CN114752302A - High-transparency super-hydrophobic spray coating and preparation method thereof - Google Patents
High-transparency super-hydrophobic spray coating and preparation method thereof Download PDFInfo
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Images
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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
- 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
- C09D183/16—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 in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a high-transparency super-hydrophobic spray coating and a preparation method thereof, wherein the high-transparency super-hydrophobic spray coating comprises a binder and a nano filler dispersion liquid; the adhesive comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent; the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent. Forming micron-scale roughness on the surface of a target by using a binder, wherein the hydrophobic modified nano-scale filler is concentrated at an interface due to low surface energy of the filler to form nano-scale roughness above the micron-scale roughness, and finally forming a 3D micro-nano topological structure required by the super-hydrophobic characteristic; the refractive indexes of the binder and the nano filler are close, so that the coating can keep high transparency, and the modified target surface cannot be influenced after construction.
Description
Technical Field
The invention relates to the technical field of super-hydrophobic materials, in particular to a high-transparency super-hydrophobic spray coating and a preparation method thereof.
Background
The super-hydrophobic material has wide application prospects in the fields of self-cleaning, adhesion prevention and control, oil-water separation, controlled release drugs and the like, and the super-hydrophobic property of the material is mainly based on the combined action of a micro-nano composite structure with a delicate surface and chemical functional groups with extremely low surface energy. According to these two basic features, the main strategies for preparing superhydrophobic surfaces include: artificially constructing a micro-nano composite structure on the surface and changing the chemical composition of the surface of the material so as to increase the real contact angle of the surface of the material.
For example, Sun M H project group uses lotus leaves as templates, the micro-nano structure on the lotus leaf surface is copied by using a nano casting technology to obtain a negative template with a topological structure opposite to that of the lotus leaf surface, and then the negative template is copied and molded to prepare a micro-nano three-dimensional rough structure which is completely the same as that of the lotus leaf surface, and the micro-nano structure also endows the molded material of the template with super-hydrophobic property. Luo Z and the like prepare a Polytetrafluoroethylene (PTFE)/polyphenylene sulfide (PPS) coating with stable superhydrophobic performance through a chemical etching method, and the group finds that a micro-nano composite multi-stage structure can be formed on the surface of a substrate through chemical etching by simulating acid rain, and the change of surface chemical groups can be caused simultaneously when the micro-nano structure on the surface is changed through photoetching with specific wavelength. Although the micro-nano structure construction method can form complex structure control on the surface of the material, the preparation process is complex, the cost is high, and the large-scale industrial application of the super-hydrophobic material is greatly restricted.
However, the appearance of the target surface can be seriously changed by changing the chemical composition of the material surface through the existing spraying method, and most application scenes need the surface coating not to change the appearance of the target surface from the industrial application of hydrophobic surface modification; and the existing spray type super-hydrophobic coating has complex preparation process and high cost, and most of the existing spray type super-hydrophobic coatings are difficult to achieve high transparency.
Accordingly, there is a need for improvements and developments in the art.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a high-transparency super-hydrophobic spray coating and a preparation method thereof, and aims to solve the problems that when a spray type super-hydrophobic coating is prepared in the prior art, the hydrophobic effect is poor, the cost is high, the high transparency cannot be achieved, and the original appearance of a target surface is influenced.
The technical scheme of the invention is as follows:
a high-transparency super-hydrophobic spray coating comprises a binder and a nano filler dispersion liquid;
the binder comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent;
the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent.
The high-transparency super-hydrophobic spray coating is characterized in that the volume ratio of the binder to the nano filler dispersion is 1:1000-100: 1.
The high-transparency super-hydrophobic spray coating is prepared by mixing polysiloxane, vinyl polysiloxane, methyl hydrogen silicone oil, epoxy-terminated polysiloxane and polyvinyl silicone oil, and then spraying the mixture on a substrate.
The high-transparency super-hydrophobic spray coating layer is characterized in that the polysilazane is selected from one or more of inorganic polysilazane DS-3001, organic polysilazane IOTA 9118 and organic polysilazane IOTA-OPSZ-9150.
The high-transparency super-hydrophobic spray coating layer is characterized in that the first solvent is one or more selected from methyl trichlorosilane, octamethyl tetrasiloxane, polyester diol, ethanol, acetone and methyl trimethoxy silane.
The high-transparency super-hydrophobic spray coating is characterized in that the nano filler is one or more selected from silicon dioxide, zinc oxide, titanium dioxide, aluminum oxide, clay and glass powder, and the particle size of the nano filler is 1-500 nm.
The high-transparency super-hydrophobic spray coating is characterized in that the nano filler is hollow or solid, and the shape of the nano filler is spherical, rod-shaped, four-needle-shaped or sheet-shaped.
The high-transparency super-hydrophobic spray coating layer is characterized in that the hydrophobic modifier is selected from one or more of long-chain alkylamine and fluorine-containing silane coupling agent; the second solvent is selected from one or more of ethanol, acetone, heptane and toluene.
A preparation method of the high-transparency super-hydrophobic spray coating comprises the following steps:
mixing polysiloxane, polysilazane, a flatting agent and a first solvent to obtain a binder;
mixing the nano filler, the hydrophobic modifier and the second solvent to obtain nano filler dispersion liquid;
mixing the binder and the nanofiller dispersion to prepare high-transparency super-hydrophobic spraying slurry;
and atomizing the high-transparency super-hydrophobic spraying slurry by using a pressure spray gun, spraying the atomized high-transparency super-hydrophobic spraying slurry on the surface of a target substrate, and curing to form the high-transparency super-hydrophobic spraying coating.
The preparation method of the high-transparency super-hydrophobic spray coating comprises the following steps of:
and sequentially cleaning the surface of the base material by using deionized water and ethanol.
Has the beneficial effects that: the invention provides a high-transparency super-hydrophobic spray coating and a preparation method thereof, wherein the high-transparency super-hydrophobic spray coating comprises a binder and a nano filler dispersion liquid; the binder comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent; the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent. According to the invention, a bonding agent is utilized to form micron-scale roughness on the surface of a target, and the hydrophobic modified nano-scale filler in the nano-filler dispersion liquid is concentrated at an interface due to low surface energy to form nano-scale roughness above the micron-scale roughness, so that a 3D micro-nano topological structure required by super-hydrophobic characteristics is finally formed; the refractive indexes of the binder and the nano filler are close, so that the coating can keep high transparency, and the modified target surface cannot be influenced after construction.
Drawings
FIG. 1 is a schematic surface view of a highly transparent superhydrophobic spray coating of the present invention;
FIG. 2 is a graph showing contact angle measurements of modified surfaces of glass slides according to example 1 (left) and example 2 (right) of the present invention;
FIG. 3 is a graph of light transmittance data (wavelength range 300-800 nm) of a glass slide modified according to the method of example 2;
FIG. 4 is a graph of light transmittance data (wavelength range 300-800 nm) of a glass slide modified according to the method of example 3;
FIG. 5 is a graph of the self-cleaning properties of the modified surface of a slide according to the invention using example 3, as compared to the self-cleaning properties of the unmodified slide surface.
Detailed Description
The invention provides a high-transparency super-hydrophobic spray coating and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In the embodiments and claims, the articles "a", "an", "the" and "the" may include plural forms as well, unless the context specifically dictates otherwise. If there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including 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 will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The spraying method is simple in operation, can realize rapid large-area surface modification, and is suitable for surface treatment of building materials, power transmission lines and the like. Generally, to achieve the super-hydrophobic property modification of the surface by one-step spraying, a curable binder is required to stably fix the hydrophobic particles to the target surface. For example, Wu et al prepared inorganic-organic composite thiol-ene superhydrophobic coatings by continuous spray deposition and photocuring, which incorporate an inorganic-organic thiol-ene resin consisting of pentaerythritol tetrakis (PETMP), polyurethane (TTT), TMTVSi, and hydrophobically modified fumed carbon black nanoparticles. The chemical composition of the spray precursor has low surface energy, and continuous spray deposition can create a surface with micro-scale and nano-scale roughness on the surface of the substrate, but coatings based on this technique can seriously alter the appearance of the target surface; from the industrial application of hydrophobicized surface modification, most application scenarios require that the surface coating does not alter the appearance of the target surface as much as possible.
And (b) and (c). The existing spraying type super-hydrophobic coating utilizes a two-layer or multi-layer structure, has complex preparation process and high cost, and is difficult to realize high transparency; the construction of the target surface can greatly affect the original appearance of the target surface and restrict the commercialization and popularization of the target surface.
Based on the method, the invention provides a high-transparency super-hydrophobic spray coating, which comprises a binder and a nano filler dispersion liquid;
the adhesive comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent;
the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent.
In the invention, a transparent low-surface-energy binder capable of being cured at normal temperature and a low-surface-energy nano filler dispersion liquid are uniformly mixed and sprayed to prepare the high-transparency super-hydrophobic spray coating; the atomized adhesive is used for forming micron-scale roughness, and meanwhile, the nano filler modified by the hydrophobic modifier in the nano filler dispersion liquid is concentrated on an interface due to low surface energy to form the nano-scale roughness above the micron-scale roughness, so that a 3D micro-nano topological structure required by the super-hydrophobic characteristic is finally formed. In the components, because the refractive indexes of the binder and the nano filler are close to each other, when the spray coating is prepared by mixing the components in parts by mass, the coating can keep high transparency, and the modified target cannot be influenced after construction.
Preparing a binder and a nano filler dispersion liquid according to the mass parts, and uniformly mixing the binder and the nano filler dispersion liquid to prepare a high-transparency super-hydrophobic spray coating, wherein the super-hydrophobic surface contact angle of the high-transparency super-hydrophobic spray coating can reach more than 156 degrees; the glass sprayed with the high-transparency super-hydrophobic spray coating has an obvious super-hydrophobic effect, water drops are spherical on the glass, the glass has good transparency and is not influenced by the high-transparency super-hydrophobic spray coating, and writing below the glass is clear and visible.
In some embodiments, the volume ratio of the binder to the nanofiller dispersion is between 1:1000-100: 1.
In a preferred embodiment, the volume ratio of the binder to the nanofiller dispersion is between 1:1 and 1: 10. The super-hydrophobic surface contact angle of the high-transparency super-hydrophobic spray coating prepared by mixing according to the volume ratio is larger, and the hydrophobic effect is better; and the high-transparency super-hydrophobic spray coating has high transparency and cannot influence the original appearance of the target surface.
In some embodiments, the polysiloxane is selected from one or more of polydimethylsiloxane, vinyl polysiloxane, methyl hydrogen silicone oil, epoxy-terminated polysiloxane, polyvinyl silicone oil.
In some embodiments, the polysilazane is selected from one or more of the group consisting of inorganic (perhydro) polysilazane DS-3001, organic polysilazane IOTA 9118, and organic polysilazane IOTA-OPSZ-9150.
According to the invention, the polysiloxane and the polysilazane have the characteristics of transparency and solidification at normal temperature, when the high-transparency super-hydrophobic spray coating is constructed by one-step spraying, the bonding agent formed by the polysiloxane and the polysilazane can form micron-scale roughness on the target surface after atomization, and the nano-filler modified by the hydrophobic modifier can form nano-scale roughness on the micron-scale roughness, so that super-hydrophobic performance is realized.
In some embodiments, the first solvent can be any solvent and siloxane monomer that can completely dissolve the polysiloxane and polysilazane; optionally, the first solvent is selected from one or more of methyltrichlorosilane, octamethyltetrasiloxane, polyester diol, ethanol, acetone, methyltrimethoxysilane.
In some embodiments, the nano filler is selected from one or more of silica, zinc oxide, titanium dioxide, alumina, clay and glass powder, and the particle size of the nano filler is 1 to 500 nm. The contact angle of the super-hydrophobic surface of the high-transparency super-hydrophobic spray coating can reach more than 156 degrees, and the super-hydrophobic performance of the coating is improved.
In some embodiments, the nanofiller is hollow or solid and the shape of the nanofiller includes, but is not limited to, spherical, rod-like, tetrapod-like, or platelet. The nano filler with the shape has larger specific surface area, and is beneficial to completely modifying the nano filler by a hydrophobic modifier, thereby improving the hydrophobic property.
In some embodiments, the hydrophobic modifier is selected from one or more of long chain alkyl amines and fluorine-containing silane coupling agents; the second solvent is selected from one or more of ethanol, acetone, heptane and toluene. The second solvent provides a reaction environment for the hydrophobic modifier to modify the nano-filler, and is beneficial to improving the modification success rate of the hydrophobic modifier to the nano-filler.
In some embodiments, the leveler is a silicone-based leveler, including but not limited to GS-1333, GS-1308.
In addition, the invention also provides a preparation method of the high-transparency super-hydrophobic spray coating, which comprises the following steps:
step S10: mixing polysiloxane, polysilazane, a flatting agent and a first solvent to obtain a binder;
step S20: mixing the nano filler, the hydrophobic modifier and the second solvent to obtain nano filler dispersion liquid;
Step S30: mixing the binder and the nanofiller dispersion to prepare high-transparency super-hydrophobic spraying slurry;
step S40: and atomizing the high-transparency super-hydrophobic spraying slurry by using a pressure spray gun, spraying the atomized high-transparency super-hydrophobic spraying slurry on the surface of a target substrate, and curing to form the high-transparency super-hydrophobic spraying coating.
In the preparation method of the high-transparency super-hydrophobic spray coating, the binder prepared according to the mass parts of the binder and the nano filler dispersion liquid is uniformly mixed with the nano filler dispersion liquid to obtain high-transparency super-hydrophobic spray coating slurry; then, when the high-transparency superhydrophobic spraying slurry is atomized by a pressure spray gun, as shown in fig. 1, firstly, the atomized binder forms micron-scale roughness on the surface of a target, then, the nanofiller modified by the hydrophobic modifier concentrates at a junction due to low surface energy to form nanoscale roughness above the micron-scale roughness, and finally, the high-transparency superhydrophobic spraying coating with a 3D micro-nano topological structure is obtained; due to the surface aggregation of the low-surface-energy substances, the preparation method can form a super-hydrophobic surface in one step; and because the refractive indexes of the adhesive and the nano filler are similar, the super-hydrophobic spray coating can keep high transparency, and the appearance and the light transmission effect of the target surface are not influenced.
The preparation method of the high-transparency super-hydrophobic spray coating can perform super-hydrophobic modification on the target surface in a large area at low cost, and the prepared high-transparency super-hydrophobic spray coating has high transparency and cannot influence the appearance of the target.
In some embodiments, before step S40 (i.e., before spraying the high-transparency superhydrophobic spray slurry on the surface of the target substrate), the method further comprises the steps of: and sequentially cleaning the surface of the base material by using deionized water and ethanol. Provides a substrate with clean surface, is beneficial to the adsorption of the coating, is not easy to fall off, and improves the service life of the high-transparency super-hydrophobic spray coating.
In some embodiments, the curing in step S40 is specifically: standing the target substrate sprayed with the high-transparency super-hydrophobic spraying slurry and curing in air at normal temperature for 18-24 hours to obtain a high-transparency super-hydrophobic spraying coating after the high-transparency super-hydrophobic spraying slurry is cured; it should be noted that: during the curing process, excessive moisture is prevented from contacting the coating which is not dried out, and the hydrophobicity is prevented from being deteriorated due to excessive contact with moisture.
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings.
Example 1
S1 preparation of a low surface energy adhesive curable at room temperature
Uniformly mixing 1ml of methyl hydrogen-containing silicone oil (hydrogen content is 1.4%) with 2ml of ASF-51 fluorosilicone oil, adding 4ml of IOTA 9150 polysilazane into the mixed solution, performing ultrasonic dispersion for 5min, then adding 5ml of MTMS (methyl trimethoxy silane) monomer and 0.01ml of 17FAS as dispersion solvents, performing ultrasonic dispersion for 5min, adding 0.01ml of GS-1333 flatting agent, and performing ultrasonic dispersion for 5min to obtain the low-surface-energy binder.
S2 preparation of low surface energy nano filler dispersion liquid
0.5g of 7-40nm hydrophilic gas phase nano silicon dioxide and 200ml of ethanol are uniformly mixed, 10ml of 1H,1H,2H, 2H-perfluorodecyl triethoxysilane is added into the system after 5min of ultrasonic dispersion, and then the ultrasonic dispersion is carried out for 5min, thus obtaining the low surface energy nano filler dispersion liquid.
S3 preparation of atomized high-transparency super-hydrophobic spraying slurry
And adding 0.5ml of low-surface-energy binder into 2ml of low-surface-energy nano filler dispersion liquid, and performing ultrasonic dispersion for 5min to obtain the atomized high-transparency super-hydrophobic spraying slurry.
S4, forming the high-transparency super-hydrophobic spray coating by one-time spraying
Slides (25X75mm) were cleaned with ethanol and blown dry with clean air. After the glass slide is fixed by a clamp, 0.5ml of atomized high-transparency super-hydrophobic slurry is put into a low-pressure air pump spray gun, the distance between the spray gun head and the surface of a target in the spraying process is 5cm-10cm, and the spraying speed is 0.5 ml/min. After uniform spraying, the glass slide is placed in a fume hood and cured for 24 hours at normal temperature to obtain the high-transparency super-hydrophobic spray coating.
Example 2
S1 preparation of a Low surface energy adhesive curable at Normal temperature
Uniformly mixing 1ml of methyl hydrogen-containing silicone oil (hydrogen content is 1.4%) and 0.5ml of monohydroxy terminated dimethyl active silicone oil, adding 1ml of IOTA 9150 polysilazane into the mixed solution, performing ultrasonic dispersion for 5min, then adding 5ml of MTMS monomer and 0.01ml of 17FAS as dispersion solvents, performing ultrasonic dispersion for 5min, adding 0.42ml of GS-1308 leveling agent, and performing ultrasonic dispersion for 5min to obtain the low-surface-energy binder.
S2 preparation of low surface energy nano filler dispersion liquid
0.5g of 7-40nm hydrophilic gas phase nano silicon dioxide, 0.15g of 40-70 nm hydrophilic gas phase nano silicon dioxide and 200ml of ethanol are uniformly mixed, 10ml of 1H,1H,2H, 2H-perfluorodecyl triethoxysilane is added into the system after 5min of ultrasonic dispersion, and then the ultrasonic dispersion is carried out for 5min, thus obtaining the low surface energy nano filler dispersion liquid.
S3 preparation of atomized high-transparency super-hydrophobic slurry
And adding 0.04ml of low-surface-energy binder into 1ml of low-surface-energy nano filler dispersion liquid, and performing ultrasonic dispersion for 5min to obtain the atomized high-transparency super-hydrophobic slurry.
S4, forming the high-transparency super-hydrophobic spray coating by one-time spraying
Slides (25X75mm) were cleaned with ethanol and blown dry with clean air. After the glass slide is fixed by a clamp, 0.5ml of atomized super-hydrophobic slurry is put into a low-pressure air pump spray gun, the distance between the spray gun head and the target surface is 5cm-10cm in the spraying process, and the spraying speed is 0.5 ml/min. After uniform spraying, the glass slide is placed in a fume hood and cured for 24 hours at normal temperature to obtain the high-transparency super-hydrophobic spray coating.
Example 3
S1 preparation of a low surface energy adhesive curable at room temperature
Uniformly mixing 1ml of methyl hydrogen-containing silicone oil (the hydrogen content is 1.4%) with 0.5ml of ASF-51 fluorosilicone oil, adding 2ml of IOTA9150 polysilazane into the mixed solution, performing ultrasonic dispersion for 5min, then adding 5ml of MTMS monomer and 0.01ml of 17FAS as dispersion solvents, performing ultrasonic dispersion for 5min, adding 0.02ml of GS-1333 flatting agent, and performing ultrasonic dispersion for 5min to obtain the low-surface-energy binder.
S2 preparation of low surface energy nano filler dispersion liquid
0.5g of 7-40nm hydrophilic gas phase nano silicon dioxide and 200ml of ethanol are uniformly mixed, 2ml of 1H,1H,2H, 2H-perfluorodecyl triethoxysilane is added into the system after 5min of ultrasonic dispersion, and the low surface energy nano filler dispersion liquid is obtained after 5min of ultrasonic dispersion.
S3 preparation of atomization type high-transparency super-hydrophobic slurry
And adding 0.5ml of low-surface-energy binder into 2ml of low-surface-energy nano filler dispersion liquid, and performing ultrasonic dispersion for 5min to obtain the atomized high-transparency super-hydrophobic slurry.
S4, forming the high-transparency super-hydrophobic spray coating by one-time spraying
Slides (25X75mm) were cleaned with ethanol and blown dry with clean air. After the glass slide is fixed by a clamp, 0.5ml of atomized super-hydrophobic slurry is put into a low-pressure air pump spray gun, the distance between the spray gun head and the target surface is 5cm-10cm in the spraying process, and the spraying speed is 0.5 ml/min. After uniform spraying, the glass slide is placed in a fume hood and cured for 24 hours at normal temperature to obtain the high-transparency super-hydrophobic spray coating.
The high-transparency super-hydrophobic spray coatings formed by one-time spraying prepared in examples 1 to 3 were subjected to performance tests, which specifically comprise the following steps:
contact angle test: the high transparency superhydrophobic spray coatings prepared in examples 1 and 2 were subjected to a contact angle test with deionized water as the test liquid and a water drop volume of 2 ul. As can be seen from fig. 2, the contact angles of the superhydrophobic surfaces obtained in example 1 and example 2 can reach 156 ° or more.
And (3) testing light transmittance: the light transmittance of the samples in the examples 2 and 3 is measured by adopting an ultraviolet-visible spectrophotometer, the scanning wavelength range is 300-800 nm, and the scanning interval is 2 nm. As can be seen from FIG. 3, the transmittance of the surface prepared in example 2 can reach 60% -80% in the wavelength band of 500-800 nm, but the transmittance decreases slightly with the increase of the number of sprayed layers. As can be seen from FIG. 4, the superhydrophobic prepared in example 3 also has high transparency, the transmittance of the superhydrophobic on the surface of the glass slide can reach 60% -80% in a wave band of 400-800 nm, and the transmittance is reduced slightly with the increase of the number of sprayed layers.
Testing the self-cleaning property of the surface: the method comprises the steps of utilizing convex-concave attapulgite (clay with high water absorption) as simulated dust pollutants, respectively placing a proper amount of the obtained convex-concave attapulgite on the surfaces of a modified glass slide and an unmodified glass slide, cleaning the surfaces of the modified glass slide and the unmodified glass slide by using deionized water, and observing the adhesiveness of the convex-concave attapulgite on different surfaces. As shown in FIG. 5 (group A is a glass slide with an untreated surface, group B is a glass slide with a surface sprayed with the high-transparency super-hydrophobic spray coating, 0S, 1S, 3S and 5S respectively represent 0 second, 1 second, 3 second and 5 second), experiments prove that the modified glass slide (example 3) has better self-cleaning property compared with the unmodified glass slide, and after being cleaned by deionized water, convex-concave clavulanic dust is quickly carried away by the water and almost has no residue, while the surface of the glass slide without surface modification is difficult to remove simulated dust pollution by the deionized water, and the surface has a large amount of mud-like residue.
Hydrophobicity and transparency test: the modified (examples 1 and 2) and unmodified slides were placed on the same background and different colored drops were added drop wise to the surface, with the brown, pink, light blue and orange liquids being cola, red plum juice, jalapa sports drink and fenda soda respectively. It was found that the water droplets spread substantially completely over the untreated slide; the modified glass slide has an obvious super-hydrophobic effect, water drops are spherical on the glass, the modified glass still has good transparency, and the writing below the glass is clear and visible.
In summary, the present invention provides a high-transparency superhydrophobic spray coating and a preparation method thereof, wherein the high-transparency superhydrophobic spray coating comprises a binder and a nanofiller dispersion; the binder comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent; the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent. According to the invention, a bonding agent is utilized to form micron-scale roughness on the surface of a target, and the hydrophobic modified nano-scale filler in the nano-filler dispersion liquid is concentrated at an interface due to low surface energy to form nano-scale roughness above the micron-scale roughness, so that a 3D micro-nano topological structure required by super-hydrophobic characteristics is finally formed; the refractive indexes of the binder and the nano filler are close, so that the coating can keep high transparency, and the modified target surface cannot be influenced after construction.
It will be understood that the invention is not limited to the examples described above, but that modifications and variations will occur to those skilled in the art in light of the above teachings, and that all such modifications and variations are considered to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A high-transparency super-hydrophobic spray coating is characterized by comprising a binder and a nano filler dispersion liquid;
the adhesive comprises the following components in parts by weight: 1-90 parts of polysiloxane, 0.1-90 parts of polysilazane, 0.02-10 parts of flatting agent and 1-200 parts of first solvent;
the nano filler dispersion liquid comprises the following components in parts by weight: 1-90 parts of nano filler, 1-90 parts of hydrophobic modifier and 1-2000 parts of second solvent.
2. The high transparency superhydrophobic spray coating of claim 1, wherein the volume ratio of the binder to the nanofiller dispersion is between 1:1000 and 100: 1.
3. The high transparency superhydrophobic spray coating according to claim 2, wherein the polysiloxane is selected from one or more of polydimethylsiloxane, vinyl polysiloxane, methyl hydrogen silicone oil, epoxy terminated polysiloxane, polyvinyl silicone oil.
4. The high transparency superhydrophobic spray coating according to claim 2, wherein the polysilazane is selected from one or more of inorganic polysilazane DS-3001, organic polysilazane IOTA 9118, organic polysilazane IOTA-OPSZ-9150.
5. The high transparency superhydrophobic spray coating according to claim 2, wherein the first solvent is selected from one or more of methyltrichlorosilane, octamethyltetrasiloxane, polyester diol, ethanol, acetone, methyltrimethoxysilane.
6. The high-transparency superhydrophobic spray coating of claim 2, wherein the nano-filler is selected from one or more of silica, zinc oxide, titanium dioxide, alumina, clay, and glass powder, and the particle size of the nano-filler is 1-500 nm.
7. The high transparency superhydrophobic spray coating of claim 6, wherein the nanofiller is hollow or solid and the nanofiller is spherical, rod-like, tetrapod-like or plate-like in shape.
8. The high transparency superhydrophobic spray coating according to claim 2, wherein the hydrophobic modifier is selected from one or more of long chain alkyl amine and fluorine-containing silane coupling agent; the second solvent is selected from one or more of ethanol, acetone, heptane and toluene.
9. A method for preparing a high transparency superhydrophobic spray coating according to any one of claims 1-8, comprising the steps of:
mixing polysiloxane, polysilazane, a flatting agent and a first solvent to obtain a binder;
mixing the nano filler, the hydrophobic modifier and the second solvent to obtain nano filler dispersion liquid;
mixing the binder and the nano filler dispersion liquid to prepare high-transparency super-hydrophobic spraying slurry;
and atomizing the high-transparency super-hydrophobic spraying slurry by using a pressure spray gun, spraying the atomized high-transparency super-hydrophobic spraying slurry on the surface of a target substrate, and curing to form the high-transparency super-hydrophobic spraying coating.
10. The method for preparing a high-transparency superhydrophobic spray coating according to claim 9, further comprising the steps of, before spraying the high-transparency superhydrophobic spray coating on a target substrate surface:
and cleaning the surface of the base material by using deionized water and ethanol in sequence.
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