Preparation method of glass frosting liquid and application thereof

Abstract

The application discloses a preparation method of glass frosting liquid and application thereof. Water, polyhydric alcohol, ammonium hydrogen fluoride, ammonium fluoride and calcium fluoride are uniformly pre-stirred, then, silica, iron salt, potassium nitrate, potassium fluoride and cationic surfactant are added, and sealed aging stirring is conducted to obtain the glass frosting liquid. The application of the frosting liquid prepared by the preparation method in preparation of AG glass. The glass is flowed and frosted in an inclined manner to obtain the AG glass. The polyhydric alcohol and the cationic surfactant in the application are synergistic 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 more than 15%, and the yield of the produced AG glass is increased by more than 11%.

Description

Technical Field

[0001] This invention relates to AG glass for medical, industrial control, and automotive display applications, belonging to the field of glass surface processing technology, specifically to a method for preparing glass frosting liquid and its application. Background Technology

[0002] Anti-glare glass, often referred to as AG glass or anti-reflective glass, is made by specially treating the glass surface to change the specular reflection of a glossy surface into diffuse reflection of a matte surface, thus achieving the effect of reducing glare or reflection. With the continuous upgrading of electronic products, anti-glare glass has been widely used in automotive displays, laptops, and other electronic product screens, and the demand continues to increase.

[0003] In the AG glass manufacturing industry, frosting solution is a key processing material, and its service life and utilization efficiency have always been important factors restricting production efficiency. Existing frosting solutions suffer from problems such as rapid depletion of effective components and susceptibility to performance degradation due to impurities, leading to frequent replacements. This not only increases production costs but also disrupts production continuity and efficiency due to frequent adjustments. Although some related technologies have attempted to improve the performance of frosting solutions, there are still shortcomings in significantly extending service life and optimizing overall performance. For example, Chinese patent CN113880447B discloses a low flash point AG glass surface treatment composition and its application. Glass treated with this composition not only has a low flash point but also exhibits good anti-glare effects. However, the effective components of the frosting solution in this method are consumed quickly during production, leading to a decline in its performance. Furthermore, during wet frosting, a layer of residual water remains on the glass surface after cleaning, which can seep into the frosting solution, further reducing its viscosity and easily causing water ripples on the glass surface, resulting in a shorter service life. Chinese patent CN116606077A discloses a glass frosting solution, its preparation method, and its application. This solution reduces volatilization by lowering the operating temperature of the frosting solution, extending its service life, and also reuses the waste frosting solution, improving its utilization rate. However, this method requires a significant amount of time for debugging to reuse the waste frosting solution, which is detrimental to improving production efficiency and process stability.

[0004] Disadvantages of existing technology: Short service life of frosting solution: The effective components of existing frosting solutions are consumed quickly during use. The consumption cannot be fully replenished by simply adding frosting solution. As production progresses, the performance gradually declines, requiring frequent replacement, which leads to increased production costs and hinders production continuity.

[0005] Limited production efficiency: Due to the lack of a slow-release agent in the frosting solution, its performance is unstable and requires frequent adjustments and replacements, leading to frequent interruptions in the production process and greatly affecting production efficiency. In wet frosting, the glass needs to be moistened with water, but the glass surface contains a water film, and the existing process is prone to producing defective products with water ripples. Summary of the Invention

[0006] The technical problem solved by this invention is the short service life of frosting liquid, low utilization rate of frosting liquid, and the easy occurrence of water ripple defects, which limits the production efficiency and yield.

[0007] To solve the above problems, this application provides the following technical solution:

[0008] A method for preparing a glass frosting solution includes the following steps:

[0009] After pre-stirring water, polyhydroxy alcohol, ammonium bifluoride, ammonium fluoride and calcium fluoride evenly, silicon dioxide, iron salt, potassium nitrate, potassium fluoride and cationic surfactant are added, and the mixture is sealed and matured by stirring to obtain glass frosting solution.

[0010] Preferably, the pre-stirring rate is 50-80 rpm and the stirring time is 15-30 min.

[0011] Preferably, the maturation stirring rate is 30~50 rpm, and the stirring time for a single cycle is 25~50 min.

[0012] The polyhydroxy alcohol is one or more of ethylene glycol, diethylene glycol, and trimethylolpropane.

[0013] The iron salt is one of ferric acetate or ferric citrate.

[0014] In the AG glass frosting solution, by mass ratio, ammonium bifluoride: ammonium fluoride: iron salt: calcium fluoride: silicon dioxide: polyhydroxy 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.

[0015] The silica is micron-sized silica with a particle size of 3~100 μm.

[0016] The curing temperature is 45℃~55℃.

[0017] The ripening time is 24~32 hours.

[0018] The cationic surfactant is either hexadecyltrimethylammonium bromide or hexadecyltrimethylammonium chloride.

[0019] The application of the frosting solution prepared by the aforementioned method in the preparation of AG glass.

[0020] The specific preparation method for preparing AG glass using frosting solution also includes the following steps;

[0021] AG glass is obtained by frosting glass sheets at an angle.

[0022] Preferably, the frosting time is 50~100s.

[0023] Preferably, the sanding tilt angle is 1-8°.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0025] 1. In the frosting solution, iron salts and ammonium fluoride react to form ammonium hexafluoroferrite. As fluoride ions are consumed, ammonium hexafluoroferrite slowly releases F. - and H + This enhances the etching stability of the solution. Simultaneously, the polyhydroxy alcohols in the frosting solution bind with water molecules through hydrogen bonds, forming a three-dimensional network structure. This eliminates the influence of water films containing impurities on the wet-process frosted glass surface. The polyhydroxy alcohols, on the one hand, control the slow release of effective components such as fluoride and hydrogen ions from the frosting solution, and on the other hand, balance the viscosity of the solution, ensuring the continuous and stable flow of the frosting solution on the glass surface and preventing etching defects such as water ripples from forming on the glass surface.

[0026] 2. In this 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 interaction, avoiding uneven frosting defects caused by reduced viscosity. The cationic surfactant can be one of hexadecyltrimethylammonium bromide (CTAB) and hexadecyltrimethylammonium chloride (CTAC).

[0027] Compared to bentonite, polyhydroxy alcohols do not suffer from uneven surface and microstructure due to impurity particles, which facilitates production control. The synergistic effect of the polyol and cationic surfactant in this invention, along with the optimized frosting solution formulation, extends the service life of the frosting solution, resulting in a frosting area increase of over 15%, and a yield rate of AG glass production increase of over 11%.

[0028] 3. The extended service life and improved production efficiency of the frosting solution significantly reduce the amount of frosting solution used and production costs, while also reducing scrap costs due to product quality issues. The frosting solution in this invention is highly efficient, stable, and can be used for extended periods, improving production efficiency, reducing production costs, and enhancing the quality stability of glass frosting products. Detailed Implementation

[0029] Preferably, the AG glass is purchased from Rainbow Group Special Glass Co., Ltd., with specifications of 1520*955*1.1mmCG01PRO+, and the water carrying capacity of the AG glass is 0.05~0.15 kg per square meter.

[0030] In the embodiments and comparative examples of the present invention, when the glass is transported to the frosting machine in an inclined manner for frosting, AG glass is obtained.

[0031] The sandblasting machine was purchased from Weiliuda Machinery Equipment Co., Ltd., model: AG line.

[0032] In the following embodiments, an acid-resistant film is applied to the glass surface that does not require frosting before frosting. After frosting, the acid-resistant film is removed. Unless otherwise specified, the raw materials added to the frosting solution in the following embodiments are by weight parts.

[0033] Example 1

[0034] By mass ratio, 17 parts water, 5 parts ethylene glycol, 24 parts ammonium bifluoride, 10 parts ammonium fluoride, and 7 parts calcium fluoride were pre-stirred at 60 rpm for 20 min until homogeneous. Then, 6.4 parts silica, 9.2 parts ferric citrate, 12 parts potassium nitrate, 8 parts potassium fluoride, and 1.4 parts hexadecyltrimethylammonium bromide (a cationic surfactant) were added. The mixture was then placed in a sealed container and aged at 50°C for 32 h. During aging, the mixture was stirred for 30 min every 4 hours to promote the full reaction and fusion of the components in the frosting solution, thus preparing 400 kg of frosting solution #1.

[0035] Each piece of glass is tilted at a 3.5° angle, and the frosting time is 70 seconds.

[0036] Example 2

[0037] Compared to Example 1, the difference is that ethylene glycol is replaced with trimethylolpropane.

[0038] The mass ratio of water to trimethylolpropane is 16:6:24:10:6.4:6:10:10:1.6.

[0039] Each piece of glass is tilted at a 4° angle, and the frosting time is 60 seconds.

[0040] With other conditions remaining unchanged, prepare 400 kg of frosting solution #2.

[0041] Example 3

[0042] The difference from Example 1 is that hexadecyltrimethylammonium bromide is replaced with hexadecyltrimethylammonium chloride.

[0043] The mass ratio of 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.

[0044] Each piece of glass is tilted at a 3° angle, and the frosting time is 65 seconds.

[0045] With other conditions remaining unchanged, prepare 400 kg of frosting solution #3.

[0046] Example 4

[0047] Compared to Example 1, the difference is that ethylene glycol is replaced with diethylene glycol, and ferric citrate is replaced with ferric acetate, while other conditions remain unchanged.

[0048] The mass ratio of water to diethylene glycol to ammonium bifluoride to ammonium fluoride to calcium fluoride to silicon dioxide to ferric acetate to potassium nitrate to potassium fluoride to cetyltrimethylammonium chloride is 16:5:25:10:8:5:9:13:8:1.

[0049] Each piece of glass is tilted at a 5° angle, and the frosting time is 65 seconds.

[0050] With other conditions remaining unchanged, prepare 400 kg of frosting solution #4.

[0051] Comparative Example 1

[0052] Compared with Example 1, the difference is that ethylene glycol is not added, while other conditions remain unchanged, and 400 kg of frosting solution #5 is prepared.

[0053] Comparative Example 2

[0054] Compared with Example 1, the difference is that the cationic surfactant cetyltrimethylammonium bromide was not added, and other conditions remained unchanged, to obtain 400 kg of frosting solution #6.

[0055] Comparative Example 3

[0056] Compared with Example 1, the difference is that ferric citrate is replaced with ferric nitrate to prepare 400kg of frosting solution #7.

[0057] Comparative Example 4

[0058] Compared with Example 1, the difference is that ferric citrate is replaced with ferric chloride to prepare 400kg of frosting solution #8.

[0059] Comparative Example 5

[0060] Compared with Example 1, the difference is that no pre-stirring is performed. Ethylene glycol, ammonium bifluoride, ammonium fluoride, calcium fluoride, silicon dioxide, ferric citrate, potassium nitrate, potassium fluoride, and hexadecyltrimethylammonium bromide are directly mixed, aged, and stirred. After filtration, there are particulate substances, the solution is paste-like, and a uniform frosting solution cannot be obtained.

[0061] The performance tests of the frosting solutions prepared in Examples 1-4 and Comparative Examples 1-5 are shown in Table 1 below:

[0062]

[0063] The measuring instruments and models used for the measurement parameters in Table 1 above are shown in Table 2 below:

[0064] Table 2

[0065]

[0066] The above data were obtained using conventional testing methods in this field.

Claims

1. A method for preparing a glass frosting solution, characterized in that, Includes the following steps: After pre-stirring water, polyhydroxy alcohol, ammonium fluoride, ammonium fluoride and calcium fluoride evenly, silicon dioxide, iron salt, potassium nitrate, potassium fluoride and cationic surfactant are added, and the mixture is sealed and matured by stirring to obtain glass frosting solution. The iron salt is one of ferric acetate and ferric citrate; In the glass frosting solution, by mass ratio, ammonium bifluoride: ammonium fluoride: iron salt: calcium fluoride: silicon dioxide: polyhydroxy 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.

2. The method for preparing a glass frosting solution according to claim 1, characterized in that, The polyhydroxy alcohol is one or more of ethylene glycol, diethylene glycol, and trimethylolpropane.

3. The method for preparing a glass frosting solution according to claim 1, characterized in that, The silica is micron-sized silica with a particle size of 3~100 μm.

4. The method for preparing a glass frosting solution according to claim 1, characterized in that, The curing temperature is 45℃~55℃.

5. The method for preparing a glass frosting solution according to claim 1, characterized in that, The ripening time is 24~32 hours.

6. The method for preparing a glass frosting solution according to claim 1, characterized in that, The cationic surfactant is either hexadecyltrimethylammonium bromide or hexadecyltrimethylammonium chloride.

7. The application of the frosting solution prepared by the preparation method according to any one of claims 1 to 6 in the preparation of AG glass.

8. The application according to claim 7, characterized in that, The specific preparation method for preparing AG glass using frosting solution also includes the following steps; AG glass is obtained by frosting glass sheets at an angle.

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