CN114516729A - Frosting liquid and preparation method thereof, frosted glass and glass cover plate - Google Patents
Frosting liquid and preparation method thereof, frosted glass and glass cover plate Download PDFInfo
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- CN114516729A CN114516729A CN202011314023.1A CN202011314023A CN114516729A CN 114516729 A CN114516729 A CN 114516729A CN 202011314023 A CN202011314023 A CN 202011314023A CN 114516729 A CN114516729 A CN 114516729A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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Abstract
The application discloses a frosting solution and a preparation method thereof, frosted glass and a glass cover plate, wherein the frosting solution comprises the following components in parts by weight: 39-62 parts of fluoride; 35-70 parts of fluorosilicate, wherein the fluorosilicate comprises potassium fluosilicate; 5-10 parts of ferrous salt; 34-58 parts of inorganic acid, wherein the inorganic acid comprises boric acid; 25-46 parts of organic acid, wherein the organic acid comprises methanesulfonic acid and citric acid; 6-18 parts of an additive; and 30-50 parts of water. In this application, fluorosilicate and ferrous ion generate the crystal adhesion of ferrous fluorosilicate on the glass surface, are favorable to improving the crystal appearance on frosting surface to citric acid, methanesulfonic acid and boric acid stabilize the pH valve of frosting liquid, are favorable to controlling frosting glass surface's growth, improve frosting glass's frosting effect.
Description
Technical Field
The invention relates to the technical field of glass surface treatment, in particular to a frosting liquid and a preparation method thereof, frosted glass and a glass cover plate.
Background
The glass has the unique advantages of good transparency, high mechanical strength, uniform texture, smooth surface and the like, and is widely applied to the industries of buildings, decorations, instruments, daily necessities, electronics and the like. The glass is applied to the electronic industries such as televisions, computers, mobile phones and the like in a super large scale, and an industrial production system of related industries is formed. However, due to the imperfection of glass product manufacture, high intensity light pollution is caused, so that the electronic product poses a threat to the eyesight health of people. At present, the method of glass frosting is adopted to eliminate the problem of light pollution of glass products and improve the hazy feeling of frosted glass so as to improve the aesthetic feeling of decoration, and corresponding frosting liquid is developed aiming at different cover plate glass materials.
The frosted glass processed by the existing frosting liquid has low roughness, high haze and low glass transmittance, and the frosted glass integrally shows the matte effect of low roughness and high haze, so that the frosted glass cannot be matched with a high-brightness glare membrane to achieve the actual glare effect.
Disclosure of Invention
In view of the above-mentioned drawbacks and deficiencies of the prior art, it is desirable to provide a frosting solution, a preparation method thereof, a frosted glass and a glass cover plate.
In a first aspect, the invention provides a frosting solution, which comprises the following components in parts by weight:
39-62 parts of fluoride;
35-70 parts of fluorosilicate, wherein the fluorosilicate comprises potassium fluosilicate;
5-10 parts of ferrous salt;
34-58 parts of inorganic acid, wherein the inorganic acid comprises boric acid;
25-46 parts of organic acid, wherein the organic acid comprises methanesulfonic acid and citric acid;
6-18 parts of an additive;
and 30-50 parts of water.
Alternatively, the fluoride includes at least one of magnesium fluoride, ammonium fluoride, sodium fluoride, ammonium bifluoride, potassium fluoride, and sodium bifluoride.
Optionally, the fluorosilicate further comprises at least one of ammonium fluorosilicate, sodium fluorosilicate, potassium fluorosilicate, magnesium fluorosilicate, iron fluorosilicate, and calcium fluorosilicate.
Optionally, the ferrous salt comprises ferrous sulfate and/or ferrous nitrate.
Optionally, the inorganic acid further comprises sulfuric acid and/or nitric acid.
Optionally, the organic acid further comprises oxalic acid.
Optionally, the additive comprises a thickener and/or dispersant; wherein the thickening agent comprises at least one of carboxymethyl cellulose and xanthan gum; the dispersant comprises at least one of diisobutyl naphthalene sulfonate, methylene dinaphthalene sodium sulfonate and deflocculant.
Optionally, the frosting solution further comprises 4-8 parts of calcium salt, wherein the calcium salt comprises calcium sulfate and/or calcium nitrate.
Preferably, the frosting solution comprises the following components in parts by weight:
15-24 parts of ammonium fluoride, 5-11 parts of magnesium fluoride, 19-27 parts of potassium hydrogen fluoride, 12-24 parts of ammonium fluosilicate, 5-10 parts of sodium fluosilicate, 6-11 parts of potassium fluosilicate, 5-10 parts of magnesium fluosilicate, 7-15 parts of ferric fluosilicate, 5-10 parts of ferrous sulfate and/or ferrous nitrate, 20-30 parts of nitric acid, 14-28 parts of boric acid, 15-26 parts of methanesulfonic acid, 10-20 parts of citric acid, 2-5 parts of a thickening agent and 4-11 parts of a dispersing agent.
In a second aspect, the present invention provides a method for preparing a frosting solution according to the first aspect, including:
adding the additive and the organic acid into water according to the weight ratio, and uniformly mixing to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I according to the weight ratio, and uniformly stirring to obtain a mixture II;
and adding the inorganic acid into the mixture II according to the weight ratio, and uniformly stirring to obtain the frosting liquid.
In a third aspect, the invention provides frosted glass, which is obtained by performing frosting treatment on glass by using the frosting liquid of the first aspect.
Alternatively, the frosted glass has a roughness of 1.0 μm to 3.0. mu.m.
Alternatively, the frosted glass has a haze of 40% to 80%.
In a fourth aspect, the present invention provides a glass cover plate, at least a portion of which is composed of the frosted glass of the third aspect.
The application provides a fluoride produces the fluorinion in solution in the frosting liquid, the fluorinion combines with hydrogen ion to generate hydrofluoric acid, hydrofluoric acid etches the glass surface, fluorosilicate and ferrous ion generate ferrous fluorosilicate's crystal adhesion on the glass surface, be favorable to improving the crystal appearance on frosting surface, and adopt citric acid, methanesulfonic acid and boric acid cooperation in this application, stabilize the pH valve of frosting liquid, be favorable to controlling the growth on frosting glass surface, make frosting glass demonstrate the flash point effect that the diamond is like.
Detailed Description
The present application will be described in further detail with reference to examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the invention are shown in the embodiments.
It should be noted that, in the present application, the embodiments and features of the embodiments may be combined with each other without conflict. The present application will be described in detail with reference to examples.
The prior art discloses a frosting liquid with the following mixture ratio: 6.5-9.6 parts of hydrofluoric acid, 2-6 parts of ammonium fluoride, 5.5-8 parts of ammonium bifluoride, 4-7 parts of water, 2-5 parts of sulfuric acid, 3-5.5 parts of sodium carbonate, 1-2.5 parts of silicon dioxide and 1-4 parts of calcium fluoride. The frosting solution has low hydrofluoric acid content, mild reaction and long frosting time; and the frosted product has low roughness and high haze, the roughness is 0.1-1 mu m, the haze is 80-100%, and the glass transmittance is low. The glass wholly appears for the low roughness high haze's of frosting back glass matt effect, and above characteristics lead to frosting back glass can't realize some through the cooperation high brightness dazzling light diaphragm and dazzle light effect.
Based on the above problems, the embodiment of the invention provides a frosting solution, which comprises the following components in parts by weight:
39-62 parts of fluoride;
35-70 parts of fluorosilicate, wherein the fluorosilicate comprises potassium fluosilicate;
5-10 parts of ferrous salt;
34-58 parts of inorganic acid, wherein the inorganic acid comprises boric acid;
25-46 parts of organic acid, wherein the organic acid comprises methanesulfonic acid and citric acid;
6-18 parts of an additive;
and 30-50 parts of water.
Fluoride in the frosting liquid provided by the invention generates fluoride ions in the solution, the fluoride ions and hydrogen ions are combined to generate hydrofluoric acid, the hydrofluoric acid etches the glass surface, crystals of fluorosilicate and ferrous ions which generate ferrous fluorosilicate are adhered to the glass surface, and the crystal morphology of the frosting surface is favorably improved.
The fluoride may be at least one of magnesium fluoride, hydrogen fluoride, ammonium fluoride, sodium fluoride, ammonium bifluoride, potassium fluoride, and sodium hydrogen fluoride; the fluorosilicate can be at least one of ammonium fluorosilicate, sodium fluorosilicate, potassium fluorosilicate, magnesium fluorosilicate, iron fluorosilicate and calcium fluorosilicate; the ferrous salt can be any one of ferrous sulfate, ferrous nitrate and ferrous chloride; the inorganic acid may be at least one of nitric acid, hydrochloric acid and sulfuric acid; the additives may be various dispersants, deflocculants and thickeners.
Preferably, the ferrous salt comprises ferrous sulfate and/or ferrous nitrate.
Preferably, the mineral acid further comprises sulfuric acid and/or nitric acid.
Preferably, the additive comprises a thickener and/or dispersant; wherein the thickening agent comprises at least one of carboxymethyl cellulose and xanthan gum; the dispersant comprises at least one of diisobutyl naphthalene sulfonate, methylene dinaphthalene sodium sulfonate and deflocculant. Wherein the deflocculant can be diatomaceous earth, tartrate, deflocculant D91(wgwin series auxiliary agent)
Preferably, the frosting solution also comprises 4 to 8 parts of calcium salt, and the calcium salt comprises calcium sulfate and/or calcium nitrate.
In a preferred embodiment, the frosting solution comprises the following components in parts by weight:
15-24 parts of ammonium fluoride, 5-11 parts of magnesium fluoride, 19-27 parts of potassium hydrogen fluoride, 12-24 parts of ammonium fluosilicate, 5-10 parts of sodium fluosilicate, 6-11 parts of potassium fluosilicate, 5-10 parts of magnesium fluosilicate, 7-15 parts of ferric fluosilicate, 4-8 parts of calcium sulfate, 5-10 parts of ferrous sulfate, 20-30 parts of nitric acid, 14-28 parts of boric acid, 15-26 parts of methanesulfonic acid, 10-20 parts of citric acid, 2-5 parts of a thickening agent (such as xanthan gum), 3-8 parts of methylene dinaphthalene sodium sulfonate (a diffusant NNO), 3-3 parts of an anti-flocculant D911 and 30-50 parts of water.
It should be noted that ammonium fluoride, magnesium fluoride, and potassium bifluoride function as an etchant for fluorine ions to provide water-soluble fluorine ions; fluorosilicate is used as a particle sanding agent and is attached to the surface of glass after etching reaction, and then a 'sand layer' is formed on the etched surface through chemical reaction; nitric acid is used as a hydrogen ion providing agent and is combined with fluorine ions to generate hydrofluoric acid, the hydrofluoric acid reacts with the surface of the glass to generate silicon fluoride gas, the silicon fluoride gas further reacts with the hydrofluoric acid to generate fluosilicate, the fluosilicate is combined with ferrous ions provided by ferrous salt in the frosting liquid, calcium ions provided by calcium salt are combined to generate precipitates, and the combination of the fluosilicate in the frosting liquid is favorable for improving the crystal morphology of the surface of the glass; the methanesulfonic acid, the citric acid and the boric acid are used as acidity regulators, can provide hydrogen ions, play a role in acidity regulation, can generate hydrofluoric acid with fluoride ions for etching reaction of glass, and simultaneously control the acidity degree and the etching efficiency of the etching solution, so that the problems that the reaction rate is too high, the hydrofluoric acid is volatile and extremely corrosive, prismatic crystal forms cannot be formed and the use is unsafe due to the fact that the hydrofluoric acid is directly added into the frosting solution are solved; boric acid can also be used as a surfactant, which is beneficial to forming uniform frosting on the surface of the glass; the xanthan gum in the additive is mainly used as a thickening agent, is matched with a diffusant NNO and a deflocculant D91 for use, can ensure that the frosting liquid has proper viscosity and fluidity after being cured in curing agent water, and ensures the uniformity and stability of the whole system.
The appearance of ammonium fluosilicate and potassium fluosilicate in the fluosilicate is spherical, the appearance of sodium fluosilicate is angular, the appearance of magnesium fluosilicate is rhombic or acicular, and the fluosilicate has great influence on the surface appearance of frosted glass and is beneficial to generating different crystal forms. Because of the existence of ferrous ions in the frosting solution, under the action of fluosilicate in the frosting solution, crystals of ferrous fluosilicate generated by the frosting solution in the frosting process are adhered to the surface of the glass, thereby being beneficial to improving the crystal morphology of the surface of the glass.
Wherein the weight ratio of the ammonium fluoride is 15-24 parts, such as: 15 parts, 17 parts, 18 parts, 20 parts, 22 parts, 23 parts and 24 parts; the weight ratio of the magnesium fluoride is 5-11 parts, for example: 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts and 11 parts; the weight ratio of the potassium bifluoride is 19-27 parts, for example: 19 parts, 20 parts, 22 parts, 23 parts, 24 parts, 26 parts and 27 parts; the weight ratio of the ammonium fluosilicate is 12-24 parts, for example: 12 parts, 13 parts, 15 parts, 17 parts, 20 parts, 22 parts and 24 parts; the weight ratio of the sodium fluosilicate is 5-10 parts, for example: 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10 parts; the weight ratio of the potassium fluosilicate is 6-11 parts, for example: 6 parts, 7 parts, 8 parts, 9 parts, 10 parts and 11 parts; the weight ratio of the magnesium fluosilicate is 5-10 parts, for example: 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10 parts; the weight ratio of the fluorine-containing ferric silicate is 7-15 parts, for example: 7 parts, 8 parts, 9 parts, 11 parts, 13 parts, 14 parts and 15 parts; the weight ratio of the calcium sulfate is 4-8 parts, for example: 4 parts, 5 parts, 6 parts, 7 parts and 8 parts; the weight ratio of the ferrous sulfate is 5-10 parts, for example: 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10 parts; the weight ratio of the nitric acid is 20-30 parts, for example: 20 parts, 22 parts, 23 parts, 25 parts, 27 parts, 29 parts and 30 parts; the boric acid is 14-28 parts by weight, for example: 14 parts, 16 parts, 17 parts, 20 parts, 22 parts, 25 parts, 26 parts and 28 parts; the weight ratio of the methanesulfonic acid is 15-26 parts, for example: 15 parts, 16 parts, 18 parts, 19 parts, 21 parts, 23 parts, 25 parts and 26 parts; the weight ratio of the citric acid is 10-20 parts, for example: 10 parts, 12 parts, 14 parts, 16 parts, 17 parts, 19 parts and 20 parts; the weight ratio of the xanthan gum is 2-5 parts, such as: 2 parts, 3 parts, 4 parts and 5 parts; the weight ratio of the NNO as the diffusant is 3-8 parts, for example: 3 parts, 4 parts, 5 parts, 6 parts, 7 parts and 8 parts; the weight ratio of the deflocculant D91 is 1 part to 3 parts, such as 1 part, 2 parts and 3 parts; the weight ratio of water is 30-50 parts, for example: 30 parts, 32 parts, 35 parts, 37 parts, 40 parts, 42 parts, 45 parts, 47 parts, 48 parts, 49 parts and 50 parts.
According to the frosting solution disclosed by the embodiment of the invention, the methanesulfonic acid, the citric acid and the boric acid are used as acidity regulators, so that the frosting solution is beneficial to achieving proper pH value in the use process, and glass can be effectively corroded; on the other hand, compared with the traditional hydrofluoric acid, the methanesulfonic acid, the lemon and the boric acid can slowly release hydrogen ions, so that the etching reaction is mild, and the phenomenon that the etching surface is not uniform and a good crystal shape cannot be generated due to over-strong local reaction is prevented.
Due to the existence of fluosilicate and ferrous salt (such as potassium fluosilicate and ferrous sulfate) in the frosting liquid, the frosting liquid provided by the embodiment of the invention is beneficial to promoting the formation of ferrous fluosilicate crystals on the frosting surface in the use process of the frosting liquid, and improves the crystal morphology of the surface of the frosting by combining the effects of other fluosilicate and additives. The frosting solution provided by the embodiment of the invention not only enables the frosted glass to have the frosting effect and realize the fingerprint and glare preventing effect, but also ensures that the frosted glass surface forms the pearly luster effect due to the crystal morphology on the surface of the frosting.
In a second aspect, an embodiment of the present invention provides a method for preparing a frosting solution, including:
adding the additive and the organic acid into water according to the weight ratio, and uniformly mixing to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I according to the weight ratio, and uniformly stirring to obtain a mixture II;
and adding the inorganic acid into the mixture II according to the proportion, and uniformly stirring to obtain the frosting liquid.
In particular, the method comprises the following steps of,
adding an additive and organic acid into water at the temperature of 30-40 ℃ and stirring for 10-20 min to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I at the temperature of 40-60 ℃, and stirring for 10-20 min to obtain a mixture II;
adding inorganic acid into the mixture II, and stirring for 30min-60min to obtain the frosting solution.
According to the preparation method of the frosting solution provided by the embodiment of the invention, because the solubility of the salts such as ammonium fluoride and ammonium fluorosilicate in water is far higher than that of the salts in acid, the fluoride, the fluorosilicate and the like are mixed and stirred uniformly with water, and then the inorganic acid is added, so that the frosting solution can be prevented from generating new large insoluble ammonium nitrate crystals due to violent reaction with nitric acid.
In a third aspect, the invention provides frosted glass, which is obtained by performing frosting treatment on glass by using the frosting solution of the first aspect.
The frosting treatment may be any treatment method, such as soaking, showering, or the like. This embodiment is not particularly limited thereto.
As a preferred embodiment, the glass is subjected to a frosting treatment by using the frosting solution of the first aspect, which specifically comprises the following steps:
putting the prepared frosting liquid into a stirrer for curing, opening the stirrer every 2 hours, stirring for 5-15 min, and taking out after keeping for 48-72 hours;
pretreating glass, removing oil stains, impurities and a silicon oxide film on the surface of the glass, and washing the glass clean by using clear water;
soaking the pretreated glass in the cured frosting solution, continuously stirring the frosting solution, and swinging the glass to perform frosting treatment on the glass;
and cleaning the glass after the frosting treatment to obtain the frosted glass.
Further, the frosted glass has a roughness of 1.0 μm to 3.0. mu.m. For example: 1.0. mu.m, 1.1. mu.m, 1.3. mu.m, 1.5. mu.m, 1.8. mu.m, 1.9. mu.m, 2.0. mu.m, 2.3. mu.m, 2.5. mu.m, 2.7. mu.m, 2.9. mu.m and 3.0. mu.m. Preferably, the frosted glass has a roughness of 1.3 μm to 3.0. mu.m. The frosted glass provided by the embodiment of the invention has higher roughness, can be widely applied to the building industry and the decoration industry, reduces optical pollution, keeps the pearl effect and improves the attractiveness.
Furthermore, the haze of the frosted glass is 40-80%. For example: 40%, 45%, 50%, 51%, 55%, 60%, 65%, 70%, 75%, 76%, 78% and 80%. Preferably, the frosted glass has a haze of 51% to 80%. The frosted glass provided by the embodiment of the invention has a good frosting effect.
In a fourth aspect, embodiments of the present invention provide a glass cover plate, at least a portion of which is formed from the frosted glass of the third aspect. It will be appreciated by those skilled in the art that the frosted glass has all the features and advantages of the method of making a frosted glass as described above and will not be described in any greater detail herein.
The present invention is illustrated below by way of specific examples, which are intended to be illustrative only and not to limit the scope of the present invention in any way, and reagents and materials used therein are commercially available, unless otherwise specified, and conditions or steps thereof are not specifically described.
Example 1
Selecting the raw materials of the frosting liquid according to the following weight ratio:
20 parts of ammonium fluoride, 8 parts of magnesium fluoride and 22 parts of potassium bifluoride;
20 parts of ammonium fluosilicate, 7 parts of sodium fluosilicate, 9 parts of potassium fluosilicate, 8 parts of magnesium fluosilicate and 7 parts of iron fluosilicate;
4 parts of calcium sulfate and 6 parts of ferrous sulfate;
26 parts of nitric acid and 17 parts of boric acid;
19 parts of methanesulfonic acid and 14 parts of citric acid;
2 parts of xanthan gum, 3 parts of a dispersing agent NNO and 911.2 parts of a deflocculant D;
water: and 47 parts.
Preparing a frosting solution:
adding the additive and the organic acid into water at 30 ℃ and stirring for 10min to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I at 45 ℃ and stirring for 15min to obtain a mixture II;
adding inorganic acid into the mixture II, and stirring for 30min to obtain a frosting solution;
curing the frosting solution:
placing the prepared frosting liquid in a stirrer, opening the stirrer every 2 hours to stir for 10min, and curing after 48 h;
glass pretreatment:
soaking glass in 15% alkaline detergent for 5min to clean oil stain on the surface, then cleaning the glass in 5% hydrofluoric acid detergent for 5min to remove a silicon oxide film on the surface of the glass, and rinsing the glass with pure water for 1 min to remove residual acid liquor on the surface of the pickled glass;
glass frosting treatment:
mounting the pretreated glass on a mechanical arm, putting the glass into the frosting solution, soaking for 90s, continuously stirring the frosting solution, controlling the mechanical arm to continuously swing the glass, and keeping the glass frosting temperature at 10 ℃ and the swinging speed at 18 m/min;
cleaning treatment:
and putting the frosted glass into a 10% sodium carbonate solution for first rinsing for 15s, and then performing second rinsing in pure water for 30 s.
Example 2
Selecting the raw materials of the frosting liquid according to the following weight ratio:
22 parts of ammonium fluoride, 5 parts of magnesium fluoride and 26 parts of potassium bifluoride;
24 parts of ammonium fluosilicate, 5 parts of sodium fluosilicate, 6 parts of potassium fluosilicate, 9 parts of magnesium fluosilicate and 14 parts of iron fluosilicate;
6 parts of calcium sulfate and 8 parts of ferrous sulfate;
30 parts of nitric acid and 14 parts of boric acid;
16 parts of methanesulfonic acid and 15 parts of citric acid;
2 parts of xanthan gum, 3 parts of a dispersing agent NNO and 912 parts of a deflocculant D;
water: 30 parts of.
Preparing a frosting solution:
adding the additive and the organic acid into water at 30 ℃ and stirring for 15min to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I at 50 ℃ and stirring for 15min to obtain a mixture II;
adding inorganic acid into the mixture II, and stirring for 30min to obtain a frosting solution;
curing the frosting solution:
placing the prepared frosting liquid in a stirrer, opening the stirrer every 2 hours, stirring for 10min, and curing after lasting for 60 hours;
glass pretreatment:
soaking glass in 15% alkaline detergent for 5min to clean oil stain on the surface, then cleaning the glass in 5% hydrofluoric acid detergent for 5min to remove a silicon oxide film on the surface of the glass, and then rinsing the glass for 1 min by using pure water to remove residual acid liquor on the surface of the glass after acid cleaning;
glass frosting treatment:
mounting the pretreated glass on a mechanical arm, soaking the glass in the frosting solution for 90s, continuously stirring the frosting solution, controlling the mechanical arm to continuously swing the glass, and keeping the glass frosting temperature at 10 ℃ at the swing speed of 18 m/min;
cleaning treatment:
and putting the frosted glass into a 10% sodium carbonate solution for first rinsing for 15s, and then performing second rinsing in pure water for 30 s.
Example 3
The frosting liquid is prepared from the following raw materials in parts by weight:
20 parts of ammonium fluoride, 8 parts of magnesium fluoride and 24 parts of potassium bifluoride;
24 parts of ammonium fluosilicate, 9 parts of sodium fluosilicate, 9 parts of potassium fluosilicate, 9 parts of magnesium fluosilicate and 9 parts of ferric fluosilicate;
7 parts of calcium sulfate and 7 parts of ferrous sulfate;
28 parts of nitric acid and 15 parts of boric acid;
16 parts of methanesulfonic acid and 15 parts of citric acid;
3 parts of xanthan gum, 3 parts of a dispersing agent NNO and 911 parts of a deflocculant;
water: 50 parts of the raw materials.
Preparing a frosting solution:
adding the additive and the organic acid into water at 40 ℃ and stirring for 15min to obtain a mixture I;
adding fluoride, fluosilicate and ferrous salt into the mixture I at 55 ℃ and stirring for 16min to obtain a mixture II;
adding inorganic acid into the mixture II, and stirring for 40min to obtain a frosting solution;
curing the frosting solution:
placing the prepared frosting liquid in a stirrer, opening the stirrer every 2 hours to stir for 10min, and curing after 72 h;
glass pretreatment:
soaking glass in 15% alkaline detergent for 5min to clean oil stain on the surface, then cleaning the glass in 5% hydrofluoric acid detergent for 5min to remove a silicon oxide film on the surface of the glass, and rinsing the glass with pure water for 1 min to remove residual acid liquor on the surface of the pickled glass;
glass frosting treatment:
mounting the pretreated glass on a mechanical arm, putting the glass into the frosting solution, soaking for 90s, continuously stirring the frosting solution, controlling the mechanical arm to continuously swing the glass, and keeping the glass frosting temperature at 10 ℃ and the swinging speed at 18 m/min;
cleaning treatment:
and putting the frosted glass into a 10% sodium carbonate solution for first rinsing for 15s, and then performing second rinsing in pure water for 30 s.
Example 4
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
15 parts of ammonium fluoride, 11 parts of magnesium fluoride and 19 parts of potassium bifluoride;
12 parts of ammonium fluosilicate, 10 parts of sodium fluosilicate, 7 parts of potassium fluosilicate, 5 parts of magnesium fluosilicate and 10 parts of iron fluosilicate;
8 parts of calcium sulfate and 9 parts of ferrous sulfate;
20 parts of nitric acid and 22 parts of boric acid;
25 parts of methanesulfonic acid and 10 parts of citric acid;
5 parts of xanthan gum, 7 parts of a dispersing agent NNO and 913 parts of a deflocculant D;
water: 35 parts of (A).
Example 5
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
24 parts of ammonium fluoride, 6 parts of magnesium fluoride and 27 parts of potassium bifluoride;
23 parts of ammonium fluosilicate, 9 parts of sodium fluosilicate, 7 parts of potassium fluosilicate, 15 parts of magnesium fluosilicate and 9 parts of ferric fluosilicate;
5 parts of calcium sulfate and 10 parts of ferrous sulfate;
20 parts of nitric acid and 22 parts of boric acid;
26 parts of methanesulfonic acid and 19 parts of citric acid;
4 parts of xanthan gum, 6 parts of a dispersing agent NNO and 912.5 parts of a deflocculant D;
water: 42 parts of the raw materials.
Example 6
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
20 parts of ammonium fluoride, 8 parts of magnesium fluoride and 22 parts of potassium bifluoride;
20 parts of ammonium fluosilicate, 7 parts of sodium fluosilicate, 9 parts of potassium fluosilicate, 8 parts of magnesium fluosilicate and 7 parts of iron fluosilicate;
4 parts of calcium nitrate and 6 parts of ferrous nitrate;
26 parts of nitric acid and 17 parts of boric acid;
19 parts of methanesulfonic acid and 14 parts of citric acid;
2 parts of xanthan gum, 3 parts of a dispersing agent NNO and 911.2 parts of a deflocculant D;
water: and 47 parts.
Example 7
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
20 parts of ammonium fluoride, 8 parts of magnesium fluoride and 22 parts of potassium bifluoride;
20 parts of ammonium fluosilicate, 7 parts of sodium fluosilicate, 9 parts of potassium fluosilicate, 8 parts of magnesium fluosilicate and 7 parts of iron fluosilicate;
4 parts of calcium sulfate and 6 parts of ferrous sulfate;
26 parts of nitric acid and 17 parts of boric acid;
19 parts of methanesulfonic acid and 14 parts of citric acid;
2 parts of carboxymethyl cellulose, 2 parts of nekal BX1 parts, 3 parts of a dispersing agent NNO and 911.2 parts of a deflocculant;
water: and 47 parts.
Example 8
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
20 parts of ammonium fluoride, 8 parts of magnesium fluoride and 22 parts of potassium bifluoride;
20 parts of ammonium fluosilicate, 7 parts of sodium fluosilicate, 9 parts of potassium fluosilicate, 8 parts of magnesium fluosilicate and 7 parts of iron fluosilicate;
4 parts of calcium sulfate and 6 parts of ferrous sulfate;
26 parts of sulfuric acid and 17 parts of boric acid;
19 parts of methanesulfonic acid and 14 parts of oxalic acid;
2 parts of xanthan gum, 3 parts of a dispersing agent NNO and 911.2 parts of a deflocculant D;
water: and 47 parts.
Example 9
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
20 parts of sodium fluoride, 8 parts of magnesium fluoride and 22 parts of ammonium bifluoride;
20 parts of ammonium fluosilicate, 7 parts of sodium fluosilicate, 17 parts of potassium fluosilicate and 7 parts of ferric fluosilicate;
4 parts of calcium sulfate and 6 parts of ferrous sulfate;
26 parts of sulfuric acid and 17 parts of boric acid;
19 parts of oxalic acid and 14 parts of citric acid;
2 parts of carboxymethyl cellulose, 3 parts of a dispersing agent NNO and 911.2 parts of a deflocculant;
water: and 47 parts.
Example 10
The difference between the embodiment and the embodiment 1 is that the raw materials of the frosting liquid are selected according to the following weight ratio:
20 parts of sodium fluoride, 8 parts of potassium bifluoride and 22 parts of ammonium fluoride;
20 parts of ammonium fluosilicate, 14 parts of sodium fluosilicate and 17 parts of potassium fluosilicate;
4 parts of calcium nitrate and 6 parts of ferrous nitrate;
26 parts of nitric acid and 17 parts of boric acid;
19 parts of methanesulfonic acid and 14 parts of oxalic acid;
2 parts of nekal BX, 3 parts of a diffusant NNO and 911.2 parts of a deflocculant;
water: 50 parts of the raw materials.
Comparative example 1
The difference between the comparative example and the example 1 is that the frosting solution does not contain ferrous salt, namely ferrous sulfate;
comparative example 2
The difference between the comparative example and the example 1 is that the molysite in the frosting solution is 30 parts, namely 30 parts of ferrous sulfate;
comparative example 3
This comparative example differs from example 1 in that the frosting solution does not include fluorosilicates;
comparative example 4
This comparative example differs from example 1 in that the frosting solution does not include boric acid and organic acids (methanesulfonic acid and citric acid);
comparative example 5
Selecting the raw materials of the frosting liquid according to the following weight ratio:
6.5 parts of hydrofluoric acid, 6 parts of ammonium fluoride, 5.5 parts of ammonium bifluoride, 4 parts of water, 2 parts of sulfuric acid, 3 parts of sodium carbonate, 1 part of silicon dioxide and 1 part of calcium fluoride.
The frosted glass processed by the above examples 1 to 10 and comparative examples 1 to 5 is added with 10pcs glass, the roughness of the surface of the frosted glass is measured by GB/T131-1993, the test point is the center of the product, and the test result is shown in Table 1:
TABLE 1 roughness test results of examples 1 to 10, and comparative examples 1 to 5, in μm
Further, the frosted glasses obtained in examples 1 to 10 and comparative examples 1 to 5 were tested for haze using GB T2410-2008, and the test results are shown in table 2:
table 2 haze test results of examples 1 to 10, and comparative examples 1 to 5
From the results of table 1, it can be derived:
the results of the roughness of the frosted glass prepared in example 1 and comparative example 2 gave: the roughness of the frosted glass prepared in the comparative example 2 is far greater than that of the frosted glass prepared in the example 1, which shows that excessive ferrous salt causes a large number of crystals to be formed on the surface of the frosted glass, and the roughness is increased. Therefore, the weight range of the ferrous salt in the embodiment of the invention is beneficial to the frosted glass to have proper roughness and ensure the pearlescent effect.
The results of the roughness of the frosted glass prepared in example 1 and comparative example 3 gave: the roughness of the frosted glass prepared in the comparative example 3 is far lower than that of the frosted glass prepared in the example 1, and the frosted glass prepared in the comparative example 3 is analyzed to be lower in roughness because the frosted liquid lacks a sand-applying agent and crystals are difficult to form on the surface of the glass because the frosted liquid does not contain fluosilicate; the results of the roughness of the frosted glass prepared in example 1 and comparative example 4 gave: the frosting solution of comparative example 4 does not include boric acid and organic acid, only contains inorganic strong acid, and cannot adjust the acidity of the frosting solution, so that the reaction is too fast, the glass surface is seriously etched, and the roughness of the frosted glass is too large. Therefore, the frosting liquid component provided by the embodiment of the invention is beneficial to the frosted glass to have proper roughness, and has good pearling effect and attractive appearance while reducing light pollution, preventing fingerprints and preventing glare.
The frosted glass prepared in examples 1-10 has a roughness much greater than that of the frosted glass prepared in comparative example 5. The results in table 1 show that the frosting solution provided by the invention is beneficial to improving the roughness of frosted glass, and has good pearling effect and attractive appearance while reducing light pollution, preventing fingerprints and preventing glare.
From the roughness results of examples 1-10, it can be concluded that: the components of the frosting solution and the content change of each component have great influence on the roughness of the frosted glass, and the roughness of the frosted glass obtained by treating the frosting solution is more than 1.4, which shows that the components of the frosting solution in the embodiment of the invention are beneficial to improving the roughness of the frosted glass, thereby being beneficial to improving the frosting effect of the frosted glass.
From the results of table 2, it can be seen that: the haze of the frosted glass prepared in the examples 1 to 10 is smaller than that of the frosted glass prepared in the comparative examples 1 to 5, and the haze of the frosted glass prepared in the comparative examples 1 to 5 is large, so that the pearlescence effect of the glass is influenced. Therefore, the frosting solution provided by the embodiment of the invention is beneficial to ensuring that the haze of the frosted glass is in a proper range, so that the frosted glass has a better frosting effect, and has a good pearling effect while reducing light pollution, preventing fingerprints and preventing glare.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (14)
1. The frosting solution is characterized by comprising the following components in parts by weight:
39-62 parts of fluoride;
35-70 parts of fluorosilicate, wherein the fluorosilicate comprises potassium fluosilicate;
5-10 parts of ferrous salt;
34-58 parts of inorganic acid, wherein the inorganic acid comprises boric acid;
25-46 parts of organic acid, wherein the organic acid comprises methanesulfonic acid and citric acid;
6-18 parts of an additive;
and 30-50 parts of water.
2. The frosting solution of claim 1, wherein the fluoride comprises at least one of magnesium fluoride, ammonium fluoride, sodium fluoride, ammonium bifluoride, potassium fluoride and sodium bifluoride.
3. The frosting solution of claim 1, wherein the fluorosilicate further comprises at least one of ammonium fluorosilicate, sodium fluorosilicate, potassium fluorosilicate, magnesium fluorosilicate, iron fluorosilicate, and calcium fluorosilicate.
4. The frosting solution according to claim 1, wherein the ferrous salt comprises ferrous sulfate and/or ferrous nitrate.
5. The frosting solution according to claim 1, wherein the inorganic acid further comprises sulfuric acid and/or nitric acid.
6. The frosting solution of claim 1, wherein the organic acid further comprises oxalic acid.
7. The frosting solution according to claim 1, wherein the additive comprises a thickener and/or a dispersant; wherein the thickening agent comprises at least one of carboxymethyl cellulose and xanthan gum; the dispersing agent comprises at least one of diisobutyl naphthalene sulfonate, methylene dinaphthalene sodium sulfonate and a deflocculant.
8. The frosting solution of claim 1, further comprising 4-8 parts of a calcium salt, wherein the calcium salt comprises calcium sulfate and/or calcium nitrate.
9. The frosting solution according to any one of claims 1 to 8, wherein the frosting solution comprises the following components in parts by weight:
15-24 parts of ammonium fluoride, 5-11 parts of magnesium fluoride, 19-27 parts of potassium hydrogen fluoride, 12-24 parts of ammonium fluosilicate, 5-10 parts of sodium fluosilicate, 6-11 parts of potassium fluosilicate, 5-10 parts of magnesium fluosilicate, 7-15 parts of ferric fluosilicate, 5-10 parts of ferrous sulfate and/or ferrous nitrate, 20-30 parts of nitric acid, 14-28 parts of boric acid, 15-26 parts of methanesulfonic acid, 10-20 parts of citric acid, 2-5 parts of a thickening agent and 4-11 parts of a dispersing agent.
10. A method of preparing a frosting fluid according to any of claims 1 to 9, comprising:
adding the additive and the organic acid into the water according to the weight ratio, and uniformly mixing to obtain a mixture I;
adding the fluoride, the fluosilicate and the ferrous salt into the mixture I according to the weight ratio, and uniformly stirring to obtain a mixture II;
and adding the inorganic acid into the mixture II according to the weight ratio, and uniformly stirring to obtain the frosting solution.
11. A frosted glass obtained by subjecting a glass to a frosting treatment using the frosting solution according to any one of claims 1 to 9.
12. The frosted glass of claim 11, wherein the frosted glass has a roughness of 1.0 μ ι η to 3.0 μ ι η.
13. The frosted glass according to claim 11, wherein the frosted glass has a haze of 40% to 80%.
14. A glass cover plate, characterized in that at least a part of the glass cover plate is composed of the frosted glass according to any of claims 11 to 13.
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| CN115321827A (en) * | 2022-08-31 | 2022-11-11 | 郑州恒昊光学科技有限公司 | Etching solution with diamond sand sparkling effect and manufacturing process of mobile phone rear shell glass of etching solution |
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| CN114516729B (en) | 2023-10-17 |
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