Preparation method and application of glass frosting liquid

By preparing a frosting solution containing polyhydroxy alcohols and cationic surfactant, the short service life and water ripple problems of frosting solution are solved, and the service life and production efficiency of frosting solution are extended, the production cost is reduced and the glass quality is improved.

CN120271242AActive Publication Date: 2025-07-08YICHANG NANBO DISPLAY +1
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Patent Information

Application Number
CN202510524752.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-24
Publication Date
2025-07-08
Estimated Expiration
2045-04-24

AI Technical Summary

Technical Problem

The existing frosting liquid has a short service life and low utilization rate, which is prone to water corrugation defective products, affecting production efficiency and cost.

Method used

By preparing a frosted solution containing water, polyhydroxy alcohol, ammonium hydrogen fluoride, ammonium fluoride, calcium fluoride, iron salt, potassium nitrate, potassium fluoride and cationic surfactant, a sustained release F- and H+ of ammonium hexafluoride ferrate is formed, combined with polyhydroxy alcohol to form a three-dimensional network structure, enhance etching stability, and use cationic surfactant to improve adhesion and avoid a decrease in viscosity.

Benefits of technology

Extend the service life of frosting liquid by more than 15%, improve the yield of AG glass by 11%, reduce production costs and product quality issues, and improve production efficiency and glass surface quality.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method and application of glass frosting liquid. The preparation method comprises the following steps: uniformly pre-stirring water, polyhydroxy alcohol, ammonium bifluoride, ammonium fluoride and calcium fluoride, then adding silicon dioxide, ferric salt, potassium nitrate, potassium fluoride and a cationic surfactant, sealing, curing and stirring to obtain the glass frosting liquid. The invention also discloses application of the frosting liquid prepared by the preparation method in preparation of AG glass. The glass is subjected to tape-out frosting in an inclined mode, and the AG glass is obtained. The polyol and the cationic surface active agent cooperate with each other, and the optimized frosting liquid formula can prolong the service life of the frosting liquid, i.e., the frosting area is increased by 15% or more, and the yield of the produced AG glass is increased by 11% or more.
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Description

Technical Field

[0001] The present invention relates to AG glass for display fields such as medical, industrial control, and vehicle-mounted, belonging to the technical field of glass surface processing, and specifically relates to a preparation method and application of a glass frosting solution. Background Art

[0002] Anti-glare glass is often also called AG glass (Anti Glare Glass) or anti-reflection glass. It is achieved by specially treating the glass surface to change the specular reflection of the bright surface into diffuse reflection of the matte surface, thereby achieving the effects of anti-glare or anti-reflection. With the update and iteration of electronic products, anti-glare glass has been widely used in the display screens of electronic products such as vehicle-mounted displays and laptop computers, and the demand has been increasing continuously.

[0003] In the AG glass production industry, as a key treatment material, the service life and utilization efficiency of the frosting solution have always been important factors restricting production efficiency. In the process of using the existing frosting solution, there are problems such as rapid consumption of effective components and performance degradation easily affected by impurities, resulting in frequent replacement of the frosting solution. This not only increases production costs but also affects production continuity and efficiency due to frequent debugging. Although some related technologies have tried to improve the performance of the frosting solution, there are still deficiencies in significantly improving the service life and optimizing the comprehensive performance. For example, Chinese Patent CN113880447B discloses a low flash point AG glass surface treatment composition and its application. The glass treated with this composition not only has a low flash point but also has a good anti-glare effect. However, the effective components of the frosting solution in this solution consume quickly during production, and the performance of the frosting solution degrades. At the same time, during wet frosting, a layer of water remains on the glass surface after cleaning, and the water will enter the frosting solution, further causing the viscosity of the frosting solution to deteriorate, and it is extremely easy to cause water ripples on the glass surface, with a short service life; Chinese Patent CN116606077A discloses a glass frosting solution, its preparation method and application. This solution reduces volatilization by lowering the use temperature of the frosting solution, prolongs the service life of the frosting solution, and at the same time reuses the waste of the frosting solution to improve the utilization rate of the frosting solution. However, reusing the waste of the frosting solution in this solution requires a lot of time for debugging, which is not conducive to improving production efficiency and process stability.

[0004] Disadvantages of the prior art: Short service life of the frosting solution: In the process of using the existing frosting solution, the effective components consume quickly. By simply adding the frosting solution, the consumption during the process cannot be completely replenished. As production progresses, the performance gradually degrades, and frequent replacement is required, resulting in increased production costs and hindered production continuity.

[0005] Limited production efficiency: Due to the lack of a slow-release agent in the frosting solution and its unstable performance, frequent debugging and replacement are required, resulting in frequent interruptions in the production process and greatly affecting production efficiency. In wet frosting, the glass needs to be wetted with water, but there is a water film on the glass surface, and the glass produced by the existing process is prone to water ripple defects. Summary of the Invention

[0006] The technical problem solved by the present invention is the problem of short service life of the frosting solution, low utilization rate of the frosting solution, and limited production efficiency and yield due to easy occurrence of water ripple defects.

[0007] To solve the above problems, the present application is achieved through the following technical solutions: A preparation method of a glass frosting solution, comprising the following steps: After pre-stirring water, polyhydric alcohol, ammonium bifluoride, ammonium fluoride and calcium fluoride evenly, then adding silicon dioxide, iron salt, potassium nitrate, potassium fluoride and cationic surfactant, and sealing and aging and stirring to obtain a glass frosting solution.

[0008] Preferably, the pre-stirring rate is 50-80 rpm, and the stirring time is 15-30 min.

[0009] Preferably, the aging and stirring rate is 30-50 rpm, and the single stirring time is 25-50 min.

[0010] The polyhydric alcohol is one or more of ethylene glycol, diethylene glycol, and trimethylolpropane.

[0011] The iron salt is one of iron acetate and iron citrate.

[0012] In the AG glass frosting solution, by mass ratio, ammonium bifluoride: ammonium fluoride: iron salt: calcium fluoride: silicon dioxide: polyhydric alcohol: potassium nitrate: potassium fluoride: cationic surfactant: water = 20-28: 5-12: 4-13: 4-10: 2-8: 0.8-10: 10-14: 8-12: 0.8-5: 8-20.

[0013] The silicon dioxide is micron silicon dioxide, and the particle size of the micron silicon dioxide is 3-100 um.

[0014] The aging temperature is 45°C-55°C.

[0015] The aging time is 24-32 h.

[0016] The cationic surfactant is any one of cetyltrimethylammonium bromide and cetyltrimethylammonium chloride.

[0017] Application of the frosting solution prepared by the described preparation method in the preparation of AG glass.

[0018] The specific preparation method of frosting solution for preparing AG glass further includes the following steps; The glass is sliced and frosted in an inclined manner to obtain AG glass.

[0019] Preferably, the frosting time is 50 - 100 s.

[0020] Preferably, the frosting inclination angle is 1 - 8°.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. In the frosting solution, iron salt reacts with ammonium fluoride to form ammonium hexafluoroferrate. As fluoride ions are consumed, ammonium hexafluoroferrate slowly releases F - and H + , enhancing the etching stability of the solution. At the same time, the polyhydric alcohol in the frosting solution combines with water molecules through hydrogen bonds to form a three-dimensional network structure, which can eliminate the influence of the impurity water film entrained on the surface of the wet-frosted glass. On the one hand, the polyhydric alcohol controls the slow release of effective components such as fluoride ions and hydrogen ions in the frosting solution, and on the other hand, it can balance the viscosity of the solution, making the fluidity of the frosting solution on the glass surface continuously stable and not easily causing etching defects such as water ripples on the glass surface.

[0022] 2. In the present invention, a cationic surfactant is added to the frosting solution. The cationic surfactant enhances the adhesion between the frosting solution and the glass through electrostatic action, avoiding the defect of uneven frosting caused by the reduction of viscosity. The cationic surfactant can be one of cetyltrimethylammonium bromide (CTAB) and cetyltrimethylammonium chloride (CTAC).

[0023] Compared with bentonite, polyhydric alcohol will not cause unevenness of the apparent microstructure due to the influence of impurity particles, which is conducive to production control. The polyhydric alcohol and the cationic surfactant in the present invention cooperate with each other, and the optimized frosting solution formula can extend the service life of the frosting solution, that is, the frosting area is increased by more than 15%, and the yield of the produced AG glass is increased by more than 11%.

[0024] 3. The extension of the service life of the frosting solution and the improvement of production efficiency significantly reduce the usage amount and production cost of the frosting solution, and at the same time reduce the scrap cost caused by product quality problems. The high efficiency, stability and long-term use of the frosting solution in the present invention improve production efficiency, reduce production costs, and at the same time improve the quality stability of glass frosted products. Specific Embodiments

[0025] Preferably, the AG glass is purchased from Rainbow Group Special Glass Co., Ltd., with the specification model of 1520*955*1.1mm CG01PRO+, and the water content per square meter of the AG glass is 0.05 - 0.15 kg.

[0026] In the embodiments of the present invention and the comparative examples, when the glass is transported to the sandblasting machine in an inclined manner for sandblasting during chip flow, AG glass is obtained.

[0027] Among them, the sandblasting machine was purchased from Weiliuda Machinery Equipment Co., Ltd., model: AG line.

[0028] In the following embodiments, an acid-resistant film is pasted on the surface of the glass that does not need to be sandblasted before sandblasting, and the acid-resistant film is torn off after sandblasting. In the following embodiments, unless otherwise specified, the raw materials added to the sandblasting solution are in parts by mass.

[0029] Example 1 In terms of the ratio by mass, 17 parts of water, 5 parts of ethylene glycol, 24 parts of ammonium bifluoride, 10 parts of ammonium fluoride and 7 parts of calcium fluoride are pre-stirred at 60 rpm for 20 min until uniform, and then 6.4 parts of silicon dioxide, 9.2 parts of ferric citrate, 12 parts of potassium nitrate, 8 parts of potassium fluoride and 1.4 parts of cetyltrimethylammonium bromide (cationic surfactant) are added. After mixing the above raw materials, they are placed in a sealed container and cured at 50 °C for 32 h. During the curing process, stir for 30 min every 4 hours to promote the full reaction and fusion of the components of the sandblasting solution, and prepare 400 kg of sandblasting solution #1.

[0030] The inclination angle of each piece of glass is 3.5°, and the sandblasting time is 70 s.

[0031] Example 2 Compared with Example 1, the difference is that ethylene glycol is replaced by trimethylolpropane. In terms of the ratio by mass, water:trimethylolpropane:ammonium bifluoride:ammonium fluoride:calcium fluoride:silicon dioxide:ferric citrate:potassium nitrate:potassium fluoride:cetyltrimethylammonium bromide = 16:6:24:10:6.4:6:10:10:10:1.6.

[0032] The inclination angle of each piece of glass is 4°, and the sandblasting time is 60 s.

[0033] Under other unchanged conditions, 400 kg of sandblasting solution #2 is prepared.

[0034] Example 3 Compared with Example 1, the difference is that cetyltrimethylammonium bromide is replaced by cetyltrimethylammonium chloride. In terms of the ratio by mass, water:ethylene glycol:ammonium bifluoride:ammonium fluoride:calcium fluoride:silicon dioxide:ferric citrate:potassium nitrate:potassium fluoride:cetyltrimethylammonium chloride = 18:5:26:12:4.5:6:7:12:8:1.5.

[0035] The inclination angle of each piece of glass is 3°, and the sandblasting time is 65 s.

[0036] Keep other conditions unchanged and prepare 400 kg of frosting solution #3.

[0037] Example 4 Compared with Example 1, the difference is that ethylene glycol is replaced by diethylene glycol, and ferric citrate is replaced by ferric acetate. Keep other conditions unchanged. By mass ratio, water: diethylene glycol: ammonium bifluoride: ammonium fluoride: calcium fluoride: silicon dioxide: ferric acetate: potassium nitrate: potassium fluoride: cetyltrimethylammonium chloride = 16:5:25:10:8:5:9:13:8:1.

[0038] The tilt angle of each piece of glass is 5°, and the frosting time is 65 s.

[0039] Keep other conditions unchanged and prepare 400 kg of frosting solution #4.

[0040] Comparative Example 1 Compared with Example 1, the difference is that ethylene glycol is not added. Keep other conditions unchanged and prepare 400 kg of frosting solution #5.

[0041] Comparative Example 2 Compared with Example 1, the difference is that the cationic surfactant cetyltrimethylammonium bromide is not added. Keep other conditions unchanged and prepare 400 kg of frosting solution #6.

[0042] Comparative Example 3 Compared with Example 1, the difference is that ferric citrate is replaced by ferric nitrate, and 400 kg of frosting solution #7 is prepared.

[0043] Comparative Example 4 Compared with Example 1, the difference is that ferric citrate is replaced by ferric chloride, and 400 kg of frosting solution #8 is prepared.

[0044] Comparative Example 5 Compared with Example 1, the difference is that no pre-stirring is carried out. Ethylene glycol, ammonium bifluoride, ammonium fluoride, calcium fluoride, silicon dioxide, ferric citrate, potassium nitrate, potassium fluoride, and cetyltrimethylammonium bromide are directly mixed and aged and stirred. After filtration, there are granular substances and the solution is in a paste state, and a uniform frosting solution cannot be prepared.

[0045] The performance tests of the frosting solutions prepared in the above Examples 1 to 4 and Comparative Examples 1 to 5 are as shown in Table 1 below:

[0046] The measuring instruments and models used for the measuring parameters in the above Table 1 are as shown in Table 2 below: Table 2

[0047] The above data are obtained by using conventional testing methods in the art.

Claims

1. A method for preparing a glass frosting solution, characterized in that, It includes the following steps: After premixing water, polyhydric alcohol, ammonium bifluoride, ammonium fluoride and calcium fluoride evenly, then add silicon dioxide, iron salt, potassium nitrate, potassium fluoride and cationic surfactant, and seal and age and stir to obtain the glass frosting solution.

2. The preparation method of a glass frosting liquid according to claim 1, characterized in that The polyhydric alcohol is one or more of ethylene glycol, diethylene glycol, trimethylolpropane.

3. The preparation method of a glass frosting liquid according to claim 1, characterized in that, The iron salt is one of iron acetate and iron citrate.

4. The preparation method of a glass frosting liquid according to claim 1, characterized in that, In the AG glass frosting solution, by mass ratio, ammonium bifluoride: ammonium fluoride: iron salt: calcium fluoride: silicon dioxide: polyhydric alcohol: potassium nitrate: potassium fluoride: cationic surfactant: water = 20-28: 5-12: 4-13: 4-10: 2-8: 0.8-10: 10-14: 8-12: 0.8-5: 8-20.

5. The preparation method of a glass frosting liquid according to claim 1, characterized in that, The silicon dioxide is micron silicon dioxide, and the particle size of the micron silicon dioxide is 3-100 um.

6. The preparation method of a glass frosting solution according to claim 1, characterized in that, The aging temperature is 45°C to 55°C.

7. The preparation method of a glass frosting liquid according to claim 1, characterized in that, The aging time is 24-32 h.

8. The preparation method of a glass frosting liquid according to claim 1, wherein, The cationic surfactant is any one of cetyltrimethylammonium bromide and cetyltrimethylammonium chloride.

9. The application of the frosting solution prepared by the preparation method according to any one of claims 1 to 8 in the preparation of AG glass.

10. The application according to claim 9, characterized in that, The specific preparation method of using the frosting solution to prepare AG glass further includes the following steps; Flow and frost the glass in an inclined manner to obtain AG glass.

Citation Information

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