CN106800885A - A kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating - Google Patents

A kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating Download PDF

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CN106800885A
CN106800885A CN201611192769.3A CN201611192769A CN106800885A CN 106800885 A CN106800885 A CN 106800885A CN 201611192769 A CN201611192769 A CN 201611192769A CN 106800885 A CN106800885 A CN 106800885A
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super
coating
transparent
hydrophobic
amphiphobic coating
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张俊平
李步成
高子茜
于勃
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • C08G77/04—Polysiloxanes
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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Abstract

The invention discloses a kind of transparent hydrophobic or the large-scale preparation method of super-amphiphobic coating; it is first by nano-particle ultrasonic disperse in alcohol water mixed system; again under acid or base catalysis; nano-particle is hydrolyzed with floride-free or fluorine-containing organic silicon alkane, condensation reaction, the transperent suspension liquid of floride-free or fluorine-containing organic silicon alkane polymer nano-particle compound is obtained；Then the composite transparent suspension is imposed on by substrate material surface by spraying or dip-coating, obtains transparent hydrophobic of good performance or super-amphiphobic coating.The present invention can complete 10 100 m in 1 hour2The preparation of transparent hydrophobic or super-amphiphobic coating, realizes that large-area transparent is super-hydrophobic or prepare with scale of super-amphiphobic coating first, and with low cost, process is simple；The coating of preparation has excellent super-hydrophobic or ultra-amphosphobic energy, preferable mechanical stability, chemical stability and environmental stability, is with a wide range of applications.

Description

A kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating
Technical field
The present invention relates to a kind of super-hydrophobic or super-amphiphobic coating preparation, more particularly to a kind of transparent hydrophobic or super-amphiphobic The large-scale preparation method of coating, belongs to surface biomimetic coat preparing technology field.
Background technology
Lotus leaf just has the good reputation of " going out mud without dye " in China from ancient times.Water droplet is in Cassie- in lotus leaf surface Baxter states, can tumble from lotus leaf surface, while taking away the particulate pollutant of lotus leaf surface.Therefore, lotus leaf has mystery Self_cleaning effect.Inspired by lotus leaf self_cleaning effect, the research of bionic super-hydrophobic coating is of great interest, at present There are a large amount of reports about super-hydrophobic coat.Research shows, appropriate surface micro-nano structure and low-surface energy substance is combined Can be prepared by super-hydrophobic coat.Although super-hydrophobic coat has high contact angle and relatively low roll angle to water droplet, easily Soaked by low-energy liquid, so as to lose its self-cleaning performance.
Super-amphiphobic coating is respectively provided with high contact angle and relatively low roll angle to water and low-energy liquid, but relative to Super-hydrophobic coat is more difficult to prepare in theory and technically；Low-energy liquid often only has contact angle higher, but jail Adhere and invest surface, drop is in Wenzel states, so that simultaneously without unique self-cleaning performance.Only a small amount of research at present By designing unique surface texture, such as " overhang " structure, " re-entrant " structure, candle ash and organosilan polymerization Thing nanofiber etc., is prepared for the super-amphiphobic coating with high contact angle and relatively low roll angle.Due to its unique automatically cleaning Performance, super-hydrophobic, super-amphiphobic coating has wide in fields such as self-cleaning surface, water-oil separating, fluid drag-reduction, freezing and anti-corrosions Wealthy application prospect.
However, super-hydrophobic or super-amphiphobic coating preparation generally existing problems with：
（1）The opaque or transparency is not high.High transparency is super-hydrophobic or super-amphiphobic coating is in window, optical device and glasses etc. One of important performance applied in substrate of glass.However, super-hydrophobic or super-amphiphobic coating surface has micro-nano structure, This frequently can lead to scattering of the light in coating surface, reduce the light transmittance of coating, or even opaque.Research shows, works as surface Roughness less than visible wavelength a quarter, i.e. 100nm when, be significantly reduced scattering of the light in visible region, from And improve the transparency of coating.At present, there are reports by method systems such as vapour deposition process, template and LBL self-assemblies For transparency super-amphiphobic coating higher.The B of patent CN 101407648 disclose it is a kind of prepared by electrophoresis it is transparent super thin The method of water silica dioxide coating：Silicon dioxide colloid is deposited in conductive substrates first, then is heat-treated, most afterwards through dredging Water process is obtained super-hydrophobic transparent coating.The B of patent CN 101519278 by base treatment, solution preparation, LBL self-assembly, The step such as heat treatment and decorating hydrophobic substances is prepared for transparent hydrophobic coating, with preferable ultra-hydrophobicity and light transmittance.Specially The B of sharp CN 103060773 are disperseed by powder, are prepared for transparent surpassing into steps such as initiator, spraying and chemical vapor depositions Hydrophobic coating.The B of patent CN 102140251 disclose a kind of transparent hydrophobic coating with hydrogen containing silicone oil cured as matrix Preparation method, is obtained by the cured shaping of the titania modified particle that fluorine silicon segment is added in polymeric matrix. The B of patent CN 103524053 are prepared by base treatment, core shell structure, micro-nano structure is assembled, coating is heat-treated and hydrophobe The steps such as matter modification, are prepared for transparent hydrophobic coating.The B of patent CN 103553359 deposit one layer of cigarette ash first in substrate, Then through vapour deposition, go templating and gas phase modification be prepared for transparent hydrophobic coating.The B of patent CN 104231916 are with third Ketone is prepared for silica dioxide granule and silicon rubber pre-polymer solution for solvent, water is added after the two is mixed, by spraying process It is prepared for transparent hydrophobic coating.It is template that the B of patent CN 103626403 use carbon black and CNT, by sol-gel The steps such as change, spraying, high-temperature oxydation decomposition and the modification of surface silicon fluoride, are prepared for super-amphiphobic coating, drop roll angle<10 °, thoroughly Light rate>75%.
（2）Preparation method complex and expensive, it is difficult to carry out large area preparation.Although above-mentioned report disclose it is various prepare it is transparent Super-hydrophobic or super-amphiphobic coating method, but there is preparation method complex and expensive（Vapour deposition）, need multistep reaction and step（Layer Layer self assembly, micro-nano structure construct-surface modification protocols）, be confined to single base material（Conductive substrates, high temperature resistant substrate）With Small size base material, the problems such as transparency is not high.
（3）Stability is poor.It is existing about transparent hydrophobic or the document and patent report of super-amphiphobic coating, it is high by complexity Expensive method has been obtained transparent hydrophobic or super-amphiphobic coating, but there is mechanical stability, chemical stability and environmental stability Critical defect in terms of poor equistability, this strongly limits transparent hydrophobic or the practical application of super-amphiphobic coating.
Therefore, the transparent hydrophobic or super-amphiphobic coating of stabilization how to be obtained by simple method, realizes transparent super thin The prepare with scale of water or super-amphiphobic coating is this area problem in the urgent need to address, can promote the reality of bionical automatic cleaning coating Apply on border.
The content of the invention
The invention aims to solve what existing transparent hydrophobic or super-amphiphobic coating performance and technical elements were present A kind of problem, there is provided the large-scale preparation method of transparent hydrophobic or super-amphiphobic coating.
（One）The prepare with scale of transparent hydrophobic/super-amphiphobic coating
The large-scale preparation method of transparent hydrophobic/super-amphiphobic coating of the present invention, is first by nano-particle ultrasonic disperse in alcohol-water In mixed system, then under alkali or acid catalysis, nano-particle is set to be hydrolyzed with free-floride/fluorine-containing organic silicon alkane, be condensed instead Should, the transperent suspension liquid of free-floride/fluorine-containing organic silicon alkane polymer-nanoparticle compound is obtained；Then by spraying or dip-coating The composite transparent suspension is imposed on into substrate material surface, transparent hydrophobic/super-amphiphobic coating is obtained.
The nano-particle be montmorillonite, hectorite, attapulgite, hydrotalcite, kaolinite, silica, titanium dioxide, At least one in zinc oxide, aluminum oxide, CNT, graphene oxide or nano-cellulose；The particle diameter of nano-particle be 5 ~ 60 nm。
In the alcohol-water mixed system, alcohol is at least one in methyl alcohol, ethanol, propyl alcohol and ethylene glycol；The body of alcohol and water Product is than being 80:1~2:1.Mass percent of the nano-particle in alcohol-water mixed system is 0.01 ~ 2.5%；It is floride-free/fluorine-containing organic Percentage by volume of the silane body in alcohol-water mixed system is 0.02% ~ 25%.
The alkali as catalyst be ammoniacal liquor, ethylenediamine, triethylamine, NaOH, potassium hydroxide, sodium methyl silicate and At least one in potassium methyl silicate；The acid as catalyst is at least in hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, formic acid Kind；Mass percent of the catalyst in alcohol-water mixed system is 0.2% ~ 10%.
The hydrolysis of the free-floride/fluorine-containing organic silicon alkane and nano-particle, condensation reaction are that 1 ~ 48 h is carried out at 0 ~ 80 DEG C.
The base material is smooth or coarse glass, ceramics, stone material, concrete, metal, plastics, rubber, timber, Leather or fabric.
It in spray pressure is 0.1 ~ 0.6 MPa that the spraying is, under conditions of spray distance is 10 ~ 150 cm, will be compound Thing suspension spray is in substrate material surface.
The dip-coating is to impregnated in base material to keep 1 ~ 10 min in compound suspension, then dry naturally or 3 ~ 30 min are processed at 60 ~ 150 DEG C.
The fluorine-containing organic silicon alkane is perfluoro capryl trichlorosilane, perfluoro capryl trimethoxy silane, the second of perfluoro capryl three TMOS, perfluoro decyl trichlorosilane, perfluoro decyl trimethoxy silane, perfluoro decyl triethoxysilane, perfluoro capryl Dimethylchlorosilane, perfluoro capryl dimethyl methoxy silane, perfluoro decyl dimethylchlorosilane, perfluoro decyl dimethyl methoxy At least one in base silane.The coating for using fluorine-containing organic silicon alkane to prepare is transparent super-amphiphobic coating.Transparent super-amphiphobic coating Light transmittance be more than 90%（600nm）；Contact angle of the 5 μ L water droplets on above-mentioned coating is 160 ° ~ 166 °, and roll angle is 1 ~ 3 °； Contact angle of the 5 μ L n-decanes drops on above-mentioned coating is 153 ° ~ 165 °, and roll angle is 5 ~ 8 °；10kPa water columns wash away 10min, After immersion 5 days, laboratory are placed 180 days or ultraviolet irradiation 96h in saturated sodium-chloride, liquid-drop contact angle>155 °, roll angle< 10°。
The floride-free organosilan be MTMS, MTES, ethyl trimethoxy silane, Ethyl triethoxysilane, vinyltrimethoxy silane, VTES, phenyltrimethoxysila,e, phenyl Triethoxysilane, octyl group trimethoxy silane, octyltri-ethoxysilane, dodecyltrimethoxysilane, dodecyl Triethoxysilane, hexadecyl trimethoxy silane, hexadecyl, 3- (methacryloxypropyl) propyl group three Methoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, aminopropyl trimethoxysilane, aminopropyl-triethoxy At least one in silane, tetraethyl orthosilicate and methyl silicate.Coating prepared by floride-free organosilan is used for transparent super thin Water coating.The light transmittance of transparent hydrophobic>88%（600nm）；Contact angle of the 5 μ L water droplets on above-mentioned coating is 157 ° ~ 160 °, Roll angle is 1 ~ 6 °；10kPa water columns wash away in 10min, saturated sodium-chloride and soak 5 days, laboratory placement 180 days or ultraviolet irradiation After 96h, water droplet contact angle>155 °, roll angle<10°.
In sum, the present invention has advantages below compared with the prior art：
1st, coating prepared by the present invention has excellent super-hydrophobic/ultra-amphosphobic energy, the transparency, preferable mechanical stability, change Stability and environmental stability are learned, photovoltaic panel, glass curtain wall, windshield, ceramics, stone material, concrete, gold is can be applied to The material surfaces such as category, plastics, rubber, timber, leather or fabric；
2nd, the present invention can complete 10 ~ 100 m in 1 hour2The preparation of transparent hydrophobic/super-amphiphobic coating, realizes big first The prepare with scale of area transparent hydrophobic/super-amphiphobic coating；
3rd, preparation method of the invention is with low cost, process is simple, applied widely, it is easy to which industrialization and scale are applied.
Brief description of the drawings
Fig. 1 is the ESEM on the transparent hydrophobic surface of preparation in embodiment 1 in photo.
Fig. 2 is the digital photograph on the transparent hydrophobic surface of preparation in embodiment 2.
Fig. 3 is the digital photograph of transparent super-double-hydrophobic surface prepared by embodiment 4.
Fig. 4 is the transmission electron microscope photo of transparent super-amphiphobic suspension prepared by embodiment 5.
Specific embodiment
Further is made to the preparation of transparent hydrophobic of the present invention or super-amphiphobic coating and performance below by specific embodiment Explanation.
Embodiment 1
Weigh 0.5g attapulgites, be added in 100mL conical flasks, then measure respectively 34mL ethanol, 2mL ammoniacal liquor and 14mL go from Sub- water, magnetic agitation 10min, ultrasonic 10min.2.1mL tetraethyl orthosilicates and 5.2mL MTMSs are measured afterwards, It is added in conical flask, stirring reaction 16h obtains translucent g., jelly-like gel at room temperature；50 times, warp are diluted using absolute ethyl alcohol After 10 min of ultrasound, super-hydrophobic transparent suspension is obtained.100 mL super-hydrophobic transparent suspension are measured, spray pressure is controlled 0.3MPa, spray distance are sprayed at the glass surface of 50cm × 50cm in 40cm, obtain transparent hydrophobic glass（ESEM Figure is shown in Fig. 1）.
The light transmittance of transparent hydrophobic glass is 88.6%（600nm）；The contact angle of 5 μ L water droplets is 162 °, and roll angle is 3°；10kPa water columns wash away in 10min, saturated sodium-chloride soak 5 days, laboratory place 180 days or ultraviolet irradiation 96h after, water droplet Contact angle>155 °, roll angle<10°.
Embodiment 2
Weigh 1.0g Nano particles of silicon dioxide, be added in 250mL conical flasks, then measure respectively 84mL ethanol, 2mL acetic acid and 14mL deionized waters, magnetic agitation 10min, ultrasonic 20min.1.2mL tetraethyl orthosilicates, the second of 0.5mL aminopropyls three are measured afterwards TMOS and 7.2mL hexadecyl trimethoxy silanes, are added in conical flask, and stirring reaction 12h obtains semi-transparent at 40 DEG C Bright g., jelly-like gel；Using absolute ethyl alcohol dilute 70 times, through ultrasonic 10 min after, obtain super-hydrophobic transparent suspension.Measure 2L Super-hydrophobic transparent suspension, control spray pressure 0.5MPa, spray distance are sprayed at 3 pieces of 1m × 1m's in 100cm, 30min Glass surface, obtains 3m2Transparent hydrophobic glass（Digital photograph figure is shown in Fig. 2）.
The light transmittance of transparent hydrophobic glass is 89.6%（600nm）；The contact angle of 5 μ L water droplets is 158 °, and roll angle is 4°；10kPa water columns wash away in 10min, saturated sodium-chloride soak 5 days, laboratory place 180 days or ultraviolet irradiation 96h after, water droplet Contact angle>155 °, roll angle<10°.
Embodiment 3
Weigh 1.0g graphene oxides, be added in 500mL round-bottomed flasks, then measure respectively 180mL ethanol, 50mL ethylene glycol, 1mL hydrochloric acid and 19mL deionized waters, magnetic agitation 10min, ultrasonic 10min.Measure afterwards 5mL MTESs, 0.2mL aminopropyl triethoxysilanes, 2.0mL tetraethyl orthosilicates and 9mL dodecyltrimethoxysilanes, are added to round bottom burning In bottle, stirring reaction 8h obtains brown g., jelly-like gel at 50 DEG C；Using absolute ethyl alcohol dilute 100 times, through ultrasonic 10 min after, Obtain super-hydrophobic transparent suspension.Measure 300mL super-hydrophobic transparent suspension respectively, control spray pressure 0.4MPa, spraying away from From being 120cm, glass, marble, timber and the aluminum alloy surface of 1m × 1m are sprayed in 30min, on 4 kinds of base materials To transparent hydrophobic coating.Or the polyester textile and leather of 1m × 1m impregnated in 5L super-hydrophobic transparent suspension keep 5min, then processes 15 min at 60 DEG C.
The light transmittance of transparent hydrophobic glass is 90.2%（600nm）, the transparency of coating phase therewith on other base materials When；Contact angle of the 5 μ L water droplets on above-mentioned coating is 160 °, and roll angle is 1 ~ 6 °；10kPa water columns wash away 10min, saturation chlorination After immersion 5 days, laboratory are placed 180 days or ultraviolet irradiation 96h in sodium, water droplet contact angle>155 °, roll angle<10°.
Embodiment 4
5g hectorites are weighed, is added in 10L reactors, then measure 4L ethanol, 0.1L methyl alcohol, 0.25L ethylene glycol, 50mL respectively Ammoniacal liquor and 0.6L deionized waters, mechanical agitation 10min, ultrasonic 20min.6mL tetraethyl orthosilicates, 20mL γ-shrink are measured afterwards Glycerine ether oxygen propyl trimethoxy silicane and 6mL perfluoro capryl trimethoxy silanes, are added in reactor, 40 DEG C of stirring reactions 12h obtains super-amphiphobic transperent suspension liquid.250mL super-amphiphobic transperent suspension liquid, control spray pressure 0.5MPa, spraying are measured respectively Distance is 100cm, and glass, ceramics and the polytetrafluoro plate surface of 1m × 1m are sprayed in 20min, is obtained on 3 kinds of base materials Transparent super-amphiphobic coating（Digital photograph figure is shown in Fig. 3）.
The light transmittance of transparent super-amphiphobic glass is 89.4%（600nm）, the transparency of coating phase therewith on other base materials When；Contact angle of the 5 μ L water droplets on above-mentioned coating is 162 ° ~ 168 °, and roll angle is 1 ~ 2 °；5 μ L n-decanes drops are in above-mentioned painting Contact angle on layer is 155 ° ~ 163 °, and roll angle is 6 ~ 8 °；10kPa water columns wash away in 10min, saturated sodium-chloride soak 5 days, After laboratory is placed 180 days or ultraviolet irradiation 96h, liquid-drop contact angle>155 °, roll angle<10°.
Embodiment 5
Weigh 5.0g Nano particles of silicon dioxide, be added in 500mL round-bottomed flasks, then be separately added into 50mL deionized waters, 0.2g potassium hydroxide, 200mL ethanol and 10mL propyl alcohol, magnetic agitation 10min, ultrasonic 20min.The second of 2mL phenyl three is measured afterwards TMOS, 0.5mL aminopropyl triethoxysilanes, 1.0mL tetraethyl orthosilicates and 6mL perfluoro decyl triethoxysilanes, plus Enter in round-bottomed flask, stirring reaction 12h obtains translucent g., jelly-like gel at room temperature；60 times, warp are diluted using absolute ethyl alcohol After 10 min of ultrasound, super-amphiphobic transperent suspension liquid is obtained（Transmission electron microscope photo is shown in Fig. 4）.Measure the suspension of 500mL super-hydrophobic transparents Liquid, controls spray pressure 0.4MPa, spray distance for 100cm, is sprayed in 30min on 2 blocks of glass of 1m × 1m and obtains transparent Super-amphiphobic coating.Or 5min is kept during the polyester textile of 1m × 1m impregnated in into 4L super-amphiphobic transperent suspension liquid, then in room temperature Dry, obtain final product transparent super-amphiphobic glass.
The light transmittance of transparent super-amphiphobic glass is 90.1%（600nm）, the transparency of coating is suitable therewith on polyester textile；5 Contact angle of the μ L water droplets on above-mentioned coating is 160 ° ~ 166 °, and roll angle is 1 ~ 3 °；5 μ L n-decanes drops are on above-mentioned coating Contact angle be 153 ° ~ 165 °, roll angle be 5 ~ 8 °；10kPa water columns wash away in 10min, saturated sodium-chloride and soak 5 days, experiment After room is placed 180 days or ultraviolet irradiation 96h, liquid-drop contact angle>155 °, roll angle<10°.
Embodiment 6
50g montmorillonites are weighed, is added in 100L reactors, then measure 45L ethanol, 1L methyl alcohol, 0.5L propyl alcohol, 25mL ammonia respectively Water, 5g sodium methyl silicates and 8L deionized waters, mechanical agitation 10min, ultrasonic 20min.Measure afterwards 20mL tetraethyl orthosilicates, 15mL phenyl triethoxysilanes, 10mL aminopropyl trimethoxysilanes, 60mL perfluoro capryls trimethoxy silane and 10mL are complete Fluorine decyl dimethyl methoxylsilane, is added in reactor, and stirring reaction 24h obtains super-amphiphobic transperent suspension liquid at room temperature. Control spray pressure 0.6MPa, spray distance for 150cm, the above-mentioned super-amphiphobic transperent suspension liquid of 30L is sprayed at 80m in 60min2 On glass surface, transparent super-amphiphobic coating is obtained.
The light transmittance of transparent super-amphiphobic glass is 90.7%（600nm）；Contact angle of the 5 μ L water droplets on above-mentioned coating be 165 °, roll angle is 1 ~ 2 °；Contact angle of the 5 μ L n-decanes drops on above-mentioned coating is 158 °, and roll angle is 5-7 °；10kPa Water column wash away in 10min, saturated sodium-chloride soak 5 days, laboratory place 180 days or ultraviolet irradiation 96h after, liquid-drop contact angle> 155 °, roll angle<10°.

Claims (10)

1. a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, is first by nano-particle ultrasonic disperse in alcohol-water In mixed system, then under acid or base catalysis, nano-particle is set to be hydrolyzed with free-floride/fluorine-containing organic silicon alkane, be condensed instead Should, the transperent suspension liquid of free-floride/fluorine-containing organic silicon alkane polymer-nanoparticle compound is obtained；Then by spraying or dip-coating The composite transparent suspension is imposed on into substrate material surface, transparent hydrophobic/super-amphiphobic coating is obtained.
2. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Receive Rice corpuscles be montmorillonite, hectorite, attapulgite, hydrotalcite, kaolinite, silica, titanium dioxide, zinc oxide, aluminum oxide, At least one in CNT, graphene oxide or nano-cellulose；The particle diameter of nano-particle is 5 ~ 60 nm.
3. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute Fluorine-containing organic silicon alkane is stated for perfluoro capryl trichlorosilane, perfluoro capryl trimethoxy silane, perfluoro capryl triethoxysilane, complete Fluorine decyltrichlorosilane, perfluoro decyl trimethoxy silane, perfluoro decyl triethoxysilane, perfluoro capryl dimethyl chloride silicon In alkane, perfluoro capryl dimethyl methoxy silane, perfluoro decyl dimethylchlorosilane, perfluoro decyl dimethyl methoxy silane It is at least one；The floride-free organosilan is MTMS, MTES, ethyl trimethoxy silicon Alkane, ethyl triethoxysilane, vinyltrimethoxy silane, VTES, phenyltrimethoxysila,e, benzene Ethyl triethoxy silicane alkane, octyl group trimethoxy silane, octyltri-ethoxysilane, dodecyltrimethoxysilane, dodecane Ethyl triethoxy silicane alkane, hexadecyl trimethoxy silane, hexadecyl, 3- (methacryloxypropyl) propyl group Trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, aminopropyl trimethoxysilane, the ethoxy of aminopropyl three At least one in base silane, tetraethyl orthosilicate and methyl silicate.
4. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute State in alcohol-water mixed system, alcohol is at least one in methyl alcohol, ethanol, propyl alcohol and ethylene glycol；Alcohol is 80 with the volume ratio of water:1 ~2:1。
5. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Receive Mass percent of the rice corpuscles in alcohol-water mixed system is 0.01 ~ 2.5%；Free-floride/fluorine-containing organic silicon alkane body is mixed in alcohol-water Percentage by volume in zoarium system is 0.02% ~ 25%.
6. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute It is ammoniacal liquor, ethylenediamine, triethylamine, NaOH, potassium hydroxide, sodium methyl silicate and potassium methyl silicate to state as the alkali of catalyst In at least one；The acid as catalyst is at least one in hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, formic acid；Catalyst Mass percent in alcohol-water mixed system is 0.2% ~ 10%.
7. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Nothing The hydrolysis of fluorine/fluorine-containing organic silicon alkane and nano-particle, condensation reaction are that 1 ~ 48 h is carried out at 0 ~ 80 DEG C.
8. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute It is smooth or coarse glass, ceramics, stone material, concrete, metal, plastics, rubber, timber, leather or fabric to state base material.
9. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute State spraying be spray pressure be 0.1 ~ 0.6 MPa, spray distance be 10 ~ 150 cm under conditions of, compound suspension is sprayed It is applied to substrate material surface.
10. as claimed in claim 1 a kind of large-scale preparation method of transparent hydrophobic/super-amphiphobic coating, it is characterised in that：Institute It is to keep 1 ~ 10 min during base material impregnated in into compound suspension to state dip-coating, is then dried naturally or at 60 ~ 150 DEG C 3 ~ 30 min for the treatment of.
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