CN111849349A - Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module - Google Patents

Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module Download PDF

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Publication number
CN111849349A
CN111849349A CN202010771504.9A CN202010771504A CN111849349A CN 111849349 A CN111849349 A CN 111849349A CN 202010771504 A CN202010771504 A CN 202010771504A CN 111849349 A CN111849349 A CN 111849349A
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coating liquid
antireflection
antireflection coating
hole sealing
sealing agent
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乔仁静
游芳芳
康正辉
郭玉楠
刘迪
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Wujiang CSG Glass Co Ltd
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Wujiang CSG Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • 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
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • 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
    • C08G77/42—Block-or graft-polymers containing polysiloxane sequences
    • C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/004—Reflecting paints; Signal paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662—Synthetic film-forming substance
    • C09D5/1675—Polyorganosiloxane-containing compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1687—Use of special additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02—Details
    • H01L31/0216—Coatings
    • H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • H01L31/054—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00—Crosslinking
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/52—PV systems with concentrators

Abstract

The invention discloses a sealant for improving the anti-fouling performance of an antireflection coating, a preparation method thereof and an antireflection coating liquid, wherein the sealant comprises the following components in percentage by mass: 10-40% of low hydrogen silicone oil, 25-35% of allyl polyether, 30-60% of solvent and 10-20ppm of catalyst. According to the anti-reflection coating liquid prepared by the invention, the hole sealing agent for improving the anti-fouling performance of the anti-reflection coating glass is added, the hole sealing agent has low surface energy, is added into the anti-reflection coating liquid and is easy to migrate to the surface of the film layer, and can be crosslinked with organic silicon resin in the coating liquid in a high-temperature curing process to form a compact structure, so that the hole sealing effect is realized on the surface of the film layer, the bonding force between media such as an EVA (ethylene vinyl acetate) film and sealing silica gel and the surface group of the film layer is reduced, and the anti-reflection coating liquid is applied to the anti-reflection coating and provides excellent anti-fouling performance on the basis.

Description

Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module
Technical Field
The invention relates to the technical field of solar cell module packaging glass and coating liquid, in particular to antireflection coating liquid for improving the anti-fouling performance of glass, a preparation method of the antireflection coating liquid, antireflection coating glass prepared by the antireflection coating liquid and a photovoltaic module comprising the antireflection glass.
Background
Anti-reflection films (Anti-reflection coatings) have been widely used in the fields of display screens, optical lenses, high-energy laser windows, automobile and building glass, etc. as a surface optical treatment technology, and mainly have the effect of reducing the reflection of light by an interface. The preparation method of the anti-reflection film mainly comprises a chemical method, a physical method and a chemical physical method. The sol-gel method is the most common process at present, and has the main advantages of simple equipment, low cost and no need of specific vacuum environment at normal temperature and normal pressure. Because the weatherability of organosilicon polymer is poor, after the coating liquid is formed on the surface of glass and other materials, a film surface structure mainly comprising Si-O-Si is obtained through high-temperature calcination treatment.
The sol-gel method takes an organic silicon monomer with high chemical activity as a precursor, adds a solvent, water and an acid or alkali catalyst, forms a stable and transparent sol system in a solution through hydrolysis and condensation chemical reactions, and finally forms gel with a three-dimensional network structure after the sol is aged and slowly polymerized. Because the intermolecular acting force is weaker, after the antireflection coating liquid is coated on the surface of glass, the organic silicon prepolymer and the functional resin in the antireflection coating liquid are generally subjected to high-temperature calcination treatment to form a film.
The antireflection coating liquid in the current market mainly improves the glass transmittance by controlling a porous structure, but pollutants or water vapor in the environment easily enter the film or adhere to the surface of the film, so that the anti-fouling performance of the film is influenced. In addition, a large number of hydroxyl groups exist on the surface of the inorganic silicon dioxide anti-reflection film, and the surface activity is high, so that pollutants are easy to adhere to the film surface. In the production process of the photovoltaic module, the glass surface is easily adhered with module sealing silica gel or an EVA (ethylene vinyl acetate) adhesive film used in the packaging process, and the module sealing silica gel or the EVA adhesive film is remained on the surface of the film layer and is tightly combined with the film layer through high-temperature lamination and is difficult to remove.
In order to solve the above problems, the following two solutions are available:
firstly, Ti is added to form a super-hydrophilic structure, but if the addition amount is too low, the anti-fouling performance of the membrane surface cannot be effectively improved; however, when the amount of the surfactant added exceeds a certain value, the permeability of the film surface is remarkably decreased.
And secondly, forming a micro-nano structure on the surface of the glass by a sputtering method, and improving the anti-fouling performance of the film surface. Therefore, there is a need for a glass that can effectively improve the anti-staining property of the surface of the anti-reflection coating.
Disclosure of Invention
In view of the above, in order to overcome the defects of the prior art, the present invention aims to provide an anti-reflection coating liquid for improving the anti-fouling performance of glass, a preparation method thereof, and anti-reflection glass and a photovoltaic module prepared by using the anti-reflection coating liquid.
In order to achieve the purpose, the invention adopts the following technical scheme:
the anti-reflection coating liquid comprises the following components in percentage by mass:
Figure BDA0002616794070000021
the hole sealing agent comprises the following components in percentage by mass:
Figure BDA0002616794070000022
wherein the solvent is alcohol and/or high boiling point solvent, and the alcohol solvent is one or more of isopropanol, ethanol and n-butanol; the high boiling point solvent is one or more of propylene glycol methyl ether acetate, propylene glycol methyl ether, propylene glycol diacetate and butyl acetate. In some embodiments, isopropanol and propylene glycol methyl ether acetate may be used. Isopropanol and propylene glycol methyl ether acetate with higher boiling point are used, so that benzene solvents or acetone with higher toxicity is avoided, the boiling point of a mixed solvent in the reaction is higher than the reaction temperature, and meanwhile, reactants and products can be dissolved in the solvent.
The catalyst is a platinum-carrying catalyst, and the dosage of the catalyst accounts for 10-20ppm of the total reactant mass. The platinum-carrying catalyst comprises a speier or Karstedt catalyst, such as a chloroplatinic acid catalyst.
The fluorine-containing acrylate is one or more of hexafluorobutyl methacrylate, trifluoroethyl acrylate and trifluorobutyl methacrylate.
The allyl polyether is one or more of allyl alcohol polyoxyalkyl ether, allyl polyoxyethylene polyoxypropylene methyl ether, allyl polyoxyethylene polyoxypropylene propyl ether, allyl polyoxyethylene epoxy ether, allyl polyoxyethylene polyoxypropylene butyl ether and allyl polyoxyethylene acetate.
The hydrogen content of the low hydrogen-containing silicone oil is 0.1-1.0%. Specifically, the hydrogen content of the low hydrogen silicone oil is one or more of 0.10%, 0.18%, 0.2%, 0.3% and 0.80%. Such as heptamethyl tridylene oxide, the hydrogen content of which is 0.44 percent, belongs to low hydrogen silicone oil.
The diluent is preferably isopropanol.
According to some preferred aspects of the invention, the mass ratio of allyl polyether to fluoroacrylate is 30 to 80: 1.
according to some preferred aspects of the present invention, the molar ratio of active hydrogen in the low hydrogen silicone oil to C ═ C in the allyl polyether is 1: 0.5-1.2. More preferably, the molar ratio of active hydrogen in the low hydrogen silicone oil to C ═ C in the allyl polyether is 1: 1-1.2. The amount of allyl polyether is not preferably too high because of isomerization of the allyl polyether. When the amount of allyl polyether is increased, the conversion rate of the hydrogen-containing silicone oil is reduced. And the residual silicon-hydrogen bond is relatively active, which easily causes the stability of the product to be poor.
According to some preferred aspects of the present invention, the pore former comprises the raw materials: the acrylic resin and the propylene glycol methyl ether acetate are mixed according to a mass ratio of 1: 0.5-1.5. Preferably, the mass ratio of the acrylic resin to the propylene glycol methyl ether acetate is 1: 1. The acrylic resin preferably has a solids content of 30 to 35%.
The invention also provides a preparation method of the antireflection coating liquid for improving the anti-fouling performance of the glass, which comprises the following steps: mixing the hole sealing agent with the film forming material and the pore forming agent, adding an auxiliary agent, and diluting with a diluent to obtain the antireflection coating liquid;
the preparation method of the hole sealing agent comprises the following steps:
(1) adding low-hydrogen silicone oil into a mixed solvent of alcohol such as isopropanol and a high-boiling point solvent such as propylene glycol monomethyl ether acetate, stirring the solution at the rotating speed of 60-200rpm, introducing nitrogen into a reaction kettle, and displacing air in the system for 30min-1 h;
(2) heating the reaction system of the step (1) to 80-120 ℃ under the protection of nitrogen, and reacting according to the molar ratio of active hydrogen in the low-hydrogen silicone oil to C ═ C in the allyl polyether of 1: 0.5-1.2, mixing allyl polyether and platinum-carrying catalyst, and controlling the mass ratio of allyl polyether to fluorine-containing acrylate such as hexafluorobutyl acrylate to be 30-80: 1, the dosage of the platinum-carrying catalyst is 10-20ppm of the total mass of hydrogen-containing silicone oil, allyl polyether and hexafluorobutyl acrylate, the mixed solution of the allyl polyether and the platinum-carrying catalyst and fluorine-containing acrylate are simultaneously and slowly dripped into the reaction system in the step (1), the dripping time is controlled to be 0.5-1.5h, after the dripping is finished, the reaction is carried out for 5.0-8.0h by heat preservation, the temperature is reduced, the nitrogen introduction is stopped, and the hole sealing agent is obtained after the reaction is finished.
According to some preferable aspects of the invention, the reaction temperature when the mixed solution of the allyl polyether and the catalyst and the fluoroacrylate are added dropwise in the preparation of the hole sealing agent is 80 to 120 ℃, and the stirring speed is 80 to 200 rpm. The hydrosilylation reaction already occurs at the reaction temperature of 70 ℃, the higher the reaction temperature is, the higher the conversion rate of the hydrogen-containing silicone oil is, the reaction temperature is continuously increased, the conversion rate of the hydrogen-containing silicone oil is not greatly increased, and therefore, the temperature is optimally selected to be 85-95 ℃. The stirring speed affects the conversion rate of the hydrosilylation reaction, and the higher the stirring speed, the higher the conversion rate of the side reaction, so the conversion rate is optimally controlled to be 80-100 rpm.
The preparation method of the film forming material comprises the following steps:
(1) adding a silicon source, a siloxane coupling agent, water, a catalyst and a solvent into a reaction kettle, mixing and stirring uniformly, and then adding the catalyst; the mass ratio of the total mass of the silicon source and the siloxane coupling agent to the solvent, the water and the catalyst is 1: 0.50-3: 0.1-1:0.0001-0.001.
(2) And (2) carrying out hydrolytic polycondensation on the solution prepared in the step (1) at the reaction temperature of 20-80 ℃, reacting for 2-6h, and cooling to room temperature to obtain the film-forming substance.
The silicon source in the step is one or two of methyl orthosilicate and ethyl orthosilicate; the silane coupling agent is two or more than two of methyl triethoxysilane, methyl trimethoxysilane, vinyl triethoxysilane, dimethyl diethoxy silane, phenyl trimethoxysilane, gamma-glycidyl ether oxypropyl trimethoxysilane or gamma-methacryloxypropyl trimethoxysilane; the water is deionized water; the catalyst is one or more than two of hydrochloric acid, acetic acid, nitric acid, sulfuric acid, citric acid, oxalic acid, ammonia water, ethylamine and ethylenediamine; the solvent is one or more than two of methanol, ethanol, normal propyl alcohol, isopropanol, glycerol and ethylene glycol monobutyl ether.
According to some preferred aspects of the present invention, the method for preparing the pore-forming agent comprises the steps of: uniformly dispersing acrylic resin in propylene glycol monomethyl ether acetate and isopropanol, stirring and uniformly mixing, and standing. Specifically, 1 part by mass of an acrylic resin was uniformly dispersed in 1 part by mass of propylene glycol monomethyl ether acetate and 3 parts by mass of isopropyl alcohol, stirred for 30min, and then allowed to stand. The acrylic resin preferably has a solids content of 30 to 35%.
According to some preferred aspects of the invention, the process for the preparation of the adjuvant comprises the steps of: and mixing and stirring the amine-containing auxiliary agent and the isopropanol uniformly. Specifically, 1 part by mass of an amine-containing auxiliary agent and 2 parts by mass of isopropanol are mixed and stirred for 30min for later use.
The amine-containing auxiliary agent is one or more than two of ammonia water, monoethanolamine, diethanolamine, triethanolamine, ethylamine, diethylamine and triethylamine.
The invention also provides antireflection coated glass, wherein one surface of the antireflection coated glass is provided with an antireflection coating prepared from the antireflection coating liquid. The preparation process comprises the following steps: and coating the antireflection coating liquid on the surface of the super-white patterned glass by any coating method of spraying, rolling coating, lifting, roller coating and spin coating, curing at 250 ℃ for 2-5min through 100-.
The invention also provides a photovoltaic module which sequentially comprises the front plate glass, the front packaging layer, the battery layer, the rear packaging layer and the back plate from top to bottom, wherein the front plate glass is the antireflection coated glass, and one side of the antireflection coated glass, which is far away from the battery layer, is provided with an antireflection coating.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following benefits:
(1) the hole sealing agent is co-modified by polyether and polyester, has low surface energy, is added into the antireflection coating liquid, is easy to migrate to the surface of the film layer, can be crosslinked with organic silicon resin in the coating liquid in the high-temperature curing process to form a compact structure, and can be used for sealing holes of the antireflection film layer;
(2) according to the hole sealing agent prepared by the method, the allyl polyether modified silicone oil is grafted with the allyl polyether branched chain on the silicone oil, so that the hole sealing agent can have alcohol solubility, and the compatibility with film forming substances, pore forming agents and the like in a film coating liquid is improved;
(3) the hole sealing agent prepared by the method grafts fluorine on the silicone oil branched chain, so that the hole sealing agent is further ensured to have low surface energy and can easily migrate to the surface of the membrane layer along with the volatilization of the solvent in the curing process;
(4) the antireflection coating obtained by the prepared antireflection coating liquid can effectively prevent pollutants or water vapor in the environment from entering due to the compact structure of the film layer, reduce the binding force between media such as an EVA (ethylene vinyl acetate) film, sealing silica gel and the like and surface groups of the film layer, and has anti-fouling performance when applied to antireflection coating liquid glass;
(5) the antireflection coating liquid prepared by the invention can adopt a roll coating process in the application process, is suitable for large-area coating of packaging glass for solar cells, has low raw material and manufacturing cost and high production efficiency, and provides excellent anti-fouling performance on the basis of ensuring high transmittance of a film layer.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 hole sealing agent and method for preparing the same
The hole sealing agent in the embodiment comprises the following components:
Figure BDA0002616794070000051
Figure BDA0002616794070000061
the hydrogen content of the low hydrogen silicone oil in this example was 0.10%. The solvent is a mixed solvent of isopropanol and propylene glycol methyl ether acetate. Isopropanol and propylene glycol methyl ether acetate with higher boiling point are used, so that benzene solvents or acetone with higher toxicity is avoided, the boiling point of a mixed solvent in the reaction is higher than the reaction temperature, and meanwhile, reactants and products can be dissolved in the solvent.
In other embodiments, the low hydrogen silicone oil has a hydrogen content of 0.1 to 1.0%; the solvent is alcohol solvent and/or high boiling point solvent, wherein the alcohol solvent is one or more of isopropanol, ethanol and n-butanol. The high boiling point solvent is one or more of propylene glycol methyl ether acetate, propylene glycol methyl ether, propylene glycol diacetate and butyl acetate; the allyl polyether is one or more of allyl alcohol polyoxyalkyl ether, allyl polyoxyethylene polyoxypropylene methyl ether, allyl polyoxyethylene polyoxypropylene propyl ether, allyl polyoxyethylene epoxy ether, allyl polyoxyethylene polyoxypropylene butyl ether, allyl polyoxyethylene acetate and heptamethyltrisiloxane; the fluorine-containing acrylate is one or more of hexafluorobutyl methacrylate, trifluoroethyl acrylate and trifluorobutyl methacrylate.
The preparation method of the hole sealing agent in the embodiment comprises the following steps:
(1) 55g of isopropanol, 5g of propylene glycol monomethyl ether acetate and 13g of low hydrogen silicone oil with the hydrogen content of 0.10 percent are added into a three-neck flask, the stirring speed is controlled at 60rpm, nitrogen is introduced into the three-neck flask for 1h, and the air in the system is replaced.
(2) Heating the system to 90 ℃, mixing 27g of allyl alcohol polyoxyalkyl ether F6 (molecular weight 2000, double key value ≧ 0.5mmol/g) and 1.4g of Speier catalyst, and adding into a dropping funnel; and adding 0.4g of trifluoroethyl methacrylate into the other dropping funnel, simultaneously opening the two dropping funnels, controlling the dropping speed to ensure that the dropping is finished within 1h, preserving the temperature for reacting for 5h after the dropping is finished, cooling, stopping introducing nitrogen, and finishing the reaction to obtain the hole sealing agent.
Example 2 antireflection coating solution and method for producing the same
The antireflection coating liquid in the embodiment comprises the following components:
Figure BDA0002616794070000062
the preparation method comprises the following steps:
method for preparing film-forming material
(1) 20g of ethyl orthosilicate, 160g of methyltriethoxysilane, 32g of vinyltriethoxysilane, 61g of water and 316g of isopropanol are added into a reaction kettle, mixed and stirred uniformly, 0.08g of hydrochloric acid solution is added, and stirring is continued.
In other embodiments, the silicon source is one or both of methyl orthosilicate and ethyl orthosilicate; the silane coupling agent is two or more than two of methyl triethoxysilane, methyl trimethoxysilane, vinyl triethoxysilane, dimethyl diethoxy silane, phenyl trimethoxysilane, gamma-glycidyl ether oxypropyl trimethoxysilane or gamma-methacryloxypropyl trimethoxysilane; the water is deionized water; the catalyst is one or more than two of hydrochloric acid, acetic acid, nitric acid, sulfuric acid, citric acid, oxalic acid, ammonia water, ethylamine and ethylenediamine; the solvent is one or more than two of methanol, ethanol, n-propanol, isopropanol, glycerol and ethylene glycol monobutyl ether.
(2) And (2) carrying out hydrolytic polycondensation on the solution prepared in the step (1) at the reaction temperature of 60 ℃, reacting for 4 hours, and cooling to room temperature to obtain the film-forming substance.
Preparation method of (II) pore-forming agent
100g of acrylic resin is evenly dispersed in 100g of propylene glycol methyl ether acetate and 300g of isopropanol, stirred for 30min and then kept stand for standby.
Preparation method of (III) auxiliary agent
Mixing 10g triethanolamine and 20g isopropanol, stirring for 30min, and standing. In other embodiments, the amine-containing auxiliary agent is selected from one or more of ammonia, monoethanolamine, diethanolamine, triethanolamine, ethylamine, diethylamine and triethylamine.
Preparation method of (IV) coating liquid
(1) Mixing 0.6g of the hole sealing agent prepared in the example 1, 30g of the film forming material prepared in the step (I) and 12g of the pore forming agent prepared in the step (II);
(2) and then 0.3g of the auxiliary agent prepared in the step (III) is added, and diluted by 57.1g of isopropanol to obtain the antireflection coating liquid with the solid content of 4% by mass, which is marked as coating liquid # 1.
Example 3 hole sealing agent and method of preparing the same
The hole sealing agent in the embodiment comprises the following components:
Figure BDA0002616794070000071
Figure BDA0002616794070000081
the hydrogen content of the low hydrogen silicone oil in this example was 0.18%. The solvent is a mixed solvent of isopropanol and butyl acetate.
The preparation method of the hole sealing agent in the embodiment comprises the following steps:
(1) 25g of isopropanol, 5g of butyl acetate and 36.91g of low-hydrogen silicone oil with the hydrogen content of 0.18 percent are added into a three-neck flask, the stirring speed is controlled at 90rpm, nitrogen is introduced into the three-neck flask for 1h, and the air in the system is replaced.
(2) The system was warmed to 100 ℃ and 33.17g of allyl polyethylene glycol methyl ether AEM-10 (molecular weight 498, pure EO structure) and 2.8g of Karstedt's catalyst were mixed and added to one dropping funnel; and adding 1.02g of hexafluorobutyl acrylate into the other dropping funnel, simultaneously opening the two dropping funnels, controlling the dropping speed, ensuring that the dropping is finished within 1.5h, preserving heat for reacting for 4.5h after the dropping is finished, cooling, stopping introducing nitrogen, and finishing the reaction to obtain the hole sealing agent.
Example 4 antireflection coating solution and method for producing the same
The antireflection coating liquid in the embodiment comprises the following components:
Figure BDA0002616794070000082
the preparation method comprises the following steps:
method for preparing film-forming material
(1) Adding 29g of ethyl orthosilicate, 142g of methyltriethoxysilane, 34g of vinyltriethoxysilane, 63g of water and 303g of isopropanol into a reaction kettle, uniformly mixing and stirring, adding 0.08g of hydrochloric acid solution, and continuously stirring.
(2) And (2) carrying out hydrolytic polycondensation on the solution prepared in the step (1) at the reaction temperature of 60 ℃, reacting for 3 hours, and cooling to room temperature to obtain the film-forming substance.
Preparation method of (II) pore-forming agent
100g of acrylic resin is evenly dispersed in 200g of propylene glycol methyl ether acetate and 200g of isopropanol, stirred for 30min and then kept stand for standby.
Preparation method of (III) auxiliary agent
10g of diethanolamine and 20g of isopropanol are mixed and stirred for 30min and then kept stand for standby.
Preparation method of (IV) coating liquid
(1) 0.5g of the sealing agent prepared in example 3, 30g of the film-forming material prepared in the step (one), and 16g of the pore-forming agent prepared in the step (two) were mixed.
(2) Then 0.30g of the auxiliary agent prepared in the step (III) is added, and diluted by 53.2g of isopropanol to obtain the antireflection coating liquid with the solid content of 4% by mass, which is marked as coating liquid # 2.
Comparative examples 1 and 2
Comparative example 1 is substantially the same as example 2 except that no pore sealing agent is added to the coating solution of comparative example 1, and is marked as comparative example #1, and the preparation method thereof is substantially the same as example 2.
Comparative example 2 is substantially the same as example 4 except that no pore sealing agent is added to the coating solution of comparative example 2, and is labeled as comparative example #2, and the preparation method thereof is substantially the same as example 4.
Example 5 evaluation of the Properties of antireflection coating solution
(1) Measuring the transmittance of the coating liquid:
the coating liquid prepared in the embodiment 2, the embodiment 4 and the comparative examples 1 and 2 is coated on the super white solar embossed glass with the light transmittance Y/T of 91.84/91.80 and the thickness of 3.2mm in a rolling way, the super white solar embossed glass is cured by a curing furnace (150 ℃ C. and 200 ℃ C.), finally the glass is toughened at the temperature of 650 ℃ C. and 700 ℃ C. for 2min to obtain a film layer with the film thickness of 120nm, and the film layer is tested by an air floatation bench type spectral transmittance test system, the light transmittance Y/T value is 91.65%/91.30% according to the standard ISO9050-2003, and the test coefficient is 0.983 coating.
(2) Performance testing of the film layer
1) And (3) testing pencil hardness: according to the national standard GB/T3098.1-2015, the hardness is required to be higher than 3H.
2) Testing of 3M tape: A3M Scotch610-1PK type adhesive tape is used for rapid testing, the testing method comprises the steps of flatly laying the 3M adhesive tape and adhering the 3M adhesive tape to the surface of a film layer, forcibly extruding and grinding the adhesive tape by using dust-free cloth, then vertically tearing the adhesive tape at 90 degrees, and judging the adhesive tape to be 1-5 grade, 1 grade without mark, 2 grade to be very slight, 3 grade to be obvious, 4 grade residual white and bright marks and 5 grade degumming, wherein the larger the grade is, the worse the dirt resistance is.
3) Testing of polyethylene-vinyl acetate polymer (EVA) adhesive films: cleaning and drying the coated glass, and placing three pieces of coated glass with the area of about 2.5cm on the surface of the glass2The 3M polyethylene-vinyl acetate copolymer (EVA) adhesive film is prepared by placing a coated glass sample sheet with EVA in an oven (with the temperature set at 150 ℃), baking for 30min, taking out and cooling to room temperature, tearing off the EVA adhesive film on the surface of the glass by using tweezers, wiping with alcohol, observing whether the film surface has marks, judging the film surface to be 1-3 grade according to the depth of the marks on the residual surface, judging the film surface to be 1 grade without marks to have no change, judging the film surface to be 2 grade with slight marks to have light color, and judging the film surface to be 3 grade with obvious white marks, wherein the film surface color cannot be seen. The larger the number of stages, the worse the fouling resistance of the membrane surface.
4) Testing of the solar sealing silica gel: cleaning and drying coated glass, coating a round solar sealing silica gel with the diameter of about 10cm on the surface of the glass, standing for 10min at normal temperature, wiping with alcohol, observing whether marks are left on the film surface, judging the marks to be 1-5 levels according to the depths of the marks on the residual surface, judging the marks to be 1-5 levels, judging the marks to be 1 level, judging the 2 levels to be very slight, judging the 3 levels to be more obvious round spots, judging the marks to be white and bright on the 4 levels, degumming the 5 levels, and indicating that the larger the level is, the worse the dirt resistance of.
5) Testing handprints: cleaning and drying the coated glass, pressing a fingerprint at the center of the surface of the glass, putting a coated glass sample wafer with the fingerprint into an oven (with the temperature set at 150 ℃), baking for 30min, taking out and cooling to room temperature, wiping with alcohol, observing whether the mark is left on the film surface, judging the mark to be 1-5 grade, 1 grade without mark, 2 grade with very slight mark, 3 grade with slight mark, 4 grade with relatively clear mark and 5 grade with very clear mark according to the depth of the residual surface mark. The larger the number of stages, the worse the fouling resistance of the membrane surface.
Table 1 results of various performance tests of the anti-reflective coating liquid
Figure BDA0002616794070000101
As can be seen from Table 1, the results of the change in the visible light transmittance before and after examples 2 and 4 are: the light transmittance was increased by Δ T/Δ Y of 2.23/2.54. Here, the transmittance is measured as the average transmittance TE in the range of 380-1100 nm. The hole sealing agents prepared in the embodiments 1 and 3 are added into the coating liquid, namely the coating liquid #1 and the coating liquid #2, so that the film surface antireflection and hardness, the adhesive tape print and the handprint are not influenced, and the performances of the film surface anti-EVA adhesive film and the solar sealing silica gel can be improved. The film surface EVA adhesive film test result and the solar sealing silica gel test result of the comparative sample #1 and the comparative sample #2 which are not added with the sealant are poor.
The prior art for improving the anti-fouling performance of the antireflection coated glass has the following technical defects: (1) ti is added to form a super-hydrophilic structure, and if the addition amount is too low, the anti-fouling performance of the membrane surface cannot be effectively improved; but the addition amount exceeds a certain value, the permeability increasing rate of the film surface can be obviously reduced; (2) the method has the advantages that the thickness of the film layer is easy to control, but the sputtering method is high in cost, and the difficulty of large-area film coating production is high. The hole sealing agent for improving the anti-fouling performance of the anti-reflection coated glass, which is prepared by the invention, has low surface energy, is added into the anti-reflection coating liquid, is easy to migrate to the surface of the film layer, can be crosslinked with organic silicon resin in the coating liquid in a high-temperature curing process to form a compact structure, further plays a hole sealing role on the surface of the film layer, reduces the binding force between media such as EVA (ethylene vinyl acetate) glue films and sealing silica gel and the like and the surface group of the film layer, and provides excellent anti-fouling performance on the basis of ensuring the high transmittance of the film layer when being applied to the anti-reflection coating.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.

Claims (10)

1. The anti-reflection coating liquid is characterized by comprising the following components in percentage by mass:
Figure FDA0002616794060000011
the hole sealing agent comprises the following components in percentage by mass:
Figure FDA0002616794060000012
2. the antireflection coating liquid of claim 1 wherein the mass ratio of the allyl polyether to the fluoroacrylate is 30-80: 1.
3. the antireflection coating liquid of claim 1 wherein the molar ratio of active hydrogen in the low hydrogen silicone oil to C ═ C in the allyl polyether is 1: 0.5-1.2.
4. The antireflection coating solution of claim 1 wherein the pore former comprises the following raw materials: the acrylic resin and the propylene glycol methyl ether acetate are mixed according to a mass ratio of 1: 0.5-1.5.
5. The antireflection coating solution of claim 1 wherein the solvent is an alcohol solvent and/or a high boiling point solvent, and the high boiling point solvent is one or more of propylene glycol methyl ether acetate, propylene glycol methyl ether, propylene glycol diacetate, and butyl acetate.
6. The method for preparing the antireflection coating liquid according to claim 1, characterized by comprising the steps of: mixing the hole sealing agent with the film forming material and the pore forming agent, adding an auxiliary agent, and diluting with a diluent to obtain the antireflection coating liquid;
the preparation method of the hole sealing agent comprises the following steps:
(1) adding low-hydrogen silicone oil into a solvent, stirring, introducing inert gas, and replacing air in the system;
(2) under the protection of inert gas, heating the reaction system in the step (1) to 80-120 ℃, mixing allyl polyether and a catalyst in proportion, controlling the proportion of the allyl polyether to fluoroacrylate, slowly dropwise adding the mixed solution of the allyl polyether and the catalyst and the fluoroacrylate into the system in the step (1), after dropwise adding, keeping the temperature for reaction, and cooling to obtain the hole sealing agent.
7. The method for preparing the antireflection coating liquid according to claim 6, wherein the reaction temperature when the mixed solution of the allyl polyether and the catalyst and the fluorine-containing acrylate are added dropwise in the preparation of the hole sealing agent is 80 to 120 ℃, and the stirring speed is 80 to 200 rpm.
8. The method for preparing the antireflection coating liquid according to claim 6, wherein the method for preparing the pore-forming agent comprises the following steps: uniformly dispersing acrylic resin in propylene glycol monomethyl ether acetate and isopropanol, stirring and uniformly mixing, and standing.
9. An antireflection coated glass characterized in that one surface of the antireflection coated glass has an antireflection coating prepared by the antireflection coating liquid described in any one of claims 1 to 5.
10. A photovoltaic module, which comprises a front glass, a front packaging layer, a battery layer, a rear packaging layer and a back plate in sequence from top to bottom, wherein the front glass is the antireflection coated glass according to claim 9, and one side of the antireflection coated glass, which is far away from the battery layer, is provided with an antireflection coating.
CN202010771504.9A 2020-08-04 2020-08-04 Antireflection coating liquid, preparation method thereof, antireflection coated glass and photovoltaic module Pending CN111849349A (en)

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