 Super-hydrophobic coating and preparation method thereof Pending CN114985234A (en)

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