CN115806755A - Super-hydrophobic coating designed based on compact accumulation theory and preparation method thereof - Google Patents
Super-hydrophobic coating designed based on compact accumulation theory and preparation method thereof Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention relates to the technical field of super-hydrophobic coatings, in particular to a super-hydrophobic coating designed based on a compact stacking theory and a preparation method thereof. The invention provides a super-hydrophobic coating designed based on a compact stacking theory and a preparation method thereof. The invention solves the problem that the hydrophobicity of the exposed new surface is reduced or lost due to the damage of low surface energy substances or coarse structures of the super-hydrophobic coating in the process of mechanical external force or outdoor use, and improves the durability of the super-hydrophobic coating.
Description
Technical Field
The invention relates to the technical field of super-hydrophobic coatings, in particular to a super-hydrophobic coating designed based on a compact stacking theory and a preparation method thereof.
Background
The information in this background section is only for enhancement of 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 that is already known to a person of ordinary skill in the art.
In nature, the leaf surfaces of many plants, waterfowl feathers, etc. exhibit superhydrophobicity, the most typical of which is the "lotus effect". On one hand, the low-surface-energy wax-like substance on the lotus leaf surface and the mastoid coarse structure reduce the contact area between water drops and the lotus leaf surface, and the water drops tend to exist in a spherical shape on the lotus leaf surface under the action of surface tension, so that the super-hydrophobic effect is shown; on the other hand, due to the existence of the low-surface-energy wax-like substance, the filth is not easy to firmly adhere to the surface of the wax-like substance and is easily taken away by falling water drops, so that the self-cleaning effect is realized. In recent years, due to the unique super-hydrophobic property and self-cleaning property, the super-hydrophobic surface has wide application prospect in various fields of building, corrosion protection, biomedicine, pipeline transportation and the like.
Based on the special structure of the super-hydrophobic surface, low surface energy and a micro-nano rough structure are two important parameters for constructing the super-hydrophobic surface. The commonly used method for constructing the super hydrophobic surface comprises the following steps: (1) Constructing a micro-or nano-scale micro-rough structure on the surface of a low-surface-energy substrate, and (2) reducing the surface energy of the surface with the micro-nano rough structure. The method specifically 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 complicated process, high cost, small preparation amount, incapability of large-scale production and use and the like. For example, etching methods often have special limitations on the types of substrates (e.g., copper, iron, glass, etc.); phase separation methods also generally require components or require the use of large amounts of solvents; the stencil method is complicated in process and relates to the steps of selecting and removing the stencil and the like.
The micro-nano rough structure of the surface of the coating is constructed by doping the filler into the low-surface-energy material, so that the method for preparing the super-hydrophobic 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 super-hydrophobic coating prepared by the method is easy to have the phenomenon of low surface energy substance loss or surface micro-nano coarse structure damage under the external force damage or in the outdoor use process, so that the super-hydrophobic performance of the coating is reduced or even lost, and the long-term use effect of the coating is influenced. Therefore, improving the durability of the super-hydrophobic coating to meet the actual field use requirement becomes a key factor for realizing the industrialization process of the super-hydrophobic coating.
The currently used methods for improving the durability of the super-hydrophobic coating mainly include the following three methods: firstly, preparing a self-repairing super-hydrophobic coating, wherein the coating can recover performance again when damaged, and the performance is mainly realized by rebuilding of a micro-nano coarse structure or migration of a low-surface-energy substance to the surface; secondly, covalent bonds are introduced between the coating and the base material or components of the coating, so that the acting force between the coating and the base material is increased, and the durability of the coating is improved; and thirdly, an adhesive is used to increase the adhesion among the components in the coating and between the components and the base material. However, the use of the self-repairing super-hydrophobic coating generally requires specific environmental conditions such as temperature induction and infrared light induction to realize the restoration of the super-hydrophobicity, so that the application environment and the application scene of the coating are limited; the method of introducing covalent bond or adhesive layer enhances the adhesion of each component in the coating and the base material, improves the durability of the super-hydrophobic coating to a certain extent, but can not resist the damage of strong external force such as knife scraping and the like to the coating.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a super-hydrophobic coating designed based on a dense packing theory and a preparation method thereof. The super-hydrophobic coating can realize that micro-nano structures and low-surface-energy components uniformly penetrate through the whole system of the coating, the effect that the internal structure and the external structure of the coating are consistent is achieved, and even if the surface structure is damaged by external force, the exposed new surface still has the same structure as the original surface, so that the aim of improving the durability of the coating is fulfilled.
According to the invention, after the spherical filler is subjected to hydrophobic modification by adopting the modifier, dense accumulation of the solid filler in the super-hydrophobic coating is realized by matching spherical particles with different particle sizes, a rough structure of the surface of the coating is constructed, and a low-surface-energy film forming matter is mixed with the solid filler to coat the spherical particles, so that the super-hydrophobic coating with uniform inner and outer structures is constructed. The invention solves the problem that the hydrophobicity of the exposed new surface is reduced or lost because the low surface energy substance or the coarse structure is damaged in the process of using the super hydrophobic coating by mechanical external force or outdoors, and improves the durability of the super hydrophobic coating.
In order to realize the purpose, the invention is realized by the following technical scheme:
in a first aspect, the invention provides a super-hydrophobic coating, which is composed of a component A and a component B in a ratio of 10 to 1, wherein the component A comprises a low-surface-energy film-forming substance, 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 substance.
In a second aspect, the invention provides a preparation method of the super hydrophobic coating, which comprises the following steps:
s1, dispersing a low-surface-energy film forming matter into one third of organic solvent mixed liquor, and stirring and dispersing to obtain a film forming matter dispersion liquid;
s2, dispersing the modified particles into two-thirds of the organic solvent mixed solution, adding a wetting dispersant, uniformly stirring, shearing and dispersing, adding half of the film forming matter dispersion liquid, and continuously shearing to obtain a modified particle dispersion liquid;
s3, ultrasonically dispersing 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 flatting agent and a film-forming assistant, stirring to obtain a component A, and mixing with a component B in proportion to obtain the super-hydrophobic coating.
In a third aspect, the invention provides the super-hydrophobic coating and application of a product prepared by the preparation method of the super-hydrophobic coating in the fields of buildings, corrosion protection, biomedicine, pipeline transportation and the like.
The beneficial effects obtained by one or more technical schemes of the invention are as follows:
(1) According to the application, the super-hydrophobic coating is prepared by adopting a compact stacking theoretical design, uniform distribution of micro-nano coarse structures and low-surface-energy film forming substances in a coating system is realized, a super-hydrophobic coating with consistent internal and external structures is obtained, the destructive capacity of the super-hydrophobic coating against external force is enhanced, and the durability of the super-hydrophobic coating is improved.
(2) The spherical particles with different particle diameters are used for realizing the compact accumulation of the solid filler in a coating system, the compactness of the super-hydrophobic coating is improved, the porosity of the coating is reduced, and the capability of the super-hydrophobic coating for resisting external environments such as water vapor and corrosive atmosphere is improved.
(3) The method realizes compact accumulation of the solid filler in the super-hydrophobic coating, reduces the porosity of the coating, reduces the application of low-surface-energy film forming substances, and reduces the production cost of the coating.
(4) The method is simple in operation method, low in cost, universal and easy for large-scale production, and promotes the industrialization process of the super-hydrophobic coating.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to illustrate an exemplary embodiment of the invention and not to limit the invention.
FIG. 1 is a model of a single size spherical particle packing;
FIG. 2 is a model of two sizes of spherical particle packing;
FIG. 3 is a model of the packing of spherical particles of three sizes;
FIG. 4 is a two-dimensional surface topography of a coating formed from the superhydrophobic coating prepared in example 2;
FIG. 5 is a three-dimensional surface topography of a coating formed from the superhydrophobic coating prepared in example 2.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. 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 invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Two requirements are constructed based on the super-hydrophobic coating: first, low surface energy materials; the second is the rough structure of the surface. By combining the dense packing theory of spherical filler, as shown in fig. 1, when spherical particles with a single particle size are used, the dense packing rate of the coating is 62%, but because the spherical particles with a single size cannot construct a micro-nano coarse structure on the surface of the coating, the super-hydrophobic effect cannot be realized; as shown in fig. 2, when spherical particles with two particle sizes are used, the particle size of the large spherical particles is 4-6 times of that of the small spherical particles, and 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%, the particle size of the large spherical particles can be matched with that of the small spherical particles to form a rough structure on the surface of the coating, and the preparation of the super-hydrophobic coating can be realized by matching with a low-surface-energy film-forming substance; as shown in FIG. 3, when spherical particles of three sizes are used as the solid filler, the particle size difference of the spherical particles is 4-6 times, and the quantity ratio is 6-8:1-2:1-3, the effective filling of the small balls to the big ball pores can be realized, the close packing rate of the coating can reach 94.6%, and the super-hydrophobic effect of the coating can be realized by matching with a low-surface-energy film forming matter.
The super hydrophobic coating is characterized by comprising a component A and a component B in a ratio of 10-40.
In one or more embodiments of this embodiment, component a is comprised of the following raw materials in parts by weight: low surface energy film-forming material: 25% -40%, organic solvent: 15% -26%, modified particles: 30-50% of wetting dispersant: 0.5% -3%, defoaming agent: 0.5-1.5%, leveling agent: 1% -1.5%, coupling agent: 1% -2%, film-forming additive: 0.5 to 2 percent.
In one or more embodiments of this embodiment, the low surface energy film-forming substance 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, normal 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 defoaming agent is one or more of BYK-052N, BYK-053N, BYK-077 and BYK-1752;
the flatting 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 consist of 2 to 3 modified particles of different particle sizes.
In one or more embodiments of this embodiment, when the modified particles are comprised of 2 modified particles of different particle sizes, the modified particle size ratio is from 4 to 6:1 and the quantity ratio is from 6 to 8:2 to 4.
In one or more embodiments of this embodiment, when the modified particles consist of 3 modified particles of different particle sizes, the modified particle size ratio is from 16 to 36, from 4 to 6:1, and from 6 to 8:1 to 2:1-3.
In a second exemplary embodiment of the present invention, the method for preparing the super hydrophobic coating is characterized by comprising the following steps:
s1, dispersing a low-surface-energy film forming matter into one third of organic solvent mixed liquor, and stirring and dispersing to obtain a film forming matter dispersion liquid;
s2, dispersing the modified particles into two-thirds of the organic solvent mixed solution, adding a wetting dispersant, uniformly stirring, shearing and dispersing, adding half of the film forming matter dispersion liquid, and continuously shearing to obtain a modified particle dispersion liquid;
s3, ultrasonically dispersing the modified particle dispersion liquid, mechanically stirring, then adding the rest of the film forming matter dispersion liquid, and continuously stirring;
and S4, adding a coupling agent, a defoaming agent, a flatting agent and a film-forming assistant, stirring to obtain a component A, and mixing with a component B in proportion to obtain the super-hydrophobic coating.
One or more embodiments of this embodiment further include a method of making the modified particle:
dispersing particles of silicon oxide, titanium oxide or aluminum oxide and the like into an ethanol solution, and dispersing for 10-20min under mechanical stirring at 500-800r/min to obtain a particle dispersion liquid;
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 of ultrasonic waves for ultrasonic dispersion for 20-30min;
transferring the particle dispersion liquid into an oil bath at 70-90 ℃, dropwise adding modifier hydrolysate with pH of 3-5 under continuous stirring, and continuously stirring for reaction for 12-36h to obtain modified particles;
and centrifugally washing the modified particles by using ethanol for more than 3 times, and transferring the modified particles to a 60 ℃ drying oven 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; adding the film forming material dispersion liquid and stirring for 0.5-1.5h.
In one or more embodiments of this embodiment, the stirring time in step S4 is from 1 to 3 hours.
In a third exemplary embodiment of the present invention, the super hydrophobic coating and/or the product obtained by the preparation method of the super hydrophobic coating are applied to the fields of building, corrosion protection, biomedicine, pipeline transportation, and the like.
In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the technical scheme of the present invention will be described in detail below by combining specific examples and comparative examples.
Example 1
Preparing modified silicon oxide spherical particles:
(1) Dispersing the silicon oxide spherical particles into an ethanol solution, and dispersing for 10min under the mechanical stirring of 500r/min to obtain a particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid for 30min at the rotating speed of 2000r/min, and then transferring to ultrasonic dispersion of 1000W for 20min;
(3) Preparing modifier hydrolysate and regulating pH to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysate under continuous stirring, and continuously stirring for reacting for 24 hours after dropwise adding to obtain modified silicon oxide spherical particles;
(5) The modified silicon oxide spherical particles are centrifugally washed by ethanol for more than 3 times and then transferred to a 60 ℃ drying oven for drying and standby.
The component A comprises:
fluorocarbon resin: 30% (GK 570)
Organic solvent: 23% (mixture of ethyl acetate and xylene)
Modified silica spherical particles: 43% (5 μm:1 μm = 7:3)
Wetting and dispersing agent: 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 blocked isocyanate curing agent.
Preparing super hydrophobic paint:
(1) Preparing a mixed solution of ethyl acetate and xylene according to the 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 liquor 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 the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid subjected to shearing dispersion under 1000W of ultrasonic waves for dispersing for 15min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring for 30min at the rotating speed of 1000r/min, adding the rest of the film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a flatting 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.
Example 2
Preparing modified silicon oxide spherical particles:
(1) Dispersing the silicon oxide spherical particles into an ethanol solution, and dispersing for 10min under the mechanical stirring of 500r/min to obtain a particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid at the rotating speed of 2000r/min for 30min, and then transferring to ultrasonic dispersion of 1000W for 20min;
(3) Preparing modifier hydrolysate and regulating pH to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysate under continuous stirring, and continuously stirring for reacting for 24 hours after dropwise adding to obtain modified silicon oxide spherical particles;
(5) The modified silicon oxide spherical particles are centrifugally washed by ethanol for more than 3 times and then transferred to a 60 ℃ drying oven for drying and standby.
The component A comprises:
fluorine-silicon resin: 25% (Hualin chemical industry)
Organic solvent: 23% (mixture of ethyl acetate and xylene)
Modified silica spherical particles: 47% (5 μm:1 μm:0.2 μm =7
Wetting and dispersing agent: 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 blocked isocyanate curing agent.
Preparing super hydrophobic paint:
(1) Preparing a mixed solution of ethyl acetate and xylene according to the 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 liquor 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 the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid subjected to shearing dispersion under 1000W of ultrasonic waves for dispersing for 15min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring the particle dispersion liquid for 30min at the rotating speed of 1000r/min, adding the rest film forming matter dispersion liquid, and continuously stirring the mixture for 1h;
(6) Adding a coupling agent, a defoaming agent, a flatting 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.
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 the rotating speed of 2000r/min for 40min, and then transferring to ultrasonic dispersion of 1000W for 40min;
(3) Preparing modifier hydrolysate and regulating pH to 3.5;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysate under continuous stirring, and continuously stirring for reacting for 24 hours after dropwise adding to obtain modified titanium oxide spherical particles;
(5) The modified titanium oxide spherical particles are centrifugally washed by ethanol for more than 3 times and then transferred to a 60 ℃ drying oven for drying and standby.
The component A comprises:
silicone resin: 28% (XJY 8205C)
Organic solvent: 20% (mixed solution of butyl acetate and xylene)
Modified titanium oxide spherical particles: 45% (5 μm:1 μm:0.2 μm =7
Wetting and dispersing agent: 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 organic silicon resin curing agent.
Preparing super hydrophobic paint:
(1) Preparing a mixed solution of butyl acetate and xylene according to the 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 liquor 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 the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid after shearing dispersion under 1000W of ultrasonic waves for dispersion for 10-15min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring for 30min at the rotating speed of 1000r/min, adding the rest of the film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a flatting agent and a film-forming assistant into the coating system according to the proportion in 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 18.
Example 4
Preparing modified alumina spherical particles:
(1) Dispersing the alumina spherical particles into an ethanol solution, and dispersing for 10min under mechanical stirring at 600r/min to obtain a particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid for 30min at the rotating speed of 2000r/min, and then transferring to ultrasonic dispersion of 1000W 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 hydrolysate under continuous stirring, and continuously stirring for reacting for 24 hours after dropwise adding to obtain modified alumina spherical particles;
(5) The modified alumina spherical particles are centrifugally washed by ethanol for more than 3 times and then transferred to a 60 ℃ oven for drying for later use.
The component A comprises:
silicone rubber: 25% (Sylgard 184)
Organic solvent: 15% (mixed solution of butyl acetate and xylene)
Modified alumina spherical particles: 50% (5 μm:1 μm:0.2 μm =7
Wetting and dispersing agent: 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 a silicone rubber curing agent.
Preparing super hydrophobic paint:
(1) Preparing a mixed solution of butyl acetate and xylene according to the 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 liquor 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 at the rotating speed of 1200r/min for 10min, adding half of the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid subjected to shearing dispersion under 1200W of ultrasonic waves for dispersion for 12min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring for 30min at the rotating speed of 800r/min, adding the rest of the film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding a coupling agent, a defoaming agent, a flatting 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 40.
Example 5
The modified silica spherical particles were prepared as described in example 2.
The modified titania spherical particles were prepared as described in example 3.
The modified alumina spherical particles were prepared as described in example 4.
The component A comprises:
fluorocarbon resin: 27% (GK 570)
Organic solvent: 15% (mixture of ethyl acetate and xylene)
Modified silica spherical particles: 35% (5 μm)
Modified titanium oxide spherical particles: 5% (1 μm)
Modified alumina spherical particles: 10% (0.2 μm)
Wetting and dispersing agent: 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 blocked isocyanate curing agent.
The preparation method of the super-hydrophobic coating comprises the following steps:
(1) Preparing a mixed solution of ethyl acetate and xylene according to the 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 two thirds of organic solvent mixed liquor 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 the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid subjected to shearing dispersion under 1000W of ultrasonic waves for dispersing for 15min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring for 30min at the rotating speed of 1000r/min, adding the rest of the film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding coupling agent, defoaming agent, flatting agent, film-forming assistant and other components into the coating system according to the proportion in 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 18.
Comparative example 1
Preparing modified silicon oxide spherical particles:
(1) Dispersing the silicon oxide spherical particles into an ethanol solution, and dispersing for 10min under the mechanical stirring of 500r/min to obtain a particle dispersion liquid;
(2) Shearing and dispersing the particle dispersion liquid for 30min at the rotating speed of 2000r/min, and then transferring to ultrasonic dispersion of 1000W for 20min;
(3) Preparing modifier hydrolysate and regulating pH to 4.0;
(4) Transferring the particle dispersion liquid into an oil bath at 80 ℃, dropwise adding the modifier hydrolysate under continuous stirring, and continuously stirring for reacting for 24 hours after dropwise adding to obtain modified silicon oxide spherical particles;
(5) The modified silicon oxide spherical particles are centrifugally washed by ethanol for more than 3 times and then transferred to a 60 ℃ drying oven for drying and standby.
The component A comprises:
fluorocarbon resin: 40% (GK 570)
Organic solvent: 26% (mixed solution of ethyl acetate and xylene)
Modified silica spherical particles: 30% (5 μm)
Wetting and dispersing agent: 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 blocked isocyanate curing agent.
Preparing super hydrophobic coating:
(1) Preparing a mixed solution of ethyl acetate and xylene according to the 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 liquor 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 the film forming matter dispersion liquid, and continuing shearing for 10min;
(4) Transferring the particle dispersion liquid subjected to shearing dispersion under 1000W of ultrasonic waves for dispersing for 15min;
(5) Transferring the particle dispersion liquid to a mechanical stirrer, mechanically stirring for 30min at the rotating speed of 1000r/min, adding the rest of the film forming matter dispersion liquid, and continuously stirring for 1h;
(6) Adding coupling agent, defoaming agent, flatting agent, film-forming assistant and other components 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.
Experimental example 1
The super-hydrophobic coating obtained in comparative example 1 and examples 1 to 5 is sprayed on the surface of a glass sheet to form a coating, and the surface morphology characterization is performed by taking example 2 as an example, and the results are shown in fig. 4 and 5, so that the coating prepared based on the dense packing theory design can construct a micro-nano coarse structure in the coating, so that the surface of the coating is rough, and the super-hydrophobic effect is achieved.
The super-hydrophobic effect of the coating is measured by detecting the contact angle and the rolling angle, and the external force damage resistance of the super-hydrophobic property of the coating is measured by the change of the surface hydrophobic property of the coating after being polished by sand paper. The coatings of comparative example 1 and examples 1 to 5 were tested for initial water repellency and water repellency after sanding, and the results are shown in table 1.
TABLE 1 test results of the performance of the superhydrophobic coatings of comparative example 1 and examples 1-5 of the present invention
As shown in table 1, comparative example 1 contains only spherical particles having a single particle size, and cannot construct a micro-nano roughness structure in the coating layer, so the coating layer does not have a super-hydrophobic effect. The examples 1-5 all contain two or more kinds of spherical particles, so that the rough structure of the coating can be effectively constructed, and the super-hydrophobic effect is realized under the coordination of the low-surface-energy film-forming substance. The contact angles of the coatings are all larger than 150 degrees, and the rolling angles are smaller than 10 degrees. The coating prepared in the embodiment 1 only contains spherical particles with two sizes, the external force damage resistance of the coating is insufficient, and the hydrophobicity of the coating is reduced after sanding; the spherical particles with three sizes are contained in the examples 2-5, the porosity of the coating is low, the close packing rate is high, the external damage resistance effect is strong, after sanding, the coating still keeps super-hydrophobic effect, the contact angle is more than 150 degrees, and the rolling angle is less than 10 degrees.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The super-hydrophobic coating is characterized by comprising a component A and a component B in a ratio of 10 to 1-40, wherein the component A comprises a low-surface-energy film-forming substance, 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 substance.
2. The super hydrophobic paint as claimed in claim 1, wherein the component A is composed of the following raw materials by weight: low surface energy film-forming material: 25% -40%, organic solvent: 15% -26%, modified particles: 30-50% of wetting dispersant: 0.5% -3%, defoaming agent: 0.5-1.5%, leveling agent: 1% -1.5%, coupling agent: 1% -2%, film-forming additive: 0.5 to 2 percent.
3. The super hydrophobic coating as claimed in claim 1, wherein the low surface energy film forming material is one or more of fluorine-containing resin and organosilicon material;
the organic solvent is one or more of ethyl acetate, butyl acetate, toluene, xylene, normal 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 defoaming agent is one or more of BYK-052N, BYK-053N, BYK-077 and BYK-1752;
the flatting 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.
4. The superhydrophobic coating of claim 1, wherein the modified particles consist of 2-3 modified particles of different sizes.
5. The superhydrophobic coating of claim 4, wherein when the modified particles are composed of 2 types of modified particles with different particle sizes, the modified particle size ratio is 4-6:1 and the quantity ratio is 6-8:2-4.
6. The superhydrophobic coating of claim 4, wherein, when the modified particles consist of 3 modified particles of different sizes, the ratio of modified particle size to diameter is from 16 to 36: 1, the quantity ratio is 6-8:1-2:1-3.
7. The method for preparing the super hydrophobic coating as claimed in any one of claims 1 to 6, comprising the steps of:
s1, dispersing a low-surface-energy film forming matter into one third of organic solvent mixed liquor, and stirring and dispersing to obtain a film forming matter dispersion liquid;
s2, dispersing the modified particles into two-thirds of the organic solvent mixed solution, adding a wetting dispersant, uniformly stirring, shearing and dispersing, adding half of the film forming matter dispersion liquid, and continuously shearing to obtain a modified particle dispersion liquid;
s3, ultrasonically dispersing the modified particle dispersion liquid, mechanically stirring, then adding the rest of the film forming matter dispersion liquid, and continuously stirring;
and S4, adding a coupling agent, a defoaming agent, a flatting agent and a film-forming assistant, stirring to obtain a component A, and mixing with a component B in proportion to obtain the super-hydrophobic coating.
8. The method for preparing the superhydrophobic coating according to claim 7, further comprising a method for preparing the modified particles:
dispersing particles of silicon oxide, titanium oxide or aluminum oxide and the like into an ethanol solution, and dispersing for 10-20min under mechanical stirring at 500-800r/min to obtain a particle dispersion liquid;
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 of ultrasonic waves for ultrasonic dispersion for 20-30min;
transferring the particle dispersion liquid into an oil bath at 70-90 ℃, dropwise adding modifier hydrolysate with pH of 3-5 under continuous stirring, and continuously stirring for reaction for 12-36h to obtain modified particles;
and centrifugally washing the modified particles by using ethanol for more than 3 times, and transferring the particles to a 60 ℃ drying oven for later use.
9. The method for preparing the superhydrophobic coating of claim 7, wherein the stirring speed in the step S1 is 500-800r/min for 5-10min;
or, in the step S2, the shearing dispersion rotating speed is 800-1500r/min, and the time is 10-20min;
or in the step S3, the ultrasonic dispersion power is 800-1500W, and the time is 10-20min; the mechanical stirring speed is 800-1000r/min, and the time is 20-40min; adding the film forming matter dispersion liquid and stirring for 0.5-1.5h;
or, the stirring time in the step S4 is 1-3h.
10. Use of the superhydrophobic coating of any one of claims 1-6 and/or the product of the process for the preparation of the superhydrophobic coating of any one of claims 7-9 in the fields of construction, corrosion protection, biomedicine, pipeline transportation, etc.
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