A kind of frosting powder for etching AG glass produced by atomization spraying method and its preparation method and use method

CN118084339BActive Publication Date: 2026-10-27XINXIANG ANJILAI NEW MATERIAL CO LTD +1
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Patent Information

Application Number
CN202410099784.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-24
Publication Date
2026-10-27
Estimated Expiration
2044-01-24

AI Technical Summary

Technical Problem

[0006]为了解决现有的AG玻璃生产采用喷涂法涂层易剥落、耐磨性能差,采用常规蚀刻法工艺复杂、良率低等技术问题,本发明提供一种用于雾化喷涂法生产蚀刻AG玻璃的蒙砂粉及其制备方法和应用,本发明将蒙砂粉和水配成透明的蚀刻液,通过喷涂法的工艺设备实现蚀刻AG玻璃的生产,可以满足市场需求

Benefits of technology

1、本发明制备的AG玻璃耐候性强,AG玻璃的粗糙度大小可以控制在0.03-3.0μm,通过该种工艺生产的AG玻璃表面效果好,硬度高(莫氏硬度为5.5),质量稳定,适合批量化生产。

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Abstract

The application provides a kind of frosting powder for etching AG glass produced by atomization spraying method and its preparation method and use method, and the frosting powder is composed of one or more components of a plurality of substances including ammonium fluoride, ammonium hydrogen fluoride, ammonium sulfate, high molecular glue powder, sorbitol, citric acid, sucrose, carbomer and the like.The use method includes: adding one or more of a plurality of substances including pure water, diethylene glycol butyl ether, glycerol, phosphoric acid, hydrofluoric acid and the like in the batching tank.Add the frosting powder to mature, after the end of maturation, take the supernatant, which is the etching liquid;The etching liquid is uniformly sprayed onto the glass surface by low-pressure atomization spray gun, to ensure that the etching liquid sprayed onto the glass surface forms a uniform water film;The etching liquid reacts on the glass surface for 5-350 seconds, and the AG glass finished product is obtained after treatment.The AG glass prepared by the application has strong weather resistance, good surface effect, high hardness, scratch resistance and stable quality, and is suitable for mass production.
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Description

Technical Field

[0001] This invention relates to the field of glass surface treatment technology, specifically to a frosting powder for producing etched AG glass by atomization spraying method, and its preparation and application methods. Background Technology

[0002] AG glass production methods include spraying, etching, sandblasting, and coating.

[0003] The spraying method for AG glass involves applying nano-silica coating to the glass surface using spraying equipment, creating a coating layer to achieve an anti-glare effect. In AG glass prepared by spraying, the silica in the coating is bonded to the glass through molecular bonds, resulting in poor weather resistance and scratch resistance, primarily limiting its use to the low-end market. According to industry insiders, AG glass prepared by spraying has several unsatisfactory aspects during use. Firstly, environmental and usage factors can cause the coating to peel off. Secondly, the coating's abrasion resistance is poor; a steel wire ball rubbing test only yields about 4856 cycles (approximately 5000 cycles), which is three times less abrasion resistant than chemically etched AG glass.

[0004] Etching involves using hydrofluoric acid to etch glass, creating uneven, dotted surfaces that generate diffuse reflection and reduce the glass's reflectivity. Because the AG glass produced by etching is formed by etching the glass surface with hydrofluoric acid, the AG film is strong, has good weather resistance, and is highly scratch-resistant, making it very popular in the market.

[0005] Currently, AG glass etching production methods include the immersion method, the horizontal curtain method, the horizontal curtain method combined with multi-pipe spraying, and the oblique curtain method. The immersion method uses multiple underground PVC tanks with overhead cranes. The frosting and polishing solutions are both placed in the PVC tanks. The glass is mounted on the cranes and undergoes processes such as water washing, acid washing, water washing, frosting, water washing, hydrofluoric acid polishing, water washing, cleaning machine washing, and drying to produce AG glass. This method is relatively rudimentary, generates a lot of wastewater, the workshop cannot be completely sealed, and waste gas treatment is incomplete, polluting the environment. Furthermore, the solids in the frosting solution fall downwards during the immersion process, scratching the glass surface and leaving marks. These scratches are still visible after the AG glass is polished and thinned. Therefore, this process can only produce low-end AG glass and is currently used by small companies. The horizontal curtain method is a type of fully automated production line. This method uses a horizontal production line where the chemicals pass through a curtain fabric. The equipment has good sealing and a good production environment, but the equipment is complex and expensive, making it difficult for small and medium-sized manufacturers to afford. Currently, this process is mainly used by large companies. A fatal flaw of this process is the significant impact of the frosting solution as the glass passes through the curtain. The frosting solution contains a large number of undissolved crystals, causing defects such as swirl marks, scratches, and tear ducts on the frosted surface, resulting in a low yield. The horizontal curtain combined with multi-pipe spraying process involves the glass, after being cleaned and dewatered, quickly passing through a chemical curtain and then entering a spray chamber. The spray chamber contains a row of six PVC pipes with a diameter of 2-4 cm, spaced 10-30 cm apart. These pipes are fixed to a guide rail and reciprocate along the rail during operation. The frosting solution is sprayed onto the glass surface via a pump, plastic hoses, and PVC pipes. The disadvantages of this method are that the impact of the chemical solution is too great, easily forming swirl marks on the glass surface. Furthermore, if the forward speed of the glass and the reciprocating oscillation speed of the six spray pipes are not properly matched, defects such as S-shaped patterns can easily appear on the glass surface. The oblique curtain method and the horizontal curtain method are similar in process, except for the frosting section. In this method, the frosting section is oblique, with an inclination of approximately 10 degrees, and 3-5 curtains are used for fabric application. The subsequent polishing section is the same. The disadvantages are similar to those of the horizontal curtain method. Furthermore, the above-mentioned etching methods for producing AG glass are all wet processes, meaning a water film is applied to the glass surface before frosting liquid is applied and etching begins. If these processes are combined with currently available mainstream frosting powders, and the glass is etched after surface drying, the result is that large areas of the glass are not etched, making it impossible to obtain a good AG glass product. Summary of the Invention

[0006] To address the technical problems of easy peeling and poor wear resistance of coatings in existing AG glass production methods, such as the complexity and low yield of conventional etching methods, this invention provides a frosting powder for producing etched AG glass using atomized spraying, its preparation method, and its application. This invention mixes the frosting powder with water to form a transparent etching solution, which is then used in a spraying process to produce etched AG glass, thus meeting market demands.

[0007] The present invention adopts the following technical solution: A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances in parts by weight: 5-15 parts ammonium fluoride, 40-55 parts ammonium bifluoride, 1-5 parts ammonium sulfate, 1-7 parts polymer powder, 0-30 parts sorbitol, 5-20 parts citric acid, 0-25 parts sucrose, and 1-5 parts carbomer.

[0008] Furthermore, the frosting powder is composed of the following substances in parts by weight: 5-10 parts ammonium fluoride, 40-55 parts ammonium bifluoride, 3-5 parts ammonium sulfate, 5 parts polymer powder, 5-20 parts sorbitol, 10-20 parts lemon, 3-15 parts sucrose, and 2 parts carbomer.

[0009] Furthermore, the polymer powder is modified cellulose.

[0010] Furthermore, the modified cellulose is microcrystalline cellulose or xanthan gum.

[0011] A method for preparing frosting powder for producing etched AG glass using an atomized spraying method includes the following steps: Step 1-1: Weigh out the ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the weight proportions described in claim 1, add them to a mixing mixer and stir. After stirring evenly, pulverize them with a Raymond mill to obtain component A. Component A is packaged separately. Steps 1-2: Weigh out the polymer powder, sorbitol, citric acid, sucrose, and carbomer according to the weight proportions described in claim 1, put them into a mixer and stir for 20-40 minutes to obtain component B. Component B is packaged separately. Steps 1-3: The total amount of each substance in the frosting powder according to claim 1 is 100 parts, which is divided into two components, A and B.

[0012] Furthermore, in step 1-1, the mixing time for adding ammonium fluoride, ammonium bifluoride, and ammonium sulfate into the mixing mixer is 20-40 minutes.

[0013] Furthermore, the particle size of the material pulverized using the Raymond mill in step 1-1 is less than or equal to 80 mesh.

[0014] A method for using frosting powder for producing etched AG glass by atomized spraying, wherein the method employs a dry process, specifically, after the glass is cleaned and dried, the aforementioned frosting powder for producing etched AG glass by atomized spraying or the frosting powder prepared by the aforementioned method for producing etched AG glass by atomized spraying is used for etching.

[0015] Furthermore, the method of use specifically includes the following steps: Step 2-1: Preparation of etching solution: Add 50-150 kg of purified water, 0-60 kg of diethylene glycol butyl ether, 0-150 kg of glycerol, 0-30 kg of phosphoric acid, and 0-15 kg of hydrofluoric acid to a mixing tank. Start stirring, then add 25-150 kg of frosting powder. Begin aging at room temperature for 65-80 hours. At the beginning of aging, the stirring speed is 1800-2200 rpm. After half an hour, reduce the stirring speed to 70-90 rpm and continue stirring during aging. After aging, stop stirring and wait for the temperature of the frosting solution to return to room temperature and clarify naturally. Take the supernatant, which is the etching solution. Furthermore, the room temperature curing time is 72 hours, the stirring speed is 2000 rpm at the beginning of curing, and the stirring speed is reduced to 80 rpm after half an hour; The phosphoric acid used in step 2-1 is industrial-grade phosphoric acid with a concentration of approximately 85%; the hydrofluoric acid is industrial-grade with a concentration of approximately 55%.

[0016] Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is sprayed evenly onto the glass surface through an atomizing spray gun, preferably a low-pressure atomizing spray gun (the air pressure of the low-pressure spray gun is 0.1-0.3 MPa, while the air pressure of the ordinary spray gun is 0.4-0.6 MPa). The air-liquid ratio is adjusted so that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 5-350 seconds. The solution is then recovered. The glass is then washed with water, polished with hydrofluoric acid, washed and dried, and inspected to obtain the finished AG glass product.

[0017] The nozzle of the low-pressure spray gun used in this invention is made of 316L, which has excellent corrosion resistance.

[0018] Furthermore, the gas-liquid ratio is 1000-1500:1.

[0019] The etching solution prepared by this invention has almost completely dissolved all components, resulting in a transparent solution that can be atomized and sprayed using a low-pressure atomizing spray gun. In contrast, most ordinary etching solutions are suspensions, and frosting solutions have a high solid content with a solid-liquid ratio of around 2:1, which easily clogs the spray gun and makes them unusable.

[0020] The commonly used method for producing AG glass is the curtain etching process. The etching solution is pumped to a cloth feeder, then forms a curtain through a guide plate. The glass quickly passes through the curtain, coating the glass surface with the etching solution. After the reaction, it is rinsed off with water. The disadvantage of this method is that the impact force of the etching solution from the curtain is too great, easily creating scratches, tear tracks, and other defects on the glass surface. The atomization method, on the other hand, atomizes the etching solution into very small water droplets, which then fall onto the glass surface, forming a uniform etching solution water film. This avoids the aforementioned defects. Furthermore, this invention allows etching to be performed after the glass surface is dried, preventing the etching solution from being diluted. The etching solution can be recovered simply by tilting the glass.

[0021] Existing AG glass prepared by spraying has a coating layer on the surface, which has poor weather resistance, poor UV resistance, and the coating is easy to peel off in high-salt and high-humidity environments, and is not scratch-resistant; while the AG glass prepared by this invention has strong weather resistance.

[0022] Compared with the prior art, the present invention has the following technical effects: 1. The AG glass prepared by this invention has strong weather resistance, and the roughness of the AG glass can be controlled within 0.03-3.0μm. The AG glass produced by this process has good surface effect, high hardness (Mohs hardness of 5.5), stable quality, and is suitable for mass production.

[0023] 2. Existing AG glass production mainly employs a wet process, namely glass washing - acid washing - water washing - water control - etching solution coating. This invention, however, uses a dry process: glass washing - acid washing - water washing - drying - etching solution coating. This invention has the following advantages: (1) The AG glass prepared by the present invention has uniform surface parameters.

[0024] The wet process uses a tilted water control process, resulting in different thicknesses of the water film on the upper and lower surfaces of the glass. When the etching solution is applied, the uneven thickness of the water film causes a significant difference in the roughness of the upper and lower surfaces after etching. The lower part, where the water film is thicker, has a larger roughness, while the upper part, where the water film is thinner, has a smaller roughness, which affects product quality.

[0025] (2) The solution of the present invention is stable.

[0026] The dry process of this invention, because the glass surface is dried and water-free, results in a slow and stable change in the concentration of the recycled etching solution during production. In contrast, the wet process, because water remains on the glass surface, dilutes the etching solution, causing the recycled etching solution to be diluted further, gradually decreasing its concentration and affecting its stability, requiring continuous adjustments.

[0027] (3) The AG glass prepared by the present invention has good surface effect.

[0028] Wet etching processes mostly use curtain-type or multi-tube reciprocating oscillating fabrics, resulting in high chemical impact and easily causing defects such as chemical wash marks, tear tracks, and bright lines on the glass surface. In contrast, the atomization process fixes multiple low-pressure spray guns on a single axis, spaced 10-30 cm apart. During operation, the low-pressure spray guns atomize the etching solution into tiny water droplets. By adjusting the gas-liquid ratio of the spray guns, the etching solution sprayed from each gun forms fan-shaped sprays that intersect each other, creating a complete fog screen. The glass passes uniformly under this fog screen, and the etching solution falls onto the glass surface, forming a uniform water film. Therefore, the etched surface is uniform and defect-free.

[0029] 3. The etching solution prepared by this invention is a transparent solution that can be atomized and sprayed using a low-pressure spray gun. Most etching solutions currently available on the market, formulated with frosting powder, are suspensions with a high solid content, which easily clogs the spray gun and renders them unusable. Detailed Implementation

[0030] The present invention will be further described below with reference to specific embodiments.

[0031] Example 1 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 5 kg ammonium fluoride, 40 kg ammonium bifluoride, 3 kg ammonium sulfate, 5 kg microcrystalline cellulose, 20 kg sorbitol, 10 kg citric acid, 15 kg sucrose, and 2 kg carbomer, totaling 100 kg.

[0032] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out the ammonium fluoride, ammonium bifluoride, and ammonium sulfate according to the above weights, add them to a mixing mixer and stir for 30 minutes. Then, use a Raymond mill to pulverize the mixture until the particle size is 80 mesh to obtain component A. Component A is packaged separately. Steps 1-2: Weigh out microcrystalline cellulose, sorbitol, citric acid, sucrose, and carbomer according to the above weight in kilograms, add them to a mixer and stir for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0033] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 80 kg of purified water, 10 kg of diethylene glycol butyl ether, and 90 kg of glycerol to the mixing tank, start stirring, and slowly add 100 kg of frosting powder. Start aging at room temperature for 72 hours. At the beginning of aging, the stirring speed is 2000 rpm. After half an hour, the stirring speed is reduced to 80 rpm. Stirring is maintained during aging. After aging, stop stirring and let it settle naturally. Some undissolved crystals will settle to the bottom of the tank. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 20 seconds, and the glass is tilted to recover the etching solution. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0034] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 100-110 GU, a roughness RA of 0.04-0.05 μm, and a uniform AG surface without defects.

[0035] Example 2 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 5 kg ammonium fluoride, 55 kg ammonium bifluoride, 3 kg ammonium sulfate, 5 kg microcrystalline cellulose, 10 kg sorbitol, 10 kg citric acid, 10 kg sucrose, 2 kg carbomer, totaling 100 kg.

[0036] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the above weights and add them to a mixing mixer. Stir for 30 minutes, then pulverize with a Raymond mill. The particle size of the pulverized material is 80 mesh, which is component A. Component A is packaged separately. Steps 1-2: Weigh out microcrystalline cellulose, sorbitol, citric acid, sucrose, and carbomer according to the above weight (in kilograms) and put them into a mixer for stirring for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0037] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 100 kg of purified water, 10 kg of diethylene glycol butyl ether, 60 kg of glycerol, and 8 kg of phosphoric acid to the mixing tank. Start stirring and slowly add 100 kg of frosting powder. Start aging at room temperature for 72 hours. The stirring speed is 2000 rpm at the beginning of aging. After half an hour, the stirring speed is reduced to 80 rpm. Stirring is maintained during aging. After aging, stop stirring and let it settle naturally. A small amount of undissolved crystals will settle to the bottom of the tank. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 30 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0038] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 100-110 GU, a roughness RA of 0.1-0.2 μm, and a uniform AG surface without defects.

[0039] Example 3 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 10 kg ammonium fluoride, 50 kg ammonium bifluoride, 5 kg ammonium sulfate, 5 kg xanthan gum powder, 5 kg sorbitol, 13 kg citric acid, 10 kg sucrose, 2 kg carbomer, totaling 100 kg.

[0040] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the above weights and add them to a mixing mixer. Stir for 30 minutes, then pulverize with a Raymond mill. The particle size of the pulverized material is 80 mesh, which is component A. Component A is packaged separately. Steps 1-2: Weigh out xanthan gum powder, sorbitol, citric acid, sucrose, carbomer, etc. according to the above weight in kilograms, put them into a mixer and stir for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0041] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 110 kg of purified water, 10 kg of diethylene glycol butyl ether, 50 kg of glycerol, 8 kg of phosphoric acid, and 4 kg of hydrofluoric acid to the mixing tank. Start stirring and slowly add 100 kg of frosting powder. Start aging at room temperature for 72 hours. The stirring speed is 2000 rpm at the beginning of aging. After half an hour, the stirring speed is reduced to 80 rpm. Stirring is maintained during aging. After aging, stop stirring and let it settle naturally. A small amount of undissolved crystals will settle to the bottom of the tank. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 60 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0042] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 100-110 GU, a roughness RA of 0.2-0.3 μm, and a uniform AG surface without defects.

[0043] Example 4 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 10 kg ammonium fluoride, 45 kg ammonium bifluoride, 5 kg ammonium sulfate, 5 kg microcrystalline cellulose, 5 kg sorbitol, 15 kg citric acid, 13 kg sucrose, and 2 kg carbomer, totaling 100 kg.

[0044] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the above weights and add them to a mixing mixer. Stir for 30 minutes, then pulverize with a Raymond mill. The particle size of the pulverized material is 80 mesh, which is component A. Component A is packaged separately. Steps 1-2: Weigh out the polymer powder, sorbitol, citric acid, sucrose, and carbomer according to the above weight in kilograms, put them into a mixer and stir for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0045] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 120 kg of purified water, 10 kg of diethylene glycol butyl ether, 40 kg of glycerol, 4 kg of phosphoric acid, and 4 kg of hydrofluoric acid to the mixing tank. Start stirring and slowly add 100 kg of frosting powder. Start aging at room temperature for 72 hours. The stirring speed is 2000 rpm at the beginning of aging. After half an hour, the stirring speed is reduced to 80 rpm. Stirring is maintained during aging. After aging, stop stirring and let it settle naturally. A small amount of undissolved crystals will settle to the bottom of the tank. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 120 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0046] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 100-110 GU, a roughness RA of 0.35-0.45 μm, and a uniform AG surface without defects.

[0047] Example 5 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 10 kg ammonium fluoride, 55 kg ammonium bifluoride, 5 kg ammonium sulfate, 5 kg microcrystalline cellulose, 10 kg sorbitol, 10 kg citric acid, 3 kg sucrose, and 2 kg carbomer, totaling 100 kg.

[0048] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the above weights and add them to a mixing mixer. Stir for 30 minutes, then pulverize with a Raymond mill. The particle size of the pulverized material is 80 mesh, which is component A. Component A is packaged separately. Steps 1-2: Weigh out microcrystalline cellulose, sorbitol, citric acid, sucrose, and carbomer according to the above weight in kilograms, put them into a mixer and stir for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0049] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 150 kg of purified water, 10 kg of diethylene glycol butyl ether, and 8 kg of phosphoric acid to the mixing tank. Start stirring, then slowly add 100 kg of frosting powder. Begin aging at room temperature for 72 hours. At the beginning of aging, the stirring speed is 2000 rpm. After half an hour, reduce the stirring speed to 80 rpm, and continue stirring throughout the aging process. After aging is complete, stop stirring and allow the solution to settle naturally. A small amount of undissolved crystals will settle to the bottom of the tank. Collect the supernatant, which is the etching solution. Step 2-2: The glass is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 180 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0050] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 60-80 GU, a roughness RA of 0.5-0.8 μm, and a uniform AG surface without defects.

[0051] Example 6 A frosting powder for producing etched AG glass by atomization spraying method, the frosting powder is composed of the following substances by weight: 10 kg ammonium fluoride, 55 kg ammonium bifluoride, 5 kg ammonium sulfate, 5 kg microcrystalline cellulose, 15 kg citric acid, 8 kg sucrose, 2 kg carbomer, totaling 100 kg.

[0052] The preparation method of the above-mentioned frosting powder includes the following steps: Step 1-1: Weigh out ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the above weights and add them to a mixing mixer. Stir for 30 minutes, then pulverize with a Raymond mill. The particle size of the pulverized material is 80 mesh, which is component A. Component A is packaged separately. Steps 1-2: Weigh out microcrystalline cellulose, citric acid, sucrose, and carbomer according to the above weight in kilograms, put them into a mixer and stir for 30 minutes to obtain component B. Component B is packaged separately. Components A and B are packaged separately and then mixed to obtain 100 kg of frosting powder before use.

[0053] The method of using the above-mentioned frosting powder includes the following steps: Step 2-1: Preparation of etching solution: Add 150 kg of purified water, 10 kg of diethylene glycol butyl ether, and 10 kg of phosphoric acid to the mixing tank, start stirring, and slowly add 100 kg of frosting powder. Start aging at room temperature for 72 hours. At the beginning of aging, the stirring speed is 2000 rpm. After half an hour, the stirring speed is reduced to 80 rpm. Stirring is maintained during aging. After aging, stop stirring and let it settle naturally. A small amount of undissolved crystals will settle to the bottom of the tank. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 300 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0054] Upon inspection, the AG glass product prepared in this embodiment has a gloss of 40-50, a roughness RA of 0.8-1.2μm, and a uniform AG surface without defects.

[0055] Comparative Example 1 Purchase frosting powder, model NC-01, from a manufacturer on the market for use in the production of etched AG glass on a horizontal curtain-type automated line. The usage includes the following steps: Step 2-1: Preparation of etching solution: Add 120 kg of purified water, 10 kg of diethylene glycol butyl ether, 40 kg of glycerol, 4 kg of phosphoric acid, and 4 kg of hydrofluoric acid to the mixing tank. Start stirring, then slowly add 100 kg of the above-mentioned NC-01 frosting powder and start stirring again. At the beginning of curing, the stirring speed is 2000 rpm. After half an hour, the stirring speed is reduced to 80 rpm. Curing is carried out for 72 hours, with stirring maintained during curing. After curing is completed, stop stirring and allow it to cure naturally. Many undissolved crystals will settle to the bottom of the tank. Take the supernatant for later use.

[0056] Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 60 seconds, and the chemical solution is recovered. Then, the glass undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

[0057] Upon inspection, all AG glass prepared in this embodiment was found to be defective; most of the glass surface was not etched, while some had very shallow etching.

[0058] Comparative Example 2 Purchase frosting powder, model NC-01, from a manufacturer on the market for use in the production of etched AG glass on a horizontal curtain-type automated line. The usage includes the following steps: Includes the following steps: Step 2-1: Preparing the etching solution: Add 120 kg of purified water, 10 kg of diethylene glycol butyl ether, 40 kg of glycerol, 4 kg of phosphoric acid, and 4 kg of hydrofluoric acid to a mixing tank. Start stirring, then slowly add 100 kg of the above-mentioned NC-01 frosting powder. Initially, the stirring speed is 2000 rpm. After half an hour, reduce the stirring speed to 80 rpm. Allow to mature for 72 hours, maintaining stirring throughout the maturation process. After maturation, stop stirring and allow to mature naturally. Many undissolved crystals will settle to the bottom of the tank. When using, start the stirrer to mix the solution thoroughly and set aside.

[0059] Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After the glass is washed with water, acid washed, washed with water, washed with deionized water and dried, it enters the spraying chamber. The etching solution prepared in step 2-1 is sprayed through a low-pressure atomizing spray gun. As a result, the solution quickly clogs the low-pressure spray gun and the spraying cannot be completed.

[0060] Comparative Examples 1 and 2 both used the same manufacturer and model of frosting powder. The difference between Comparative Examples 1 and 2 was that in Comparative Example 1, the supernatant was discarded after preparing the etching solution for use in step 2-1, while in Comparative Example 2, the etching solution was a solid-liquid mixture, which was stirred evenly before use in step 2-1. The experimental results showed that when only the supernatant was used to prepare the etching solution with the frosting powder and sprayed using a low-pressure atomizing spray gun, all the prepared AG glass was defective. Furthermore, directly using the solid-liquid mixture of etching solution for low-pressure atomizing spraying would clog the nozzle, making it impossible to complete the experiment.

[0061] Comparative Example 3 Purchase frosting powder, model HS-06P, from a manufacturer on the market for use in the production of etched AG glass on a horizontal curtain-type automated production line. The usage includes the following steps: Step 2-1: Preparation of etching solution: Add 110 kg of purified water, 10 kg of diethylene glycol butyl ether, 50 kg of glycerol, 8 kg of phosphoric acid, and 4 kg of hydrofluoric acid to the mixing tank. Start stirring and slowly add 100 kg of the above-mentioned HS-06P frosting powder. The stirring speed is 2000 rpm at the beginning. After half an hour, the stirring speed is reduced to 80 rpm. Let it mature for 72 hours, keeping the stirring constant during maturation. After maturation, stop stirring and let it mature naturally. Many undissolved crystals will settle to the bottom of the tank. Take the supernatant for later use.

[0062] Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through a low-pressure atomizing spray gun. The air-liquid ratio is adjusted, with an air usage of 60L / min and a chemical usage of 50mL / min, to ensure that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 90 seconds, the chemical solution is recovered, and then the glass is washed, polished, and inspected to obtain the finished AG glass product.

[0063] Upon inspection, all AG glass prepared in this embodiment was found to be defective; most of the glass surface was not etched, while some had very shallow etching.

[0064] Comparative Example 4 Purchase frosting powder, model HS-06P, for etched AG glass used in multi-pipe spraying from a certain manufacturer. The usage includes the following steps: Step 2-1: Preparation of etching solution: Add 110 kg of purified water, 10 kg of diethylene glycol butyl ether, 50 kg of glycerol, 8 kg of phosphoric acid, and 4 kg of hydrofluoric acid to the mixing tank. Start stirring, then slowly add 100 kg of the above-mentioned HS-06P frosting powder. Initially, the stirring speed is 2000 rpm. After half an hour, reduce the stirring speed to 80 rpm. Allow to mature for 72 hours, maintaining stirring throughout the maturation process. After maturation, stop stirring and allow to mature naturally. Many undissolved crystals will settle to the bottom of the tank. When using, start stirring to mix the solution thoroughly and set aside.

[0065] Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 1 is used for spraying through a low-pressure atomizing spray gun. As a result, the solution quickly clogs the low-pressure spray gun, making it impossible to complete the spraying. The experiment failed.

[0066] Comparative Examples 3 and 4 both used the same manufacturer and model of frosting powder. The difference between Comparative Examples 3 and 4 was that in Comparative Example 3, the supernatant was discarded after preparing the etching solution for use in step 2-1, while in Comparative Example 4, the etching solution was a solid-liquid mixture, which was stirred evenly before use in step 2-1. The experimental results show that when only the supernatant was used to prepare the etching solution with the frosting powder and sprayed using a low-pressure atomizing spray gun, all the prepared AG glass was defective. Furthermore, directly using the solid-liquid mixture of etching solution for low-pressure atomizing spraying would clog the nozzle, making it impossible to complete the experiment.

[0067] The embodiments described above are merely preferred embodiments of the present invention and are only used to explain the present invention. They are not intended to limit the scope of the present invention. For those skilled in the art, other implementation methods can be easily made by substitution or modification based on the technical content disclosed in this specification. Therefore, all changes and improvements made to the principles and process conditions of the present invention should be included in the scope of the patent application of the present invention.

Claims

1. A frosting powder for producing etched AG glass using an atomization spraying method, characterized in that, The frosting powder is composed of the following substances in parts by weight: 5-15 parts ammonium fluoride, 40-55 parts ammonium bifluoride, 1-5 parts ammonium sulfate, 1-7 parts polymer powder, 0-30 parts sorbitol, 5-20 parts citric acid, 0-25 parts sucrose, and 1-5 parts carbomer. The polymer powder is modified cellulose, and the modified cellulose is microcrystalline cellulose.

2. The frosting powder for producing etched AG glass by atomization spraying method according to claim 1, characterized in that, The frosting powder is composed of the following substances in parts by weight: 5-10 parts ammonium fluoride, 40-55 parts ammonium bifluoride, 3-5 parts ammonium sulfate, 5 parts polymer powder, 5-20 parts sorbitol, 10-20 parts citric acid, 3-15 parts sucrose, and 2 parts carbomer.

3. The method for preparing frosting powder for producing etched AG glass by atomization spraying according to claim 1, characterized in that, Includes the following steps: Step 1-1: Weigh out the ammonium fluoride, ammonium bifluoride and ammonium sulfate according to the weight proportions described in claim 1, add them to a mixing mixer and stir. After stirring evenly, pulverize them with a Raymond mill to obtain component A. Component A is packaged separately. Steps 1-2: Weigh out the polymer powder, sorbitol, citric acid, sucrose, and carbomer according to the weight proportions described in claim 1, put them into a mixer and stir for 20-40 minutes to obtain component B. Component B is packaged separately. Steps 1-3: The total amount of each substance in the frosting powder according to claim 1 is 100 parts, which is divided into two components, A and B.

4. The method for preparing frosting powder for producing etched AG glass by atomization spraying according to claim 3, characterized in that, In step 1-1, the ammonium fluoride, ammonium bifluoride, and ammonium sulfate are added to the mixing mixer and stirred for 20 to 40 minutes.

5. The method for preparing frosting powder for producing etched AG glass by atomized spraying according to claim 3, characterized in that, The particle size of the material after being pulverized using a Raymond mill in step 1-1 is less than or equal to 80 mesh.

6. A method for using frosting powder in the production of etched AG glass by atomization spraying, characterized in that, Specifically, after the glass is cleaned and dried, the frosting powder prepared by the method of producing etched AG glass by atomization spraying as described in any one of claims 1 to 2 or the method of preparing frosting powder for producing etched AG glass by atomization spraying as described in any one of claims 3 to 5 is used for etching by atomization spraying.

7. The method of using frosting powder for producing etched AG glass by atomization spraying according to claim 6, characterized in that, The method of use specifically includes the following steps: Step 2-1: Preparation of etching solution: Add 50-150 kg of purified water, 0-60 kg of diethylene glycol butyl ether, 0-150 kg of glycerol, 0-30 kg of phosphoric acid, and 0-15 kg of hydrofluoric acid to a mixing tank. Start stirring, then add 25-150 kg of frosting powder. Begin aging at room temperature for 65-80 hours. At the beginning of aging, the stirring speed is 1800-2200 rpm. After half an hour, reduce the stirring speed to 70-90 rpm and continue stirring during aging. After aging, stop stirring and wait for the temperature of the frosting solution to return to room temperature and clarify naturally. Take the supernatant, which is the etching solution. Step 2-2: The glass tin surface is coated with a protective film and placed on the AG glass spraying production line. After water washing, acid washing, water washing, deionized water washing, and drying, the glass enters the spraying chamber. The etching solution prepared in Step 2-1 is evenly sprayed onto the glass surface through an atomizing spray gun. The gas-liquid ratio is adjusted so that the etching solution sprayed onto the glass surface forms a uniform water film. The etching solution reacts on the glass surface for 5-350 seconds. The solution is then recovered. The glass then undergoes water washing, hydrofluoric acid polishing, water washing and drying, and inspection to obtain the finished AG glass product.

8. The method of using frosting powder for producing etched AG glass by atomization spraying according to claim 7, characterized in that, The gas-liquid ratio is 1000-1500:1.

Citation Information

Patent Citations

  • Frosting etching composition and preparation method and application thereof

    CN115677229A