CN115806755B - Ultraphobic coating designed based on dense stacking theory and preparation method thereof - Google Patents
Ultraphobic coating designed based on dense stacking theory and preparation method thereof Download PDFInfo
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- CN115806755B CN115806755B CN202211434934.7A CN202211434934A CN115806755B CN 115806755 B CN115806755 B CN 115806755B CN 202211434934 A CN202211434934 A CN 202211434934A CN 115806755 B CN115806755 B CN 115806755B
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Abstract
The invention relates to the technical field of ultraphobic paint, in particular to an ultraphobic paint designed based on a dense stacking theory and a preparation method thereof. The invention provides an ultraphobic coating designed based on a dense accumulation theory and a preparation method thereof, wherein after spherical fillers are subjected to hydrophobic modification by adopting a modifier, dense accumulation of solid fillers in the ultraphobic coating is realized by collocating spherical particles with different particle diameters, a coarse structure of the surface of the coating is constructed, and a film forming material with low surface energy is mixed with the solid fillers to realize coating of the spherical particles, so that the ultraphobic coating with uniform internal and external structures is constructed. The invention solves the problem that the hydrophobicity of the exposed new surface is reduced or lost due to the destruction of low surface energy substances or coarse structures in the process of mechanical external force or outdoor use of the ultraphobic coating, and improves the durability of the ultraphobic coating.
Description
Technical Field
The invention relates to the technical field of ultraphobic paint, in particular to an ultraphobic paint designed based on a dense stacking theory and a preparation method thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
In nature, many plant leaf surfaces, waterfowl feathers, etc. exhibit superhydrophobicity, the most typical of which is the "lotus leaf effect". The low surface energy waxy substance and the mastoid-shaped coarse structure on the lotus leaf surface reduce the contact area of water drops and the lotus leaf surface, and the water drops tend to be spherical on the surface under the action of surface tension, so that the super-hydrophobic effect is shown; on the other hand, the existence of the low-surface energy waxy substance ensures that the filth is not easy to firmly adhere to the surface of the material and is extremely easy to be taken away by the rolled water drops, thereby realizing the self-cleaning effect. In recent years, the ultraphobic surface has wide application prospect in various industries such as building, corrosion protection, biological medicine, pipeline transportation and the like due to the unique ultraphobic property and self-cleaning property.
Based on the specific structure of the superhydrophobic surface, low surface energy and micro-nano roughness structures are two important parameters for constructing the superhydrophobic surface. The methods commonly employed to construct ultraphobic surfaces include: (1) A micro-rough structure with micro-or nano-scale is constructed on the surface of the low-surface-energy substrate, and (2) the surface energy of the surface with the micro-nano rough structure is reduced. Specifically, the method comprises a sol-gel method, a phase separation method, an etching method, a deposition method, a template method and the like. However, the preparation methods generally have the problems of complex process, high cost, small preparation amount, incapability of large-scale production and use and the like. For example, etching methods often have special restrictions on the type of substrate (e.g., copper, iron, glass, etc.); phase separation processes also typically require components or require the use of large amounts of solvents; the template method has complex process and relates to the steps of template selection, template removal and the like.
The micro-nano rough structure of the coating surface is constructed by doping the filler into the low-surface-energy material, so that the preparation method of the ultraphobic coating has the advantages of simple process, low cost, batch preparation and the like, and has the prospect of commercial popularization and application. However, the ultraphobic coating prepared by the method is easy to lose low-surface energy substances or damage the micro-nano rough structure of the surface under the condition of external force damage or in the outdoor use process, so that the ultraphobic performance of the coating is reduced or even lost, and the long-term use effect of the coating is affected. Thus, increasing the durability of ultraphobic coatings to meet practical field use requirements has become a key factor in achieving an ultraphobic coating industrialization process.
The methods currently in common use for improving the durability of ultraphobic coatings are mainly three: firstly, preparing a self-repairing ultraphobic coating, wherein the performance of the coating can be restored again when the coating is damaged, and the self-repairing ultraphobic coating is mainly realized through the reconstruction of a micro-nano coarse structure or the migration of a low-surface energy substance to the surface; secondly, covalent bonds are introduced between the coating and the substrate or between the components of the coating, so that the acting force between the coating and the substrate is increased, and the durability of the coating is improved; and thirdly, an adhesive is used to increase the adhesion between each component in the coating and the adhesion between each component and the substrate. The use of self-healing ultraphobic coatings generally requires specific environmental conditions such as temperature induction, infrared light induction, etc. to achieve ultraphobic recovery, resulting in limited application environments and application scenarios for the coating; the method of introducing covalent bonds or adhesive layers enhances the adhesion of the components of the coating and the coating to the substrate, to a degree that improves the durability of the ultraphobic coating, but does not resist the damaging effects of strong external forces such as knife scraping on the coating.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an ultraphobic coating designed based on a dense stacking theory and a preparation method thereof. The ultraphobic coating can realize that the micro-nano structure and the low surface energy component uniformly penetrate through the whole system of the coating, achieves the effect of consistent internal and external structures of the coating, and even if the surface structure is destroyed by external force, the exposed new surface still has the same structure as the original surface, thereby achieving the purpose of improving the durability of the coating.
According to the invention, after the spherical filler is subjected to hydrophobic modification by adopting the modifier, dense accumulation of solid filler in the ultraphobic coating is realized by collocating spherical particles with different particle diameters, a coarse structure of the surface of the coating is constructed, and a film forming material with low surface energy is mixed with the solid filler to realize coating of the spherical particles, so that the ultraphobic coating with uniform internal and external structures is constructed. The invention solves the problem that the hydrophobicity of the exposed new surface is reduced or lost due to the destruction of low surface energy substances or coarse structures in the process of mechanical external force or outdoor use of the ultraphobic coating, and improves the durability of the ultraphobic coating.
In order to achieve the above object, the present invention is realized by the following technical scheme:
In a first aspect, the invention provides an ultraphobic coating, which comprises a component A and a component B in a ratio of 10:1-40:1, wherein the component A comprises a low surface energy film forming material, an organic solvent, modified particles, a wetting dispersant, a defoaming agent, a leveling agent, a coupling agent and a film forming auxiliary agent, and the component B is a curing agent for the low surface energy film forming material.
In a second aspect, the present invention provides a method of preparing the above ultraphobic coating material comprising the steps of:
S1, dispersing a low-surface-energy film forming material into one third of organic solvent mixed liquid, and stirring and dispersing to obtain film forming material dispersion liquid;
S2, dispersing the modified particles into two thirds of organic solvent mixed liquid, adding a wetting dispersant, stirring uniformly, shearing and dispersing, adding half of film forming matter dispersion liquid, and continuing shearing to obtain modified particle dispersion liquid;
S3, performing ultrasonic dispersion and mechanical stirring on the modified particle dispersion liquid, then adding the rest film forming matter dispersion liquid, and continuously stirring;
and S4, adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent, stirring to obtain a component A, and mixing the component A with a component B in proportion to obtain the ultraphobic coating.
In a third aspect, the present invention provides the use of the ultraphobic coatings described above and products produced by the process for producing the ultraphobic coatings described above in the fields of construction, corrosion protection, biomedical, plumbing, and the like.
The beneficial effects obtained by one or more of the technical schemes of the invention are as follows:
(1) The application adopts the dense stacking theory design to prepare the ultraphobic coating, realizes the uniform distribution of micro-nano coarse structure and low surface energy film forming matters in a coating system, obtains the ultraphobic coating with consistent internal and external structures, enhances the damage resistance of the ultraphobic coating to external force and improves the durability of the ultraphobic coating.
(2) The spherical particles with different particle diameters are used in the application to realize compact accumulation of solid filler in a coating system, improve the compactness of the ultraphobic coating, reduce the porosity of the coating and improve the capability of the ultraphobic coating to resist external environments such as water vapor, corrosive atmosphere and the like.
(3) The application realizes compact accumulation of solid filler in the ultraphobic coating, reduces the porosity of the coating, reduces the application of low surface energy film forming matters and reduces the production cost of the coating.
(4) The method has the advantages of simplicity, low cost, universality and easiness in large-scale production, and promotes the industrialization process of the ultraphobic paint.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a single size spherical particle packing model;
FIG. 2 is a graph of two sizes of spherical particle packing models;
FIG. 3 is a three-dimensional spherical particle packing model;
FIG. 4 is a two-dimensional surface topography of an ultraphobic coating formed from example 2;
fig. 5 is a three-dimensional surface topography of the ultraphobic coating produced in example 2 to form a coating.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
Two requirements based on ultraphobic coating construction: first, a low surface energy substance; and secondly, a rough structure of the surface. In combination with the theory of dense packing of spherical fillers, as shown in fig. 1, when spherical particles with a single particle diameter are used, the close packing rate of the coating is 62%, but the ultra-hydrophobic effect cannot be realized because spherical particles with a single size cannot construct a micro-nano coarse structure on the surface of the coating; as shown in FIG. 2, spherical particles with two particle sizes are used, the particle size of the large spherical particles is 4-6 times that of the small spherical particles, and when the number ratio of the large spherical particles to the small spherical particles is 6-8:2-4, the small spherical particles can be filled into gaps of the large spherical particles, the close packing rate of the coating is improved to 85.6%, a coarse structure can be constructed on the surface of the coating by matching the particle sizes of the large spherical particles, and the ultra-hydrophobic coating can be prepared by matching with a low surface energy film forming material; as shown in FIG. 3, when spherical particles with three sizes are used as solid fillers, the particle sizes of the spherical particles are 4-6 times different, and when the number ratio is 6-8:1-2:1-3, the effective filling of the pores of the big spheres can be realized, the close packing rate of the coating can reach 94.6%, and the ultraphobic effect of the coating can be realized by matching with a low surface energy film forming material.
In a first exemplary embodiment of the present invention, an ultraphobic coating composition is characterized by comprising a component A and a component B in a ratio of 10:1 to 40:1, wherein the component A comprises a low surface energy film former, an organic solvent, modified particles, a wetting dispersant, an antifoaming agent, a leveling agent, a coupling agent, and a film-forming aid, and the component B is a curing agent for the low surface energy film former.
In one or more examples of this embodiment, the a component is composed of the following raw materials in parts by weight: low surface energy film former: 25% -40% of organic solvent: 15% -26%, modified particles: 30% -50%, wetting dispersant: 0.5 to 3 percent of defoaming agent: 0.5 to 1.5 percent of flatting agent: 1 to 1.5 percent of coupling agent: 1% -2%, film forming auxiliary agent: 0.5 to 2 percent.
In one or more embodiments of this embodiment, the low surface energy film former is one or more of a fluorine-containing resin and an organosilicon material;
The organic solvent is one or more of ethyl acetate, butyl acetate, toluene, xylene, n-hexane, cyclohexane and acetone;
the modified particles are one or more of spherical silicon oxide, titanium oxide and aluminum oxide which are subjected to hydrophobic modification;
the wetting dispersant is one or more of BYK-101N, BYK-W940 and BYK-2150;
the defoamer is one or more of BYK-052N, BYK-053N, BYK-077 and BYK-1752;
The leveling agent is one or more of BYK-397 and BYK-3550;
the coupling agent is one or more of siloxane-based coupling agents KH550, KH560 and KH 570;
The film forming aid is OE300.
In one or more embodiments of this embodiment, the modified particles are comprised of 2-3 different particle size modified particles.
In one or more examples of this embodiment, when the modified particles are composed of 2 modified particles of different particle sizes, the modified particles have a particle size ratio of 4-6:1 and a number ratio of 6-8:2-4.
In one or more examples of this embodiment, when the modified particles are composed of 3 different particle sizes of modified particles, the modified particles have a particle size ratio of 16-36:4-6:1 and a quantitative ratio of 6-8:1-2:1-3.
In a second exemplary embodiment of the present invention, a method for preparing the ultraphobic coating material described above is characterized by comprising the steps of:
S1, dispersing a low-surface-energy film forming material into one third of organic solvent mixed liquid, and stirring and dispersing to obtain film forming material dispersion liquid;
S2, dispersing the modified particles into two thirds of organic solvent mixed liquid, adding a wetting dispersant, stirring uniformly, shearing and dispersing, adding half of film forming matter dispersion liquid, and continuing shearing to obtain modified particle dispersion liquid;
S3, performing ultrasonic dispersion and mechanical stirring on the modified particle dispersion liquid, then adding the rest film forming matter dispersion liquid, and continuously stirring;
and S4, adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent, stirring to obtain a component A, and mixing the component A with a component B in proportion to obtain the ultraphobic coating.
In one or more embodiments of this embodiment, the method of preparing the modified particle further comprises:
dispersing particles such as silicon oxide, titanium oxide or aluminum oxide into ethanol solution, and dispersing for 10-20min under mechanical stirring of 500-800r/min to obtain particle dispersion;
shearing and dispersing the particle dispersion liquid for 20-60min at the rotating speed of 1500-3000 r/min;
transferring the particle dispersion liquid to 1000W ultrasonic wave for ultrasonic dispersion for 20-30min;
Transferring the particle dispersion liquid into 70-90 ℃ oil bath, dropwise adding modifier hydrolysis liquid with pH of 3-5 under continuous stirring, and continuing stirring for reacting for 12-36h after the dropwise adding is finished to obtain modified particles;
And (3) centrifugally washing the modified particles with ethanol for more than 3 times, and transferring the modified particles into a 60 ℃ oven for drying for later use.
In one or more embodiments of this embodiment, the stirring speed in step S1 is 500-800r/min for 5-10min.
In one or more embodiments of this embodiment, the shear dispersion speed in step S2 is 800-1500r/min for 10-20min.
In one or more embodiments of this embodiment, the ultrasonic dispersion power in step S3 is 800-1500W for 10-20min; the mechanical stirring speed is 800-1000r/min, and the time is 20-40min; the stirring time is 0.5-1.5h after the film forming matter dispersion liquid is added.
In one or more embodiments of this embodiment, the stirring time in step S4 is 1-3 hours.
In a third exemplary embodiment of the present invention, the ultraphobic coatings and/or the products of the process for preparing the ultraphobic coatings described above find use in construction, corrosion protection, biomedical, plumbing, and the like.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail below with reference to specific examples and comparative examples.
Example 1
Preparing modified silicon oxide spherical particles:
(1) Dispersing spherical silica particles into an ethanol solution, and dispersing for 10min under mechanical stirring of 500r/min to obtain a particle dispersion;
(2) Shearing and dispersing the particle dispersion liquid for 30min at a rotating speed of 2000r/min, and then transferring the particle dispersion liquid to 1000W ultrasonic waves for 20min;
(3) Preparing modifier hydrolysate, and regulating the pH value to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysis liquid under continuous stirring, and continuing stirring for reaction for 24 hours after the addition of the modifier hydrolysis liquid is finished to obtain modified silicon oxide spherical particles;
(5) And (3) centrifugally washing the modified silicon oxide spherical particles with ethanol for more than 3 times, and transferring the particles into a 60 ℃ oven for drying for later use.
And (3) a component A:
fluorocarbon resin: 30% (GK 570)
Organic solvent: 23% (mixture of ethyl acetate and xylene)
Spherical particles of modified silica: 43% (5 μm:1 μm=7:3)
Wetting dispersant: 1% (BYK-W940)
Defoaming agent: 0.5% (BYK-052N)
Leveling agent: 1% (BYK-397)
Coupling agent: 1% (KH 560)
Film forming auxiliary agent: 0.5% (OE 300)
The component B is a closed isocyanate curing agent.
Preparation of ultraphobic coatings:
(1) Preparing a mixed solution of ethyl acetate and dimethylbenzene according to a mass ratio of 4:6;
(2) Dispersing fluorocarbon resin into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 10min at the rotating speed of 800 r/min;
(3) Dispersing the modified silicon oxide spherical particles into two thirds of organic solvent mixed liquid according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at the rotating speed of 1000r/min, adding half of film forming matter dispersing liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing for 15min under 1000W ultrasonic wave;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And (3) fully stirring and uniformly mixing the component A and the component B according to the proportion of 16:1 to obtain the ultraphobic coating.
Example 2
Preparing modified silicon oxide spherical particles:
(1) Dispersing spherical silica particles into an ethanol solution, and dispersing for 10min under mechanical stirring of 500r/min to obtain a particle dispersion;
(2) Shearing and dispersing the particle dispersion liquid for 30min at a rotating speed of 2000r/min, and then transferring the particle dispersion liquid to 1000W ultrasonic waves for 20min;
(3) Preparing modifier hydrolysate, and regulating the pH value to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysis liquid under continuous stirring, and continuing stirring for reaction for 24 hours after the addition of the modifier hydrolysis liquid is finished to obtain modified silicon oxide spherical particles;
(5) And (3) centrifugally washing the modified silicon oxide spherical particles with ethanol for more than 3 times, and transferring the particles into a 60 ℃ oven for drying for later use.
And (3) a component A:
Fluorosilicone resin: 25% (Hua Lin chemical industry)
Organic solvent: 23% (mixture of ethyl acetate and xylene)
Spherical particles of modified silica: 47% (5 μm:1 μm:0.2 μm = 7:1:2)
Wetting dispersant: 1.5% (BYK-2150)
Defoaming agent: 0.5% (BYK-053N)
Leveling agent: 1% (BYK-397)
Coupling agent: 1% (KH 550)
Film forming auxiliary agent: 1% (OE 300)
The component B is a closed isocyanate curing agent.
Preparation of ultraphobic coatings:
(1) Preparing a mixed solution of ethyl acetate and dimethylbenzene according to a mass ratio of 4:6;
(2) Dispersing fluorocarbon resin into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 10min at the rotating speed of 800 r/min;
(3) Dispersing the modified silicon oxide spherical particles into two thirds of organic solvent mixed liquid according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at the rotating speed of 1000r/min, adding half of film forming matter dispersing liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing for 15min under 1000W ultrasonic wave;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And (3) fully stirring and uniformly mixing the component A and the component B according to the proportion of 20:1 to obtain the ultraphobic coating.
Example 3
Preparing modified titanium oxide spherical particles:
(1) Dispersing titanium oxide spherical particles into an ethanol solution, and dispersing for 15min under mechanical stirring at 700r/min to obtain a particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid at a rotating speed of 2000r/min for 40min, and then transferring the particle dispersion liquid to 1000W ultrasonic waves for 40min;
(3) Preparing modifier hydrolysate, and regulating the pH value to 3.5;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysis liquid under continuous stirring, and continuing stirring for reaction for 24 hours after the addition of the modifier hydrolysis liquid is finished to obtain modified titanium oxide spherical particles;
(5) And (3) centrifugally washing the modified titanium oxide spherical particles with ethanol for more than 3 times, and transferring the particles into a 60 ℃ oven for drying for later use.
And (3) a component A:
silicone resin: 28% (XJY 8205C)
Organic solvent: 20% (mixture of butyl acetate and xylene)
Modified titanium oxide spherical particles: 45% (5 μm:1 μm:0.2 μm = 7:1:2)
Wetting dispersant: 2% (BYK-101N)
Defoaming agent: 1% (BYK-053N)
Leveling agent: 1% (BYK-3550)
Coupling agent: 1% (KH 550)
Film forming auxiliary agent: 2% (OE 300)
The component B is an organosilicon resin curing agent.
Preparation of ultraphobic coatings:
(1) Preparing a mixed solution of butyl acetate and dimethylbenzene according to a mass ratio of 2:8;
(2) Dispersing the organic silicon resin into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 10min at the rotating speed of 700 r/min;
(3) Dispersing the modified titanium oxide spherical particles into two thirds of organic solvent mixed liquid according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at the rotating speed of 1000r/min, adding half of film forming matter dispersing liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing under 1000W ultrasonic wave for 10-15min;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And fully stirring and uniformly mixing the component A and the component B according to the proportion of 18:1 to obtain the ultraphobic coating.
Example 4
Preparing modified alumina spherical particles:
(1) Dispersing alumina spherical particles into ethanol solution, and dispersing for 10min under mechanical stirring at 600r/min to obtain particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid for 30min at a rotating speed of 2000r/min, and then transferring the particle dispersion liquid to 1000W ultrasonic waves for 30min;
(3) Preparing modifier hydrolysate, and regulating the pH value to 4;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysis liquid under continuous stirring, and continuing stirring for reaction for 24 hours after the addition of the modifier hydrolysis liquid is finished to obtain modified alumina spherical particles;
(5) And (3) centrifugally washing the modified alumina spherical particles with ethanol for more than 3 times, and transferring the particles into a 60 ℃ oven for drying for later use.
And (3) a component A:
silicone rubber: 25% (Sylgard 184)
Organic solvent: 15% (mixture of butyl acetate and xylene)
Modified alumina spherical particles: 50% (5 μm:1 μm:0.2 μm=7:1:2)
Wetting dispersant: 3% (BYK-2150)
Defoaming agent: 1.5% (BYK-1752)
Leveling agent: 1.5% (BYK-397)
Coupling agent: 2% (KH 570)
Film forming auxiliary agent: 2% (OE 300)
The component B is an organic silicon rubber curing agent.
Preparation of ultraphobic coatings:
(1) Preparing a mixed solution of butyl acetate and dimethylbenzene according to a mass ratio of 1:1;
(2) Dispersing the organic silicon rubber into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 8min at the rotating speed of 650 r/min;
(3) Dispersing the modified alumina spherical particles into two thirds of organic solvent mixed liquid according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at the rotating speed of 1200r/min, adding half of film forming matter dispersing liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing under 1200W ultrasonic wave for 12min;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 800r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And (3) fully stirring and uniformly mixing the component A and the component B according to the ratio of 40:1 to obtain the ultraphobic coating.
Example 5
The preparation of the modified silica spherical particles was the same as described in example 2.
The preparation of the modified titanium oxide spherical particles was the same as described in example 3.
The preparation of the modified alumina spherical particles was the same as described in example 4.
And (3) a component A:
Fluorocarbon resin: 27% (GK 570)
Organic solvent: 15% (mixture of ethyl acetate and xylene)
Spherical particles of modified silica: 35% (5 μm)
Modified titanium oxide spherical particles: 5% (1 μm)
Modified alumina spherical particles: 10% (0.2 μm)
Wetting dispersant: 2.5% (BYK-1162)
Defoaming agent: 1% (BYK-077)
Leveling agent: 1% (BYK-397)
Coupling agent: 1.5% (KH 560)
Film forming auxiliary agent: 2% (OE 300)
The component B is a closed isocyanate curing agent.
The ultraphobic coating described in this example was prepared as follows:
(1) Preparing a mixed solution of ethyl acetate and dimethylbenzene according to a mass ratio of 4:6;
(2) Dispersing fluorocarbon resin into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 10min at the rotating speed of 800 r/min;
(3) Dispersing spherical particles of modified silicon oxide, titanium oxide and aluminum oxide into a mixed solution of two thirds of organic solvents according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at a rotating speed of 1000r/min, adding half of film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing for 15min under 1000W ultrasonic wave;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding components such as a coupling agent, a defoaming agent, a leveling agent, a film-forming auxiliary agent and the like into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And fully stirring and uniformly mixing the component A and the component B according to the proportion of 18:1 to obtain the ultraphobic coating.
Comparative example 1
Preparing modified silicon oxide spherical particles:
(1) Dispersing spherical silica particles into an ethanol solution, and dispersing for 10min under mechanical stirring of 500r/min to obtain a particle dispersion;
(2) Shearing and dispersing the particle dispersion liquid for 30min at a rotating speed of 2000r/min, and then transferring the particle dispersion liquid to 1000W ultrasonic waves for 20min;
(3) Preparing modifier hydrolysate, and regulating the pH value to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysis liquid under continuous stirring, and continuing stirring for reaction for 24 hours after the addition of the modifier hydrolysis liquid is finished to obtain modified silicon oxide spherical particles;
(5) And (3) centrifugally washing the modified silicon oxide spherical particles with ethanol for more than 3 times, and transferring the particles into a 60 ℃ oven for drying for later use.
And (3) a component A:
fluorocarbon resin: 40% (GK 570)
Organic solvent: 26% (mixture of ethyl acetate and xylene)
Spherical particles of modified silica: 30% (5 μm)
Wetting dispersant: 0.5% (BYK 101N)
Defoaming agent: 0.5% (BYK-077)
Leveling agent: 1% (BYK-397)
Coupling agent: 1% (KH 550)
Film forming auxiliary agent: 1% (OE 300)
The component B is a closed isocyanate curing agent.
Preparation of ultraphobic coatings:
(1) Preparing a mixed solution of ethyl acetate and dimethylbenzene according to a mass ratio of 4:6;
(2) Dispersing fluorocarbon resin into one third of the organic solvent mixed solution according to the proportion in the component A, and stirring and dispersing for 10min at the rotating speed of 800 r/min;
(3) Dispersing the modified silicon oxide spherical particles into two thirds of organic solvent mixed liquid according to the proportion in the component A, adding a wetting dispersant according to the proportion in the component A, stirring and dispersing, shearing and dispersing for 10min at the rotating speed of 1000r/min, adding half of film forming matter dispersing liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing and dispersing for 15min under 1000W ultrasonic wave;
(5) Transferring the particle dispersion liquid to mechanical stirring, mechanically stirring for 30min at a rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding components such as a coupling agent, a defoaming agent, a leveling agent, a film-forming auxiliary agent and the like into the coating system according to the proportion of the component A, and continuously stirring for 2 hours;
(7) And (3) fully stirring and uniformly mixing the component A and the component B according to the proportion of 12:1 to obtain the ultraphobic coating.
Experimental example 1
The ultraphobic coatings obtained in comparative example 1 and examples 1-5 were sprayed onto the surface of a glass sheet to form a coating, and the surface morphology was characterized using example 2 as an example, and as shown in fig. 4 and 5, it can be seen that the coating prepared based on the dense packing theory design was able to build micro-nano coarse structures in the coating, making the coating surface rough, thereby having an ultraphobic effect.
The coating ultraphobic effect was measured by contact angle and roll angle measurements, and the change in hydrophobicity of the coating surface after sanding was used to measure the resistance of the coating to external damage. The coatings of comparative example 1 and examples 1-5 were tested for initial hydrophobicity and hydrophobicity after sanding, and the results are shown in Table 1.
TABLE 1 ultra-hydrophobic coating Performance test results for comparative example 1 and examples 1-5 of the present invention
As shown in Table 1, comparative example 1 contained only spherical particles of a single particle size, and was unable to build micro-nano coarse structure in the coating, and thus the coating did not have ultraphobic effect. Examples 1-5 each contain two or more spherical particles that are effective in creating a rough texture in the coating and achieving ultraphobic effects with low surface energy film formers. The contact angle of the coating is larger than 150 degrees, and the rolling angle is smaller than 10 degrees. In example 1, the coating contains spherical particles with two sizes, the coating has insufficient external damage resistance, and the hydrophobicity of the coating is reduced after sanding; examples 2-5 contained spherical particles of three sizes, the coating had low porosity, high close packing fraction, strong resistance to external damage, and the coating remained ultraphobic after sanding, with a contact angle greater than 150 ° and a roll angle less than 10 °.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The ultraphobic coating is characterized by comprising a component A and a component B in a ratio of 10:1-40:1, wherein the component A comprises a low-surface-energy film forming material, an organic solvent, modified particles, a wetting dispersant, a defoaming agent, a leveling agent, a coupling agent and a film forming auxiliary agent, and the component B is a curing agent for the low-surface-energy film forming material;
The component A consists of the following raw materials in percentage by weight: low surface energy film former: 25% -40%, organic solvent: 15% -26% of modified particles: 30% -50%, wetting dispersant: 0.5% -3%, defoamer: 0.5% -1.5% of leveling agent: 1% -1.5%, coupling agent: 1% -2% of film forming auxiliary agent: 0.5% -2%;
the modified particles are one or more of spherical silicon oxide, titanium oxide and aluminum oxide which are subjected to hydrophobic modification;
the modified particles consist of 3 modified particles with different particle diameters, wherein the particle diameter ratio of the modified particles is 5 mu m to 1 mu m to 0.2 mu m, and the number ratio is 7:1:2;
the low surface energy film forming material is one or more of fluorine-containing resin and organic silicon materials;
The organic solvent is one or more of ethyl acetate, butyl acetate, toluene, xylene, n-hexane, cyclohexane and acetone.
2. The ultraphobic coating of claim 1 wherein the wetting dispersant is one or more of BYK-101N, BYK-W940, BYK-2150;
the defoamer is one or more of BYK-052N, BYK-053N, BYK-077 and BYK-1752;
the leveling agent is one or more of BYK-397 and BYK-3550;
the coupling agent is one or more of siloxane-based coupling agents KH550, KH560 and KH 570;
The film forming aid is OE300.
3. A method of preparing an ultraphobic coating as claimed in any one of claims 1 to 2, comprising the steps of:
S1, dispersing a low-surface-energy film forming material into one third of organic solvent mixed liquid, and stirring and dispersing to obtain film forming material dispersion liquid;
S2, dispersing the modified particles into two thirds of organic solvent mixed liquid, adding a wetting dispersant, stirring uniformly, shearing and dispersing, adding half of film forming matter dispersion liquid, and continuing shearing to obtain modified particle dispersion liquid;
S3, performing ultrasonic dispersion on the modified particle dispersion liquid, mechanically stirring, then adding the rest film forming matter dispersion liquid, and continuously stirring;
and S4, adding a coupling agent, a defoaming agent, a leveling agent and a film-forming auxiliary agent, stirring to obtain a component A, and mixing the component A with a component B in proportion to obtain the ultraphobic coating.
4. The method of preparing the ultraphobic coating of claim 3, further comprising the step of preparing modified particles:
dispersing silica, titanium oxide or aluminum oxide particles into ethanol solution, and dispersing 10-20 min under mechanical stirring of 500-800 r/min to obtain particle dispersion;
shearing and dispersing the particle dispersion liquid at a rotating speed of 1500-3000 r/min for 20-60 min;
transferring the particle dispersion liquid to 1000W of ultrasonic waves for ultrasonic dispersion of 20-30 min;
Transferring the particle dispersion liquid into 70-90 ℃ oil bath, dropwise adding modifier hydrolysis liquid with pH of 3-5 under continuous stirring, and continuing stirring reaction for 12-36 h after the dropwise addition is finished to obtain modified particles;
and (3) centrifugally washing the modified particles with ethanol for more than 3 times, and transferring the modified particles into a 60 ℃ oven for drying for later use.
5. A method of preparing an ultraphobic coating according to claim 3 wherein the stirring speed in step S1 is 500-800 r/min for a period of time of 5-10 min.
6. A method of preparing an ultraphobic coating according to claim 3 wherein the shear dispersion in step S2 is carried out at a speed of 800 to 1500 r/min for a period of 10 to 20 min.
7. The method of preparing the ultraphobic coating material according to claim 3, wherein the ultrasonic dispersion power in step S3 is 800-1500W for 10-20 min; the mechanical stirring speed is 800-1000 r/min, and the time is 20-40 min; the stirring time after the film forming material dispersion is added is 0.5-1.5 h.
8. A method of preparing an ultraphobic coating according to claim 3 wherein the agitation time in step S4 is from 1 to 3 h.
9. Use of the ultraphobic coating according to any of claims 1-2 and/or the product obtained by the process for the preparation of the ultraphobic coating according to any of claims 3-8 in the fields of construction, corrosion protection, biological medicine, pipeline transportation.
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