CN108587447B - Preparation method of durable transparent super-hydrophobic coating suitable for various substrates - Google Patents

Preparation method of durable transparent super-hydrophobic coating suitable for various substrates Download PDF

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CN108587447B
CN108587447B CN201810209419.6A CN201810209419A CN108587447B CN 108587447 B CN108587447 B CN 108587447B CN 201810209419 A CN201810209419 A CN 201810209419A CN 108587447 B CN108587447 B CN 108587447B
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coating
super
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durable transparent
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CN108587447A (en
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董兵海
张艳平
王世敏
赵丽
万丽
王二静
李静
李文路
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Hubei University
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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
    • C09D183/04—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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention relates to a durable transparent super-hydrophobic coating suitable for various substrates and a preparation method thereof. The preparation method of the invention is that the nano-scale is prepared by mixingSiO of (2)2Reacting the particles with a silane coupling agent at room temperature, acidifying to obtain sol precursor solution, and drying at high temperature to obtain powder with super-hydrophobic property. SiO with super-hydrophobic property2The powder and polydimethylsiloxane are mixed in an alkane solvent, dispersed by ultrasonic waves, coated on the surface of a base material, and subjected to heat treatment to obtain the transparent super-hydrophobic coating. The invention has simple process, low reaction temperature, wide product adaptability and large-scale industrial production. Has good thermal stability, chemical stability and mechanical property stability, and can meet the requirements of outdoor environment.

Description

Preparation method of durable transparent super-hydrophobic coating suitable for various substrates
Technical Field
The invention relates to the technical field of coating preparation, in particular to a transparent super-hydrophobic coating which has certain durability and is suitable for various substrates and a preparation method thereof.
Background
The transparent super-hydrophobic coating is used as a functional coating and has great application potential in the aspects of microfluid, pollution prevention, corrosion resistance, oil-water separation and the like. The method has great application value particularly on optical automobile windshields, solar cells, safety goggles of electronic equipment and windows.
Silica is stable under ultraviolet light and the preparation method is simple, so it is often used to prepare superhydrophobic coatings in various ways. Chemically, since the silica surface has a large number of hydroxyl groups and can be grafted with various hydrophobic groups, the surface energy of the silica surface can be adjusted according to the grafted groups; and for physical properties, silica may exhibit excellent stability at high temperature, which may allow its surface to be grafted with different groups. In addition, when the particle size of the silicon dioxide is less than 100nm, high transparency is shown, and even the function of anti-reflection can be achieved by adjusting the thickness of the silicon dioxide film.
Patent applications are numerous for the preparation of transparent superhydrophobic coatings, such as patent applications of publication numbers CN103803814A, CN103524053A, CN101362632, CN101519278, CN103553359A, CN 103060773A. However, these methods mostly adopt perfluorosilane as a modifier, and form a film at high temperature, which consumes a lot of energy and has a complex film forming process, and the coatings prepared by these methods have poor thermal stability and chemical stability, and cannot meet the requirements of outdoor environment.
The super-hydrophobic coating has poor adhesion force between the coating and a base material, the rough structure is very fragile, the super-hydrophobic performance is lost when the mechanical actions such as impact, friction and the like from the surface are easily damaged, and in addition, when the coating is exposed outdoors, the coating needs to have good durability so as to meet the requirements of industrial application.
Disclosure of Invention
In view of the above, the invention provides a durable transparent super-hydrophobic coating which has simple preparation process and low production cost and is suitable for various substrates and a preparation method thereof2A super-hydrophobic coating prepared by compounding PDMS with SiO2The PDMS is uniformly dispersed in the solvent, so that the hydrophobic silicon dioxide is partially wrapped by the PDMS, the loss of hydrophobic groups can be reduced in a severe outdoor environment, in addition, the adhesion force between the coating and the substrate is enhanced by adding the PDMS, the thermal stability, the chemical stability and the mechanical property stability of the coating are improved, the applicability of the prepared coating is wide, the transparency is high, the preparation method is simple and feasible, and the industrial application range of the super-hydrophobic coating is greatly improved.
In a first aspect, the present invention provides a method for preparing a durable transparent superhydrophobic coating that is adaptable to a variety of substrates, comprising the steps of:
s1, taking nano SiO2Dissolving the particles in an alcohol solvent, and performing ultrasonic dispersion for 2-8 h to obtainUniformly dispersed SiO2Suspending liquid;
s2, taking SiO2Adding an alkyl chain silane coupling agent and a hydrochloric acid solution into the suspension in a stirring state, and performing ultrasonic dispersion stirring for 2-8 hours to obtain a sol precursor solution; the addition volume of the alkyl chain silane coupling agent and SiO2The volumes of the suspension liquid are equal;
s3, centrifugally drying the precursor solution to obtain white powder, and drying in vacuum to obtain partially methyl-modified SiO2Powder;
s4, selecting SiO in step S32Dissolving the powder in an alkane solvent, adding silicone into the solution, and stirring and ultrasonically treating for 2-4 h to obtain a dispersion liquid, wherein the adding mass of the silicone and SiO2The mass ratio of the powder is 0-0.7: 0.3;
and S5, coating the dispersion liquid on a substrate, drying the substrate by hot air, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
In a second aspect, the present invention provides coatings prepared using the above-described method for preparing durable transparent superhydrophobic coatings that are adaptable to a variety of substrates.
Compared with the prior art, the invention has the beneficial effects that:
1. the durable transparent super-hydrophobic coating prepared by the invention has simple preparation method and low cost;
2. the durable transparent super-hydrophobic coating prepared by the method has higher transparency, and the highest transmittance of the durable transparent super-hydrophobic coating can reach 80%;
3. the durable transparent super-hydrophobic coating prepared by the invention can still keep the super-hydrophobic characteristic at the low temperature of-15 ℃ and the high temperature of 500 ℃;
4. the durable transparent super-hydrophobic coating prepared by the invention can still keep the super-hydrophobic characteristic in acidic, alkaline, neutral and salt environments;
5. the durable transparent super-hydrophobic coating prepared by the invention can still keep the super-hydrophobic characteristic when the durable transparent super-hydrophobic coating passes through water flow and gravel washing;
6. the durable transparent super-hydrophobic coating prepared by the invention can be applied to various substrates such as wood, paper, copper mesh, glass and the like.
The invention has simple process, low production cost and wide coating adaptability, and can be used for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a scan of the superhydrophobic coatings prepared in examples 5 and 2, wherein a is a scan of the coating obtained in example 6 and b is a scan of the coating obtained in example 2.
FIG. 2 is an atomic force microscope image of the superhydrophobic coating prepared in example 5 and example 2; wherein a is the AFM image of the coating obtained in example 6, and b is the AFM image of the coating obtained in example 2.
FIG. 3 is a diagram of a transparent superhydrophobic film on a different substrate prepared in example 2; wherein, the base material in a is A4 paper, the base material in b is wood, the base material in c is glass, the base material in d is cotton cloth, and the base material in e is copper mesh.
Fig. 4 is a graph of transparency of the super-hydrophobic coatings prepared in examples 2 and 5 after spraying on a glass slide, wherein the glass slide is coated with an uncoated coating, coated with an uncoated PDMS coating, and coated with 0.3g of PDMS coating.
Fig. 5 is a thermal stability diagram of the superhydrophobic coating prepared in example 2.
Fig. 6 is a graph of the contact angle of the superhydrophobic coating prepared in example 2 after being soaked in an acid-base solution and then washed with water and gravel, wherein a is the graph of the contact angle without treatment, b is the graph of the contact angle after being soaked in a solution with pH of 2 for 2h, c is the graph of the contact angle after being soaked in a solution with pH of 12 for 2h, d is the graph of the contact angle after being washed with water, and e is the graph of the contact angle after being washed with gravel.
Detailed Description
In a first aspect, the present invention provides a method for preparing a durable transparent superhydrophobic coating that is adaptable to a variety of substrates, comprising the steps of:
s1, taking nano SiO2Dissolving the particles in an alcohol solvent, and performing ultrasonic dispersion for 2-8 h to obtain uniformly dispersed SiO2Suspending liquid;
s2, taking SiO2Adding an alkyl chain silane coupling agent and a hydrochloric acid solution into the suspension in a stirring state, and performing ultrasonic dispersion stirring for 2-8 hours to obtain a sol precursor solution; the addition volume of the alkyl chain silane coupling agent and SiO2The volumes of the suspension liquid are equal;
s3, centrifugally drying the precursor solution to obtain white powder, and drying in vacuum to obtain partially methyl-modified SiO2Powder;
s4, selecting SiO in step S32Dissolving the powder in an alkane solvent, adding silicone into the solution, and stirring and ultrasonically treating for 2-4 h to obtain a dispersion liquid, wherein the adding mass of the silicone and SiO2The mass ratio of the powder is 0-0.7: 0.3;
and S5, coating the dispersion liquid on a substrate, drying the substrate by hot air, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
PDMS (polydimethylsiloxane) is a hydrophobic organic silicon material, has good wear resistance, chemical stability, physiological inertia, electric insulation, no toxicity and no odor, is a low-surface-energy material, is colorless and transparent, can be used for preparing a transparent super-hydrophobic layer, has certain adhesive force and can improve the binding force between a coating and a base material. By mixing PDMS and SiO2And by compounding, the thermal stability, the chemical stability and the mechanical property stability of the super-hydrophobic coating can be effectively improved, the durability of the super-hydrophobic coating is enhanced, and the industrial application range of the transparent super-hydrophobic coating is expanded.
The invention relates to SiO modified by silane coupling agent2Uniformly dispersed in the solution with PDMS to make PDMS partially wrap SiO2The particles reduce the exposure of hydrophobic groups, ensure super-hydrophobicity, and simultaneously enhance the thermal stability, chemical stability and SiO of the super-hydrophobic coating2Surface residual hydroxyl groupsThe coating is hydrogen bonded with hydroxyl on the surface of PDMS, so that the adhesive force of the coating is improved, and the durability of the super-hydrophobic coating is further improved.
Preferably, the SiO of nanometer scale in step S12The particles are SiO with the particle size of 20 nm-100 nm2Particles. Specifically, it may be 20nm, 40nm, 70nm or 100nm SiO2One or a mixture of several of the particles mixed according to any proportion.
More preferably, the alcoholic solvent in step S1 is one or a mixture of ethanol, methanol, n-propanol or isopropanol mixed in any proportion; the SiO2The ratio of the mass of the particles to the volume of the alcohol solvent is 1: 9-11 g/mL.
Preferably, the alkyl chain silane coupling agent in step S2 is one or a mixture of several of methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, methyltriethoxysilane and aminopropyltriethoxysilane mixed in any proportion.
Preferably, the hydrochloric acid solution in the step S2 is a hydrochloric acid solution with a mass fraction of 25-28%, and the addition volume of the hydrochloric acid solution and SiO are2The volume ratio of the suspension is 0.1-0.3: 2.
Preferably, the silicone in step S4 is one or both of silicone 184 and silicone 181. The silicone is a series of polydimethylsiloxanes with different molecular weights, and the preferred silicone of the invention is silicone 184, which has a mass ratio of the A component (PDMS) to the B component (curing agent) of 10: 1.
Preferably, the alkane solvent in step S4 is one or two of n-hexane and n-heptane.
Preferably, in step S5, the coating method is selected from spray coating, spin coating, dip coating and the like, and the preferred method is spray coating, the spray speed of a spray gun is 2-4cm/S, and the spray distance is 15-20 cm; the temperature of the hot air is 115-125 ℃.
In a second aspect, the present invention provides coatings prepared using the above-described method for preparing durable transparent superhydrophobic coatings that are adaptable to a variety of substrates.
In order to facilitate understanding of the present invention, the present invention will be described more fully and in detail below with reference to the accompanying drawings and examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specified, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by an existing method, and for example, the used raw materials silicone 184 and silicone 181 are commercially available.
Example 1
This example provides a method for preparing a durable transparent superhydrophobic coating that can be applied to a variety of substrates by incorporating nanoscale SiO2Reacting the particles with a silane coupling agent at room temperature, acidifying to obtain sol precursor solution, and drying at high temperature to obtain powder with super-hydrophobic property. Mixing the super-hydrophobic powder with polydimethylsiloxane in an alkane solvent, and ultrasonically dispersing to partially wrap the PDMS with SiO2And (4) obtaining a dispersion liquid, coating the surface of the base material, and performing heat treatment to obtain the super-hydrophobic coating. The method specifically comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 5h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is obtained by mixing ethanol and n-propanol according to the volume ratio of 2: 1.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring is carried out for 5 hours to obtain sol precursor solution; the alkyl chain silane coupling agent is obtained by mixing methyl trimethoxy silane and ethyl trimethoxy silane according to the volume ratio of 1: 1.
(3) Centrifugally drying the precursor solution in the same amount of the step (2) to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) 0.3g of SiO in step (3) was taken2Dissolving the powder in 20ml of alkane solvent, adding 0.1g of silicone 184 (the mass ratio of the component A to the component B is 10: 1) into the solution, stirring and ultrasonically treating for 3 hours to uniformly divide PDMS and SiO2Uniformly dispersing the particles in a solvent to obtain a dispersion liquid; the alkane solvent is n-hexane.
(5) Spraying the dispersion liquid on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
Example 2
The embodiment provides a preparation method of a durable transparent super-hydrophobic coating suitable for various substrates, which comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 6h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is isopropanol.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring is carried out for 6 hours to obtain sol precursor solution; the alkyl chain silane coupling agent is aminopropyl triethoxysilane.
(3) Centrifugally drying the precursor solution in the same amount of the step (2) to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) 0.3g of SiO in step (3) was taken2Dissolving the powder in 20ml of alkane solvent, adding 0.3g of silicone 184 (the mass ratio of the component A to the component B is 10: 1) into the solution, and stirring and ultrasonically treating for 3 hours to obtain PDMS and SiO2Uniformly dispersing in a solvent to obtain a dispersion liquid; the alkane solvent is n-hexane.
(5) Spraying the dispersion liquid on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
The scanning image of the superhydrophobic coating prepared in this example is shown in fig. 1, the atomic force microscope image of the obtained coating is shown in fig. 2, the transparency image of the superhydrophobic coating after being sprayed on a glass slide is shown in fig. 4, the transmittance ratio pairs of different addition amounts of PDMS at the wavelengths of 550nm and 800nm are shown in table 1, and the thermal stability image of the superhydrophobic coating is shown in fig. 5.
TABLE 1 comparison of the transmittance at wavelengths of 550nm and 800nm for different amounts of PDMS added
Figure BDA0001596770110000071
The dispersion obtained in this example was sprayed onto different substrates, the transparent superhydrophobic film pattern of which is shown in fig. 3, the substrates are respectively a4 paper, wood, glass, cotton cloth, and copper mesh, and specifically, the contact angles on the different substrates are as follows: the contact angle on A4 paper was 154 °, the contact angle on glass was 155 °, the contact angle on copper mesh was 153 °, the contact angle on wood was 152 °, and the contact angle on cotton was 153 °; the spraying process comprises the following steps: the spraying speed of the spray gun is 2-4cm/s, and the spraying distance is 15-20 cm.
After the superhydrophobic coating obtained in this embodiment is soaked in an acid-base solution, a contact angle graph of water flow and gravel after scouring is shown in fig. 6, as can be seen from fig. 6, the contact angle when the superhydrophobic coating is not treated is 155 °, the contact angle is 152 ° after the superhydrophobic coating is soaked in a solution with PH 2 for 2 hours, the contact angle is 153 ° after the superhydrophobic coating is soaked in a solution with PH 12 for 2 hours, the contact angle is 152 ° after the superhydrophobic coating is washed by water flow, and the contact angle is 151 ° after the superhydrophobic coating is scoured by gravel.
Example 3
The embodiment provides a preparation method of a durable transparent super-hydrophobic coating suitable for various substrates, which comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 3h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is a mixture of methanol and n-propanol.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring is carried out for 8 hours, and sol precursor solution is obtained; the alkyl chain silane coupling agent is propyl trimethoxyA silane.
(3) Centrifugally drying the precursor solution in the same amount of the step (2) to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) 0.3g of SiO in step (3) was taken2Dissolving the powder in 20ml of alkane solvent, adding 0.5g of silicone 184 (the mass ratio of the component A to the component B is 10: 1) into the solution, stirring and ultrasonically treating for 4h, and mixing PDMS with SiO2Uniformly dispersing in a solvent to obtain a dispersion liquid; the alkane solvent is n-heptane.
(5) Spraying the dispersion liquid on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
Example 4
The embodiment provides a preparation method of a durable transparent super-hydrophobic coating suitable for various substrates, which comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 8h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is ethanol.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring for 3h to obtain sol precursor solution; the alkyl chain silane coupling agent is methyl triethoxysilane.
(3) Centrifugally drying the precursor solution in the same amount of the step (2) to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) dissolving 0.3g of the super-hydrophobic powder obtained in the step (3) in 20ml of alkane solvent, adding 0.7g of silicone 184 (the mass ratio of the component A to the component B is 10: 1) into the solution, and stirring and ultrasonically treating for 2 hours to obtain PDMS and SiO2Uniformly dispersing in a solvent to obtain a dispersion liquid; the alkane solvent is obtained by mixing n-hexane and n-heptane according to the volume ratio of 1: 1.
(5) Spraying the dispersion liquid on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
Example 5
The embodiment provides a preparation method of a durable transparent super-hydrophobic coating suitable for various substrates, which comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 5h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is isopropanol.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring is carried out for 5 hours to obtain sol precursor solution; the alkyl chain silane coupling agent is aminopropyl triethoxysilane.
(3) Washing and filtering the precursor solution in the same amount of the step (2) by a sand core funnel to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) 0.3g of SiO in step (3) was taken2Dissolving the powder in 20ml of alkane solvent, and stirring and ultrasonically treating for 3 hours to obtain a super-hydrophobic spray; the alkane solvent is n-hexane.
(5) Spraying the spray on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for many times to obtain the transparent super-hydrophobic coating.
In order to contrast with other examples, this example is used as a comparative example, and the PDMS content in the preparation step is 0.
Example 6
The embodiment provides a preparation method of a durable transparent super-hydrophobic coating suitable for various substrates, which comprises the following steps:
(1) taking nano-scale SiO2Dissolving 2g of particles in 20ml of solvent alcohol, and ultrasonically dispersing for 8h to obtain uniformly dispersed SiO2Suspending liquid; the solvent alcohol is ethanol.
(2) Equivalent SiO of step (1)22ml of an alkyl chain silane coupling agent and 0.1ml of a 28% hydrochloric acid solution were added to the suspension under stirring. Ultrasonic dispersion stirring for 3h to obtain sol precursor solution; the alkyl chain silane coupling agent is methyl triethoxy siliconAn alkane.
(3) Centrifugally drying the precursor solution in the same amount of the step (2) to obtain white powder, and drying in vacuum to obtain partially methylated SiO2Powder;
(4) dissolving 0.3g of the super-hydrophobic powder obtained in the step (3) in 20ml of alkane solvent, adding 0.7g of silicone 181 into the solution, stirring and ultrasonically treating for 2 hours to obtain PDMS and SiO2Uniformly dispersing in a solvent to obtain a dispersion liquid; the alkane solvent is obtained by mixing n-hexane and n-heptane according to the volume ratio of 1: 1.
(5) Spraying the dispersion liquid on various substrates, drying the substrates by using hot air at 120 ℃, and circulating for multiple times to obtain the transparent super-hydrophobic coating.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. A preparation method of a durable transparent super-hydrophobic coating suitable for various substrates is characterized by comprising the following steps: the method comprises the following steps:
s1, taking nano SiO2Dissolving the particles in an alcohol solvent, and performing ultrasonic dispersion for 2-8 h to obtain uniformly dispersed SiO2Suspending liquid;
s2, taking SiO2Adding an alkyl chain silane coupling agent and a hydrochloric acid solution into the suspension under the stirring state, and performing ultrasonic dispersion stirring for 2-8 hours to obtain a sol precursor solution; the addition volume of the alkyl chain silane coupling agent and SiO2The volumes of the suspension liquid are equal;
s3, centrifugally drying the precursor solution to obtain white powder, and drying in vacuum to obtain partially methyl-modified SiO2Powder;
s4, taking the SiO with partial methyl modification in the step S32Dissolving the powder in an alkane solvent, adding silicone into the solution, and stirring and ultrasonically treating for 2-4 h to obtain a dispersion liquid, wherein the adding mass of the silicone and SiO2The mass ratio of the powder is 0.1-0.7: 0.3;
s5, converting the result of the step S4Coating the dispersion liquid on a substrate, drying the substrate by hot air, and circulating for multiple times to obtain a transparent super-hydrophobic coating; step S2, the hydrochloric acid solution is 25-28% by mass, and the addition volume of the hydrochloric acid solution and SiO2The volume ratio of the suspension is 0.1-0.3: 2.
2. The method of claim 1 for preparing a durable transparent superhydrophobic coating that can accommodate a variety of substrates, comprising: step S1 of nano-scale SiO2The particles are SiO with the particle size of 20 nm-100 nm2Particles.
3. The method of claim 2, wherein the durable transparent superhydrophobic coating comprises: step S1, the alcohol solvent is one or more of ethanol, methanol, n-propanol or isopropanol; the SiO2The ratio of the mass of the particles to the volume of the alcohol solvent is 1: 9-11 g/mL.
4. The method of claim 1 for preparing a durable transparent superhydrophobic coating that can accommodate a variety of substrates, comprising: the alkyl chain silane coupling agent in the step S2 comprises methyltrimethoxysilane and/or methyltriethoxysilane.
5. The method of claim 1 for preparing a durable transparent superhydrophobic coating that can accommodate a variety of substrates, comprising: step S4 the silicone is one or both of silicone 184 and silicone 181.
6. The method of claim 1 for preparing a durable transparent superhydrophobic coating that can accommodate a variety of substrates, comprising: in the step S4, the alkane solvent is one or two of n-hexane and n-heptane.
7. The method of claim 1 for preparing a durable transparent superhydrophobic coating that can accommodate a variety of substrates, comprising: in the step S5, the coating mode is spraying, the spraying speed of a spray gun is 2-4cm/S, and the spraying distance is 15-20 cm; the temperature of the hot air is 115-125 ℃.
8. A coating prepared by the method of claim 1 for preparing a durable transparent superhydrophobic coating that is conformable to a variety of substrates.
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