Anti-glare etching glass and preparation method thereof

Abstract

The invention discloses anti-dazzle etching glass and a preparation method thereof, belongs to the technical field of etching glass, and is used for solving the technical problems that in the prior art, an existing etching process cannot further enhance the anti-dazzle performance of the glass and how to improve the uniformity of a frosting effect of the glass so that the glass has excellent anti-dazzle performance at different angles. A preparation method of anti-dazzle etching glass comprises the following steps: S1, cleaning a glass substrate with an organic solvent, and pasting corrosion-resistant glue for local protection and whole-surface protection to obtain a protected glass sample; s2, immersing the protected glass sample into frosting liquid for etching and polishing to obtain a finished product; s3, anti-dazzle emulsion is sprayed on the upper surface of the finished product, and an anti-dazzle layer is formed; and drying at room temperature to form a film to prepare the anti-glare etching glass. The anti-dazzle etching glass prepared by the invention has the advantages of uniform frosting effect and strong anti-dazzle capability.

Description

Technical Field

[0001] The invention relates to the technical field of etched glass, and in particular to an anti-glare etched glass and a preparation method thereof. Background Art

[0002] In recent years, as personal mobile phones, tablet computers, electronic watches and other personal portable electronic products have become more and more popular, for these electronic products, the flat glass has a strong reflection of ambient light, which affects the color display of the display screen to a certain extent and affects the user experience of the product. At present, the common methods used by the industry to solve this problem include chemical frosting, glass spraying, glass sandblasting, etc.

[0003] Patent application CN108549502A discloses an anti-glare electronic-grade glass and its manufacturing process. The glass body uses a spray gun to generate a high-pressure liquid flow and spray it onto the surface of the glass body to produce fine lines with a specific roughness; then chemical etching is performed to obtain an anti-glare layer; the etched glass has the advantage of more precise control of haze and glossiness. However, the chemical etching liquid used in the anti-glare electronic-grade glass prepared above is a conventional etching liquid, which can only enhance the etching accuracy but cannot enhance the anti-glare property of the glass. In addition, how to improve the uniformity of the glass frosting effect so that it has excellent anti-glare properties at different angles is also a technical problem that needs to be solved urgently.

[0004] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention

[0005] The purpose of the present invention is to provide an anti-glare etched glass and a preparation method thereof, which are used to solve the technical problems in the prior art that when synthesizing anti-glare glass, the existing etching process cannot enhance the anti-glare property of the glass and how to improve the uniformity of the glass frosting effect so that it has excellent anti-glare property at different angles.

[0006] The purpose of the present invention can be achieved through the following technical solutions: A method for preparing anti-glare etched glass comprises the following steps: S1. The glass substrate is cleaned with an organic solvent and affixed with corrosion-resistant adhesive for local protection and full-surface protection to obtain a protected glass sample; S2, the protected glass sample is immersed in a frosting solution for etching and polishing to obtain a finished product; S3, spraying the anti-glare emulsion on the upper surface of the finished product to form an anti-glare layer; drying the anti-glare emulsion at room temperature to form a film, thereby preparing an anti-glare etched glass.

[0007] In the present invention, a glass substrate of a certain specification is pre-cleaned, and then local protection and overall protection (applying corrosion-resistant glue) are successively carried out on the non-etching surface and the non-etching positions (the part where the camera is installed at the etching position) to obtain a protected glass sample. The protected glass sample is successively subjected to etching and polishing treatments to obtain a finished product. In order to further improve the anti-glare ability of the prepared etched glass, an anti-glare emulsion is sprayed on the finished product to form an anti-glare layer, and finally, anti-glare etched glass is prepared.

[0008] Further, in step S1, the glass substrate is soda-lime glass or aluminosilicate glass, and the specification is 300 mm × 300 mm × (0.5 - 1) mm; Further, in step S2, the preparation method of the frosting solution includes the following steps: A1. Zinc chloride solution of 0.1 - 0.2 mol / L and sodium hydroxide solution are mixed and strongly stirred to obtain a reaction product; the reaction product is centrifuged to obtain a solid; ethanol, the solid and a surfactant are mixed and stirred, and then left standing to obtain a precipitate; the precipitate is centrifuged, dried and ground into powder to obtain zinc oxide particles modified with a surfactant; A2. Hydrochloric acid, barium sulfate, ammonium sulfate and zinc oxide particles modified with a surfactant are mixed evenly, and then deionized water and sodium fluoride are added to obtain a mixture; the mixture is cured at 25 - 30 °C for 1 - 2 h to obtain the frosting solution.

[0009] Further, in step A1, the concentration of the sodium hydroxide solution is 1 mol / L, the dosage ratio of the zinc chloride solution to the sodium hydroxide solution is 15 - 20 mL:2 mL, and the stirring duration is 20 - 30 min; the surfactant is sodium dodecylbenzenesulfonate, and the dosage ratio of the ethanol, the solid and the surfactant is 100 mL:2 - 3 g:0.3 - 0.5 g; in step A2, the dosage ratio of the hydrochloric acid, the barium sulfate, the ammonium sulfate and the zinc oxide particles modified with a surfactant is 10 - 15 g:2.5 - 5 g:2 - 3 g:2 - 5 g.

[0010] Further, in step S2, the etching temperature is 25 °C, the etching duration is 20 - 30 min; the polishing solution is hydrofluoric acid, and the polishing duration is 5 - 10 min.

[0011] Further, in step S1, the preparation method of the anti-glare coating emulsion includes the following steps: B1. CH 3 OH, CH 2 (OCH 3 ) 2 and CH 3Mix Cl and heat to 45 - 50 °C to obtain a mixed gas; continuously introduce the mixed gas into the Si - CuCl catalyst and continue the reaction at 45 - 50 °C to obtain a mixed product; the mixed product and deionized water undergo an alcoholysis reaction at 25 °C, collect the liquid to obtain a polysiloxanol mixture; Through the above Rochow reaction, the synthesized mixed product mainly includes HSi(OCH 3 ), 3 Si(OCH 3 ), 4 CH 3 Si(OCH 3 ), 3 etc. gas - liquid mixtures. The gas - liquid mixture undergoes hydrolysis to obtain a polysiloxanol mixture.

[0012] Mix B2, the polysiloxanol mixture, acrylic acid and p - toluenesulfonic acid evenly to obtain a reaction system; the reaction system undergoes a condensation reflux reaction at 80 - 85 °C for 24 h to obtain a polysiloxanol mixture containing terminal double bonds; Using p - toluenesulfonic acid as the catalyst for the esterification reaction, the polysiloxanol mixture and acrylic acid undergo a transesterification reaction to modify its terminal group to a double bond, obtaining a polysiloxanol mixture containing terminal double bonds.

[0013] B3. Mix the polysiloxanol mixture containing terminal double bonds and deionized water evenly to obtain a mixture; mix the mixture, styrene and initiator, react at 60 - 70 °C for 5 - 10 h, then stop the reaction, stir and discharge to obtain a solid; the solid undergoes post - process treatment to obtain an anti - glare coating solution.

[0014] The polysiloxane organic resin containing terminal double bonds, styrene and methyl methacrylate undergo a polymerization reaction to obtain a solid; the solid is blended with a polyurethane emulsion to prepare an anti - glare coating solution.

[0015] Furthermore, in step B1, the mass ratio of CH 3 OH, CH 2 (OCH 3 ), 2 and CH 3 Cl is 1:1:1, the mass of the Si - CuCl catalyst is 3 - 5 g; the feeding rate of the mixed gas is 1 mL / min, and the feeding duration is 20 - 30 min; the reaction duration is 24 - 48 h; the duration of the alcoholysis reaction is 3 - 6 h.

[0016] Further, in step B2, the dosage ratio of the polysiloxanol mixture, acrylic acid, and p-toluenesulfonic acid is 10 - 20 mL: 15 - 35 mL: 0.5 - 1 g; in step B3, the initiator is azobisisobutyronitrile; the dosage ratio of the polysiloxanol mixture containing terminal double bonds, deionized water, styrene, and the initiator is 20 - 30 mL: 50 mL: 5 - 10 g: 0.1 - 0.2 g; the post-process treatment steps include: washing the solid with deionized water 3 - 5 times, and then drying it under vacuum at 70 - 80 °C to constant weight to obtain the anti-glare coating emulsion; mixing the anti-glare coating emulsion and the polyurethane emulsion in a mass ratio of 1: 2 - 3 to obtain the anti-glare coating solution.

[0017] As another aspect of the present invention, an anti-glare etched glass prepared by the method for preparing anti-glare etched glass.

[0018] The present invention has the following beneficial effects: 1. The present invention provides a processing technology for anti-glare etched glass, which specifically includes the following steps: cleaning the glass substrate - local protection and overall protection - etching - polishing - coating with the anti-glare coating solution. The frosting solution components used in the etching process of the present invention include hydrochloric acid, barium sulfate, ammonium sulfate, sodium fluoride, and zinc oxide particles modified with surfactants, etc.; adding zinc oxide to the frosting solution helps control the crystal growth rate of the frosted surface, thereby making the generated crystal grains become fine, and thus reducing the roughness of the frosted surface. In addition, the zinc oxide particles modified with surfactants can replace starch to play a role in assisting film formation and improving fluidity, thereby improving the uniformity of the frosting effect.

[0019] 2. After the protected glass sample is immersed in the frosting solution for etching and polishing, a finished product is obtained; spraying the synthesized anti-glare emulsion on the polished surface of the finished product to form an anti-glare layer can further enhance the anti-glare property of the synthesized etched glass. The above anti-glare emulsion is obtained by mixing a polymer anti-glare material and a polyurethane emulsion, wherein the polymer anti-glare material is obtained by adding styrene and a polysiloxanol mixture containing terminal double bonds. In addition, the anti-glare coating emulsion prepared by the present invention has polycarboxylic acid monomers, which significantly enhance the calcium ion contact sites on the polymer chain segments, greatly enhancing the chelation effect between the carboxyl group and zinc ions, thereby effectively improving the compatibility between the anti-glare layer material provided and the glass etched surface, and thus significantly reducing the phase separation phenomenon between the inorganic glass substrate and the coated polymer glare material. In addition, the above polymer anti-glare material not only has anti-glare performance but also has superhydrophobic self-cleaning ability, which can ensure that under the premise of its high light transmittance and anti-reflection performance, the dirt adhered to the surface is removed under the action of natural conditions, which is more environmentally friendly and economical. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0021] Figure 1 This is the electron micrograph of the finished product prepared in Example 9 of the present invention with a particle size of 0.12 - 0.13 μm. Detailed implementation manners

[0022] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0023] The polyurethane emulsion used in Examples 1 - 3 of the present invention was purchased from Shenzhen Yitian Chemical Co., Ltd., with the model number 1624 and the brand name FPU1624; the Si - CuCl catalyst used in Examples 1 - 3 of the present invention was obtained by mixing catalyst copper chloride and high - purity silicon in a mass ratio of 1:1. The high - purity silicon was purchased from Nangong Shixiangfan Alloy Materials Co., Ltd., with the product number 2358 and the brand name si1, and the silicon content was ≥99%; the glass substrates used in Examples 7 - 9 of the present invention were soda - lime glass or aluminosilicate glass, customized from Dongguan Xupeng Glass Co., Ltd., and the specifications were all 300mm×300mm×0.5mm.

[0024] Example 1 This example provides a method for preparing an anti - glare coating emulsion for anti - glare etched glass, including the following steps: B1. Select a 500 - mL reactor. A quenching device is installed at the lower end of the reactor, and the quenching device is connected to a nozzle. 3 g of Si - CuCl catalyst is placed in the reactor, and then the reactor is heated to 220 °C; CH 3 OH, CH 2 (OCH 3 ) 2 and CH 3 Cl are mixed in a mass ratio of 1:1:1, heated to 45 °C to obtain a mixed gas. Then, the mixed gas is continuously introduced into the above - mentioned reactor at a rate of 1 mL / min for 20 min, and the reactor reacts at 45 °C for 24 h to obtain a mixed product.

[0025] B2. After the reaction is completed, 50 mL of deionized water is sprayed into the quenching device through a nozzle. The above-mentioned mixed product and deionized water undergo an alcoholysis reaction at 25 °C for 3 h, and the liquid is collected to obtain a polysilicon alcohol mixture.

[0026] B3. Measure 10 mL of the polysilicon alcohol mixture and add it to a three-necked flask equipped with a thermometer. Then add 15 mL of acrylic acid and 0.5 g of p-toluenesulfonic acid to the three-necked flask, and mix well to obtain a reaction system. The reaction system is subjected to a reflux condensation reaction at 80 °C for 24 h to obtain a polysilicon alcohol mixture containing terminal double bonds.

[0027] B4. Weigh 20 mL of the polysilicon alcohol mixture containing terminal double bonds and 50 mL of deionized water and add them to a 250 mL three-necked flask, and mix and stir evenly at 300 r / min to obtain a mixture. Then transfer the three-necked flask to a constant-temperature heating water bath magnetic stirrer, add 5 g of styrene and 0.1 g of initiator azobisisobutyronitrile to the three-necked flask, and carry out a mechanical stirring reaction at 60 °C for 5 h. Then stop stirring and discharge to obtain a solid. The solid is washed 3 times with deionized water and then vacuum dried at 70 °C to constant weight to obtain a high molecular anti-glare material. The above-mentioned high molecular anti-glare material and polyurethane emulsion are mixed evenly according to a mass ratio of 1:2 to obtain an anti-glare coating solution.

[0028] Example 2 This example provides a preparation method of an anti-glare coating emulsion for anti-glare etched glass, including the following steps: B1. Select a 500 mL reactor, install a quenching device at the lower end of the reactor, and the quenching device is connected to a nozzle. 4 g of Si-CuCl catalyst is installed in the reactor, and then the reactor is heated to 250 °C; CH 3 OH, CH 2 (OCH 3 ) 2 and CH 3 Cl are mixed according to a mass ratio of 1:1:1, heated to 48 °C to obtain a mixed gas. Then the mixed gas is continuously introduced into the above-mentioned reactor at a rate of 1 mL / min for 25 min, and the reactor reacts at 46 °C for 36 h to obtain a mixed product.

[0029] B2. After the reaction is completed, 50 mL of deionized water is sprayed into the quenching device through a nozzle. The above-mentioned mixed product and deionized water undergo an alcoholysis reaction at 25 °C for 5 h, and the liquid is collected to obtain a polysilicon alcohol mixture.

[0030] B3. Measure 15 mL of the polysilicon alcohol mixture and add it to a three-necked flask equipped with a thermometer. Then add 25 mL of acrylic acid and 0.8 g of p-toluenesulfonic acid to the three-necked flask, and mix well to obtain a reaction system. The reaction system is subjected to a reflux condensation reaction at 82 °C for 24 h to obtain a polysilicon alcohol mixture containing terminal double bonds.

[0031] B4. Weigh 25 mL of the polysiloxanol mixture with terminal double bonds and 50 mL of deionized water, add them to a 250 mL three-necked flask, mix and stir evenly at 400 r / min to obtain a mixture. Then transfer the three-necked flask to a constant-temperature heating water bath magnetic stirrer, add 8 g of styrene and 0.15 g of initiator azobisisobutyronitrile to the three-necked flask, mechanically stir and react at 65 °C for 8 h, then stop stirring and discharge to obtain a solid. The solid is washed 4 times with deionized water and then vacuum dried at 75 °C to constant weight to obtain a polymer anti-glare material. The above polymer anti-glare material and polyurethane emulsion are mixed evenly according to a mass ratio of 1:3 to obtain an anti-glare coating solution.

[0032] Example 3 This example provides a preparation method of an anti-glare coating emulsion for anti-glare etched glass, including the following steps: B1. Select a 500 mL reactor, install a quenching device at the lower end of the reactor, and the quenching device is connected to a nozzle. 5 g of Si-CuCl catalyst is installed in the reactor, and then the reactor is heated to 280 °C; CH 3 OH, CH 2 (OCH 3 ) 2 and CH 3 Cl are mixed according to a mass ratio of 1:1:1, heated to 50 °C to obtain a mixed gas. Then the mixed gas is continuously introduced into the above reactor at 1 mL / min for 30 min, and the reactor reacts at 50 °C for 48 h to obtain a mixed product.

[0033] B2. After the reaction is completed, spray 50 mL of deionized water into the quenching device through the nozzle, and the above mixed product and deionized water undergo an alcoholysis reaction at 25 °C for 6 h, and the liquid is collected to obtain a polysiloxanol mixture.

[0034] B3. Measure 20 mL of the polysiloxanol mixture and add it to a three-necked flask equipped with a thermometer. Then add 35 mL of acrylic acid and 1 g of p-toluenesulfonic acid to the three-necked flask, and mix evenly to obtain a reaction system. The reaction system is refluxed and condensed at 85 °C for 24 h to obtain a polysiloxanol mixture with terminal double bonds.

[0035] B4. Weigh 30 mL of the polysiloxanol mixture with terminal double bonds and 50 mL of deionized water, add them to a 250 mL three-necked flask, mix and stir evenly at 500 r / min to obtain a mixture. Then transfer the three-necked flask to a constant-temperature heating water bath magnetic stirrer, add 10 g of styrene and 0.2 g of initiator azobisisobutyronitrile to the three-necked flask, mechanically stir and react at 70 °C for 10 h, then stop stirring and discharge to obtain a solid. The solid is washed 5 times with deionized water and then vacuum dried at 80 °C to constant weight to obtain a high-molecular anti-glare material. The above high-molecular anti-glare material and polyurethane emulsion are mixed evenly according to a mass ratio of 1:3 to obtain an anti-glare coating solution.

[0036] Example 4 This example provides a preparation method of a frosting solution for anti-glare etched glass, including the following steps: A1. Measure 15 mL of 0.1 mol / L zinc chloride solution and add it to a 100 mL beaker. Then quickly add 2 mL of 1 mol / L sodium hydroxide solution under magnetic stirring conditions and stir for 20 min to obtain a product. The product is centrifuged by a centrifuge to obtain a solid.

[0037] A2. Add 100 mL of ethanol to a 250 mL three-necked flask, then add 2 g of the solid and 0.3 g of surfactant sodium dodecylbenzenesulfonate, mix and stir at 100 r / min for 10 min, then let it stand in the beaker to obtain a precipitate; the precipitate is centrifuged, dried in a petri dish at room temperature and ground into powder to obtain surfactant-modified zinc oxide particles.

[0038] A3. Mix 10 g, 1 mol / L hydrochloric acid, 2.5 g of barium sulfate, 2 g of ammonium sulfate and 2 g of surfactant-modified zinc oxide particles evenly, then add 300 g of deionized water and 15 g of sodium fluoride to obtain a mixture. Use a constant-temperature magnetic stirrer to stir the mixture evenly and cure at 25 °C for 1 h to obtain a frosting solution.

[0039] Example 5 This example provides a preparation method of a frosting solution for anti-glare etched glass, including the following steps: A1. Measure 18 mL of 0.15 mol / L zinc chloride solution and add it to a 100 mL beaker. Then quickly add 2 mL of 1 mol / L sodium hydroxide solution under magnetic stirring conditions and stir for 25 min to obtain a product. The product is centrifuged by a centrifuge to obtain a solid.

[0040] A2. Add 100 mL of ethanol into a 250 mL three-necked flask, then add 2.5 g of solid and 0.4 g of surfactant sodium dodecylbenzenesulfonate, mix and stir at 150 r / min for 17 min, then let it stand in a beaker to obtain a precipitate; centrifuge the precipitate, dry it in a petri dish at room temperature and grind it into powder to obtain zinc oxide particles modified with surfactant.

[0041] A3. Mix 12 g of 1 mol / L hydrochloric acid, 3.5 g of barium sulfate, 2.5 g of ammonium sulfate and 4 g of zinc oxide particles modified with surfactant, then add 300 g of deionized water and 18 g of sodium fluoride to obtain a mixture. Stir the mixture evenly with a constant temperature magnetic stirrer and cure it at 28 °C for 1.5 h to obtain a frosting solution.

[0042] Example 6 This example provides a preparation method of a frosting solution for anti-glare etched glass, including the following steps: A1. Measure 20 mL of 0.2 mol / L zinc chloride solution and add it into a 100 mL beaker, then quickly add 2 mL of 1 mol / L sodium hydroxide solution under magnetic stirring conditions and stir for 30 min to obtain a product. Centrifuge the product with a centrifuge to obtain a solid.

[0043] A2. Add 100 mL of ethanol into a 250 mL three-necked flask, then add 3 g of solid and 0.5 g of surfactant sodium dodecylbenzenesulfonate, mix and stir at 200 r / min for 20 min, then let it stand in a beaker to obtain a precipitate; centrifuge the precipitate, dry it in a petri dish at room temperature and grind it into powder to obtain zinc oxide particles modified with surfactant.

[0044] A3. Mix 15 g of 1 mol / L hydrochloric acid, 5 g of barium sulfate, 3 g of ammonium sulfate and 5 g of zinc oxide particles modified with surfactant, then add 300 g of deionized water and 20 g of sodium fluoride to obtain a mixture. Stir the mixture evenly with a constant temperature magnetic stirrer and cure it at 30 °C for 2 h to obtain a frosting solution.

[0045] Example 7 This example provides a preparation method of anti-glare etched glass, including the following steps: S1. Select soda-lime glass as the glass substrate, and the specification of the glass substrate is 300 mm × 300 mm × 0.5 mm; mix acetone and absolute ethanol according to a mass ratio of 1:1 to obtain an organic solvent; use the organic solvent to clean the glass substrate with a flat panel cleaning machine, the cleaning duration is 20 min, and the transmission speed is 750 mm / min to obtain a surface-treated glass substrate.

[0046] S2. One side of the surface-treated glass substrate serves as the etching surface, and the other side serves as the non-etching surface; corrosion-resistant glue is pasted on both the non-etching position of the etching surface (the position where the camera needs to be installed on the etching surface) and the non-etching surface to obtain a protected glass sample.

[0047] S3. The protected glass sample is immersed in the frosting solution prepared in Example 4 for etching, with an etching temperature of 25 °C and an etching duration of 20 min to obtain etched glass. Using hydrofluoric acid as the polishing solution, the etched glass is polished with the polishing solution for 5 min to obtain the finished product.

[0048] S4. The anti-glare emulsion prepared in Example 1 is sprayed on the upper surface of the finished product using a manual spray gun to form an anti-glare layer with a spraying thickness of 0.5 μm. After drying into a film at room temperature, an anti-glare layer is formed on the upper surface of the finished product to obtain the finished product, which is the prepared anti-glare etched glass.

[0049] Example 8 This example provides a method for preparing anti-glare etched glass, including the following steps: S1. Select soda-lime glass as the glass substrate, with the specifications of the glass substrate being 300 mm × 300 mm × 0.5 mm; acetone and absolute ethanol are mixed in a mass ratio of 1:1 to obtain an organic solvent; the glass substrate is cleaned with the organic solvent using a flat panel cleaning machine for 25 min at a transmission speed of 850 mm / min to obtain a surface-treated glass substrate.

[0050] S2. One side of the surface-treated glass substrate serves as the etching surface, and the other side serves as the non-etching surface; corrosion-resistant glue is pasted on both the non-etching position of the etching surface (the position where the camera needs to be installed on the etching surface) and the non-etching surface to obtain a protected glass sample.

[0051] S3. The protected glass sample is immersed in the frosting solution prepared in Example 5 for etching, with an etching temperature of 25 °C and an etching duration of 25 min to obtain etched glass. Using hydrofluoric acid as the polishing solution, the etched glass is polished with the polishing solution for 5 - 10 min to obtain the finished product.

[0052] S4. The anti-glare emulsion prepared in Example 2 is sprayed on the upper surface of the finished product using a manual spray gun to form an anti-glare layer with a spraying thickness of 0.6 μm. After drying into a film at room temperature, an anti-glare layer is formed on the upper surface of the finished product to obtain the finished product, which is the prepared anti-glare etched glass.

[0053] Example 9 This example provides a method for preparing anti-glare etched glass, including the following steps: S1. Select soda-lime glass as the glass substrate, with the specifications of the glass substrate being 300 mm × 300 mm × 1 mm; mix acetone and absolute ethanol in a mass ratio of 1:1 to obtain an organic solvent; use the organic solvent to clean the glass substrate with a flat panel cleaning machine for 30 minutes at a transmission speed of 1000 mm / min to obtain the surface-treated glass substrate.

[0054] S2. One side of the surface-treated glass substrate is used as the etching surface, and the other side is used as the non-etching surface; anti-corrosion glue is pasted on both the non-etching position of the etching surface (the position where the camera needs to be installed on the etching surface) and the non-etching surface to obtain the protected glass sample.

[0055] S3. Immerse the protected glass sample in the frosting solution prepared in Example 6 for etching at an etching temperature of 25 °C and an etching duration of 30 minutes to obtain the etched glass. Use hydrofluoric acid as the polishing solution, and polish the etched glass with the polishing solution for 10 minutes to obtain the finished product.

[0056] S4. Use a manual spray gun to spray the anti-glare emulsion prepared in Example 3 on the upper surface of the finished product to form an anti-glare layer with a spraying thickness of 1 μm, and dry it into a film at room temperature to form an anti-glare layer on the upper surface of the finished product to obtain the finished product, which is the prepared anti-glare etched glass.

[0057] Comparative Example 1 The difference between this comparative example and Example 9 is that when preparing the anti-glare coating emulsion, methylsilanetriol of the same mass is used to replace the polysilol mixture.

[0058] Comparative Example 2 The difference between this comparative example and Example 9 is that when preparing the anti-glare coating emulsion, step B3 is cancelled; in step B4, the polysilol mixture is used to replace the polysilol mixture containing terminal double bonds.

[0059] Comparative Example 3 The difference between this comparative example and Example 9 is that when preparing the frosting solution, no surfactant is added in step A2 to obtain zinc oxide particles.

[0060] Performance detection: 1. Use a glossmeter to sequentially measure the anti-glare etched glass prepared in Examples 7 - 9 and Comparative Examples 1 - 3 Sequentially measure their glossiness values at 20°, 30°, 70°, 90° and 120°.

[0061] Table 1. Test sample performance detection data

[0062] Data analysis: The glossiness of the anti-glare etched glass prepared in Examples 7-9 and Comparative Examples 1-3 of the present invention at 20°, 30°, 70°, 90° and 120° is within its reasonable range; according to the glossiness value detections at the above different angles, after the glass prepared in Examples 7-9 and Comparative Examples 1-3 is treated by the etching and polishing processes, its surface has uniform roughness (combined with Figure 1 , the anti-glare etched glass prepared in Example 9 of the present invention has uniform roughness on its surface). However, in Comparative Example 3, zinc oxide particles of the same mass are used to replace the zinc oxide particles modified with surfactants in the frosting solution, and the uniformity of the roughness of the prepared glass after etching is reduced.

[0063] 2. Use a haze meter to detect the haze of the anti-glare etched glass prepared in Examples 7-9 and Comparative Examples 1-3 in sequence.

[0064] 3. Use a transmittance tester to detect the transmittance of the anti-glare etched glass prepared in Examples 7-9 and Comparative Examples 1-3.

[0065] 4. Use a roughness meter to detect the roughness of the anti-glare etched glass prepared in Examples 7-9 and Comparative Examples 1-3 in sequence.

[0066] Table 2: Test data of sample performance

[0067] Data analysis: By comparing and analyzing the data in Table 2, the anti-glare etched glass prepared in Examples 7-9 of the present invention has a certain rough surface, with a lower light transmittance and a lower haze value, indicating that the prepared etched glass has excellent anti-glare performance.

[0068] However, in Comparative Example 1, when preparing the anti-glare coating emulsion, methylsilanetriol of the same mass is used to replace the polysilol mixture; compared with the polysilol mixture, methylsilanetriol of the same mass has fewer hydroxyl groups and fewer grafted styrene, resulting in a decrease in the anti-glare property of the prepared anti-glare coating solution; in Comparative Example 2, the polysilol mixture is used to replace the polysilol mixture containing terminal double bonds, so that the polysilol mixture fails to graft styrene; therefore, the haze values and transmittance values of the glass prepared in Comparative Example 1 and Comparative Example 2 both increase.

[0069] The above content is only an example and explanation of the structure of the present invention. Those skilled in the art of the present technology make various modifications or supplements or use similar methods to replace the specific embodiments described, as long as they do not deviate from the structure of the invention or exceed the scope defined by the claims of the present invention, they should all fall within the protection scope of the present invention.

[0070] In the description of this specification, the descriptions referring to terms such as "one embodiment", "example", "specific example", etc. mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in a suitable manner in any one or more embodiments or examples.

[0071] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the present invention to only the specific implementation manners. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A method for preparing anti-glare etched glass, characterized in that: The following steps are involved: S1. The glass substrate is cleaned with an organic solvent and affixed with corrosion-resistant adhesive for local protection and full-surface protection to obtain a protected glass sample; S2, the protected glass sample is immersed in a frosting solution for etching, and then polished to obtain a finished product; S3, spraying the anti-glare emulsion on the polished surface of the finished product to form an anti-glare layer, and then drying it at room temperature to form a film, thereby preparing an anti-glare etched glass.

2. The method for preparing an anti-glare etched glass according to claim 1, characterized in that: In step S1, the glass substrate is soda-lime glass or aluminosilicate glass, with a specification of 300 mm×300 mm×(0.5-1) mm.

3. The method for preparing an anti-glare etched glass according to claim 1, characterized in that: In step S2, the method for preparing the frosting liquid comprises the following steps: A1, 0.1-0.2 mol / L zinc chloride and sodium hydroxide solution are mixed and stirred to obtain a product; the product is centrifuged to obtain a solid; ethanol, the solid and a surfactant are mixed and stirred, and allowed to stand to obtain a precipitate; the precipitate is centrifuged, dried and ground into powder to obtain surfactant-modified zinc oxide particles; A2. Mix hydrochloric acid, barium sulfate, ammonium sulfate and zinc oxide particles modified by a surfactant, and then add deionized water and sodium fluoride to obtain a mixture; and ripen the mixture at 25-30° C. for 1-2 hours to obtain a frosting solution.

4. The method for preparing an anti-glare etched glass according to claim 3, characterized in that: In step A1, the concentration of the sodium hydroxide solution is 1 mol / L, the dosage ratio of zinc chloride to the sodium hydroxide solution is 15-20 mL: 2 mL, and the stirring time is 20-30 min; the surfactant is sodium dodecylbenzene sulfonate, and the dosage ratio of the ethanol, the solid and the surfactant is 100 mL: 2-3 g: 0.3-0.5 g; in step A2, the dosage ratio of hydrochloric acid, barium sulfate, ammonium sulfate and surfactant-modified zinc oxide particles is 10-15 g: 2.5-5 g: 2-3 g: 2-5 g.

5. The method for preparing an anti-glare etched glass according to claim 1, characterized in that: In step S2, the etching temperature is 25°C, the etching time is 20-30 minutes, the polishing liquid is hydrofluoric acid, and the polishing time is 5-10 minutes.

6. The method for preparing an anti-glare etched glass according to claim 1, characterized in that: In step S3, the method for preparing the anti-glare coating emulsion comprises the following steps: B1, CH3OH, CH2(OCH3)2 and CH3Cl are mixed and heated to 45-50°C to obtain a mixed gas; the mixed gas is continuously introduced into the Si-CuCl contact body and the reaction is continued at 45-50°C to obtain a mixed product; the mixed product and deionized water undergo alcoholysis reaction at 25°C, and the liquid is collected to obtain a polysilicone mixture; B2, the polysilanol mixture, acrylic acid and p-toluenesulfonic acid are mixed to obtain a reaction system; the reaction system is condensed and refluxed at 80-85° C. for 24 hours to obtain a polysilanol mixture containing terminal double bonds; B3. The polysilicone mixture containing terminal double bonds and deionized water are uniformly mixed to obtain a mixture; the mixture, styrene and an initiator are mixed and reacted at 60-70° C. for 5-10 hours, and then the reaction is stopped and the material is stirred to obtain a solid; the solid is post-processed to obtain an anti-glare coating solution.

7. The method for preparing an anti-glare etched glass according to claim 6, characterized in that: In step B1, the mass ratio of CH3OH, CH2(OCH3)2 and CH3Cl is 1:1:1, the mass of Si-CuCl contact is 3-5g; the introduction rate of the mixed gas is 1mL / min, and the introduction time is 20-30min; the reaction time is 24-48h; and the alcoholysis reaction time is 3-6h.

8. The method for preparing an anti-glare etched glass according to claim 6, characterized in that: In step B2, the dosage ratio of the polysilicone mixture, acrylic acid and p-toluenesulfonic acid is 10-20mL:15-35mL:0.5-1g; in step B3, the initiator is azobisisobutyronitrile; the dosage ratio of the polysilicone mixture containing terminal double bonds, deionized water, styrene and initiator is 20-30mL:50mL:5-10g:0.1-0.2g; the post-process treatment steps include: washing the solid with deionized water for 3-5 times, and then vacuum drying at 70-80°C to constant weight to obtain a polymer anti-glare material; the polymer anti-glare material and the polyurethane emulsion are mixed in a mass ratio of 1:2-3 to obtain an anti-glare coating solution. 9.An anti-glare etched glass, characterized in that: The anti-glare etched glass is prepared by the method for preparing the anti-glare etched glass according to any one of claims 1 to 8.

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