CN107325685A - A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica - Google Patents

A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica Download PDF

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CN107325685A
CN107325685A CN201710633923.4A CN201710633923A CN107325685A CN 107325685 A CN107325685 A CN 107325685A CN 201710633923 A CN201710633923 A CN 201710633923A CN 107325685 A CN107325685 A CN 107325685A
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sio
colloidal sol
super
preparation
hydrophobic
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宋驁天
马星
郝全勇
李振乾
张勇剑
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SHENZHEN KONGQUE TECHNOLOGY DEVELOPMENT Co Ltd
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SHENZHEN KONGQUE TECHNOLOGY DEVELOPMENT Co Ltd
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    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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    • B82—NANOTECHNOLOGY
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    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
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    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
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Abstract

The present invention relates to a kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, comprise the following steps：Monodisperse mesoporous Nano-meter SiO_2 is prepared by template2；By SiO2After colloidal sol centrifuge washing, add silane coupler and 17 fluorine decyl trimethoxy silanes are modified；Binder is added to Nano-meter SiO_22In colloidal sol, super hydrophobic coating is obtained after stirring.The super hydrophobic coating even application of the present invention is in substrate, and 25 DEG C are dried 15 36h (or 1 5h is dried at 60 DEG C) naturally at room temperature, obtain super-hydrophobic transparent coating, water droplet is more than 150 degree in contact angle on surface of coating；Coating adhesion is good, and the slide or the fan blade transparency for scribbling film are considerable, and light transmittance is up to more than 90%.

Description

A kind of preparation of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica Method
Technical field
The present invention relates to a kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, category In clear dope field.
Background technology
Super hydrophobic coating is used on glass, metal, the matrix material such as ceramics, surface is had automatically cleaning and easy cleaned Effect；Super hydrophobic surface is used for the inwall of ship, naval vessels and pipeline, can reduce the frictional resistance between surface and current, real Existing drag reduction or even the transmission of the free of losses to fluid；Super hydrophobic surface is used to reduce on satellite antenna to be produced because of the absorption of snow Raw signal interference etc..The surface of super-hydrophobic/super-oleophilic characteristic can be used for water-oil separating, have important for oil field Meaning, in addition, one important background of super hydrophobic surface are the freezings on surface, that is, postpone, reduce frost in surface heap Product.Visual transparency or anti-reflection property are the glass of the basic demand, such as building outer layer of many optical material equipment, electricity The optical glass of sub- device, optical mirror etc..For them, the ability of waterproof and self-cleaning is prerequisite. Therefore in the same surface of solids, while introducing super-hydrophobicity and optical transparency or anti-reflection property has great research valency Value.
The content of the invention
The invention provides a kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, The problems such as solving the existing hydrophobic coating transparency bad and complicated preparation technology.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, including following step Suddenly：
(1) 20-70mg triethanolamines and 300-850mg cetyl trimethylammonium bromides are added in deionized water and stirred 5-45min is mixed, oil bath is warming up to 70-95 DEG C；
(2) 1-3mL tetraethyl orthosilicates are added drop-wise in above-mentioned solution, continue that 1-3mL tetraethyl orthosilicates are added dropwise after 0.5-3h； Insulation reaction 0.5-3h obtains homogeneous dispersed nano SiO2Particle colloidal sols；
(3) by SiO2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 2 times, centrifugation is purified SiO2Colloidal sol；
(4) SiO into step (3) obtained by centrifugation2Ethanol is added in colloidal sol and hydrochloric acid carries out going template, mesoporous receive is obtained Rice SiO2Colloidal sol；
(5) by the meso-porous nano SiO obtained by step (4)2Colloidal sol centrifuge washing, is respectively centrifuged with deionized water and ethanol respectively Washing 1 time, centrifuges the SiO purified2Colloidal sol；
(6) SiO is disperseed with ethanol2SiO in colloidal sol, colloidal sol2Concentration 0.005-0.02g/mL, adds silane coupler and ten Seven fluorine decyl trimethoxy silanes, SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volume ratios are 120: 0.5-1:0.2-0.5, to mesoporous SiO2It is modified 0.5-2h；
(7) binder is added to the water magnetic agitation 1h, fully dissolving, the mass ratio of binder and water is 50-100: 1；
(8) to SiO obtained by step (6)2The gained binder aqueous solution of above-mentioned steps (7) dissolving, SiO are added in colloidal sol2It is molten The volume ratio of glue and the binder aqueous solution is 1-3:1,3-10min is stirred, transparent hydrophobic coating is made.
Further, preferred scheme of the invention is：Ethanol and hydrochloric acid volume ratio are 15 in the described technique for going template:1, 70-95 DEG C of insulation reaction 10-30h.
Further, preferred scheme of the invention is：Described SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxies Base silane volume ratio is 60:0.5:0.2.
Further, preferred scheme of the invention is：Described silane coupler is KH-550.
Further, preferred scheme of the invention is：Described centrifugation is 10000-15000 revs/min of centrifugal rotational speed, during centrifugation Between 3-20 minutes.
Further, preferred scheme of the invention is：Described binder is AB bi-component aqueous epoxy resins.
Beneficial effects of the present invention：
The super hydrophobic coating even application of the present invention is to substrate (simple glass, including glass window, glass curtain wall, family Bathroom mirror, windshield, automobile rearview mirror, vehicle rear-view glass, vehicle glass skylight, ophthalmic len and ABS plastic Deng) on, 15-36h (or 1-5h is dried at 60 DEG C) is dried naturally, obtains super-hydrophobic transparent coating, water droplet connects in coating surface Feeler is more than 150 degree；Adhesive force is good, and the slide or the flabellum transparency for scribbling film are considerable, and light transmittance is up to more than 90%.
The preparation method of the present invention is simple, and technological operation is convenient, and template pyroreaction and the 6th are gone by the 4th step The modification of step so that the hydrophobicity of prepared mesoporous silicon oxide and being greatly improved for the transparency, after coating spraying The coating arrived is big to the contact angle of water, and translucency is good.
Embodiment
Below in conjunction with the specific embodiment of the invention, technical scheme is clearly and completely described, shown So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the reality in the present invention Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made all belongs to In the scope of protection of the invention.
Embodiment 1
A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, including following step Suddenly：
(1) 35mg triethanolamines and 570mg cetyl trimethylammonium bromides are added in deionized water and stirred 10min, oil bath is warming up to 85 DEG C；
(2) 1.5mL tetraethyl orthosilicates are added drop-wise in above-mentioned solution, continue that 1.5mL tetraethyl orthosilicates, insulation is added dropwise after 1h Reaction 1h obtains homogeneous 50nm dispersed nano SiO2Particle colloidal sols；
(3) by SiO2Particle colloidal sols centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 2 times, centrifugation is obtained The SiO of purifying2Colloidal sol, centrifugal rotational speed is 10000 revs/min, and centrifugation time is 10 minutes；
(4) SiO obtained to centrifugation2Ethanol is added in colloidal sol and hydrochloric acid carries out going template, ethanol and hydrochloric acid volume ratio are 15:1,85 DEG C of insulation reaction 15h, obtains meso-porous nano SiO2Colloidal sol；
(5) by meso-porous nano SiO2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 1 time, is obtained The SiO of purifying2Colloidal sol；
(6) SiO is disperseed with ethanol2SiO in colloidal sol, colloidal sol2Concentration 0.005g/mL, adds silane coupler and the 17 fluorine last of the ten Heavenly stems Base trimethoxy silane, SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volume ratios are 60:0.5:0.2, To mesoporous SiO2Modified 1.5h；
(7) binder is added to the water magnetic agitation 1h, fully dissolving, the mass ratio of water and binder is 100:1；
(8) to SiO obtained by step (6)2The gained binder aqueous solution of above-mentioned steps (7) dissolving, SiO are added in colloidal sol2It is molten The volume ratio of glue and the binder aqueous solution is 3:1,3min is stirred, transparent hydrophobic coating is made.
The super hydrophobic coating even application of the present invention dries 24h, obtains super-hydrophobic transparent naturally on vehicle rear-view glass Coating, water droplet contact angle on surface of coating position 150 degree；Adhesive force is good, and the slide or the flabellum transparency for being coated with film can See, light transmittance is up to 93%.
Embodiment 2
A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, including following step Suddenly：
(1) 70mg triethanolamines and 850mg cetyl trimethylammonium bromides are added in deionized water and stirred 45min, oil bath is warming up to 95 DEG C；
(2) 3mL tetraethyl orthosilicates are added drop-wise in above-mentioned solution, continue that 3mL tetraethyl orthosilicates, insulation reaction is added dropwise after 1h 0.5h obtains homogeneous 30nm dispersed nano SiO2Particle colloidal sols；
(3) by SiO2Particle colloidal sols centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 2 times, centrifugation is obtained The SiO of purifying2Colloidal sol, centrifugal rotational speed is 12000 revs/min, and centrifugation time is 5 minutes；
(4) SiO obtained to centrifugation2Ethanol is added in colloidal sol and hydrochloric acid carries out going template, ethanol and hydrochloric acid volume ratio are 15:1,95 DEG C of insulation reaction 30h, obtains meso-porous nano SiO2Colloidal sol；
(5) by meso-porous nano SiO2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol once, is obtained The SiO of purifying2Colloidal sol；
(6) SiO is disperseed with ethanol2SiO in colloidal sol, colloidal sol2Concentration 0.01g/mL, adds silane coupler and the 17 fluorine last of the ten Heavenly stems Base trimethoxy silane, SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volume ratios are 240:1:1, carry out Modified-reaction 0.5h；
(7) binder is added to the water magnetic agitation 1h, fully dissolving, the mass ratio of water and binder is 75:1；
(8) to SiO obtained by step (6)2The gained binder aqueous solution of above-mentioned steps (7) dissolving, SiO are added in colloidal sol2It is molten The volume ratio of glue and the binder aqueous solution is 2:1,5min is stirred, that is, obtains transparent hydrophobic coating.
The super hydrophobic coating even application of the present invention dries 24h, obtains super-hydrophobic transparent naturally on vehicle rear-view glass Coating, water droplet contact angle on surface of coating position 151 degree；Adhesive force is good, and the slide transparency for scribbling film is considerable, and light transmittance reaches 91%.
Embodiment 3
A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, including following step Suddenly：
(1) 20mg triethanolamines and 300mg cetyl trimethylammonium bromides are added in deionized water and stir 5min, Oil bath is warming up to 70 DEG C；
(2) 1mL tetraethyl orthosilicates are added drop-wise in above-mentioned solution, continue that 1mL tetraethyl orthosilicates, insulation reaction is added dropwise after 1h 0.5h obtains homogeneous 80nm dispersed nano SiO2Particle colloidal sols；
(3) by SiO2Particle colloidal sols centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 2 times, centrifugation is obtained The SiO of purifying2Colloidal sol, centrifugal rotational speed is 14000 revs/min, and centrifugation time is 3 minutes；
(4) to the SiO for obtaining centrifugation2Ethanol is added in colloidal sol and hydrochloric acid carries out going template, ethanol and hydrochloric acid volume ratio For 15:1,70 DEG C of insulation reaction 30h, obtains meso-porous nano SiO2Colloidal sol；
(5) by meso-porous nano SiO2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 1 time, centrifugation The SiO purified2Colloidal sol；
(6) SiO is disperseed with ethanol2SiO in colloidal sol, colloidal sol2Concentration 0.02g/mL, adds silane coupler and the 17 fluorine last of the ten Heavenly stems Base trimethoxy silane, SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volume ratios are 300:2:1, carry out It is modified, react 2h；
(7) binder is added to the water magnetic agitation 1h, fully dissolving, the mass ratio of water and binder is 50:1；
(8) to SiO obtained by step (6)2The gained binder aqueous solution of above-mentioned steps (7) dissolving, SiO are added in colloidal sol2It is molten The volume ratio of glue and the binder aqueous solution is 1:1,10min is stirred, that is, obtains transparent hydrophobic coating.
The super hydrophobic coating even application of the present invention dries 1h, obtains super-hydrophobic on vehicle rear-view glass at 60 DEG C Bright coating, water droplet contact angle on surface of coating position 153 degree；Adhesive force is good, and the slide or the flabellum transparency for scribbling film can See, light transmittance is up to 90%.
Binder used is that Zhejiang stablizes the country new material Co., Ltd AB-EP-51 type AB bi-component waterbornes in above-described embodiment Epoxy resin.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (6)

1. a kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica, it is characterised in that bag Include following steps：
(1) 20-70mg triethanolamines and 300-850mg cetyl trimethylammonium bromides are added in deionized water and stir 5- 45min, oil bath is warming up to 70-95 DEG C；
(2) 1-3mL tetraethyl orthosilicates are added drop-wise in above-mentioned solution, continue that 1-3mL tetraethyl orthosilicates are added dropwise after 0.5-3h；Insulation Reaction 0.5-3h obtains homogeneous dispersed nano SiO2Particle colloidal sols；
(3) by SiO2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing of ethanol 2 times, centrifuges the SiO purified2 Colloidal sol；
(4) SiO into step (3) obtained by centrifugation2Ethanol is added in colloidal sol and hydrochloric acid carries out going template, meso-porous nano is obtained SiO2Colloidal sol；
(5) by the meso-porous nano SiO obtained by step (4)2Colloidal sol centrifuge washing, respectively with deionized water and each centrifuge washing 1 of ethanol It is secondary, centrifuge the SiO purified2Colloidal sol；
(6) SiO is disperseed with ethanol2SiO in colloidal sol, colloidal sol2Concentration 0.005-0.02g/mL, adds silane coupler and 17 fluorine Decyl trimethoxy silane, SiO2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volume ratios are 120:0.5-1: 0.2-0.5, to mesoporous SiO2It is modified 0.5-2h；
(7) binder is added to the water magnetic agitation 1h, fully dissolving, the mass ratio of binder and water is 50-100:1；
(8) to SiO obtained by step (6)2The gained binder aqueous solution of above-mentioned steps (7) dissolving, SiO are added in colloidal sol2Colloidal sol and The volume ratio of the binder aqueous solution is 1-3:1,3-10min is stirred, transparent hydrophobic coating is made.
2. a kind of preparation of super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica according to claim 1 Method, it is characterised in that：The technique that template is gone in the step (4) is：Ethanol and hydrochloric acid volume ratio are 15:1,70-95 DEG C of guarantor Temperature reaction 10-30h.
3. a kind of preparation of super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica according to claim 1 Method, it is characterised in that：SiO in the step (6)2Colloidal sol:Silane coupler:17 fluorine decyl trimethoxy silane volumes Than for 60:0.5:0.2.
4. a kind of preparation of super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica according to claim 1 Method, it is characterised in that：Described silane coupler is KH-550.
5. a kind of preparation of super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica according to claim 1 Method, it is characterised in that：Described centrifugation is 10000-15000 revs/min of centrifugal rotational speed, centrifugation time 3-20 minutes.
6. a kind of preparation of super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica according to claim 1 Method, it is characterised in that：Described binder is AB bi-component aqueous epoxy resins.
CN201710633923.4A 2017-07-29 2017-07-29 A kind of preparation method of the super-hydrophobic transparent coating based on monodisperse nanosized mesoporous silica Pending CN107325685A (en)

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Application publication date: 20171107