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CN105948521A - Etching treatment liquid for preparing antireflection glass - Google Patents

Etching treatment liquid for preparing antireflection glass Download PDF

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Publication number
CN105948521A
CN105948521A CN201610553312.4A CN201610553312A CN105948521A CN 105948521 A CN105948521 A CN 105948521A CN 201610553312 A CN201610553312 A CN 201610553312A CN 105948521 A CN105948521 A CN 105948521A
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glass
etching treatment
treatment solution
etching
reflection
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禹建丽
李金钟
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Zhengzhou University of Aeronautics
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Zhengzhou University of Aeronautics
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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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  • Surface Treatment Of Glass (AREA)

Abstract

本发明涉及一种用于制备减反射玻璃的蚀刻处理液，由以下重量百分比的原料组成：H2SO4 8.2‑9.6%、Na2SiF6 1.8‑2.2%、ZnCl2 4.5‑5.5%、NH4HF2 21.5‑22.5%、CaF2 3.6‑4.2%、(NH4)2SO4 3.6‑4.2%、K2SO4 2.1‑2.5%、十二烷基葡萄糖苷1.6‑1.8%、羟乙基纤维素2.2‑2.4%和水46‑50%。本发明的蚀刻处理液成本低且较稳定，利用本发明的蚀刻处理液制备减反射玻璃，可大幅度提高玻璃成品率，防眩效果好，并且蚀刻液处理液可回收，进行防污染处理或者回收利用。The invention relates to an etching treatment solution for preparing anti-reflection glass, which is composed of the following raw materials in weight percentage: H 2 SO 4 8.2-9.6%, Na 2 SiF 6 1.8-2.2%, ZnCl 2 4.5-5.5%, NH 4 HF 2 21.5‑22.5%, CaF 2 3.6‑4.2%, (NH 4 ) 2 SO 4 3.6‑4.2%, K 2 SO 4 2.1‑2.5%, dodecyl glucoside 1.6‑1.8%, hydroxyethyl Cellulose 2.2‑2.4% and water 46‑50%. The etching treatment solution of the present invention is low in cost and relatively stable. Using the etching treatment solution of the present invention to prepare anti-reflection glass can greatly increase the yield of glass, has a good anti-glare effect, and the etching treatment solution can be recycled for anti-pollution treatment or recycle and re-use.

Description

一种用于制备减反射玻璃的蚀刻处理液A kind of etching treatment liquid for preparing anti-reflection glass

技术领域technical field

本发明涉及减反射玻璃制备技术领域，具体涉及一种用于制备减反射玻璃的蚀刻处理液。The invention relates to the technical field of anti-reflection glass preparation, in particular to an etching treatment liquid for preparing anti-reflection glass.

背景技术Background technique

玻璃因其强度高、光学性能优良、长期工作稳定性好(不易老化)等优点，在日常生活中被广泛运用。但是由于玻璃表面较高的反射率，往往造成“眩光袭击”,也就是我们常说的“光污染”，例如我们在操作电脑时常常为显示器外面的景物在显示器表面的反射而无法看清显示内容而烦恼；当我们驻足于玻璃橱窗前探究橱窗内景物时，玻璃表面反光往往使我们无法清晰的观察到窗内景物等等，这些都是因为玻璃表面的光反射引起的。要减少玻璃发射光的影响，将玻璃进行无光处理可以起到良好的效果。Glass is widely used in daily life because of its advantages such as high strength, excellent optical properties, and good long-term working stability (not easy to age). However, due to the high reflectivity of the glass surface, it often causes "glare attack", which is what we often call "light pollution". And trouble; when we stop in front of the glass window to explore the scenery inside the window, the reflection of the glass surface often prevents us from clearly observing the scenery inside the window, etc., all of which are caused by the light reflection on the glass surface. To reduce the impact of light emitted by the glass, matting the glass can have a good effect.

目前国内外市场上所销售的减反射玻璃一般通过两种方法实现的，一种是对玻璃表面进行镀膜来实现，另一种是通过酸蚀刻玻璃表面来实现的。镀膜减反射玻璃的防眩效果较好，但是生产成本高，并且镀膜很容易脱落，表面容易留下划痕等，从而影响透明度。一般的酸蚀减反射玻璃是先对玻璃表面进行蒙砂，然后对玻璃蒙砂面进行抛光，虽然可克服镀膜易脱落、表面易划损的缺陷，但这种生产工艺相对复杂，生产周期长，成品率低。为了改进酸蚀减反射玻璃生产工艺，专利公开号为CN101654330的中国专利描述了用成分为氢氟酸、盐酸、氟化氢铵、阿拉伯树胶粉和聚乙二醇的玻璃防眩蚀刻液加工减反射玻璃的生产工艺，虽然该生产工艺简单，操作方便，但阿拉伯树胶粉价格昂贵，成本较高，且由于盐酸挥发性强，蚀刻液稳定性差，不易被回收利用。专利公开号为CN101215097的中国专利描述了用成分为盐酸或硫酸、氟化氢铵、硫酸铵、氟化钙和硫酸钾的减反射玻璃蚀刻液制备减反射玻璃的工艺，同样由于盐酸挥发性强，蚀刻液稳定性差，不易被回收利用。At present, the anti-reflection glass sold in the domestic and foreign markets is generally realized by two methods, one is to coat the glass surface, and the other is to etch the glass surface with acid. The anti-glare effect of coated anti-reflection glass is better, but the production cost is high, and the coating film is easy to fall off, and the surface is easy to leave scratches, etc., which affects the transparency. Generally, the acid-etched anti-reflection glass first frosts the glass surface, and then polishes the frosted glass surface. Although it can overcome the defects that the coating is easy to fall off and the surface is easy to scratch, the production process is relatively complicated and the production cycle is long. , The yield is low. In order to improve the production process of acid-etched anti-reflection glass, Chinese Patent Publication No. CN101654330 describes the processing of anti-reflection glass with anti-glare etching solution consisting of hydrofluoric acid, hydrochloric acid, ammonium bifluoride, gum arabic powder and polyethylene glycol. Although the production process of glass is simple and easy to operate, the gum arabic powder is expensive and the cost is high, and due to the strong volatility of hydrochloric acid and the poor stability of the etching solution, it is not easy to be recycled. The Chinese patent with the patent publication number CN101215097 describes the process of preparing anti-reflective glass with an anti-reflective glass etching solution consisting of hydrochloric acid or sulfuric acid, ammonium bifluoride, ammonium sulfate, calcium fluoride and potassium sulfate. Also due to the strong volatility of hydrochloric acid, etching Poor liquid stability, not easy to be recycled.

发明内容Contents of the invention

本发明的目的是为解决上述技术问题的不足，提供一种用于制备减反射玻璃的蚀刻处理液，克服现有方法成本高、蚀刻液不稳定的缺陷。The object of the present invention is to solve the shortcomings of the above technical problems, provide an etching treatment solution for preparing anti-reflection glass, and overcome the defects of high cost and unstable etching solution in the existing method.

本发明为解决上述技术问题的不足，所采用的技术方案是：一种用于制备减反射玻璃的蚀刻处理液，依照本蚀刻处理液制成的防眩玻璃，其透过率＞94.8%，且可大于98%；雾度＞1.4%；锐化＜72.2%，且可小于66.3%；光的反射率＜6.9%，蚀刻处理液由以下重量百分比的原料组成：H2SO4 8.2-9.6%、Na2SiF6 1.8-2.2%、ZnCl2 4.5-5.5%、NH4HF2 21.5-22.5%、CaF2 3.6-4.2%、(NH4)2SO4 3.6-4.2%、K2SO4 2.1-2.5%、十二烷基十二烷基葡萄糖苷苷1.6-1.8%、羟乙基纤维素2.2-2.4%和水46-50%。In order to solve the deficiencies of the above-mentioned technical problems, the technical solution adopted by the present invention is: an etching treatment solution for preparing anti-reflection glass, and the anti-glare glass made according to the etching treatment solution has a transmittance > 94.8%, And can be greater than 98%; Haze >1.4%; Sharpening < 72.2%, and can be less than 66.3%; Light reflectivity < 6.9%. The etching treatment solution is composed of the following raw materials in weight percentage: H 2 SO 4 8.2-9.6 %, Na 2 SiF 6 1.8-2.2%, ZnCl 2 4.5-5.5%, NH 4 HF 2 21.5-22.5%, CaF 2 3.6-4.2%, (NH 4 ) 2 SO 4 3.6-4.2%, K 2 SO 4 2.1-2.5%, lauryl lauryl glucoside 1.6-1.8%, hydroxyethyl cellulose 2.2-2.4% and water 46-50%.

作为本发明一种用于制备减反射玻璃的蚀刻处理液的进一步优化：由以下重量百分比的原料组成：H2SO48.6%、Na2SiF6 2%、ZnCl2 5%、NH4HF2 22.1%、CaF23.8%、(NH4)2SO43.8%、K2SO42.3%、十二烷基十二烷基葡萄糖苷苷1.6%、羟乙基纤维素2.2%和水48.6%。As a further optimization of the etching treatment liquid for preparing anti-reflection glass in the present invention: it is composed of the following raw materials in weight percentage: H 2 SO 4 8.6%, Na 2 SiF 6 2%, ZnCl 2 5%, NH 4 HF 2 22.1%, CaF 2 3.8%, (NH 4 ) 2 SO 4 3.8%, K 2 SO 4 2.3%, Dodecyldodecyl Glucoside 1.6%, Hydroxyethylcellulose 2.2% and Water 48.6% .

有益效果Beneficial effect

本发明的减反射玻璃制备用蚀刻液配方进行了成分以及各成分含量的优化，一方面，选择了Na2SiF6 、NH4HF2和CaF2的组合，并且优化了三种氟化物之间的配比，使其性能协同，在提高离子强度的同时储备了足够的氟离子；ZnCl2 和K2SO4 配合加入到体系中，调节了体系的盐度，促进晶核的形成和晶粒的细化，使蚀刻层变薄，保持影像的真实，在蚀刻液中加入(NH4)2SO4，相互配合能在体系中形成氢氧根离子，本发明的玻璃蚀刻液在ZnCl2 和K2SO4 和(NH4)2SO4的辅助下对玻璃的蚀刻效果更加好；另一方面，在羟乙基纤维素和十二烷基十二烷基葡萄糖苷苷的辅助下，可以有效地使蚀刻液中的不溶性填料均匀的分散在溶液中，提高蚀刻液的稳定性，并且还能够调节玻璃的蚀刻反应速度，十二烷基十二烷基葡萄糖苷苷分子上的羟基易与硫酸和玻璃之间形成氢键，因此可以作为硫酸与玻璃表面反应的媒介，以控制它们反应速度和表面反应的均匀性，从而制得的成本低且产品表面颗粒细腻，透过率高的防眩玻璃。依照本蚀刻处理液制成的防眩玻璃，其透过率＞94.8%，且可大于98%；雾度＞1.4%；锐化＜72.2%，且可小于66.3%；光的反射率＜6.9%。The formulation of the etchant for preparing anti-reflection glass of the present invention optimizes the components and the content of each component. On the one hand, the combination of Na 2 SiF 6 , NH 4 HF 2 and CaF 2 is selected, and the relationship between the three fluorides is optimized. The matching ratio makes its performance synergistic, and reserves enough fluorine ions while increasing the ionic strength; ZnCl 2 and K 2 SO 4 are added to the system to adjust the salinity of the system, promote the formation of crystal nuclei and crystal grains The thinning of the etching layer makes the etching layer thinner and keeps the image true. Add (NH 4 ) 2 SO 4 in the etching solution, and cooperate with each other to form hydroxide ions in the system. The glass etching solution of the present invention can be used in ZnCl 2 and With the assistance of K 2 SO 4 and (NH 4 ) 2 SO 4 , the etching effect on glass is better; on the other hand, with the assistance of hydroxyethyl cellulose and dodecyl dodecyl glucoside, it can Effectively disperse the insoluble filler in the etching solution evenly in the solution, improve the stability of the etching solution, and also adjust the etching reaction speed of the glass. The hydroxyl group on the dodecyl dodecyl glucoside molecule is easy to combine with Hydrogen bonds are formed between sulfuric acid and glass, so it can be used as a medium for the reaction between sulfuric acid and glass surface to control their reaction speed and uniformity of surface reaction, so as to obtain low-cost, fine-grained product surface particles, and high transmittance. Dazzling glass. The anti-glare glass made according to this etching solution has a transmittance > 94.8%, and can be greater than 98%; haze >1.4%; sharpening < 72.2%, and can be less than 66.3%; light reflectance < 6.9 %.

具体实施方式detailed description

实施例1Example 1

一种用于制备减反射玻璃的蚀刻处理液，由以下重量百分比的原料组成：H2SO48.2%、Na2SiF6 1.8%、ZnCl2 4.5%、NH4HF2 21.5%、CaF2 4.2%、(NH4)2SO4 4.2%、K2SO4 2.5%、十二烷基葡萄糖苷1.8%、羟乙基纤维素2.2%和水49.1%。An etching treatment solution for preparing anti-reflection glass, which is composed of the following raw materials in weight percentage: H 2 SO 4 8.2%, Na 2 SiF 6 1.8%, ZnCl 2 4.5%, NH 4 HF 2 21.5%, CaF 2 4.2% %, (NH 4 ) 2 SO 4 4.2%, K 2 SO 4 2.5%, Lauryl Glucoside 1.8%, Hydroxyethyl Cellulose 2.2% and Water 49.1%.

利用上述蚀刻处理液制备减反射玻璃：Utilize above-mentioned etching treatment solution to prepare anti-reflection glass:

(1)、按蚀刻液的原料配方称取各原料，将水加入H2SO4中，搅拌均匀后加入Na2SiF6 、NH4HF2 和CaF2，搅拌均匀后再加入ZnCl2 、(NH4)2SO4 和K2SO4搅拌均匀，之后加入十二烷基葡萄糖苷和羟乙基纤维素，搅拌均匀后进行陈化（陈化时间为24小时）得到减反射玻璃蚀刻液；(1) Weigh each raw material according to the raw material formula of the etching solution, add water into H 2 SO 4 , stir well, add Na 2 SiF 6 , NH 4 HF 2 and CaF 2 , stir well, then add ZnCl 2 , ( Stir NH 4 ) 2 SO 4 and K 2 SO 4 evenly, then add dodecyl glucoside and hydroxyethyl cellulose, stir evenly and then age (the aging time is 24 hours) to obtain an anti-reflective glass etching solution;

(2)、将预蚀刻的玻璃用清洗剂（清洗剂为丙酮和乙酸丁酯的1:1比例混合物）进行清洗并干燥；(2) Clean and dry the pre-etched glass with a cleaning agent (the cleaning agent is a 1:1 mixture of acetone and butyl acetate);

(3)、将清洗好的玻璃不需蚀刻的一面用石蜡覆盖；(3) Cover the side of the cleaned glass that does not need to be etched with paraffin;

(4)、将玻璃浸入配制好的蚀刻液中浸泡，控制蚀刻液的温度为20℃，蚀刻时间为10min进行蚀刻处理；(4), immerse the glass in the prepared etching solution, control the temperature of the etching solution to be 20° C., and the etching time to be 10 minutes for etching treatment;

(5)、取出玻璃制品用清水冲洗,然后放入260℃的烘干箱内，烘干70min，关闭烘箱加热开关，自然降温到50℃时从烘箱中取出，制成减反射玻璃成品。(5) Take out the glass product and rinse it with clean water, then put it into a drying oven at 260°C, dry it for 70 minutes, turn off the oven heating switch, take it out of the oven when the temperature is naturally lowered to 50°C, and make a finished anti-reflection glass product.

实施例2Example 2

一种用于制备减反射玻璃的蚀刻处理液，由以下重量百分比的原料组成：H2SO48.6%、Na2SiF6 2%、ZnCl2 5%、NH4HF2 22.1%、CaF23.8%、(NH4)2SO43.8%、K2SO42.3%、十二烷基葡萄糖苷1.6%、羟乙基纤维素1.8%和水49。An etching treatment solution for preparing anti-reflection glass, which is composed of the following raw materials in weight percentage: H 2 SO 4 8.6%, Na 2 SiF 6 2%, ZnCl 2 5%, NH 4 HF 2 22.1%, CaF 2 3.8 %, (NH 4 ) 2 SO 4 3.8%, K 2 SO 4 2.3%, Lauryl Glucoside 1.6%, Hydroxyethyl Cellulose 1.8% and Water 49%.

利用上述蚀刻处理液制备减反射玻璃：Utilize above-mentioned etching treatment solution to prepare anti-reflection glass:

(1)、按蚀刻液的原料配方称取各原料，将水加入H2SO4中，搅拌均匀后加入Na2SiF6 、NH4HF2 和CaF2，搅拌均匀后再加入ZnCl2 、(NH4)2SO4 和K2SO4搅拌均匀，之后加入十二烷基葡萄糖苷和羟乙基纤维素，搅拌均匀后进行陈化（陈化时间为24小时）得到减反射玻璃蚀刻液；(1) Weigh each raw material according to the raw material formula of the etching solution, add water into H 2 SO 4 , stir well, add Na 2 SiF 6 , NH 4 HF 2 and CaF 2 , stir well, then add ZnCl 2 , ( Stir NH 4 ) 2 SO 4 and K 2 SO 4 evenly, then add dodecyl glucoside and hydroxyethyl cellulose, stir evenly and then age (the aging time is 24 hours) to obtain an anti-reflective glass etching solution;

(2)、将预蚀刻的玻璃用清洗剂（清洗剂为丙酮和乙酸丁酯的1:1比例混合物）进行清洗并干燥；(2) Clean and dry the pre-etched glass with a cleaning agent (the cleaning agent is a 1:1 mixture of acetone and butyl acetate);

(3)、将清洗好的玻璃不需蚀刻的一面用石蜡覆盖；(3) Cover the side of the cleaned glass that does not need to be etched with paraffin;

(4)、将玻璃浸入配制好的蚀刻液中浸泡，控制蚀刻液的温度为20℃，蚀刻时间为10min进行蚀刻处理；(4), immerse the glass in the prepared etching solution, control the temperature of the etching solution to be 20° C., and the etching time to be 10 minutes for etching treatment;

(5)、取出玻璃制品用清水冲洗,然后放入260℃的烘干箱内，烘干70min，关闭烘箱加热开关，自然降温到50℃时从烘箱中取出，制成减反射玻璃成品。(5) Take out the glass product and rinse it with clean water, then put it into a drying oven at 260°C, dry it for 70 minutes, turn off the oven heating switch, take it out of the oven when the temperature is naturally lowered to 50°C, and make a finished anti-reflection glass product.

实施例3Example 3

一种用于制备减反射玻璃的蚀刻处理液，由以下重量百分比的原料组成：H2SO49.6%、Na2SiF62.2%、ZnCl2 5.5%、NH4HF2 22.5%、CaF23.6%、(NH4)2SO43.6%、K2SO42.1%、十二烷基葡萄糖苷1.6%、羟乙基纤维素2.4%和水46.9。An etching treatment solution for preparing anti-reflection glass, which is composed of the following raw materials in weight percentage: H 2 SO 4 9.6%, Na 2 SiF 6 2.2%, ZnCl 2 5.5%, NH 4 HF 2 22.5%, CaF 2 3.6% %, (NH 4 ) 2 SO 4 3.6%, K 2 SO 4 2.1%, Lauryl Glucoside 1.6%, Hydroxyethyl Cellulose 2.4% and Water 46.9%.

利用上述蚀刻处理液制备减反射玻璃：Utilize above-mentioned etching treatment solution to prepare anti-reflection glass:

(1)、按蚀刻液的原料配方称取各原料，将水加入H2SO4中，搅拌均匀后加入Na2SiF6 、NH4HF2 和CaF2，搅拌均匀后再加入ZnCl2 、(NH4)2SO4 和K2SO4搅拌均匀，之后加入十二烷基葡萄糖苷和羟乙基纤维素，搅拌均匀后进行陈化（陈化时间为24小时）得到减反射玻璃蚀刻液；(1) Weigh each raw material according to the raw material formula of the etching solution, add water into H 2 SO 4 , stir well, add Na 2 SiF 6 , NH 4 HF 2 and CaF 2 , stir well, then add ZnCl 2 , ( Stir NH 4 ) 2 SO 4 and K 2 SO 4 evenly, then add dodecyl glucoside and hydroxyethyl cellulose, stir evenly and then age (the aging time is 24 hours) to obtain an anti-reflective glass etching solution;

(2)、将预蚀刻的玻璃用清洗剂（清洗剂为丙酮和乙酸丁酯的1:1比例混合物）进行清洗并干燥；(2) Clean and dry the pre-etched glass with a cleaning agent (the cleaning agent is a 1:1 mixture of acetone and butyl acetate);

(3)、将清洗好的玻璃不需蚀刻的一面用石蜡覆盖；(3) Cover the side of the cleaned glass that does not need to be etched with paraffin;

(4)、将玻璃浸入配制好的蚀刻液中浸泡，控制蚀刻液的温度为20℃，蚀刻时间为10min进行蚀刻处理；(4), immerse the glass in the prepared etching solution, control the temperature of the etching solution to be 20° C., and the etching time to be 10 minutes for etching treatment;

(5)、取出玻璃制品用清水冲洗,然后放入260℃的烘干箱内，烘干70min，关闭烘箱加热开关，自然降温到50℃时从烘箱中取出，制成减反射玻璃成品。(5) Take out the glass product and rinse it with clean water, then put it into a drying oven at 260°C, dry it for 70 minutes, turn off the oven heating switch, take it out of the oven when the temperature is naturally lowered to 50°C, and make a finished anti-reflection glass product.

减反射玻璃检测数据Anti-reflection glass test data

将未处理的普通玻璃与实施例1-3处理后的减反射玻璃进行对比，结果如下：The untreated common glass is compared with the anti-reflection glass treated in Examples 1-3, and the results are as follows:

。 .

Claims (2)

1.一种用于制备减反射玻璃的蚀刻处理液，依照本蚀刻处理液制成的防眩玻璃，其透过率＞94.8%，且可大于98%；雾度＞1.4%；锐化＜72.2%，且可小于66.3%；光的反射率＜6.9%；其特征在于：蚀刻处理液由以下重量百分比的原料组成：H2SO4 8.2-9.6%、Na2SiF6 1.8-2.2%、ZnCl2 4.5-5.5%、NH4HF2 21.5-22.5%、CaF2 3.6-4.2%、(NH4)2SO4 3.6-4.2%、K2SO4 2.1-2.5%、十二烷基葡萄糖苷1.6-1.8%、羟乙基纤维素2.2-2.4%和水46-50%。1. An etching treatment solution for preparing anti-reflection glass, according to the anti-glare glass made by the etching treatment solution, its transmittance > 94.8%, and can be greater than 98%; haze >1.4%; sharpening < 72.2%, and can be less than 66.3%; light reflectance <6.9%; characterized in that: the etching treatment solution is composed of the following raw materials in weight percentage: H 2 SO 4 8.2-9.6%, Na 2 SiF 6 1.8-2.2%, ZnCl 2 4.5-5.5%, NH 4 HF 2 21.5-22.5%, CaF 2 3.6-4.2%, (NH 4 ) 2 SO 4 3.6-4.2%, K 2 SO 4 2.1-2.5%, dodecyl glucoside 1.6-1.8%, hydroxyethyl cellulose 2.2-2.4% and water 46-50%. 2.如权利要求1所述一种用于制备减反射玻璃的蚀刻处理液，其特征在于：由以下重量百分比的原料组成：H2SO48.6%、Na2SiF6 2%、ZnCl2 5%、NH4HF2 22.1%、CaF23.8%、(NH4)2SO43.8%、K2SO42.3%、十二烷基葡萄糖苷1.6%、羟乙基纤维素2.2%和水48.6%。2. An etching treatment solution for preparing anti-reflection glass according to claim 1, characterized in that: it consists of the following raw materials in weight percentage: H 2 SO 4 8.6%, Na 2 SiF 6 2%, ZnCl 2 5 %, NH 4 HF 2 22.1%, CaF 2 3.8%, (NH 4 ) 2 SO 4 3.8%, K 2 SO 4 2.3%, dodecyl glucoside 1.6%, hydroxyethyl cellulose 2.2% and water 48.6% %.
CN201610553312.4A 2016-07-14 2016-07-14 Etching treatment liquid for preparing antireflection glass Pending CN105948521A (en)

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