CN113003942B - Environment-friendly glass etching solution and preparation method and application thereof - Google Patents
Environment-friendly glass etching solution and preparation method and application thereof Download PDFInfo
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- CN113003942B CN113003942B CN201911318741.3A CN201911318741A CN113003942B CN 113003942 B CN113003942 B CN 113003942B CN 201911318741 A CN201911318741 A CN 201911318741A CN 113003942 B CN113003942 B CN 113003942B
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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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- 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
- C03C15/02—Surface treatment of glass, not in the form of fibres or filaments, by etching for making a smooth surface
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Abstract
The invention provides an environment-friendly glass etching solution which comprises the following components in percentage by mass: inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; metal ion complexing agent: 5 to 10 percent; the balance of water; wherein the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate; the environment-friendly glass etching solution does not contain fluorine. The components of the etching solution are non-toxic and harmless, can achieve the effect which is comparable to the current acid glass etching solution, and can be repeatedly recycled; after the service life of the waste water treatment device is finished, the waste water can be discharged only through neutralization treatment of acid liquor, and the waste water treatment cost is low. The invention also provides a preparation method of the environment-friendly glass etching solution and a method for etching glass by using the environment-friendly glass etching solution.
Description
Technical Field
The invention relates to the technical field of glass processing, in particular to an environment-friendly glass etching solution and a preparation method and application thereof.
Background
Glass etching is the etching of glass or glass articles with chemicals to meet specific requirements such as reduced thickness, flat surfaces, etc. At present, the main component of the commonly used glass etching solution is hydrofluoric acid or other fluorides, but the products have the following defects: the waste liquid generated during or after the production of the fluorine-containing etching solution contains fluoride, which can damage the environment, is inconvenient to directly discharge and needs high cost for wastewater treatment. Therefore, there is a need to provide an environmentally friendly glass etchant.
Disclosure of Invention
In view of the above, the invention provides an environment-friendly glass etching solution, the components of the etching solution are non-toxic and harmless, the use time is long, the etching solution can be discharged only by neutralization treatment with acid liquor after the service life is over, the wastewater treatment cost is low, and the etching solution can achieve the effect comparable to the current acid glass etching solution.
Specifically, in a first aspect, the invention provides an environment-friendly glass etching solution, which comprises the following components in percentage by mass: inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; metal ion complexing agent: 5 to 10 percent; the balance of water; wherein the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate; the environment-friendly glass etching solution does not contain fluorine.
The components (such as strong inorganic bases, weak strong bases and weak acid salts) in the environment-friendly glass etching solution are obviously water-soluble in view of forming a uniform solution.
Wherein the inorganic strong base is selected from one or more of sodium hydroxide, potassium hydroxide and calcium hydroxide. Preferably, the inorganic strong base is one or both of sodium hydroxide and potassium hydroxide.
In the invention, the mass percentage of the inorganic strong base is 28-35%. For example, it may be 28%, 29%, 30%, 31%, 32%, 33%, 34% or 35%.
Wherein the strong base weak acid salt is selected from one or more of water-soluble carbonate, phosphate, dibasic phosphate and acetate of sodium, potassium and calcium elements. Specifically, the strong base and weak acid salt is selected from one or more of anhydrous sodium carbonate, sodium phosphate, disodium hydrogen phosphate, sodium bicarbonate, sodium acetate, potassium carbonate, potassium phosphate, dipotassium hydrogen phosphate, potassium bicarbonate, potassium acetate and calcium acetate.
Preferably, the strong and weak acid salt is one or more of anhydrous sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
In the invention, the mass percentage of the strong alkali weak acid salt is 10-18%. For example, it may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17% or 18%. In one embodiment of the invention, the content of the strong base and the weak acid salt is 10-14% by mass.
In the invention, the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate. The existence of the metal ion complexing agent can ensure that the glass is uniformly etched, and the surface roughness of the etched glass reaches the accepted standard in the industry. The metal ion complexing agent can be 5%, 6%, 7%, 8%, 9% or 10% in percentage by mass. Preferably, the mass percentage of the metal ion complexing agent is 6-10%.
Further, the metal ion complexing agent is sodium gluconate.
In one embodiment of the invention, the environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 28 to 35 percent; anhydrous sodium carbonate: 10 to 18 percent; sodium gluconate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element. Preferably, the anhydrous sodium carbonate accounts for 10-14% by mass.
In another embodiment of the invention, the environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 28 to 35 percent; anhydrous sodium carbonate: 10 to 18 percent; sodium tartrate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element.
In another embodiment of the present invention, the environment-friendly glass etching solution comprises the following components by mass: sodium hydroxide: 28 to 35 percent; anhydrous sodium carbonate: 10 to 18 percent; sodium iminodisuccinate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element.
In another embodiment of the present invention, the environment-friendly glass etching solution comprises the following components by mass: sodium hydroxide: 28 to 35 percent; sodium bicarbonate: 10 to 18 percent; sodium gluconate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element.
In another embodiment of the present invention, the environment-friendly glass etching solution comprises the following components by mass: potassium hydroxide: 28 to 35 percent; potassium carbonate: 10 to 18 percent; sodium gluconate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element.
In the invention, the dosage of the inorganic strong base is higher than that of the strong base weak acid salt, so that a stable alkaline environment required by glass etching can be ensured. Optionally, the mass ratio of the two is (1.55-3.50): 1. preferably (1.60-1.95): 1.
the environment-friendly glass etching solution provided by the first aspect of the invention is alkaline, and each component does not contain fluorine element, wherein inorganic strong base is the main component with the largest content in the etching solution and is used as a main etching corner to provide a high-alkalinity etching environment; the strong base and weak acid salt can be used as a hydroxide buffer to stabilize the alkalinity of the etching solution and prolong the service life of the etching solution; the metal ion complexing agent (such as sodium gluconate) can better complex metal ions (such as Na) in the glass+、K+、Ca2+) The etching solution can be uniformly corroded on the surface of the glass, so that the surface roughness of the etched glass reaches the industry accepted standard. Through the synergistic effect of the components with the specific mass percentage, the obtained etching solution can achieve the effect which is comparable with that of the current acid glass etching solution. Moreover, the components of the etching solution are non-toxic and harmless, the use time is long, the etching solution can be discharged only by neutralization treatment of acid liquor after the service life is over, and the wastewater treatment cost is low.
Optionally, after the glass is treated by the environment-friendly glass etching solution, the transmittance of the etched glass is greater than 98%, and the haze of the etched glass is less than 0.5. This shows that the environment-friendly glass etching solution can uniformly etch glass, and the roughness of the etched glass is low. Optionally, the roughness Ra of the etched glass is 0.02-0.04 μm.
The environment-friendly glass etching solution provided by the first aspect of the invention is alkaline, does not contain components with fluorine elements, has no toxicity or harm, can be repeatedly recycled for multiple times, can be discharged only by neutralizing the environment-friendly glass etching solution with acid liquor after the service life of the environment-friendly glass etching solution is over, and has low wastewater treatment cost; and the etching solution can achieve the effect which is comparable with the current acid glass etching solution.
In a second aspect, the invention provides a preparation method of an environment-friendly glass etching solution, which comprises the following steps:
dissolving inorganic strong base, strong base and weak acid salt and a metal ion complexing agent in water, and uniformly stirring to obtain an environment-friendly glass etching solution; the environment-friendly glass etching solution comprises the following components in percentage by mass: inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; metal ion complexing agent: 5 to 10 percent; the balance of water; wherein the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate; the etching solution does not contain fluorine.
Wherein the water is deionized water or distilled water. The components of the etching solution are as described in the first aspect of the invention.
The preparation method of the environment-friendly glass etching solution provided by the second aspect of the invention has simple process, and the environment-friendly glass etching solution which is clear, transparent, free of insoluble substances and stable in performance can be easily prepared. After the service life of the etching solution is over, the etching solution can be discharged only by neutralizing with acid liquor, and the wastewater treatment cost is low.
In a third aspect, the present invention provides a method for etching glass, comprising:
providing an environment-friendly glass etching solution, wherein the environment-friendly glass etching solution comprises the following components in percentage by mass: inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; sodium gluconate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element;
and soaking the glass in the environment-friendly glass etching solution for etching.
Optionally, before soaking the glass in the environment-friendly glass etching solution, the method further comprises: and heating the environment-friendly glass etching solution to 60-95 ℃. Preferably to 90-95 ℃. Further, in this case, the etching time may be 10 to 30 min. In the invention, the etching time can be adjusted according to the temperature of the environment-friendly glass etching solution during etching.
Optionally, before soaking the glass in the environment-friendly glass etching solution, the method further comprises: and (4) cleaning the glass. The cleaning treatment is mainly used for removing oil stains, impurities and the like on the surface of the glass, so that the environment-friendly glass etching solution can be used for better etching.
Optionally, after the etching, further comprising: the etched glass was washed with water and dried.
According to the etching method for glass provided by the third aspect of the invention, the glass is etched by using the environment-friendly glass etching solution provided by the first aspect of the invention, so that a uniform etching effect can be formed on the surface of the glass, and the effect is comparable to that of the existing acid glass etching solution.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, reagents used in the embodiments of the present invention are commercially available.
Example 1
The environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide (NaOH): 30 percent; anhydrous sodium carbonate (molecular formula Na)2CO3): 16 percent; sodium gluconate (molecular formula C)6H11NaO7): 10 percent; water: 45 percent.
The preparation process of the etching solution is as follows: dissolving weighed inorganic strong base, strong base weak acid salt and sodium gluconate in water, and uniformly stirring and dispersing to obtain the environment-friendly glass etching solution. After being matched, the mixture is placed for standby.
The application mode of the etching solution is as follows: cleaning the surface of a glass sheet with the thickness of about 145mm multiplied by 75mm and the thickness of about 0.55mm by using a glass cleaning agent BYD-01; the etching solution was heated to 92 ℃, and then the cleaned glass was immersed in the etching solution at 92 ℃ for etching for 25 minutes. The etched glass was then taken out, washed with water and dried.
In order to highlight the beneficial effects of the invention, the following comparative examples are set:
comparative example 1 (removing sodium gluconate from example 1)
The glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 30 percent; anhydrous sodium carbonate: 16 percent; water: and 55 percent.
Comparative example 2 (conventional fluorine-containing acidic etching solution)
The glass etching solution comprises the following components in percentage by mass: hydrofluoric acid: 15 percent; ammonium acid fluoride: 5 percent; sulfuric acid: 5 percent; water: 75 percent.
The glass etching solutions of comparative examples 1-2 above were applied to etching of bulk glass in the same manner as in example 1, and then the thickness of the glass sheet before and after etching was measured using a micrometer to calculate the etching rate. And then testing the roughness of the etched glass surface by using a roughness meter to detect the flatness of the etched surface.
The results of inventive example 1 are: the thickness of the glass before etching is 0.549mm, the thickness of the glass after etching is 0.498mm, and the calculated etching speed is 0.001 mm/min; the roughness of the etched area was measured to be Ra of 0.034 μm. While the results of comparative example 1 are: the thickness of the glass before etching is 0.548mm, the thickness of the glass after etching is 0.515mm, and the calculated etching speed is 0.0007 mm/min; the roughness of the etched area was measured to be Ra of 0.089. mu.m. While the results of comparative example 2 are: the thickness of the glass before etching is 0.551mm, the thickness of the glass after etching is 0.478mm, and the calculated etching speed is 0.0015 mm/min; the roughness of the etched area was measured to be Ra of 0.029 μm.
In addition, the glass etched by the glass etching solution of the embodiment 1 of the invention has no cracks on the surface, and the transmittance (T%) is more than 98% and the haze (H) is less than 0.4. And (3) carrying out strengthening treatment on the etched glass by using a sodium potassium displacement strengthening method by using a monomer strengthening furnace of one technology and adopting potassium nitrate, wherein the strengthening temperature is 400 ℃, the strengthening time is 350min, and the glass is detected by using a FSM-6000LE glass surface stress tester after strengthening. The etched glass of example 1 was found to have a post-strengthening DOL (depth of stress layer) of 8.45 μm and a CS (stress value) of 780MP, which met the performance requirements for the glass product.
In contrast, comparative example 1 measured the etched glass to have a transmittance (T%) of 95-98%, a haze (H) of 0.7, a DOL of 7.89 μm after strengthening, and a CS of 740 MP; comparative example 2 the etched glass was found to have a transmittance (T%) of 97 to 98%, haze (H) of 0.5 to 0.6, DOL after strengthening of 8.1 μm and CS of 760 MP.
From the above results, it can be seen that the glass etching solution provided in embodiment 1 of the present invention can etch glass well, the effect of the etching solution can be substantially comparable to that of the existing fluorine-containing etching solution, and the surface effect of the etched glass is substantially consistent, but the components adopted in the present invention are more environment-friendly, free of fluorine-containing components, non-toxic, harmless, easy to treat, and easy to discharge. In addition, in the glass etching solution provided by the embodiment of the invention, a proper amount of metal ion complexing agent-sodium gluconate is added, so that metal ions in glass can be better complexed, and the surface of the glass is corroded more uniformly and rapidly.
Example 2
The environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 35 percent; anhydrous sodium carbonate: 18 percent; sodium gluconate: 10 percent; the balance being water.
The etching solution of example 2 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 2 μm/min, a transmittance of the etched glass of more than 99.5%, and a haze of less than 0.3.
Example 3
The environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 31.5 percent; anhydrous sodium carbonate: 12 percent; sodium gluconate: 8 percent; the balance being water.
The etching solution of example 3 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 0.97 μm/min, a transmittance of the etched glass of more than 98%, and a haze of less than 0.5.
Example 4
The environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 30 percent; sodium bicarbonate: 14 percent; sodium gluconate: 10 percent; the balance being water.
The etching solution of example 4 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 1 μm/min, a transmittance of the etched glass of more than 98%, and a haze of less than 0.45.
Example 5
The environment-friendly glass etching solution comprises the following components in percentage by mass: potassium hydroxide: 30 percent; anhydrous sodium carbonate: 16 percent; sodium tartrate: 10 percent; the balance being water.
The etching solution of example 5 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 1 μm/min, a transmittance of the etched glass of more than 98%, a haze of less than 0.5, and a surface roughness Ra of 0.038 μm.
Example 6
The environment-friendly glass etching solution comprises the following components in percentage by mass: potassium hydroxide: 30 percent; anhydrous sodium carbonate: 16 percent; tetrasodium iminodisuccinate: 10 percent; the balance being water.
The etching solution of example 6 was applied to the etching of the above glass sheet in the same manner as in example 1 at an etching rate of 1 μm/min, and the etched glass had a transmittance of more than 98%, a haze of less than 0.45, and a surface roughness Ra of 0.035 μm.
Example 7
The environment-friendly glass etching solution comprises the following components in percentage by mass: potassium hydroxide: 29 percent; potassium carbonate: 16 percent; sodium tartrate: 6 percent; the balance being water.
The etching solution of example 7 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 0.99 μm/min, a transmittance of the etched glass of more than 98%, a haze of less than 0.5, and a surface roughness Ra of 0.039 μm.
Example 8
The environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 28%; disodium hydrogen phosphate: 10 percent; sodium iminodisuccinate: 5 percent; the balance being water.
The etching solution of example 8 was applied to the etching of the above glass sheet in the same manner as in example 1, with an etching rate of 0.92 μm/min, a transmittance of the etched glass of more than 98%, a haze of less than 0.5, and a surface roughness Ra of 0.040 μm.
The foregoing is illustrative of the present invention and it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and are intended to be within the scope of the invention.
Claims (10)
1. The environment-friendly glass etching solution is characterized by comprising the following components in percentage by mass:
inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; metal ion complexing agent: 5 to 10 percent; the balance of water; wherein the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate; the environment-friendly glass etching solution does not contain fluorine.
2. The environment-friendly glass etching solution according to claim 1, wherein the inorganic strong base is one or more selected from sodium hydroxide, potassium hydroxide and calcium hydroxide.
3. The environment-friendly glass etching solution according to claim 1, wherein the strong base and weak acid salt is selected from one or more of water-soluble carbonates, phosphates, dibasic phosphates and acetates of sodium, potassium and calcium elements.
4. The environment-friendly glass etching solution according to claim 3, wherein the strong alkali and weak acid salt is one or more of anhydrous sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
5. The environment-friendly glass etching solution as defined in claim 1, wherein the strong alkali weak acid salt is 10-14% by mass.
6. The environment-friendly glass etching solution as claimed in claim 1, wherein the environment-friendly glass etching solution comprises the following components in percentage by mass: sodium hydroxide: 28 to 35 percent; anhydrous sodium carbonate: 10 to 18 percent; sodium gluconate: 5 to 10 percent; the balance of water; wherein, the environment-friendly glass etching solution does not contain fluorine element.
7. The preparation method of the environment-friendly glass etching solution is characterized by comprising the following steps of:
dissolving inorganic strong base, strong base and weak acid salt and a metal ion complexing agent in water, and uniformly stirring to obtain an environment-friendly glass etching solution; the environment-friendly glass etching solution comprises the following components in percentage by mass: inorganic strong base: 28 to 35 percent; strong base and weak acid salt: 10 to 18 percent; metal ion complexing agent: 5 to 10 percent; the balance of water; wherein the metal ion complexing agent is selected from one or more of sodium gluconate, sodium tartrate and sodium iminodisuccinate; the environment-friendly glass etching solution does not contain fluorine.
8. A method for etching glass, comprising the steps of:
providing the environmentally friendly glass etching solution of any one of claims 1-6;
and soaking the glass in the environment-friendly glass etching solution for etching.
9. The etching method according to claim 8, further comprising, before immersing the glass in the environmentally friendly glass etchant solution: and heating the environment-friendly glass etching solution to 60-95 ℃.
10. The etching method of claim 9, wherein the etching time is 10-30 min.
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| CN201911318741.3A CN113003942B (en) | 2019-12-19 | 2019-12-19 | Environment-friendly glass etching solution and preparation method and application thereof |
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| CN113003942B true CN113003942B (en) | 2022-02-08 |
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| CN116040952B (en) * | 2021-10-28 | 2024-06-18 | 比亚迪股份有限公司 | Glass etching liquid, glass with crystal-shining pattern and production method thereof |
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| US5382295A (en) * | 1990-11-20 | 1995-01-17 | Henkel Corporation | Method for cleaning aluminum and aluminum alloys |
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| WO2012086822A1 (en) * | 2010-12-24 | 2012-06-28 | 日本パーカライジング株式会社 | Etching agent for aluminium and aluminium alloys |
| CN109609290A (en) * | 2018-12-13 | 2019-04-12 | 蓝思科技（长沙）有限公司 | Cleaning agent and cleaning method are used after a kind of glass polishing |
| CN110453223A (en) * | 2018-05-07 | 2019-11-15 | 惠州市鸿宇泰科技有限公司 | A kind of high-effect environment-friendly type acidic etching liquid and its engraving method |
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2019
- 2019-12-19 CN CN201911318741.3A patent/CN113003942B/en active Active
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|---|---|---|---|---|
| US5382295A (en) * | 1990-11-20 | 1995-01-17 | Henkel Corporation | Method for cleaning aluminum and aluminum alloys |
| US5622569A (en) * | 1995-06-02 | 1997-04-22 | Aluminum Company Of America | Aluminum rigid container sheet cleaner and cleaning method |
| WO2012086822A1 (en) * | 2010-12-24 | 2012-06-28 | 日本パーカライジング株式会社 | Etching agent for aluminium and aluminium alloys |
| CN110453223A (en) * | 2018-05-07 | 2019-11-15 | 惠州市鸿宇泰科技有限公司 | A kind of high-effect environment-friendly type acidic etching liquid and its engraving method |
| CN109609290A (en) * | 2018-12-13 | 2019-04-12 | 蓝思科技（长沙）有限公司 | Cleaning agent and cleaning method are used after a kind of glass polishing |
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