CN113583493B - Long-acting wear-resistant nano antifogging agent and preparation method and application thereof - Google Patents
Long-acting wear-resistant nano antifogging agent and preparation method and application thereof Download PDFInfo
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- CN113583493B CN113583493B CN202110877726.3A CN202110877726A CN113583493B CN 113583493 B CN113583493 B CN 113583493B CN 202110877726 A CN202110877726 A CN 202110877726A CN 113583493 B CN113583493 B CN 113583493B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 41
- 239000002105 nanoparticle Substances 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910044991 metal oxide Inorganic materials 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 150000004706 metal oxides Chemical class 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical group CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- HDMXIELEUKTYFR-UHFFFAOYSA-N bis(2-ethylhexyl) butanedioate;sodium Chemical compound [Na].CCCCC(CC)COC(=O)CCC(=O)OCC(CC)CCCC HDMXIELEUKTYFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011258 core-shell material Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims 2
- 229920000139 polyethylene terephthalate Polymers 0.000 abstract description 7
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- -1 polyethylene terephthalate Polymers 0.000 abstract description 5
- 239000004743 Polypropylene Substances 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 229920001155 polypropylene Polymers 0.000 abstract description 2
- 239000007888 film coating Substances 0.000 abstract 1
- 238000009501 film coating Methods 0.000 abstract 1
- 239000005543 nano-size silicon particle Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229920001477 hydrophilic polymer Polymers 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
-
- 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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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a long-acting wear-resistant nano antifogging agent and a preparation method and application thereof. When in use, the nano particles are dissolved in the mixed solvent with the film forming agent and the coupling agent for film coating, thus realizing the wear-resistant anti-fog effect. The nano antifogging agent disclosed by the invention is simple in preparation method, short in preparation time, capable of reacting at normal temperature, environment-friendly and nontoxic, and can be used for antifogging and wear-resistant treatment of protective glasses and protective masks made of plastic materials such as PET (polyethylene terephthalate) and PP (polypropylene).
Description
Technical Field
The invention belongs to the technical field of lens surface modification, and particularly relates to a long-acting wear-resistant nano antifogging agent as well as a preparation method and application thereof.
Background
The optical lens has different applications in the fields of people's life, medical treatment and health, industrial and mining industry, scientific research and the like, such as glasses, medical goggles, gas masks, automobile windows and rearview mirrors, endoscopes, cameras and the like which are worn by people in daily life. In the using process of the lens, the surface of the lens is easy to scratch and generate lines, so that the service life of the lens is influenced; when the lens is used in rainy and snowy weather, winter or in an environment with heavy water vapor, the lens is easily covered by fog, so that the visual field is blurred.
In order to overcome the above disadvantages, there are several solutions, which can adopt a mechanical structure such as a wiper to solve the fog problem, or adopt an antifogging agent spraying manner, but more than spray a hydrophilic polymer antifogging agent on the surface of the lens to achieve the purpose, but the hydrophilic polymer antifogging agent has the defects of low hardness, no wear resistance, easy erosion, short service life, etc.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a long-acting wear-resistant nano antifogging agent, which has simple reaction conditions and low cost.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a long-acting wear-resistant nano antifogging agent is characterized by comprising the following steps: firstly, completely mixing alkali metal hydroxide and ethanol solution by ultrasonic to obtain transparent solution, wherein the alkali metal hydroxide is one of sodium hydroxide and potassium hydroxide;
then, adding acetate into the transparent solution according to the molar ratio of the alkali metal oxide to the acetate of 1:1-4:1, and stirring at 25-35 ℃ to prepare a colloidal solution containing the nano metal oxide, wherein the acetate is one of zinc acetate and copper acetate, and the particle size of the nano metal oxide is not more than 50nm;
adding tetraethoxysilane into colloidal solution containing nano metal oxide according to the molar ratio of tetraethoxysilane to acetate of 1:1-4:1, stirring for 0.5-3h at 25-35 ℃ to prepare colloidal mixed solution containing nano silicon dioxide coated nano metal oxide, dropwise adding acetic acid to adjust the pH of the colloidal mixed solution to be 5.5-6.5, uniformly stirring, and finally decompressing and steaming out ethanol to obtain the nano silicon dioxide shell coated nano metal oxide core-shell nano particles.
Further, the range of the particle diameter d of the nano metal oxide is as follows: 1. Ltoreq. D.ltoreq.20 nm, the particle size d may preferably be from 1 to 10, and also preferably from 10 to 20nm, for example 1nm < d < 10nm or 10nm < d < 20nm or d =20nm.
Furthermore, the particle diameter of the nano-silica coated nano-metal oxide nano-particle is 10-30nm, the diameter of the middle core of the nano-particle is 1-10nm, and the thickness of the outer shell of the nano-particle is 2-12nm.
Further, the film forming agent is at least one of acrylic resin, polyvinylpyrrolidone and sodium di (2-ethylhexyl) succinate sulfonate.
Further, the coupling agent is 3- (trimethoxysilyl) propyl methacrylate.
Further, the mixed solvent of the film forming agent is at least one of ethanol, isopropanol and water.
By adopting the scheme, the nano antifogging agent disclosed by the invention is simple in preparation method, short in preparation time, capable of reacting at normal temperature, environment-friendly and nontoxic, and can be used for antifogging and wear-resistant treatment of protective glasses and protective masks made of plastic materials such as PET (polyethylene terephthalate) and PP (polypropylene).
Another object of the invention is: the invention also provides a long-acting wear-resistant nano antifogging agent, which is characterized in that: the nano-particle comprises a core and a nano-silica shell coated on the surface of the core, wherein the core is one of zinc oxide or copper oxide, the diameter of the core is 1-10nm, and the thickness of the nano-silica shell is 2-12nm.
Further, the coating comprises a film forming agent, a coupling agent and a mixed solvent capable of dissolving the film forming agent and the coupling agent simultaneously, wherein the ratio of the film forming agent to the coupling agent is 5:1-21: 1. further, the mixed solvent is at least one of ethanol, isopropanol and water.
Further, the film forming agent is at least one of acrylic resin, polyvinylpyrrolidone and sodium bis (2-ethylhexyl) succinate, and the coupling agent is 3- (trimethoxysilyl) propyl methacrylate.
Another object of the invention is: the invention also provides a nano antifogging agent prepared by the method or an application of the nano antifogging agent in preparing an antifogging coating on the surface of an optical lens, which is characterized in that: the thickness of the antifogging coating is 5nm-500um. Preferably, 20nm to 200um.
By adopting the scheme, the coating prepared from the nano antifogging agent has the following advantages:
1) The wear resistance of the material is improved, so that the hardness of the material is increased and the service life of the material is prolonged;
2) The antifogging performance of the transparent material is improved;
3) The preparation method is simple and can be realized at normal temperature.
The invention is further described below with reference to the accompanying drawings.
Drawings
FIG. 1 is a TEM of a sample of an embodiment 4 of the present invention.
Detailed Description
Firstly, completely mixing alkali metal hydroxide and ethanol solution by ultrasonic to obtain transparent solution, then adding acetate into the transparent solution, stirring at 25-35 ℃ to prepare colloidal solution containing nano metal oxide, then adding tetraethoxysilane into the colloidal solution containing nano metal oxide, stirring at 25-35 ℃ for 0.5-3h to prepare colloidal mixed solution containing nano silicon dioxide coated nano metal oxide, dropwise adding acetic acid to adjust the pH of the colloidal mixed solution to be 5.5-6.5, stirring uniformly, and finally evaporating ethanol under reduced pressure to obtain the nano silicon dioxide shell coated nano metal oxide core-shell nano particles. When in use, 3.8g of the nanoparticles are added into a mixture containing acrylic resin and 3- (trimethoxysilyl) propyl methacrylate with the mass ratio of 5:1-21: 1, stirring for 1h to obtain the nano wear-resistant antifogging agent, wherein the mass ratio of ethanol to water is 20.
In this example, a nano wear-resistant antifogging agent was coated on a 0.5mm thick PET sheet by an applicator, dried at 70 ℃ and placed on a 80 ℃ thermostatic water bath cup, and the antifogging effect was observed by visual observation at different times (see Table 2). The thickness of the antifogging coating formed after the antifogging agent is dried can be within 5nm-500um, if the thickness of the coating is more than 500um, the light transmittance is possibly reduced, and if the thickness of the coating is less than the range, the antifogging effect cannot be achieved, the wear resistance is poor, but preferably, the thickness of the coating is within 20nm-200um, and the antifogging wear-resistant effect and the definition can be very good. In the embodiment, the antifogging effect and the wear resistance of the nano wear-resistant antifogging coating with the thickness of 55nm formed by coating are tested by taking the example as an example.
A nano wear-resistant antifogging coating is coated on a PET plastic sheet, and the scratch resistance is evaluated by a pencil hardness method (see table 3).
The specific example proportions are shown in the following table:
TABLE 1 Material proportioning Table in different examples
TABLE 2 antifogging effect after different times
Note: OK means no visible haze development on the PET sheet and Fail means visible haze development on the naked eye. As shown in fig. 1, example 4 has a nanoparticle size of about 15nm, a core diameter of about 3nm, and a shell thickness of about 6nm.
TABLE 3 Pencil hardness method for testing wear resistance of samples
The present invention is not limited to the above embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention.
Claims (8)
1. A preparation method of a long-acting wear-resistant nano antifogging agent is characterized by comprising the following steps: firstly, completely mixing alkali metal hydroxide and ethanol solution by ultrasonic to obtain transparent solution, wherein the alkali metal hydroxide is one of sodium hydroxide and potassium hydroxide;
then, adding acetate into the transparent solution according to the molar ratio of alkali metal hydroxide to acetate of 1:1-4:1, and stirring at 25-35 ℃ to prepare a colloidal solution containing nano metal oxide, wherein the acetate is one of zinc acetate and copper acetate, and the particle size of the nano metal oxide is not more than 50nm;
adding tetraethoxysilane in an amount of 1:1-4:1 according to the molar ratio of tetraethoxysilane to acetate, stirring for 0.5-3h at 25-35 ℃ to prepare a colloid mixed solution containing nano-silica coated nano-metal oxide, dropwise adding acetic acid to adjust the pH of the colloid mixed solution to be 5.5-6.5, uniformly stirring, and finally decompressing and distilling ethanol to obtain nano-silica shell coated nano-metal oxide core-shell nanoparticles, wherein the nano-silica coated nano-metal oxide nanoparticles have the particle size of 10-30nm, the diameter of a central core of the nanoparticles is 1-10nm and the thickness of a shell of the nanoparticles is 2-12nm, and when the nano-silica shell coated nano-metal oxide core-shell nanoparticles are dissolved in a mixed solvent added with a film-forming agent and a coupling agent to form a nano antifogging agent, wherein the film-forming agent is at least one of acrylic resin, polyvinylpyrrolidone and sodium di (2-ethylhexyl) succinate, and the coupling agent is 3- (trimethoxysilyl) propyl methacrylate.
2. The preparation method of the long-acting wear-resistant nano antifogging agent according to claim 1, characterized in that: the range of the particle size of the nano metal oxide is as follows: 1-20nm.
3. The preparation method of the long-acting wear-resistant nano antifogging agent according to claim 1, characterized in that: the mixed solvent is at least one of ethanol, isopropanol and water.
4. A long-acting wear-resistant nano antifogging agent prepared by the method of any one of claims 1 to 3, characterized in that: the nano-particle comprises a core and a nano-silica shell coated on the surface of the core, wherein the core is one of zinc oxide or copper oxide, the diameter of the core is 1-10nm, and the thickness of the nano-silica shell is 2-12nm.
5. The long-acting wear-resistant nano antifogging agent according to claim 4, characterized in that: the coating also comprises a film forming agent, a coupling agent and a mixed solvent capable of dissolving the film forming agent and the coupling agent simultaneously, wherein the ratio of the film forming agent to the coupling agent is 5:1-21: 1.
6. the long-acting wear-resistant nano antifogging agent according to claim 5, characterized in that: the film forming agent is at least one of acrylic resin, polyvinyl pyrrolidone and sodium di (2-ethylhexyl) succinate sulfonate; the coupling agent is 3- (trimethoxysilyl) propyl methacrylate.
7. The long-acting wear-resistant nano antifogging agent according to claim 6, characterized in that: the film forming agent is acrylic resin.
8. The application of the nano antifogging agent prepared by the method of claim 1 or the nano antifogging agent of claim 4 in preparing an antifogging coating on the surface of an optical lens is characterized in that: the thickness of the antifogging coating is 20nm-200um.
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| JP4165014B2 (en) * | 1999-03-09 | 2008-10-15 | Ｔｏｔｏ株式会社 | Hydrophilic member, method for producing the same, coating agent and apparatus for the production |
| CN101747690A (en) * | 2008-11-28 | 2010-06-23 | 3M创新有限公司 | Anti-fog coating composition, anti-fog thin film and product |
| CN103013311A (en) * | 2012-12-19 | 2013-04-03 | 王育述 | Hydrophilic anti-fogging glass coating material and preparation method thereof |
| CN108793226B (en) * | 2017-05-03 | 2021-07-13 | 北京化工大学 | Method for preparing transparent zinc oxide liquid-phase dispersion by supergravity technology |
| CN206892372U (en) * | 2017-06-06 | 2018-01-16 | 东莞唯智美新材料科技有限公司 | The underwater eyeglass of preventing atomization |
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