CN101531464A - Method for preparing low-reflection glass - Google Patents
Method for preparing low-reflection glass Download PDFInfo
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- CN101531464A CN101531464A CN200910057014A CN200910057014A CN101531464A CN 101531464 A CN101531464 A CN 101531464A CN 200910057014 A CN200910057014 A CN 200910057014A CN 200910057014 A CN200910057014 A CN 200910057014A CN 101531464 A CN101531464 A CN 101531464A
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Abstract
The invention relates to a method for preparing low-reflection glass, which is characterized in that a cleaned glass sheet covered with a PVC film on one surface is soaked into frosting powder consisting of inorganic fluorine compound, assistant and surfactant and soaked into low-reflection glass frosting liquid consisting of the frosting powder and hydrochloric acid according to a weight ratio of between 1 to 0.2 and 1 to 1 for 5 to 300 seconds; after reaction, a low-reflection glass basic sample of which light transmittance is 50 to 60 percent is formed; and then, the low-reflection glass basic sample is put into a glass low-reflection transparent liquid to react for 2 to 20 minutes, the PVC film on one surface of the glass sheet is removed, and then the low-reflection glass of which reflectivity is less than 2 percent is obtained by cleaning and airing. The whole process is quite simple and practical.
Description
Technical field
The invention provides a kind of preparation method of low-reflection glass, specially refer to the chemical constitution and the preparation method that produce low-reflection glass.
Background technology
Low-reflection glass claims anti reflection glass or glare proof glass again, is a kind of special glass that lowers luminous reflectance and light is seen through easily, has been widely used in electronic industry, high-grade picture frame mounting, every field such as measurement instrument industry.Produce low-reflection glass and adopt the surfacing that the surface spraying of glass is had low reflecting properties at present, make it have low " light " reflectivity.This kind method is big to equipment input expense, and the low reflection spraying rete of formation easily causes under high humidity environment and comes off.
Glass surface is carried out chemical reaction, and its surperficial silica structure is changed and reach the reduction luminous reflectance is that the low-reflection glass that just rises recent years is made new technology.Chinese patent ZL01126227.3 has introduced a kind of several inorganic fluoride mixture, auxiliary agent and hydrochloric acid form a kind of can be to the solution of the rapid frosting of glass cell-shell.This method can not make the reflectivity of sheet glass be reduced.
Simultaneously, Chinese patent ZL200480003081.5 discloses a kind of " manufacture method of low-reflection glass and low reflection glass plate " treatment solution by using two kinds of differing materials to form that Japan AGC Co., Ltd. proposes, same surface glass is carried out twice coating, drying treatment respectively, after 400～800 ℃ of temperature roastings, form antiradar reflectivity glass on the surface of glass by two kinds of different resins in two kinds of treatment solutions.
But, though aforementioned ZL01126227.3 patented technology mixes by ammonium bifluoride and hydrofluoric acid solution glass is carried out the method that erosion is covered on the surface, can effectively reduce the glass transmittance, but can not reduce the reflection of light rate.Though providing, ZL200480003081.5 patent described later can reach the purpose that makes sheet glass reduce reflectivity, this processing method more complicated, and tooling cost also can improve.Therefore, the making method of exploring and seek a kind of easy and suitable low-reflection glass is the demand in market, also is relevant industry scientific and technical personnel's a problem.
Summary of the invention
Purpose of the present invention: the production low-reflection glass that a kind of technology is simple and easy to do, cost of manufacture is comparatively cheap preparation method is provided, realizes the antiradar reflectivity of glasswork.
The foregoing invention purpose is achieved through the following technical solutions:
The preparation method of this low-reflection glass, it is characterized in that: incite somebody to action wash clean, and the sheet glass that one side is posted the PVC film immerses by inorganic fluoride, the frosting powder that auxiliary agent and tensio-active agent are formed, and in the low-reflection glass frosted liquid that constitutes by 1:0.2～1:1 weight ratio by above-mentioned frosting powder and hydrochloric acid 5～300 seconds, make transmittance after the reaction and be 40～60% low-reflection glass basic pattern, then again the low-reflection glass basic pattern being put into the low reflection of glass printing opacity liquid reacted 2～30 minutes, remove the PVC film on the sheet glass one side, clean and promptly get reflectivity after drying less than 2% low-reflection glass.
Described frosting powder is made up of the inorganic fluoride that accounts for total amount 65～80%, 18～33% auxiliary agent, 0.5～2% tensio-active agent.
Described frosting powder comprises and can be dissolved in the water and can produce the inorganic fluoride of fluorion, and it is in ammonium bifluoride, Neutral ammonium fluoride, potassium hydrogen fluoride, sodium bifluoride, potassium fluoborate, the Sodium tetrafluoroborate one or more; Described auxiliary agent is water-fast fluorochemical, mineral powder, vitriol composition, wherein fluorochemical is Sodium Silicofluoride, Calcium Fluoride (Fluorspan), calcium silicofluoride, magnesium silicofluoride, the mineral powder is ground barium sulfate, kaolin, wilkinite, vitriol is sal epsom, barium sulfate, and this auxiliary agent is made up of one or more compounds in fluorochemical, mineral powder, the vitriol; Described tensio-active agent is that a kind of in poly amic acid, sodium polyacrylate, Walocel MT 20.000PV, Natvosol, Xylo-Mucine, sodium alginate, Teepol, xylogen sodium sulfate, dodecylbenzene ammonium sulfate, the dodecylbenzene calcium sulfate or more than one compound are formed.
The low reflection of described glass printing opacity liquid is by hydrofluoric acid, hydrochloric acid, sulfuric acid, and nitric acid and water are pressed 2:2:1:1; 4 weight ratio is formulated, and the mass concentration of hydrofluoric acid is 40%, the mass concentration of hydrochloric acid is 31%, the vitriolic mass concentration is 96%, and the mass concentration of nitric acid is 55%.
The hydrochloric acid that preparation low-reflection glass frosted liquid uses as mass concentration at 20～31% technical-grade hydrochloric acid or 37% analytical pure hydrochloric acid.
The preparation method of this low-reflection glass that proposes according to above technical scheme, not only make the reflectivity of the low-reflection glass goods that obtain after the processing be lower than 2%, and make whole technological process very easy, can provide the good technical support for making reducing cost of low-reflection glass.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
Further set forth the present invention below in conjunction with Figure of description, and provide embodiments of the invention.
Embodiment
One, the preparation of material
1, low reflection frosting powder preparation (1) (by weight percentage)
Ammonium bifluoride 50%
Potassium hydrogen fluoride 10%
Potassium fluoborate 10%
Calcium Fluoride (Fluorspan) 10%
Ground barium sulfate 8%
Kaolin 5%
Barium sulfate 5%
Sodium polyacrylate 0.5%
Natvosol 1.5%
The inorganic fluoride that adopts in the above-mentioned frosting powder: ammonium bifluoride, potassium hydrogen fluoride, potassium fluoborate also can be dissolved in the water, also can produce the inorganic fluoride of fluorion with other: one or more mixtures of material in Neutral ammonium fluoride, sodium bifluoride, the Sodium tetrafluoroborate substitute; The auxiliary agent that adopts in the same above-mentioned frosting powder also can adopt the above-mentioned auxiliary agent of one or several mixture replacings in Sodium Silicofluoride, calcium silicofluoride, magnesium silicofluoride, wilkinite, the sal epsom except Calcium Fluoride (Fluorspan), ground barium sulfate, kaolin, barium sulfate; In addition, the tensio-active agent that adopts in the frosting powder except with adopt can also adopt sodium polyacrylate, the Natvosol in poly amic acid, Walocel MT 20.000PV, Xylo-Mucine, sodium alginate, dodecylbenzene ammonium sulfate sodium, dodecylbenzene ammonium sulfate, Teepol, the xylogen sodium sulfate one or more as an alternative.
Low reflection frosting powder preparation (2) (by weight percentage)
Ammonium bifluoride 45%
Neutral ammonium fluoride 10%
Sodium bifluoride 10%
Sodium Silicofluoride 10%
Ground barium sulfate 8%
Wilkinite 10%
Vitriolate of tartar 5%
Poly amic acid 0.5%
Walocel MT 20.000PV 1.5%
The inorganic fluoride that adopts in the above-mentioned frosting powder: ammonium bifluoride, Neutral ammonium fluoride, sodium bifluoride also can be dissolved in the water with other also can produce the inorganic fluoride of fluorion: one or more mixtures of material in potassium hydrogen fluoride, potassium fluoborate, the Sodium tetrafluoroborate substitute; The auxiliary agent that adopts in the same above-mentioned frosting powder also can adopt the above-mentioned auxiliary agent of one or several mixture replacings in Calcium Fluoride (Fluorspan), calcium silicofluoride, magnesium silicofluoride, kaolin, barium sulfate, the sal epsom except Sodium Silicofluoride, ground barium sulfate, wilkinite, vitriolate of tartar; In addition, the tensio-active agent that adopts in the frosting powder except with adopt Walocel MT 20.000PV, poly amic acid, can also adopt sodium polyacrylate, Natvosol, Xylo-Mucine, sodium alginate, dodecylbenzene ammonium sulfate sodium, dodecylbenzene ammonium sulfate, Teepol, in one or more as an alternative.
Low reflection frosting powder preparation (3) (by weight percentage)
Ammonium bifluoride 50%
Potassium hydrogen fluoride 15%
Sodium tetrafluoroborate 15%
Calcium Fluoride (Fluorspan) 4.5%
Ground barium sulfate 10%
Sal epsom 5%
Xylogen sodium sulfate 0.5%
The inorganic fluoride that adopts in the above-mentioned frosting powder: Neutral ammonium fluoride, potassium hydrogen fluoride, Sodium tetrafluoroborate, also can be dissolved in the water with other and also can produce the inorganic fluoride of fluorion: one or more mixtures of material in Neutral ammonium fluoride, sodium bifluoride, the fluoroboric acid first substitute; The auxiliary agent that adopts in the same above-mentioned frosting powder except Calcium Fluoride (Fluorspan), ground barium sulfate, sal epsom,, also can adopt the above-mentioned auxiliary agent of one or several mixture replacings in Sodium Silicofluoride, calcium silicofluoride, magnesium silicofluoride, kaolin, wilkinite, the barium sulfate; In addition, the tensio-active agent that adopts in the frosting powder except with adopt can also adopt the xylogen sodium sulfate in poly amic acid, Walocel MT 20.000PV, Natvosol, Xylo-Mucine, sodium alginate, dodecylbenzene ammonium sulfate sodium, dodecylbenzene ammonium sulfate, Teepol, the sodium polyacrylate one or more as an alternative.
2, the preparation of low-reflection glass frosted liquid
Being 20～37% hydrochloric acid with the frosting powder for preparing and mass concentration mixes in PVC or plastic containers according to the weight proportion of 1:0.2～1:1, evenly stirs after 20～48 hours and makes the low-reflection glass frosted liquid.
3, the preparation of the low reflection of glass printing opacity liquid
With mass concentration is that 40% hydrofluoric acid, concentration are that 31% hydrochloric acid, concentration are that 96% sulfuric acid, concentration are 55% nitric acid and the water low reflection of the weight ratio formulate glass printing opacity liquid according to 2:2:1:1:4.Concrete making method is: the water with proportioning places plastic containers earlier, adds hydrofluoric acid, hydrochloric acid, sulfuric acid and the nitric acid of proportioning more in regular turn, when treating that this mixing solutions is reduced to room temperature the low reflection of available glass printing opacity liquid.
Two, low-reflection glass production process
1, cleans sheet glass and simultaneously stick the PVC film at it;
2, the sheet glass of above-mentioned pad pasting is put into the container that fills the low-reflection glass frosted liquid and carried out 5～300 seconds of frosting reaction, it is clean with the clear water spray to take out the back, obtains transmittance at 40～60% reflecting glass basic pattern;
3, above-mentioned transmittance is put into the container that fills the low reflection of glass printing opacity liquid, reaction treatment 2～20 minutes at 40～60% reflecting glass basic pattern;
4, take out the reflecting glass basic pattern handled, remove the PVC film, after washing, dry this reflecting glass basic pattern of having handled and promptly get reflectivity less than 2% low-reflection glass product.
Specifically process implementing is for example down:
Example 1
Prepare 30kg frosting powder by the above-claimed cpd weight ratio: each component is weighed to be placed in PVC or the plastic containers, at the uniform velocity stirs 10 minutes, and temperature is no more than 30 ℃ in the control container.Take out frosting powder that 5kg stirs and place in the plastic containers with cover, add the technical hydrochloric acid (proportioning of powder and hydrochloric acid is 1:0.50) of 2.5kg 31%.When just beginning to add hydrochloric acid, the mixing solutions temperature drops to 2～3 ℃, changes with per minute 30 and stirs 20 hours, and mixeding liquid temperature is got back to room temperature, and the frosted liquid slaking reaction is finished.Get the thick sheet glass of 5mm of a 300 * 300mm, one side protects with the PVC film, and another side cleans with glass cleaning solution, uses water wash, and the frosted liquid that is immersed in above-mentioned slaking reacted 20 seconds.Take out washing, dry, again this sheet glass is immersed the low reflection of glass liquid reaction 8 minutes.Take out and use water wash 1 minute.Remove the PVC protective membrane, water cleans up sheet glass, promptly gets reflectivity after drying less than 2% low-reflection glass.
Example 2
Press the low-reflection glass frosting powder of the chemical constitution preparation of example 1.Getting 5.0kg places in the plastic containers with cover, the analytical pure hydrochloric acid 3.5kg (proportioning of powder and hydrochloric acid is 1:0.70) of adding 36% stirred 5 minutes, built container, allow blended frosted liquid reaction 24 hours, obtain a mixed uniformly low-reflection glass frosted liquid.Get the thick sheet glass of 5mm of a 300 * 300mm, one side is protected with the PVC film, and another side is cleaned with glass cleaning solution, uses water wash, after the drip-dry, immerses low-reflection glass frosted liquid reaction 40 seconds.Take out the sheet glass water that has reacted and clean, after the drip-dry, immerse the low reflection of glass liquid reaction 10 minutes again, take out water and cleaned 1 minute.After the drip-dry, remove the PVC protective membrane, water cleans again, dries, and obtains the low-reflection glass of a reflectivity≤2%.
Example 3
Press the low-reflection glass frosting powder of the chemical constitution preparation of example 1.Get 5.0kg and place in the plastic containers, add 24% technical hydrochloric acid 2.0kg (proportioning of powder and hydrochloric acid is 1:0.40), remain a constant speed and stirred 20 hours, obtain the low-reflection glass frosted liquid of a slaking.Get a 300 * 300mm, the sheet glass that 5mm is thick, glass surface is cleaned up, immerse low-reflection glass frosted liquid reaction 60 seconds, the taking-up water cleans, and immerses low-reflection glass printing opacity liquid again 15 minutes, takes out the water spray 2 minutes, dry, obtain a reflectivity less than 2% two-sided low-reflection glass.
Example 4
Press the low-reflection glass frosting powder of the chemical constitution preparation of example 1.Get 5.0kg and place in the plastic containers, add 31% technical hydrochloric acid 3.0kg (proportioning of powder and hydrochloric acid is 1:0.60).Remain a constant speed and stirred 24 hours, obtain the low-reflection glass frosted liquid of a slaking.Get a 300 * 300mm, the sheet glass that 5mm is thick cleans up glass surface, immerses the low-reflection glass frosted liquid and reacts 20 seconds, takes out water and cleans up, and evenly sprays 10 minutes with low-reflection glass surface printing opacity liquid again.Take out water and clean glass surface, dry, obtain a reflectivity less than 2% two-sided low-reflection glass.
Example 5
Press the low-reflection glass frosting powder of the chemical constitution preparation of example 1.Get 5.0kg and place in the plastic containers with cover, add the analytical pure hydrochloric acid (the weight ratio 1:0.80 of powder and hydrochloric acid) of 4.0kg 37%, with hydrochloric acid with after powder mixes, stir, build container, and slaking 24 hours, a mixed uniformly low-reflection glass frosted liquid obtained.The thickness of getting a 300 * 300mm is the dull and stereotyped glass sheet of 5mm glass, glass is cleaned up, after drying, with 200 purpose silk screens with the acid-proof ink silk-screen on glass, 120～160 ℃ of bakings 20～60 minutes, after drying with the low-reflection glass frosted liquid evenly spray take out water and clean up glass another side 260 seconds, immersed low-reflection glass printing opacity liquid again 25 minutes.Taking-up is placed in one 10% the sodium hydroxide solution 2 minutes removing acidproof protection printing ink with water wash, with water wash 1 minute, dry, and obtains a reflectivity less than 2% low-reflection glass.
Claims (6)
1, a kind of preparation method of low-reflection glass, it is characterized in that: incite somebody to action wash clean, and covering the sheet glass that the PVC film is arranged in one side immerses by inorganic fluoride, the frosting powder that auxiliary agent and tensio-active agent are formed, and in the low-reflection glass frosted liquid that constitutes by 1:0.2～1:1 weight ratio by above-mentioned frosting powder and hydrochloric acid 5～60 seconds, make transmittance after the reaction and be 50～60% low-reflection glass basic pattern, then again the low-reflection glass basic pattern being put into the low reflection of glass printing opacity liquid reacted 2～20 minutes, remove the PVC film on the sheet glass one side, clean and promptly get reflectivity after drying less than 2% low-reflection glass.
2, the preparation method of a kind of low-reflection glass as claimed in claim 1 is characterized in that: described frosting powder is made up of the inorganic fluoride that accounts for total amount 65～80%, 18～33% auxiliary agent, 0.5～2% tensio-active agent.
3, the preparation method of a kind of low-reflection glass as claimed in claim 1 is characterized in that: described frosting powder comprises the inorganic fluoride that can be dissolved in the water and can produce fluorion: one or more in ammonium bifluoride, Neutral ammonium fluoride, potassium hydrogen fluoride, sodium bifluoride, potassium fluoborate, the Sodium tetrafluoroborate; Described auxiliary agent is water-fast fluorochemical, mineral powder, vitriol composition, fluorochemical is Sodium Silicofluoride, Calcium Fluoride (Fluorspan), Sodium Silicofluoride, calcium silicofluoride, magnesium silicofluoride, the mineral powder is that ground barium sulfate, kaolin, wilkinite, vitriol are sal epsom, barium sulfate, and this auxiliary agent is made up of one or more compounds in fluorochemical, mineral powder, the vitriol; Described tensio-active agent is one or more in poly amic acid, sodium polyacrylate, Walocel MT 20.000PV, Natvosol, Xylo-Mucine, sodium alginate, dodecylbenzene ammonium sulfate, Teepol, xylogen sodium sulfate, dodecylbenzene calcium sulfate, the sodium polyacrylate.
4, the preparation method of a kind of low-reflection glass as claimed in claim 1 is characterized in that: the low reflection of described glass printing opacity liquid is by hydrofluoric acid, hydrochloric acid, sulfuric acid, and nitric acid and water are pressed 2:2:1:1; 4 weight ratio is formulated, and the concentration of the hydrofluoric acid that is adopted is 40%, concentration of hydrochloric acid is 31%, sulfuric acid concentration is %, and concentration of nitric acid is %
5, the preparation method of a kind of low-reflection glass as claimed in claim 1 is characterized in that: the hydrochloric acid that preparation low-reflection glass frosted liquid uses as concentration at 20～37% technical grade or analytical pure hydrochloric acid.
6, the preparation method of a kind of low-reflection glass as claimed in claim 1, it is characterized in that: described mass concentration of penetrating the hydrofluoric acid that printing opacity liquid adopts is 40%, the mass concentration of hydrochloric acid is 31%, the vitriolic mass concentration is 96%, and the mass concentration of nitric acid is 55%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913772A (en) * | 2010-09-02 | 2010-12-15 | 上海多林化工科技有限公司 | One-step method for manufacturing low-reflection glass |
| CN102674704A (en) * | 2011-03-11 | 2012-09-19 | 北京市太阳能研究所有限公司 | Preparation method of porous nano silicon dioxide anti-reflection film |
| CN102887647A (en) * | 2012-10-11 | 2013-01-23 | 郑州恒昊玻璃技术有限公司 | Process for producing anti-glare glass by using high-boron silicon and high-aluminium silicon glasses |
| CN103011610A (en) * | 2012-12-20 | 2013-04-03 | 龙岩市和达机械有限公司 | Method for processing anti-dazzle glass |
| CN105263877A (en) * | 2011-11-02 | 2016-01-20 | 康宁股份有限公司 | Method for sparkle control and articles thereof |
| CN106946467A (en) * | 2017-04-27 | 2017-07-14 | 东莞市银泰玻璃有限公司 | Make anti-dazzle mobile phone screen glass technology |
| CN108795111A (en) * | 2018-06-11 | 2018-11-13 | 张家港宝视特影视器材有限公司 | The anti-dazzle coating material of projection screen, projection screen and preparation method thereof |
| CN110981208A (en) * | 2019-12-17 | 2020-04-10 | 河南豫科光学科技股份有限公司 | Preparation process of ultra-white glass substrate |
| CN111908799A (en) * | 2020-07-30 | 2020-11-10 | 杭州玺匠文化创意股份有限公司 | Manufacturing method of extinction glass |
| CN115490436A (en) * | 2022-09-23 | 2022-12-20 | 新福兴玻璃工业集团有限公司 | Antireflection magnesium fluoride coated glass and online preparation method thereof |
| CN115636591A (en) * | 2021-12-31 | 2023-01-24 | 深圳市海风润滑技术有限公司 | Glass frosting powder and glass frosting liquid |
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2009
- 2009-04-01 CN CN200910057014A patent/CN101531464A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913772A (en) * | 2010-09-02 | 2010-12-15 | 上海多林化工科技有限公司 | One-step method for manufacturing low-reflection glass |
| CN102674704A (en) * | 2011-03-11 | 2012-09-19 | 北京市太阳能研究所有限公司 | Preparation method of porous nano silicon dioxide anti-reflection film |
| CN105263877B (en) * | 2011-11-02 | 2018-05-11 | 康宁股份有限公司 | Method and its product for control of glistening |
| CN105263877A (en) * | 2011-11-02 | 2016-01-20 | 康宁股份有限公司 | Method for sparkle control and articles thereof |
| CN102887647A (en) * | 2012-10-11 | 2013-01-23 | 郑州恒昊玻璃技术有限公司 | Process for producing anti-glare glass by using high-boron silicon and high-aluminium silicon glasses |
| CN102887647B (en) * | 2012-10-11 | 2015-10-14 | 郑州恒昊玻璃技术有限公司 | The technique of glare proof glass is produced with high borosilicate, high aluminosilicate glass |
| CN103011610A (en) * | 2012-12-20 | 2013-04-03 | 龙岩市和达机械有限公司 | Method for processing anti-dazzle glass |
| CN106946467A (en) * | 2017-04-27 | 2017-07-14 | 东莞市银泰玻璃有限公司 | Make anti-dazzle mobile phone screen glass technology |
| CN108795111A (en) * | 2018-06-11 | 2018-11-13 | 张家港宝视特影视器材有限公司 | The anti-dazzle coating material of projection screen, projection screen and preparation method thereof |
| CN110981208A (en) * | 2019-12-17 | 2020-04-10 | 河南豫科光学科技股份有限公司 | Preparation process of ultra-white glass substrate |
| CN111908799A (en) * | 2020-07-30 | 2020-11-10 | 杭州玺匠文化创意股份有限公司 | Manufacturing method of extinction glass |
| CN115636591A (en) * | 2021-12-31 | 2023-01-24 | 深圳市海风润滑技术有限公司 | Glass frosting powder and glass frosting liquid |
| CN115490436A (en) * | 2022-09-23 | 2022-12-20 | 新福兴玻璃工业集团有限公司 | Antireflection magnesium fluoride coated glass and online preparation method thereof |
| CN115490436B (en) * | 2022-09-23 | 2024-02-02 | 新福兴玻璃工业集团有限公司 | Anti-reflection magnesium fluoride coated glass and online preparation method thereof |
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