CN102352184B - Method for preparing sol for stabilizing properties of anti-reflection film of solar glass - Google Patents
Method for preparing sol for stabilizing properties of anti-reflection film of solar glass Download PDFInfo
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- CN102352184B CN102352184B CN201110186598.4A CN201110186598A CN102352184B CN 102352184 B CN102352184 B CN 102352184B CN 201110186598 A CN201110186598 A CN 201110186598A CN 102352184 B CN102352184 B CN 102352184B
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Abstract
The invention relates to the preparation of sol and aims to provide a method for preparing sol for stabilizing the properties of an anti-reflection film of solar glass. The method comprises the following steps of: adding orthosilicic acid ester into a lower aliphatic alcohol solvent with stirring, and mixing uniformly; adding water, adding a pore-forming agent, namely triton X-100, mixing, adding organic acid or inorganic acid to regulate the pH value of a solution to be 2 to 3, and reacting for 4h at the temperature of 60 DEG C; adding alkyl siloxane, mixing uniformly, and continuing to react for 2h at the temperature of 60 DEG C to obtain SiO2 polymer sol for the anti-reflection film; and adding a pH value stabilizer with the pH value of between 6.8 and 7.8, and mixing uniformly to obtain a product. By the method, the subsequent reaction speed of the system is greatly reduced, and the stability of the system is improved and the preservation time of the system is prolonged. Meanwhile, during the use of film sol, volatile weak acid in a buffer solution is volatilized and weak acid salt of the volatile weak acid is remained through the curing and heating of a film in the post-heat treatment process; and the film system becomes alkaline and is easier to cure at this time.
Description
Technical field
The present invention relates to colloidal sol preparation, particularly a kind of preparation method of colloidal sol of the stable in properties for solar energy glass anti-reflection film.
Background technology
Along with the widespread use of photovoltaic generation, sun power packaged glass is used in a large number, and sun power packaged glass anti-reflection film is a kind of optical thin film that is coated in sun power packaged glass surface and is used for increasing glass transmitance.The anti-reflective glass of sun power encapsulation is at present mainly by the application pattern of roller coat or spraying, film sol coating to be obtained through the thermal treatment of certain temperature at glass surface.From the anti-reflection principle of film, for individual layer anti-reflection anti-reflection film, to in 380～1100nm visible ray-near-infrared band, realize the highest anti-reflection performance (being best reflection preventing ability), need to meet the specific refractory power of thin-film material simultaneously and strictly control two parameters of film thickness (generally in 130nm left and right) that are coated on glass surface, and the character of painting film sol and structure are to these two parameter influence keys.Painting film sol kind for film is a lot, at present in order to obtain the anti-reflection film of high mechanical strength, for the general SiO preparing under acid catalysis condition by sol-gel method that adopts of painting film sol of film
2colloidal sol.Because being one, sol-gel process continues the process of carrying out, thereby the shortcoming of this class colloidal sol is that room temperature is deposited the physical properties of colloidal sol in process (viscosity) and structure (molecular structure) is still changing, make cycle applicable time of this class colloidal sol very short, some unsettled SiO
2its anti-reflection film performance of preparing will significantly worsen and be not suitable for being suitable for the at room temperature several days time of colloidal sol, not only caused very large waste, more had a strong impact on the performance of coated glass.Thereby how to improve this class SiO
2the stability of colloidal sol physical properties and structure, the cycle that is suitable for that extends colloidal sol are very important for the anti-reflection performance of stablizing solar energy glass anti-reflection film.
For SiO
2sol-gel process, influence process speed of response is that the factor of collosol stability is a lot of as system reactant concn, temperature, amount of water etc., wherein SiO
2sol system pH value is the most remarkable to process reaction rate, works as SiO
2sol system pH value is in neutral range (between 6.0～7.5), and system speed of response significantly reduces, and sol system is stable, but pH value is at the SiO of neutral range
2very poor being difficult to of colloidal sol film forming properties solidified, and can not prepare film.When system pH is greater than 8 under alkaline condition time, system speed of response significantly improves and easily becomes gel or solidify.The present invention adopt pH neutral scope, by the buffered soln of the alkali metal weak solution composition of volatile weak acid and its identical acid group, at SiO
2when colloidal sol is reacted to best product structure, best performance point adds this buffered soln to make solution system pH value be elevated to neutral range, significantly reduces the follow-up speed of response of system, improves stability and the shelf time of system.Meanwhile, in the use procedure of painting film sol, the curing heating by film in later stage heat treatment process, volatile weak acid volatilization and remaining its salt of weak acid in buffered soln, be now coated with film system and become alkalescence, more easily solidifies.
Summary of the invention
The technical problem to be solved in the present invention is to overcome existing acid catalysis SiO
2the poor problem of colloidal sol physicals and molecular structure stabilized under colloidal sol room temperature, from regulating pH value to start with, by the SiO preparing
2in colloidal sol, add the mode of pH value stabilization agent certain pH value, that formed by volatile weak acid and weak acid root an alkali metal salt thereof, make the pH value of reaction product colloidal sol be adjusted to neutrality, thereby significantly reduce sol-gel process speed of response, reach the object of stable sol character and structure energy.
For technical solution problem, solution of the present invention is:
The preparation method that a kind of colloidal sol of the stable in properties for solar energy glass anti-reflection film is provided, comprises the steps:
(1) under the agitation condition of 300r/min, positive silicon ester is joined in lower member ester family alcoholic solvent, mix; Then add water, then add pore former triton x-100, after mixing, add organic acid or mineral acid regulator solution pH value between 2～3, at 60 ℃, react 4h; Then add alkylsiloxane, mix rear continuation at 60 ℃ of reaction 2h, obtain anti-reflection film SiO
2polymer sol; Wherein, positive silicon ester: lower member ester family alcoholic solvent: water: triton x-100: the weight percent of alkylsiloxane is: 1～20: 50～85: 10～20: 1～5: 2～10;
(2) to above-mentioned SiO
2in polymer sol, add pH value at 6.8～7.8 pH value stabilization agent, SiO
2polymer sol: the weight percent of pH value stabilization agent is 0.1～0.5, obtains product after mixing; The agent of described pH value stabilization obtains by following manner: weak acid and the salt with metal ion with weak acid root identical with it are mixed in water by a certain percentage, make the pH value of solution between 6.8～7.8.
In the present invention, the positive silicon ester in step (1) is at least one in methyl silicate or tetraethoxy.
In the present invention, the rudimentary ester-grouped alcohol in step (1) is at least one in ethanol, Virahol or n-propyl alcohol.
In the present invention, the mineral acid in step (1) or organic acid are the one in formic acid, acetic acid, hydrochloric acid or nitric acid.
In the present invention, the alkylsiloxane in step (1) is at least one in methyltrimethoxy silane, Union carbide A-162 or ethyl triethoxysilane.
In the present invention, the weak acid in step (2) is the one in volatile weak acid formic acid, acetic acid or oxalic acid.
In the present invention, the salt with metal ion in step (2) is the one in highly basic metal-salt sylvite, sodium salt, calcium salt or lithium salts.
Compared with prior art, beneficial effect of the present invention is:
Adopt the SiO that is regulated reacting quality by pH value at the buffered soln of the volatile weak acid of neutral range (between 6.0～7.5) and the alkali metal weak solution composition of its identical acid group
2sol coating liquid pH value, make it remain on neutral range, thereby reduce further SOLUTION PROPERTIES and the product structure of the speed stable sol of reaction of colloidal sol, meanwhile, the volatilization by volatile weak acid in film thermal treating processes is that thin film system pH value becomes alkalescence and fast setting.
For SiO
2sol-gel process, influence process speed of response is that the factor of collosol stability is a lot of as system reactant concn, temperature, amount of water etc., wherein SiO
2sol system pH value is the most remarkable to process reaction rate, works as SiO
2sol system pH value is in neutral range (between 6.0～7.5), and system speed of response significantly reduces, and sol system is stable, but pH value is at the SiO of neutral range
2very poor being difficult to of colloidal sol film forming properties solidified, and can not prepare film.When system pH is greater than 8 under alkaline condition time, system speed of response significantly improves and easily becomes gel or solidify.The present invention adopt pH neutral scope, by the buffered soln of the alkali metal weak solution composition of volatile weak acid and its identical acid group, at SiO
2when colloidal sol is reacted to best product structure, best performance point adds this buffered soln to make solution system pH value be elevated to neutral range, significantly reduces the follow-up speed of response of system, improves stability and the shelf time of system.Meanwhile, in the use procedure of painting film sol, the curing heating by film in later stage heat treatment process, volatile weak acid volatilization and remaining its salt of weak acid in buffered soln, be now coated with film system and become alkalescence, more easily solidifies.
Embodiment
Below by example, the present invention is further described.
The preparation method of the solar energy glass anti-reflection film colloidal sol for the preparation of stable in properties provided by the invention, comprises the steps:
(1) under the agitation condition of 300r/min, positive silicon ester is joined in lower member ester family alcoholic solvent, mix; Then add water, then add pore former triton x-100, after mixing, add organic acid or mineral acid regulator solution pH value between 2～3, at 60 ℃, react 4h; Then add alkylsiloxane, mix rear continuation at 60 ℃ of reaction 2h, obtain anti-reflection film SiO
2polymer sol; Wherein, positive silicon ester: lower member ester family alcoholic solvent: water: triton x-100: the weight percent of alkylsiloxane is: 1～20: 50～85: 10～20: 1～5: 2～10;
(2) to above-mentioned SiO
2in polymer sol, add pH value at 6.8～7.8 pH value stabilization agent, SiO
2polymer sol: the weight percent of pH value stabilization agent is 0.1～0.5, obtains product after mixing;
The agent of described pH value stabilization obtains by following manner: weak acid and the salt with metal ion with weak acid root identical with it are mixed in water by a certain percentage, make the pH value of solution between 6.8～7.8.Testing data in each embodiment sees the following form:
Note SiO
2colloidal sol gelation time is at 40 ℃, SiO
2colloidal sol becomes the time of gel.Gelation time is longer, and colloidal sol is more stable.
Can find out from experimental result, example 7,8 does not add the colloidal sol of buffered soln relatively, and the colloidal sol gelation time that example 1～6 has added buffered soln all provides several times more than.
Finally, it is also to be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (1)
1. for the preparation method of the colloidal sol of the stable in properties of solar energy glass anti-reflection film, comprise the steps:
(1) under the agitation condition of 300r/min, 10g methyl silicate is joined in 200g ethanol, mix; Then add 10g water, then add 2.4g pore former triton x-100, after mixing, adding mineral acid HCl regulator solution pH value is 2, at 60 ℃, reacts 4h; Then add 4.4g methyltrimethoxy silane, mix rear continuation at 60 ℃ of reaction 2h, obtain anti-reflection film SiO
2polymer sol;
(2) to above-mentioned SiO
2in polymer sol, add 0.5g pH value in 6.8～7.8 pH value stabilization agent, after mixing, obtain product; The agent of described pH value stabilization obtains by following manner: weak acid HAC and the salt KAC with metal ion with weak acid root identical with it are mixed in water by a certain percentage, make the pH value of solution between 6.8～7.8.
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| CN104609738A (en) * | 2013-11-01 | 2015-05-13 | 北京有色金属研究总院 | Method used for increasing silicon dioxide antireflection film hole stability |
| CN110408070B (en) * | 2019-07-31 | 2022-03-01 | 中国工程物理研究院激光聚变研究中心 | High-threshold-value scratch-resistant high-transmittance fundamental-frequency laser film and preparation method thereof |
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| CN101805531A (en) * | 2010-02-23 | 2010-08-18 | 浙江大学 | Preparation method of organic-inorganic composite collosol for the surface corrosion prevention of metal aluminum sheet |
| CN102061112A (en) * | 2010-11-12 | 2011-05-18 | 华东师范大学 | Preparation method of composite metal organic framework material colloidal solution and application thereof in optical coatings |
| CN102079947A (en) * | 2010-12-01 | 2011-06-01 | 北京航空航天大学 | Preparation method of titanium alloy surface sol-gel conversion film |
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| CN101805531A (en) * | 2010-02-23 | 2010-08-18 | 浙江大学 | Preparation method of organic-inorganic composite collosol for the surface corrosion prevention of metal aluminum sheet |
| CN102061112A (en) * | 2010-11-12 | 2011-05-18 | 华东师范大学 | Preparation method of composite metal organic framework material colloidal solution and application thereof in optical coatings |
| CN102079947A (en) * | 2010-12-01 | 2011-06-01 | 北京航空航天大学 | Preparation method of titanium alloy surface sol-gel conversion film |
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| 吴春春 |
| 郑宏勤.硅溶胶稳定性影响因素的研究进展.《胶体与聚合物》.2011,第29卷(第2期),88-90. |
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Denomination of invention: Preparation of stable sol for antireflection coatings on solar glass Effective date of registration: 20210708 Granted publication date: 20140618 Pledgee: Bank of China Limited Longgang City sub branch Pledgor: WENZHOU KANGER CRYSTALLITE UTENSILS Co.,Ltd. Registration number: Y2021330000835 |
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