CN115678424B - Water-based anti-reflection coating liquid and preparation method and application thereof - Google Patents
Water-based anti-reflection coating liquid and preparation method and application thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 74
- 239000011248 coating agent Substances 0.000 title claims abstract description 73
- 239000007788 liquid Substances 0.000 title claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims abstract description 98
- -1 polysiloxane Polymers 0.000 claims abstract description 56
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 49
- 239000011521 glass Substances 0.000 claims abstract description 40
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 38
- 125000002091 cationic group Chemical group 0.000 claims abstract description 34
- 239000012875 nonionic emulsifier Substances 0.000 claims abstract description 17
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 13
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- 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
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 238000005496 tempering Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 4
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 4
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 3
- 239000006117 anti-reflective coating Substances 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
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- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
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- 229920000647 polyepoxide Polymers 0.000 claims description 2
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
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- 238000004132 cross linking Methods 0.000 abstract description 3
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
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- 229960000583 acetic acid Drugs 0.000 description 5
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- 239000007888 film coating Substances 0.000 description 5
- 238000009501 film coating Methods 0.000 description 5
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- 239000012362 glacial acetic acid Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000003667 anti-reflective effect Effects 0.000 description 3
- 239000005038 ethylene vinyl acetate Substances 0.000 description 3
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- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 1
- VCYDUTCMKSROID-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VCYDUTCMKSROID-UHFFFAOYSA-N 0.000 description 1
- FGZFESWHQXSPJU-UHFFFAOYSA-N 2-methyl-2-(3,3,3-trifluoropropyl)-1,3,5,2,4,6-trioxatrisilinane Chemical compound FC(F)(F)CC[Si]1(C)O[SiH2]O[SiH2]O1 FGZFESWHQXSPJU-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- ZZHNUBIHHLQNHX-UHFFFAOYSA-N butoxysilane Chemical compound CCCCO[SiH3] ZZHNUBIHHLQNHX-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- JJRDHFIVAPVZJN-UHFFFAOYSA-N cyclotrisiloxane Chemical compound O1[SiH2]O[SiH2]O[SiH2]1 JJRDHFIVAPVZJN-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 235000006408 oxalic acid Nutrition 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- ZMYXZXUHYAGGKG-UHFFFAOYSA-N propoxysilane Chemical compound CCCO[SiH3] ZMYXZXUHYAGGKG-UHFFFAOYSA-N 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
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- 239000004576 sand Substances 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
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- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
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- Paints Or Removers (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention belongs to the field of coating liquid, and discloses a water-based anti-reflection coating liquid, and a preparation method and application thereof. The anti-reflection coating liquid comprises a cross-linked polysiloxane emulsion and a template agent emulsion; the cross-linking polysiloxane emulsion comprises siloxane and an emulsifier, wherein the emulsifier is a composite emulsifier of a cationic emulsifier and a nonionic emulsifier, and the template emulsion is a cationic template emulsion. The preparation method comprises the following steps: mixing siloxane and an emulsifier to prepare a cross-linked polysiloxane emulsion; and mixing the cross-linked polysiloxane emulsion with the template emulsion to prepare the water-based anti-reflection coating liquid. The film layer formed by coating the water-based anti-reflection coating liquid on the solar anti-reflection coated glass has the advantages of good light transmittance, high mechanical strength and good dirt resistance.
Description
Technical Field
The invention belongs to the field of coating liquid, and particularly relates to a water-based anti-reflection coating liquid, and a preparation method and application thereof.
Background
Most of the anti-reflection film coating liquid in the current market takes organic solvent as a dispersion medium, a large amount of waste gas is generated during the production of the anti-reflection glass, the environment and the human health are seriously harmed, and the manufacturing cost of the anti-reflection glass is increased. If the organic solvent in the anti-reflection film coating liquid is replaced by water, the water-based anti-reflection film coating liquid is prepared, the use of organic compounds is greatly reduced, and compared with the organic solvent, the water is low in cost, and the raw material cost can be saved in a larger range, so that the water-based anti-reflection film coating liquid has great practical significance and is also a trend of market trend.
At present, some water-based anti-reflection film coating solutions in the technology are prepared by compounding silica sol and small molecular organic matters or polymer resins, and the anti-reflection film formed by firing the coating solutions is prepared from silicon dioxide (SiO) with the granularity of tens to hundreds of nanometers 2 ) The porous structure with high porosity formed by stacking nano particles has good anti-reflection performance. But due to SiO 2 The nano particles and the glass surface have few chemical bonds, the mechanical strength of the film is very low, namely the film is easy to wipe off, and the surface of the film layer inevitably has open pores which are formed after the high polymer resin is decomposed and are communicated with the atmosphere, and the pores are easy to be infiltrated by molten ethylene-vinyl acetate copolymer (EVA) when the photovoltaic module is assembled, and EVA residues are difficult to remove and clean after cooling, so that the appearance and the power generation efficiency of the photovoltaic module are affected; meanwhile, the photovoltaic module has a large number of open pores on the surface of the antireflection film, so that dust, automobile tail gas and other dirt are easily adsorbed in the outdoor use process, the light transmittance is reduced, and the power generation efficiency is reduced. The solar packaging glass is used outdoors and is often subjected to various environmental conditions such as rain and snow, hail, sand wind, automobile exhaust and the like, and high requirements are put on the mechanical strength and dirt resistance of the film, so that the anti-reflection film plated by the water-based anti-reflection film plating liquid does not meet the requirements of customers.
Based on the above, it is necessary to provide a water-based antireflective coating solution which can prepare an antireflective film having high light transmittance and good stain resistance.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides the water-based anti-reflection coating liquid which uses water as a solvent, is environment-friendly and economical, has low price, and can be coated on solar photovoltaic glass to obtain the closed-cell anti-reflection coating after curing and toughening, and the anti-reflection coating has high light transmittance and good dirt resistance.
The invention also provides a preparation method of the water-based anti-reflection coating liquid.
The invention also provides solar anti-reflection coated glass.
According to one aspect of the invention, a water-based anti-reflection coating liquid is provided, which comprises a cross-linked polysiloxane emulsion and a template agent emulsion; the cross-linked polysiloxane emulsion comprises siloxane and an emulsifier, wherein the emulsifier is a composite emulsifier of a cationic emulsifier and a nonionic emulsifier, and the template emulsion is a cationic template emulsion.
According to a preferred embodiment of the invention, there is at least the following advantageous effect:
the cross-linked polysiloxane emulsion of the invention is a cationic polysiloxane emulsion because of the composite emulsifier comprising a cationic emulsifier and a nonionic emulsifier. The emulsion system is stable (if an anionic emulsifier is adopted, stable emulsion cannot be formed, emulsion breaking and layering are easy to occur), the emulsion system has good compatibility with cationic template agent emulsion, and a core-shell structure of an organic core/inorganic shell is easier to form, so that a closed-cell type antireflection film is formed, the light transmittance of the closed-cell type antireflection film is high, and the dirt resistance is good.
In addition, the cross-linked polysiloxane emulsion provided by the invention is insensitive to acid-base and electrolyte substances due to the inclusion of the nonionic emulsifier, namely has acid-base resistance and electrolyte resistance, so that the water-based anti-reflection coating liquid is more stable. Meanwhile, the cross-linked polysiloxane emulsion prepared by adopting the cationic emulsifier and the nonionic emulsifier has smaller particle size, the cross-linked polysiloxane emulsion has smaller particle size, the prepared anti-reflection film has higher light transmittance and better dirt resistance.
In some embodiments of the invention, the mass fraction of the emulsifier in the cross-linked polysiloxane emulsion is 1-5%.
In some embodiments of the invention, the mass ratio of the cationic emulsifier to the nonionic emulsifier is (0.5-2): 1.
in some preferred embodiments of the invention, the mass ratio of the cationic emulsifier to the nonionic emulsifier is 1:1.
in some embodiments of the invention, the cationic emulsifier comprises at least one of dodecyltrimethylammonium bromide (DTAB), cetyltrimethylammonium bromide (CTAB), octadecyltrimethylammonium chloride (OTAC).
In some embodiments of the invention, the nonionic emulsifier comprises at least one of fatty alcohol polyoxyethylene ether (AEO), alkylphenol polyoxyethylene ether (OP), polyoxyethylene sorbitan fatty acid ester (Tween 40), polyoxyethylene sorbitan monostearate (Tween 60), sorbitan monooleate polyoxyethylene ether (Tween 80), and isomeric tridecanol polyoxyethylene ether (TO).
In some embodiments of the invention, the siloxane comprises at least one of a cyclic siloxane, a silicate, an alkoxysilane.
In some embodiments of the invention, the cyclic siloxane comprises at least one of hexamethyl cyclotrisiloxane, octamethyl cyclotrisiloxane, hexaphenyl cyclotrisiloxane, tetramethyl tetravinyl cyclotrisiloxane, methyl trifluoropropyl cyclotrisiloxane, decamethyl cyclopentasiloxane.
In some embodiments of the invention, the silicate comprises at least one of ethyl orthosilicate, propyl orthosilicate.
In some embodiments of the invention, the alkoxysilane comprises at least one of methoxysilane, ethoxysilane, propoxysilane, butoxysilane, methyltriethoxysilane, tetraethoxysilane.
In some preferred embodiments of the invention, the siloxane comprises octamethyl cyclotetrasiloxane (D4), ethyl orthosilicate, methyltriethoxysilane.
In some embodiments of the invention, the weight fraction of the octamethyl cyclotetrasiloxane in the cross-linked polysiloxane emulsion is 10-20%.
In some embodiments of the invention, the mass fraction of the ethyl orthosilicate in the cross-linked polysiloxane emulsion is 10-15%.
In some embodiments of the invention, the mass fraction of methyltriethoxysilane in the crosslinked polysiloxane emulsion is from 5 to 10%.
In some embodiments of the invention, the cross-linked polysiloxane emulsion further comprises a solvent.
In some embodiments of the invention, the solvent is water.
In some embodiments of the invention, the cross-linked polysiloxane emulsion comprises 49.5 to 73.95% of the solvent by mass.
The invention takes water as solvent, does not add organic solvent, effectively reduces the generation of waste gas, is friendly to environment and human health, is environment-friendly and economical, and has low price.
In some embodiments of the invention, the crosslinked polysiloxane emulsion further comprises a catalyst.
In some embodiments of the invention, the catalyst comprises at least one of tetramethylammonium hydroxide, sodium hydroxide, potassium hydroxide.
In some embodiments of the invention, the mass fraction of the catalyst in the cross-linked polysiloxane emulsion is 0.05 to 0.5%.
In some embodiments of the invention, the template emulsion comprises any one of a cationic acrylic emulsion, a cationic silicone-acrylate emulsion, a cationic polyurethane emulsion, a cationic styrene-acrylate emulsion, and a cationic epoxy resin.
In some embodiments of the invention, the solids content of the template emulsion is 20 to 60% of the solids content of the cross-linked polysiloxane emulsion.
According to a second aspect of the present invention, a method for preparing the water-based anti-reflection coating solution is provided, comprising the following steps:
s1: mixing siloxane and an emulsifier to prepare a cross-linked polysiloxane emulsion; the emulsifier is a composite emulsifier of a cationic emulsifier and a nonionic emulsifier;
s2: and (3) mixing the cross-linked polysiloxane emulsion prepared in the step (S1) with a template agent emulsion to obtain the water-based anti-reflection coating liquid.
In some embodiments of the invention, the siloxane in step S1 comprises at least one of cyclic siloxane, silicate, alkoxysilane.
In some preferred embodiments of the present invention, the siloxane in step S1 comprises octamethyl cyclotetrasiloxane, ethyl orthosilicate and methyltriethoxysilane, and the pre-emulsion is obtained by mixing with the emulsifier and the solvent.
In some preferred embodiments of the present invention, in the step S1, the octamethyl cyclotetrasiloxane has a mass fraction of 10 to 20%, the tetraethoxysilane has a mass fraction of 10 to 15%, the methyltriethoxysilane has a mass fraction of 5 to 10%, the emulsifier has a mass fraction of 1 to 5%, and the solvent has a mass fraction of 49.5 to 73.95%.
In some embodiments of the invention, the solvent is water.
The invention prepares cross-linking polysiloxane emulsion (cationic polysiloxane emulsion) by using octamethyl cyclotetrasiloxane, tetraethoxysilane and methyltriethoxysilane to carry out cationic ring-opening emulsion polymerization, and then mixes the cross-linking polysiloxane emulsion (cationic polysiloxane emulsion) with template emulsion (cationic template emulsion) to prepare stable emulsion type water-based anti-reflection coating liquid. In the coating liquid, the dispersion medium is water, no organic solvent is added, and the coating liquid is friendly to environment and human health, and simultaneously reduces the cost.
In some embodiments of the present invention, step S1 further comprises heating the pre-emulsion to 70-90 ℃, then adding a catalyst, and reacting to obtain the crosslinked polysiloxane emulsion.
In some embodiments of the invention, the catalyst is added in a mass fraction of 0.05 to 0.5%.
In some embodiments of the invention, the pre-emulsion is added to a four-necked flask equipped with a stirrer, reflux condenser and thermometer and warmed to 70-90 ℃.
In some embodiments of the invention, step S1 is reacted for 7 to 12 hours after the catalyst is added.
In some embodiments of the present invention, step S1 is performed after the catalyst is added to react, the temperature is reduced to below 40 ℃, the pH is adjusted to 4-6 with glacial acetic acid solution, and the cross-linked polysiloxane emulsion is obtained after filtration.
In some embodiments of the present invention, step S2 mixes the cross-linked polysiloxane emulsion and the template emulsion to form a mixed solution, and then adds a solvent to dilute the mixed solution, thereby obtaining the water-based anti-reflection coating solution, wherein the mass fraction of the water-based anti-reflection coating solution is 3-8%.
In some embodiments of the invention, the solvent is water.
According to a third aspect of the invention, solar anti-reflection coated glass is provided, and the solar anti-reflection coated glass is coated with the water-based anti-reflection coating liquid.
In some embodiments of the invention, the coating mode comprises coating the anti-reflection coating liquid by any one of spray coating, dip coating, lifting and rolling coating.
In some embodiments of the invention, the solar anti-reflection coated glass is obtained by curing and tempering the water-based anti-reflection coating liquid.
In some embodiments of the invention, the temperature of the curing is 80 to 250 ℃.
In some embodiments of the invention, the tempering treatment is at a temperature of 500-700 ℃.
Specifically, after the curing and toughening treatment, the template latex particles are decomposed, thereby forming a mixture of SiO 2 The ellipsoidal holes are formed in the dense film layer formed by the polymer, so that the film layer can be ensured to have higher porosity and mechanical strength, the surface of the film layer is dense, the purposes of increasing light transmittance and keeping better dirt resistance are achieved, and the water-based anti-reflection prepared by the prior art is well solvedThe film has the defects of low light transmittance and poor dirt resistance.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and is provided merely to illustrate the invention and is not to be construed as limiting the invention.
In the description of the present invention, unless explicitly defined otherwise, the terms pre-emulsification, coating, etc. should be construed broadly, and the specific meaning of the terms in the present invention can be reasonably determined by those skilled in the art in combination with the specific contents of the technical scheme.
In the description of the present invention, reference to the term "one embodiment," "some embodiments," etc., means that a particular feature, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment. Furthermore, the particular features, materials, or characteristics may be combined in any suitable manner in any one or more embodiments.
The test methods used in the examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
Example 1
The anti-reflection coating liquid 1 and the solar anti-reflection coated glass 1 are prepared in the embodiment, and the specific process is as follows:
1. preparing an anti-reflection coating liquid 1:
(1) Taking 67.95g of deionized water, 1g of cationic emulsifier CTAB, 1g of nonionic emulsifier OP-10, 15g of octamethyl cyclotetrasiloxane, 10g of tetraethoxysilane and 5g of methyltriethoxysilane, and pre-emulsifying in a high-shear emulsifying machine for 5min to obtain a pre-emulsion;
adding the pre-emulsion into a four-neck flask with a stirrer, a reflux condenser and a thermometer, heating to 80 ℃, adding 0.05g of catalyst tetramethylammonium hydroxide, performing a timing reaction for 8 hours, cooling to below 40 ℃, adjusting the pH value to 4 by using glacial acetic acid solution, and filtering to obtain the cross-linked polysiloxane emulsion.
(2) Uniformly mixing 20g of cross-linked polysiloxane emulsion and 4.5g of cationic acrylic emulsion (solid content is 40%), and adding 170.5g of water to dilute to 4%, thus obtaining the anti-reflection coating liquid 1.
2. Preparing solar anti-reflection and anti-reflection coated glass 1:
and (3) coating the anti-reflection coating liquid 1 on solar ultra-white glass in a spraying mode, then baking and curing at 120 ℃, and performing tempering treatment at 500 ℃ to obtain the solar anti-reflection coating glass 1.
Example 2
The anti-reflection coating liquid 2 and the solar anti-reflection coated glass 2 are prepared in the embodiment, and the specific process is as follows:
1. preparing an anti-reflection coating liquid 2:
(1) Pre-emulsifying 49.9g of deionized water, 3g of cationic emulsifier OTAC, 2g of nonionic emulsifier Tween40, 20g of octamethyl cyclotetrasiloxane, 15g of tetraethoxysilane and 10g of methyltriethoxysilane in a high-shear emulsifying machine for 5min to obtain a pre-emulsion;
adding the pre-emulsion into a four-neck flask with a stirrer, a reflux condenser and a thermometer, heating to 80 ℃, adding 0.1g of catalyst tetramethylammonium hydroxide, performing a timing reaction for 10 hours, cooling to below 40 ℃, adjusting the pH value to 4 by using glacial acetic acid solution, and filtering to obtain the cross-linked polysiloxane emulsion.
(2) Uniformly mixing 20g of cross-linked polysiloxane emulsion and 12g of cationic silicone-acrylate emulsion (solid content is 30%), and then adding 283g of water to dilute to 4%, thus obtaining the anti-reflection coating liquid 2.
2. Preparing solar anti-reflection and anti-reflection coated glass 2:
coating the anti-reflection coating liquid 2 on solar ultra-white glass in a dip-coating mode, then baking and curing at 150 ℃, and performing tempering treatment at 550 ℃ to obtain the solar anti-reflection coating glass 2.
Example 3
The anti-reflection coating liquid 3 and the solar anti-reflection coated glass 3 are prepared in the embodiment, and the specific process is as follows:
1. preparing an anti-reflection coating liquid 3:
(1) Pre-emulsifying 54.9g of deionized water, 2g of cationic emulsifier DTAB, 3g of nonionic emulsifier AEO-9, 20g of octamethyl cyclotetrasiloxane, 10g of tetraethoxysilane and 10g of methyltriethoxysilane in a high-shear emulsifying machine for 5min to obtain a pre-emulsion;
adding the pre-emulsion into a four-neck flask with a stirrer, a reflux condenser and a thermometer, heating to 90 ℃, adding 0.1g of catalyst tetramethylammonium hydroxide, performing a timing reaction for 12 hours, cooling to below 40 ℃, adjusting the pH value to 4 by using glacial acetic acid solution, and filtering to obtain the cross-linked polysiloxane emulsion.
(2) Uniformly mixing 20g of cross-linked polysiloxane emulsion and 12g of cationic polyurethane emulsion (solid content is 30%), and adding 200g of water to dilute to 5% to obtain the anti-reflection coating liquid 3.
2. Preparing solar anti-reflection and anti-reflection coated glass 3:
the anti-reflection coating liquid 3 is coated on solar ultra-white glass in a roll coating mode, then baked and cured at 180 ℃, and tempered at 600 ℃ to obtain the solar anti-reflection coating glass 3.
Example 4
The anti-reflection coating liquid 4 and the solar anti-reflection coated glass 4 are prepared in the embodiment, and the specific process is as follows:
1. preparing an anti-reflection coating liquid 4:
(1) Taking 54.8g of deionized water, 2.5g of cationic emulsifier CTAB, 2.5g of nonionic emulsifier TO-8, 15g of octamethyl cyclotetrasiloxane, 15g of tetraethoxysilane and 10g of methyltriethoxysilane, and pre-emulsifying in a high shear emulsifying machine for 5min TO obtain a pre-emulsion;
adding the pre-emulsion into a four-neck flask with a stirrer, a reflux condenser and a thermometer, heating to 75 ℃, adding 0.2g of catalyst tetramethylammonium hydroxide, performing a timing reaction for 10 hours, cooling to below 40 ℃, adjusting the pH value to 4 by using glacial acetic acid solution, and filtering to obtain the cross-linked polysiloxane emulsion.
(2) Uniformly mixing 20g of cross-linked polysiloxane emulsion and 10g of cationic styrene-acrylic emulsion (with the solid content of 40%), and adding 210g of water to dilute to 5% to obtain the anti-reflection coating liquid 4.
2. Preparing solar anti-reflection and anti-reflection coated glass 4:
and (3) coating the anti-reflection coating liquid 4 on solar ultra-white glass in a spraying mode, then baking and curing at 200 ℃, and performing tempering treatment at 700 ℃ to obtain the solar anti-reflection coating glass 4.
Comparative example 1
The anti-reflection coating liquid a and the anti-reflection coating glass a are prepared in the comparative example, and the difference from the example 1 is that the comparative example 1 is prepared by compounding silica sol and organic additives. The specific process is as follows:
1. preparing an anti-reflection coating liquid a:
62.6g of tetraethoxysilane was dispersed in 90g of ethanol, 43.2g of 0.5N aqueous nitric acid was added thereto, and then stirred at room temperature for 24 hours, and then the obtained silica sol was concentrated by rotary evaporation to obtain 121g, to obtain nano silica sol 1.
17.8g of tetraethoxysilane was dispersed in 108g of ethanol, and after adding 9.8g of 0.16N ammonia water, stirring was performed at room temperature for 24 hours, the obtained silica sol was concentrated by rotary evaporation to obtain 63g, to obtain nano silica sol 2.
Adding the obtained nano silica sol 2 into the nano silica sol 1, adding 450g of water, stirring at room temperature for reaction for 1h, adding 0.2-1.2 g of oxalic acid, and uniformly stirring to obtain the anti-reflection coating liquid a.
2. Preparing anti-reflection coated glass a:
and cleaning the glass substrate with purified water, drying in an oven, taking out and cooling, coating the glass substrate with the anti-reflection coating liquid a through a roll coating method, and then curing the film layer in a high-temperature furnace at the treatment temperature of 200 ℃ to obtain the anti-reflection coated glass a.
Test examples
The performance of the film layer in the antireflective coated glass prepared in the examples and comparative examples was tested in this test example. Wherein:
(1) Light transmittance test
Specifically, the "light transmittance" and the "light transmittance" of all embodiments refer to measurement of the average light transmittance T in the range of 380nm to 1100nm E The calculation formula is as follows:
wherein S is λ : AM1.5 solar light relative spectral distribution; Δλ: wavelength interval, nm; τ (λ): the film layer has an actual solar spectrum transmittance.
(2) Mechanical Strength-Pencil hardness Performance test
The pencil hardness of the coating film was measured with reference to the chinese national standard GB/T6739.
(3) Dirt resistance test of film
The 3M adhesive tape is tiled and adhered on the surface of a film layer, the film layer is pressed by force, then the adhesive tape is torn at 90 degrees perpendicular to the film layer, the adhesive tape is respectively rated as 1-5 grades according to the light weight of the marks on the surface of the residual film layer, the grade 1 is no marks, the grade 2 is very slight marks, the grade 3 is obvious marks, the grade 4 is residual white marks, the grade 5 is degummed, the higher the grade is, the worse the dirt resistance is, and the grade 3 is judged to be qualified.
The results of the test for the above properties are shown in table 1.
TABLE 1
| Transmittance of light | Hardness of | 3M offset printing | |
| Example 1 | 2.35％ | 4H | Level 1 |
| Example 2 | 2.32％ | 4H | Level 1 |
| Example 3 | 2.43％ | 3H | Level 1 |
| Example 4 | 2.29％ | 4H | Level 1 |
| Comparative example 1 | 2.08％ | HB-H | Grade 5 |
As can be seen from Table 1, the film layers in the antireflective coated glasses prepared in examples 1 to 4 have higher light transmittance and pencil hardness, and the imprinting test shows no imprinting; while the film layer of comparative example 1 was lower in light transmittance and pencil hardness, the print test showed degluing. The film layer of the anti-reflection coated glass prepared by the anti-reflection coating liquid is cured and toughened, and the template agent emulsion particles are decomposed, so that the anti-reflection coated glass is prepared by the anti-reflection coating liquid 2 The ellipsoidal holes are formed in the compact film layer formed by the polymer, so that the film layer can be ensured to have higher porosity and mechanical strength, the surface of the film layer is compact, and the purposes of increasing light transmittance and keeping better dirt resistance are achieved. While the film layer in comparative example 1 is SiO with a particle size of several tens to hundreds of nanometers 2 The porous structure with high porosity formed by stacking nano particles is formed by SiO 2 The nano particles have few chemical bonds with the surface of the glass, so that the film layerIs easy to wipe off due to low mechanical strength; meanwhile, as a large number of open pores exist on the surface of the antireflection film, dust, automobile exhaust and other dirt are easily adsorbed in the outdoor use process, so that the light transmittance is reduced, and the power generation efficiency is reduced.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (12)
1. The water-based anti-reflection coating liquid is characterized by comprising a cross-linked polysiloxane emulsion and a template agent emulsion; the cross-linked polysiloxane emulsion comprises siloxane and an emulsifier, wherein the emulsifier is a composite emulsifier of a cationic emulsifier and a nonionic emulsifier, and the template emulsion is a cationic template emulsion;
the mass ratio of the cationic emulsifier to the nonionic emulsifier is (0.5-2): 1, a step of;
the siloxane comprises octamethyl cyclotetrasiloxane, tetraethoxysilane and methyltriethoxysilane; in the cross-linked polysiloxane emulsion, the mass fraction of the octamethyl cyclotetrasiloxane is 10-20%,
the mass fraction of the tetraethoxysilane is 10-15%, and the mass fraction of the methyltriethoxysilane is 5-10%;
the cross-linked polysiloxane emulsion further comprises a solvent; the solvent is water; in the cross-linked polysiloxane emulsion, the mass fraction of the solvent is 49.5-73.95%;
in the cross-linked polysiloxane emulsion, the mass fraction of the emulsifier is 1-5%.
2. The water-based anti-reflection coating solution according to claim 1, wherein the cationic emulsifier comprises at least one of dodecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide and octadecyl trimethyl ammonium chloride.
3. The water-based anti-reflection coating solution according to claim 1, wherein the nonionic emulsifier comprises at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, polyoxyethylene sorbitan fatty acid ester, and isotridecyl alcohol polyoxyethylene ether.
4. The water-based antireflective coating solution of claim 1, wherein said cross-linked polysiloxane emulsion further comprises a catalyst; the catalyst comprises at least one of tetramethyl ammonium hydroxide, sodium hydroxide and potassium hydroxide.
5. The water-based anti-reflection coating liquid according to claim 4, wherein the mass fraction of the catalyst in the cross-linked polysiloxane emulsion is 0.05-0.5%.
6. The water-based anti-reflective coating solution according to claim 1, wherein the template emulsion comprises any one of a cationic acrylic emulsion, a cationic polyurethane emulsion, and a cationic epoxy resin.
7. The water-based anti-reflection coating solution according to claim 1, wherein the solid content of the template agent emulsion is 20-60% of the solid content of the cross-linked polysiloxane emulsion.
8. The method for preparing the water-based anti-reflection coating liquid according to any one of claims 1 to 7, which is characterized by comprising the following steps: s1: mixing siloxane and an emulsifier to prepare a cross-linked polysiloxane emulsion; the emulsifier is a composite emulsifier of a cationic emulsifier and a nonionic emulsifier;
s2: and (3) mixing the cross-linked polysiloxane emulsion prepared in the step (S1) with a template agent emulsion to obtain the water-based anti-reflection coating liquid.
9. The method according to claim 8, wherein the siloxane in step S1 comprises octamethyl cyclotetrasiloxane, ethyl orthosilicate and methyltriethoxysilane, and the pre-emulsion is obtained by mixing the emulsifier and the solvent to pre-emulsify.
10. The preparation method according to claim 9, wherein step S1 further comprises heating the pre-emulsion to 70-90 ℃, adding a catalyst, and reacting to obtain the cross-linked polysiloxane emulsion.
11. Solar anti-reflection coated glass is characterized in that the solar anti-reflection coated glass is coated with the water-based anti-reflection coating liquid according to any one of claims 1 to 6.
12. The solar anti-reflection coated glass according to claim 11, wherein the solar anti-reflection coated glass is obtained by curing and tempering the water-based anti-reflection coating liquid.
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| CN110225949A (en) * | 2017-02-06 | 2019-09-10 | 富士胶片株式会社 | Coating composition, antireflection film and its manufacturing method, laminated body and solar cell module |
| CN112919821A (en) * | 2021-02-09 | 2021-06-08 | 信义光伏产业(安徽)控股有限公司 | AR coating liquid, coated glass and preparation method thereof |
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| CN103113824A (en) * | 2013-01-18 | 2013-05-22 | 中科院广州化学有限公司 | Film-forming polysiloxane emulsion and preparation method thereof |
| JP2015174972A (en) * | 2014-03-17 | 2015-10-05 | 富士フイルム株式会社 | Aqueous coat agent, film, film production method, laminate and solar cell module |
| CN110225949A (en) * | 2017-02-06 | 2019-09-10 | 富士胶片株式会社 | Coating composition, antireflection film and its manufacturing method, laminated body and solar cell module |
| CN108300286A (en) * | 2017-09-07 | 2018-07-20 | 东莞南玻太阳能玻璃有限公司 | Mix the application and preparation of zirconium silica polymer colloidal sol and its anti-reflection anti-reflection coating liquid |
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