CN106366906B - A kind of solar energy photovoltaic glass reflection reducing coating and preparation method thereof - Google Patents
A kind of solar energy photovoltaic glass reflection reducing coating and preparation method thereof Download PDFInfo
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- CN106366906B CN106366906B CN201610717550.4A CN201610717550A CN106366906B CN 106366906 B CN106366906 B CN 106366906B CN 201610717550 A CN201610717550 A CN 201610717550A CN 106366906 B CN106366906 B CN 106366906B
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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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
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/29—Mixtures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
Using organic siliconresin and esters of silicon acis, cohydrolysis forms nano-organosilicon particle to the present invention under the action of catalyst, then the fine and close silica structure body individually hydrolyzed with esters of silicon acis mixes, the fine and close structure that inorganic silicon is wrapped in the rule of the stabilization outside organosilicon is formed when solidification, organic principle oxidation becomes carbon dioxide when photovoltaic glass tempering, leave the nanoaperture of size rule, these holes are not connected, and steam is isolated except film layer, so there is good weather resistance.In addition film surface is smooth, pollutant cannot enter inside film layer, therefore have good anti-pollution characteristic.Present invention process is simple, easily controllable, is suitable for large-scale production.
Description
Technical field
The invention belongs to new materials and new energy field, and in particular to a kind of solar energy photovoltaic glass reflection reducing coating and its
Preparation method.
Background technology
Solar energy photovoltaic glass cover board, solar cell of the crystal silicon solar battery component generally by being coated with antireflective coating
Silicon chip and battery back-sheet glue press seal with EVA film and load, and are reloaded into fixed border composition.Determine crystal silicon solar energy battery photoelectricity
The most important factor of transformation efficiency is the crystal silicon technology in photoelectric subassembly, is secondly the photovoltaic glass in protection photoelectric subassembly, by
It can not be exposed to the external environment for a long time in crystal silicon, photovoltaic glass is current protection crystal silicon and itself light transmittance is higher best
One of material, thus the optical characteristics of photovoltaic glass be the outer big important change of crystal silicon technology because.However keep and improve photovoltaic glass
The optical characteristics of glass is easy more than what the crystal silicon of exploitation more high-conversion rate came, and cost is much lower, so developing and producing light transmission
The higher photovoltaic glass of rate, no matter component manufacturer or the demand in terminal market are all very urgent.
The visible light transmittance of solar cell module packaged glass is generally 91.2~91.8%, solar energy photovoltaic glass
Single face reflectivity about 4%.If coating the antireflective coating of 110-150nm thickness in photovoltaic glass surface, it is saturating visible light can be increased
Cross rate 2.5~3.5%.
At present, most of solar energy photovoltaic glass producer is all made of roll coating process and is coated with one layer on solar energy photovoltaic glass
Uniform reflection reducing coating forms a film coating baking and curing at 150 DEG C or so, then passes through 700 DEG C or so of drying tunnel about 140
Second is by solar energy photovoltaic glass tempering, while the antireflective coating that will be coated on solar energy photovoltaic glass surface is sintered in solar energy
It lies prostrate on glass surface.This antireflective coating is a kind of hydrophilic antireflective coating.
It is later due to being occurred using the technique of reflection reducing coating coating solar energy photovoltaic glass and then tempering, too to plated film
There is presently no professional standards and national standard for positive energy photovoltaic glass, also put into effect relevant standard and regulation without other countries,
Just start only to visible light transmittance value added △ T, the pencil hardness of plated film scrubs fastness, salt spray resistance, the performances such as acid and alkali-resistance
It requires, increased weather resistances and the contaminated resistances such as moisture and hot ageing, wet jelly cycle, sand and dust test, Er Qieyao again later
Ask higher and higher.Many solar energy photovoltaic glass reflection reducing coatings of domestic and international patent disclosure at present, have been unable to meet current reality
Border application requirement.
The Chinese invention patent document of Publication No. CN102812557A discloses a kind of anti-reflection coating and its manufacturer
Method, this application are prepared for the liquid combination with the tetraethyl orthosilicate of specific quantity, polyethylene glycol, hydrochloric acid, ethyl alcohol, fourth alcohol and water
Object, is thermal decomposited or burn off using the glycol of polymerization, leaves porous silica dioxide coating.The increase of silica porosity is dropped
The low refractive index of silica, causes to be improved by the light transmission of base material.But the anti-reflection effect of film layer of this structure
Fruit is poor, and weather resistance is poor.
The Chinese invention patent document of 103627226 A of Publication No. CN discloses a kind of solar energy photovoltaic glass anti-reflection
Antifouling paint and its production method are penetrated, cladding another kind hard two on the loose silica core generated using silicate hydrolyzate
Silica shell, silicon dioxide granule has nucleocapsid structure in coating, and silica core is formed and silica shell cladding process is same
Shi Jinhang, aluminium dihydrogen phosphate and silicon phosphate enhance antireflective coating weatherability as silica curing agent, existing to solve
There are the anti-reflection property of solar energy photovoltaic glass reflection reducing coating and a problem that weatherability index is conflicting, but complex process, it is difficult
With control, it is unsuitable for producing in enormous quantities.
Antireflective coating on the market has following defect at present：1, light transmittance gain is not high, is no more than 2.3%；2, weather-proof
Property it is bad, it is wet freeze, the atmospheric exposure tests light transmission rate such as damp and hot decaying reaches 0.7% or more；3, resistance to soiling is poor, in production process
In be easy polluted by finger-marks, silica gel, EVA glue, influence the appearance and light transmission rate of film surface.
The refractive index of film layer can be reduced by increasing the voidage in silica membrane, so antireflective coating film layer
Kong Yue is more, and anti-reflective effect is better.But Kong Yue is much bigger in film layer, then the hardness of film layer, attachment fastness will decline.Together
When, Kong Yukong is communicated, and surface also has a large amount of openning shape hole, and steam passes through this some holes attack glass surfaces, glass surface sodium
Lime glass, which is chronically in damp and hot complicated adverse circumstances, can slowly occur hydrolysis, and reaction generates silicic acid gel and hydroxide
Sodium, the silicic acid gel of generation, which is attached to glass surface, influences translucency, and the sodium hydroxide of generation is stranded in film layer and glass for a long time
Silica coating and glass matrix can be further corroded between glass matrix.Due to a large amount of ringent aperture on surface, make
Dust in air, the silica gel of greasy dirt, the felt, adhesive tape and the module production process that contact in coating process all can be with small
Hole enters antireflection film layer, to influence the light transmittance of antireflective coating.
Therefore, when improving the anti-reflective effect of film layer as far as possible, hardness, the attachment jail of film layer are inevitably reduced
Degree, weatherability and resistance to soiling.How to make the protective coating to be formed in the case where not influencing light transmittance, substantially increases film layer
Hardness, attachment fastness, weatherability and resistance to soiling become the emphasis of research.
Invention content
The object of the present invention is to provide it is a kind of be provided simultaneously with high-weatherability, high resistant and high anti-reflection rate photovoltaic glass
Glass reflection reducing coating and preparation method thereof, preparation process is simple, is easy to control, and is suitable for producing in enormous quantities.
A kind of preparation method of solar energy photovoltaic glass reflection reducing coating, includes the following steps：
(1) by organic siliconresin, esters of silicon acis, catalyst, emulsifier and solvent with mass ratio be 0.5~5：0.5~5：
0.01~0.05：0.05~0.5：1~10 mixing, is added dropwise water, the mass ratio of organic siliconresin and water after being heated to 70~75 DEG C
It is 0.5~5：0.5~10, rear return stirring is added dropwise and reacts 10~30min, obtains solution A after reaction；
(2) by esters of silicon acis, stabilizer, catalyst, solvent and water with mass ratio be 5~10：0.1~5：0.01~0.05：1
~5：5~10 mixing, be stirred to react 20~40min at a reflux temperature, after reaction with amine solvent adjust pH to 6.5~
7.0, obtain solution B；
(3) solution A is added in solution B under stiring, after solvent dilution is added, curing agent and coalescents is added,
The solution A, solution B, solvent, curing agent and film forming agent mass ratio be 3~20：12~30：30~80：0.01~0.1：
1~10, the reflection reducing coating is obtained after stirring evenly.
Using organic siliconresin and esters of silicon acis, cohydrolysis forms nano-organosilicon particle to the present invention under the action of catalyst,
Then the fine and close silica structure body that is individually hydrolyzed with esters of silicon acis mixes, when solidification formed inorganic silicon be wrapped in it is steady outside organosilicon
The fine and close structure of fixed rule, organic principle, which aoxidizes, when photovoltaic glass is High temperature tempered becomes carbon dioxide, leaves size rule
Nanoaperture, these holes are not connected, and steam is isolated except film layer, so there is extraordinary weather resistance.In addition
Film surface is smooth, and pollutant cannot enter inside film layer, therefore have extraordinary anti-pollution characteristic.
Preferably, in step (1), organic siliconresin, esters of silicon acis, catalyst, emulsifier and solvent mass ratio be 1~
3：1~3：0.01~0.03：0.2~0.5：1~3.
Preferably, in step (2), esters of silicon acis, stabilizer, catalyst, solvent and water mass ratio be 5~10：0.1~
2：0.01~0.03：2~3：5~7.
The organic siliconresin has for polyethers remodeling organic siliconresin, amino-polyether modified organic siliconresin, polyester modification
Machine silicones, polyether-polyester remodeling organic siliconresin, acryl-modified silicone resin resin, epoxy modified silicone resin or alkane
The aralkyl modified organic siliconresin of base-.Preferably, the organic siliconresin is polyethers remodeling organic siliconresin, polyester modification
Organic siliconresin or polyether-polyester remodeling organic siliconresin.
The esters of silicon acis be positive quanmethyl silicate, tetraethyl orthosilicate, positive n-propyl silicate, methyltrimethoxysilane,
Methyltriethoxysilane, methyl tripropoxy silane, ethyl trimethoxy silane, ethyl triethoxysilane, ethyl 3 third
At least one of oxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane and phenyl tripropoxy silane.
Preferably, in step (1), the esters of silicon acis is positive quanmethyl silicate, tetraethyl orthosilicate or positive silicic acid positive third
Ester, and organic siliconresin, esters of silicon acis, catalyst, emulsifier and solvent mass ratio be 1~3：1~3：0.01~0.03：0.2
~0.5：1~3.
The catalyst is acid, alkali or metal soluble-salt.Wherein, the acid is hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, grass
Acid, citric acid, acetic acid, malic acid or maleic acid；The alkali be ammonium hydroxide, tetramethyl aqua ammonia, sodium hydroxide, potassium hydroxide,
Monoethanolamine, diethanol amine, triethanolamine, 2-amino-2-methyl-1-propanol, a propylamine, di-n-propylamine, tripropyl amine (TPA), 2- propylene
Amine, cyclopropylamine, acrylamide, n-butylamine, triethylamine, diethylenetriamine, cyclic ethylene imines, piperazine or morpholine；The metal
Soluble-salt is the soluble-salt of lead, cobalt, tin or iron.
The emulsifier is sorbitan fatty acid ester polyoxyethylene ether, fatty alcohol polyoxyethylene ether, alkyl phenol and ring
Oxidative ethane condensation product, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, polyoxyethylene carboxylate, polyethylene glycol, poly- third
It is one or two kinds of in glycol, ethoxylated fatty amines, sucrose alcohol stearate and glyceryl tristearate.As excellent
Choosing, the emulsifier are sorbitan fatty acid ester polyoxyethylene ether, fatty alcohol polyoxyethylene ether or Nonyl pheno
Ether.
The stabilizer is dimethyl diethoxysilane, dimethyl 2 acetoxyl group silane, dimethylformamide dimethyl oxygroup silicon
Alkane, dimethylformamide dimethyl acyloxy silane, dimethyl dipropoxy silane or dimethyl dipropyl acyloxy silane.
The amine solvent is ammonium hydroxide, monoethanolamine, diethanol amine, triethanolamine, 2-amino-2-methyl-1-propanol, one
Propylamine, di-n-propylamine, tripropyl amine (TPA), 2- allylamines, cyclopropylamine, acrylamide, n-butylamine, triethylamine, diethylenetriamine, cyclic ethylene
Imines, piperazine or morpholine.
The curing agent is organic titanate, organic aluminates, organozirconates, r- aminopropyl triethoxysilanes, gathers
Aziridine, hexa, triethylene tetramine, r- glycidyl ether oxygen propyl trimethoxy silicanes or y- methacryls
Oxygroup propyl trimethoxy silicane.Preferably, the curing agent be organic titanate, organic aluminates, organozirconates or
Polyethyleneimine.
The coalescents are N methyl pyrrolidones, ethylene glycol, propylene glycol, glycerine, pentanediol, ethylene glycol monomethyl ether, second
Glycol ether, butyl glycol ether, propylene glycol monomethyl ether, glycol methyl ether acetate, ethylene glycol ether acetate, butyl glycol ether vinegar
Acid esters, propylene glycol methyl ether acetate, ethylene glycol phenyl ether acetate or propylene glycol phenyl ether acetate.Preferably, the film forming helps
Agent is ethylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl glycol ether or propylene glycol monomethyl ether.
The solvent is methanol, ethyl alcohol, isopropanol, normal propyl alcohol, isopropanol or n-butanol.
The present invention also provides a kind of solar energy photovoltaic glass reflection reducing coatings, and the reflection reducing coating is by above method system
It is standby to obtain.
Compared with prior art, the invention has the advantages that：
A. simple production process of the present invention, is easy to control, and is suitable for producing in enormous quantities；
B. solar energy photovoltaic glass reflection reducing coating of the present invention is provided simultaneously with that anti-reflection rate is high, resistance to soiling is strong, weatherability is high
Advantage substantially increases the lasting generating efficiency of solar components；
C. all raw material that the present invention uses all is free of poisonous and harmful substance, is a kind of environmentally protective product；
D. solar energy photovoltaic glass reflection reducing coating of the present invention coating process and glass tempering on solar energy photovoltaic glass
Technique is identical as prior art, is easy industrialization and popularization and application.
Specific implementation mode
Embodiment 1
(1) by polyether-polyester modified siloxane BYK-377, tetraethyl orthosilicate TEOS, ammonium hydroxide, aliphatic alcohol polyethenoxy
Ether AEO9, absolute ethyl alcohol is with quality 2：2：0.02：0.2：2 ratio mixing, is warming up to 70~75 DEG C, deionization is then added dropwise
Water, fast after first slow when dropwise addition, the mass ratio of BYK-377 and water is 1：2, add reactant boiling reflux during water, until
Water is added, then is flowed back 20 minutes, at this moment solution becomes micro- blue light solution, and reaction terminates to obtain solution A, pour out spare；
(2) by TEOS, dimethyl diethoxysilane, oxalic acid, absolute ethyl alcohol, deionized water is with quality 6：1：0.02：3：6
Ratio mixing, be that stirring is warming up to reflux in 90 DEG C of reaction vessel in oil bath temperature, maintain the reflux for 30 minutes, reaction is tied
Beam adjusts pH value to 6.5~7.0 with piperazine, obtains solution B, pour out spare；
(3) solution A is added in solution B while stirring, absolute ethyl alcohol dilution is then added, metatitanic acid four is being added just
Butyl ester and butyl glycol ether stir evenly, and mass ratio is 10.22：16.02：60：0.05：2, obtain final reflection reducing coating C.
By the above reflection reducing coating C roller coating it is 300mm*300mm* in 10 chip sizes with solar energy photovoltaic glass roll coater
On the solar energy photovoltaic glass print of 3.2mm, cures within 3 minutes through 80~180 DEG C of heat stepwises, obtain nattier blue solar energy and subtract
Film glass is reflected, its solar energy photovoltaic glass steel process routinely was then obtained into bluish violet in 700 DEG C of tempering 140 seconds
Solar energy antireflective coating glass print.Anti-reflection performance, strength character, weather resistance test are carried out to print, as a result such as following table
It is shown：
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.7% | It is excellent |
| Adhesive force is tested | / | It is excellent |
| Pencil hardness | / | 3H passes through |
| Grease resistance | / | It is excellent |
| Resistance to adhesive tape | / | It is excellent |
| Resistance to silica gel | / | It is excellent |
| Acid resisting test | 0.2% | It is excellent |
| Salt spray test | 0.3% | It is excellent |
| Hydrothermal aging | 0.6% | It is good |
| Wet jelly recycles aging | 0.6% | It is good |
Embodiment 2
(1) by polyester modification siloxanes BYK-381, TEOS, tetramethyl aqua ammonia, nonylphenol polyoxyethylene ether TX-10,
Isopropanol is with quality 2：2：0.02：0.3：2 ratio mixing, is warming up to 70~75 DEG C, is then added dropwise deionized water, and when dropwise addition is first
Fast after slow, the mass ratio of BYK-381 and water is 1：2, add reactant boiling reflux during water, until adding water, then returns
Stream 20 minutes, the micro- blue light solution of at this moment solution change, reaction terminate to obtain solution A, pour out spare；
(2) by methyltrimethoxysilane, dimethyldimethoxysil,ne, acetic acid, isopropanol, deionized water is with quality 8：
1：0.03：3：6 ratio mixing, in the reaction vessel of 90 DEG C of oil bath temperature stirring be warming up to reflux, maintain the reflux for 30 minutes,
Reaction terminates, and adjusts pH value to 6.5-7.0 with piperazine, obtains solution B, pour out spare；
(3) solution A is added in solution B while stirring, isopropanol is then added, four positive fourth of zirconic acid is added
Ester and propylene glycol monomethyl ether stir evenly, and mass ratio is 10.32：18.03：60：0.05：2, obtain final reflection reducing coating C.
By the above reflection reducing coating C it is 300mm*300mm*3.2mm in 10 chip sizes with solar energy photovoltaic glass roll coater
Solar energy photovoltaic glass print on, cure within 3 minutes through 80~180 DEG C of heat stepwises, obtain nattier blue solar energy antireflective
Then its solar energy photovoltaic glass steel process routinely was obtained bluish violet too by film glass in 700 DEG C of tempering 140 seconds
Positive energy antireflective coating glass print.Anti-reflection performance, strength character, weather resistance test are carried out to print, the results are shown in table below：
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.4% | It is good |
| Adhesive force is tested | / | It is excellent |
| Pencil hardness | / | 5H passes through |
| Grease resistance | / | It is excellent |
| Resistance to adhesive tape | / | It is excellent |
| Resistance to silica gel | / | It is excellent |
| Acid resisting test | 0.2% | It is excellent |
| Salt spray test | 0.3% | It is excellent |
| Hydrothermal aging | 0.5% | It is excellent |
| Wet jelly recycles aging | 0.5% | It is excellent |
Embodiment 3
(1) by polyether modified siloxane BYK-373, TEOS, oxalic acid, AEO9, absolute ethyl alcohol is with quality 2：2：0.03：0.3：
2 ratio mixing, is warming up to 70~75 DEG C, is then added dropwise deionized water, fast, the quality of BYK-373 and water after when dropwise addition is first slow
Than being 1：2, add reactant boiling reflux during water, until adding water, then flow back 20 minutes, at this moment solution becomes micro- blue light
Solution, reaction terminate to obtain solution A, pour out spare；
(2) by methyltrimethoxysilane, dimethyl diethoxysilane, oxalic acid, absolute ethyl alcohol, deionized water is with quality
7：1：0.02：3：7 ratio mixing, in the reaction vessel of 90 DEG C of oil bath temperature stirring be warming up to reflux, maintain the reflux for 30 points
Clock, reaction terminate, and adjust pH value to 6.5-7.0 with monoethanolamine, obtain solution B, pour out spare；
(3) solution A is added in solution B while stirring, absolute ethyl alcohol dilution is then added, it is poly- that curing agent is added
Aziridine SP-012 and propylene glycol monomethyl ether stir evenly, and mass ratio is 10.33：18.02：60：0.03：2, finally subtracted
Reflective coating C.
By the above reflection reducing coating C it is 300mm*300mm*3.2mm in 10 chip sizes with solar energy photovoltaic glass roll coater
Solar energy photovoltaic glass print on, cure within 3 minutes through 80~180 DEG C of heat stepwises, obtain nattier blue solar energy antireflective
Then its solar energy photovoltaic glass steel process routinely was obtained bluish violet too by film glass in 700 DEG C of tempering 140 seconds
Positive energy antireflective coating glass print.
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.3% | It is good |
| Adhesive force is tested | / | It is excellent |
| Pencil hardness | / | 4H passes through |
| Grease resistance | / | It is excellent |
| Resistance to adhesive tape | / | It is excellent |
| Resistance to silica gel | / | It is excellent |
| Acid resisting test | 0.3% | It is excellent |
| Salt spray test | 0.5% | It is excellent |
| Hydrothermal aging | 0.5% | It is excellent |
| Wet jelly recycles aging | 0.5% | It is excellent |
Embodiment 4
(1) by polyether-polyester modified hydroxyl functional polydimethylsiloxanes BYK-375, TEOS, sodium hydroxide, dehydration mountain
Pears polyol fatty acid ester APEO T80, normal propyl alcohol is with quality 2：2：0.01：0.2：2 ratio mixing, is warming up to 70~75
DEG C, then it is added dropwise deionized water, fast after when dropwise addition is first slow, the mass ratio of BYK-375 and water is 1：2, it is reacted during adding water
Object boiling reflux until adding water, then flows back 20 minutes, and at this moment solution becomes micro- blue light solution, and reaction terminates to obtain solution A,
It pours out spare；
(2) by positive quanmethyl silicate, dimethyl 2 acetoxyl group silane, dilaurate diisobutyl tin, normal propyl alcohol, go from
Sub- water is with quality 5.5：1：0.015：3：6 ratio mixing, in the reaction vessel of 90 DEG C of oil bath temperature stirring be warming up to reflux,
30 minutes are maintained the reflux for, reaction terminates, and adjusts pH value to 6.5-7.0 with 2-amino-2-methyl-1-propanol AMP-95, obtains molten
Liquid B is poured out spare；
(3) solution A is added in solution B while stirring, normal propyl alcohol dilution is then added, four positive fourth of metatitanic acid is added
Ester and butyl glycol ether stir evenly, and mass ratio is 10.21：15.52：60：0.05：2, obtain final reflection reducing coating C.
By the above reflection reducing coating C roller coating it is 300mm*300mm* in 10 chip sizes with solar energy photovoltaic glass roll coater
On the solar energy photovoltaic glass print of 3.2mm, divides solidification through 80~180 DEG C of heat stepwises 3, obtain nattier blue solar energy anti-reflection
Film glass is penetrated, its solar energy photovoltaic glass steel process routinely was then obtained into bluish violet in 700 DEG C of tempering 140 seconds
Solar energy antireflective coating glass print.Anti-reflection performance, strength character, weather resistance test are carried out to print, as a result such as following table institute
Show：
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.6% | It is excellent |
| Adhesive force is tested | / | It is qualified |
| Pencil hardness | / | 3H passes through |
| Grease resistance | / | It is qualified |
| Resistance to adhesive tape | / | It is qualified |
| Resistance to silica gel | / | It is qualified |
| Acid resisting test | 0.3% | It is excellent |
| Salt spray test | 0.7% | It is good |
| Hydrothermal aging | 0.7% | It is good |
| Wet jelly recycles aging | 1.0% | It is qualified |
Embodiment 5
(1) by acrylate modified siloxanes BYK-371, TEOS, acetic acid, AEO9, absolute ethyl alcohol is with quality 2：2：0.02：
0.2:2 ratio mixing, is warming up to 70~75 DEG C, is then added dropwise deionized water, fast after when dropwise addition is first slow, BYK-371 and water
Mass ratio is 1：2, add reactant boiling reflux during water, until adding water, then flow back 20 minutes, at this moment solution becomes micro-
Blue light solution, reaction terminate to obtain solution A, pour out spare；
(2) by vinyltrimethoxysilane, dimethyl diethoxysilane, oxalic acid, absolute ethyl alcohol, deionized water is with matter
Amount 9：1：0.02：3：6 ratio mixing, in the reaction vessel of 90 DEG C of oil bath temperature stirring be warming up to reflux, maintain the reflux for 30
Minute, reaction terminates, and adjusts pH value to 6.5~7.0 with piperazine, obtains solution B, pour out spare；
(3) solution A is added in solution B while stirring, absolute ethyl alcohol dilution is then added, metatitanic acid four is being added just
Butyl ester and butyl glycol ether stir evenly, and mass ratio is 10.22：19.02：60：0.05：2, obtain final reflection reducing coating C.
By the above reflection reducing coating C roller coating it is 300mm*300mm* in 10 chip sizes with solar energy photovoltaic glass roll coater
On the solar energy photovoltaic glass print of 3.2mm, cures within 3 minutes through 80~180 DEG C of heat stepwises, obtain nattier blue solar energy and subtract
Film glass is reflected, its solar energy photovoltaic glass steel process routinely was then obtained into bluish violet in 700 DEG C of tempering 140 seconds
Solar energy antireflective coating glass print.Anti-reflection performance, strength character, weather resistance test are carried out to print, as a result such as following table
It is shown：
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.6% | It is excellent |
| Adhesive force is tested | / | It is good |
| Pencil hardness | / | 4H passes through |
| Grease resistance | / | It is good |
| Resistance to adhesive tape | / | It is good |
| Resistance to silica gel | / | It is qualified |
| Acid resisting test | 0.3% | It is excellent |
| Salt spray test | 0.7% | It is good |
| Hydrothermal aging | 0.9% | It is qualified |
| Wet jelly recycles aging | 0.9% | It is qualified |
Comparative example
The maximum similar product of dosage in the market is incited somebody to action, the above coating roll is coated in 10 with solar energy photovoltaic glass roll coater
Size is to cure within 3 minutes through 80~180 DEG C of heat stepwises, obtain on the solar energy photovoltaic glass print of 300mm*300mm*3.2mm
To nattier blue solar energy antireflective coating glass, then by its solar energy photovoltaic glass steel process routinely in 700 DEG C of steel
Change 140 seconds, obtains the solar energy antireflective coating glass print of bluish violet.Anti-reflection performance, strength character, weatherability are carried out to print
It can test, the results are shown in table below：
| Detection project | Value added/decaying | Qualified grade |
| Light transmittance | 2.3% | It is good |
| Adhesive force is tested | / | It is good |
| Pencil hardness | / | 3H passes through |
| Grease resistance | / | It is good |
| Resistance to adhesive tape | / | It is good |
| Resistance to silica gel | / | It is good |
| Acid resisting test | 0.4% | It is excellent |
| Salt spray test | 0.6% | It is good |
| Hydrothermal aging | 0.8% | It is qualified |
| Wet jelly recycles aging | 0.8% | It is qualified |
Claims (9)
1. a kind of preparation method of solar energy photovoltaic glass reflection reducing coating, which is characterized in that include the following steps：
(1) by organic siliconresin, esters of silicon acis, catalyst, emulsifier and solvent with mass ratio be 0.5~5：0.5~5：0.01~
0.05：0.05~0.5：1~10 mixing, is added dropwise water after being heated to 70~75 DEG C, and the mass ratio of organic siliconresin and water is 0.5~
5：0.5~10, rear return stirring is added dropwise and reacts 10~30min, obtains solution A after reaction；
The organic siliconresin is that organic silicon modified by polyether resin, polyester modified organic silicon resin or polyether-polyester modification are organic
Silicones；
(2) by esters of silicon acis, stabilizer, catalyst, solvent and water with mass ratio be 5~10：0.1~5：0.01~0.05：1~5：
5~10 mixing, are stirred to react 20~40min at a reflux temperature, adjust pH to 6.5~7.0 with amine solvent after reaction,
Obtain solution B；
(3) solution A is added in solution B under stiring, after solvent dilution is added, curing agent and coalescents is added, it is described
Solution A, solution B, solvent, curing agent and coalescents mass ratio be 3~20：12~30：30~80：0.01~0.1：1
~10, the reflection reducing coating is obtained after stirring evenly.
2. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that step (1)
In, organic siliconresin, esters of silicon acis, catalyst, emulsifier and solvent mass ratio be 1~3：1~3：0.01~0.03：0.2~
0.5：1~3.
3. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that step (2)
In, esters of silicon acis, stabilizer, catalyst, solvent and water mass ratio be 5~10：0.1~2：0.01~0.03：2~3：5~7.
4. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that step (1)
In, the esters of silicon acis is positive quanmethyl silicate, tetraethyl orthosilicate or positive n-propyl silicate, and organic siliconresin, esters of silicon acis, is urged
The mass ratio of agent, emulsifier and solvent is 1~3：1~3：0.01~0.03：0.2~0.5：1~3.
5. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that the catalysis
Agent is acid, alkali or metal soluble-salt.
6. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that the emulsification
Agent is sorbitan fatty acid ester polyoxyethylene ether, fatty alcohol polyoxyethylene ether or nonylphenol polyoxyethylene ether.
7. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that the solidification
Agent is organic titanate, organic aluminates, organozirconates or polyethyleneimine.
8. the preparation method of solar energy photovoltaic glass reflection reducing coating according to claim 1, which is characterized in that the film forming
Auxiliary agent is ethylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl glycol ether or propylene glycol monomethyl ether.
9. a kind of solar energy photovoltaic glass reflection reducing coating, which is characterized in that the reflection reducing coating is by claim 1~8
Method described in any one is prepared.
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| CN110591516B (en) * | 2019-08-28 | 2021-07-16 | 东莞南玻太阳能玻璃有限公司 | Anti-reflection coating liquid suitable for anti-glare patterned solar glass, preparation method of anti-reflection coating liquid and method for manufacturing solar glass by using anti-reflection coating liquid |
| CN113088116B (en) * | 2021-03-16 | 2022-06-07 | 杭州玻美文化艺术有限公司 | Solar glass panel with honeycomb-shaped color toughened coating, production method thereof and color solar photovoltaic module |
| CN115594416B (en) * | 2022-08-22 | 2023-11-14 | 宸光(常州)新材料科技有限公司 | Photovoltaic glass with light conversion and antireflection functions and preparation method thereof |
| CN115772004A (en) * | 2022-12-19 | 2023-03-10 | 东莞南玻太阳能玻璃有限公司 | Photovoltaic glaze, photovoltaic back plate glass, preparation method of photovoltaic back plate glass and double-glass photovoltaic module |
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| US6893684B2 (en) * | 2001-06-05 | 2005-05-17 | Brewer Science Inc. | Anti-reflective coating compositions for use with low k dielectric materials |
| JP2004083307A (en) * | 2002-08-23 | 2004-03-18 | Sumitomo Osaka Cement Co Ltd | Silica fine particle, coating material for low refractive index film formation, low refractive index film and method for manufacturing the same, and antireflection film |
| CN1294219C (en) * | 2005-05-27 | 2007-01-10 | 吉林大学 | High strength organic / inorganic nano composite transparent film layer materials and method for preparing same |
| US20110151222A1 (en) * | 2009-12-22 | 2011-06-23 | Agc Flat Glass North America, Inc. | Anti-reflective coatings and methods of making the same |
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| CN102690537A (en) * | 2011-03-22 | 2012-09-26 | 上海益泰能源科技有限公司 | Coating solution for reducing glass surface light reflection |
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