Environment-friendly optical anti-reflection coating material and preparation method thereof

Abstract

The invention provides the field of coatings, and particularly discloses an environment-friendly optical anti-reflection coating material and a preparation method thereof.The environment-friendly optical anti-reflection coating material is prepared from a mixed base material, a fluoride additive, a polymer, a surfactant and water; the preparation method comprises the following steps: weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight, and mixing to prepare a mixed solution; emulsifying the mixed solution through a high-shear mixer to prepare an emulsion; and filtering the emulsified liquid through filter cloth, and vacuumizing to obtain the required environment-friendly optical anti-reflection coating material. The prepared environment-friendly optical anti-reflection coating material is high in light transmittance and low in organic volatile matter.

Description

Technical Field

[0001] The present application relates to the field of coatings, and in particular to an environmentally friendly optical anti-reflection coating material and a preparation method thereof. Background Art

[0002] Optical anti-reflection coating is a special coating technology designed to increase the transmittance of optical components and reduce their reflection. Optical anti-reflection coating is widely used in various optical devices. By optimizing the characteristics of the coating, the resolution and contrast of optical instruments can be improved, and the image quality can be improved. In high-end optical lenses, optical coatings play the role of anti-reflection, anti-reflection and enhanced dispersion, effectively improving the transmittance and color reproduction performance of the lens.

[0003] In the production of optically transparent coatings, environmentally unfriendly raw materials mainly include materials containing harmful chemicals such as formaldehyde and heavy metals. These materials may release harmful substances during use, causing potential harm to the environment and human health. For example, optical plastic substrates are prone to deformation at high temperatures. Anti-fog coatings developed to solve this problem will pose a threat to the environment and human health if materials containing harmful substances such as formaldehyde are used. Based on the above statements, the present application provides an environmentally friendly optical anti-reflection coating material and a preparation method thereof. Summary of the invention

[0004] The purpose of this application is to reduce the formaldehyde emission of optical anti-reflective coating materials, improve the environmental performance of the production and use of optical anti-reflective coatings, and provide an environmentally friendly optical anti-reflective coating material and a preparation method thereof compared to the prior art.

[0005] In a first aspect, the present application provides an environmentally friendly optical antireflection coating material, comprising the following raw materials in parts by weight: 60-95 parts of a mixed base, 15-25 parts of a fluorine additive, 1-5 parts of a polymer, 1-5 parts of a surfactant, and 5-15 parts of water;

[0006] Preferably, the mixed substrate is prepared by the following method:

[0007] After tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol are uniformly mixed in a mass ratio of 10-15:20-25:3-9:2:1, pH value and ammonia water in a mass ratio of 5-15:1-2 are added for vacuum stirring, and the pH value is adjusted to 5-8, the stirring speed is 500-700r / min, and after forming a mixed base material, it is stored for standby use at a storage temperature of 5-15°C.

[0008] Preferably, the polymer comprises polylactic acid and polyhydroxyalkanoate in a mass ratio of 5-8:3.

[0009] By adopting the above technical scheme, the present application selects tetraethoxysilane, trichlorofluorosilane, acrylate, and polyurethane as the main base materials of the coating. The polyurethane / SiO2 hybrid containing modified SiO2 synthesized in situ by hydrolysis and condensation reaction can enhance the hardness and wear resistance of the coating, and can exhibit a high light transmittance even at a lower silicon content; the addition of trichlorofluorosilane can improve the hydrophobicity of the coating surface, reduce the attachment of dirt and microorganisms on the coating surface, thereby maintaining the cleanliness and functionality of the coating; the addition of acrylate can make the coating dry quickly after application, thereby reducing the curing time; the addition of polyurethane can further improve the flexibility of the coating surface, making the coating resistant to cold and heat shocks.

[0010] Preferably, the polylactic acid is prepared by the following method:

[0011] a. The collected corn and glutinous rice are mixed, washed, soaked, ground, and filtered through a fine mesh to extract the precipitated starch at the bottom;

[0012] b. Mixing starch and Lactobacillus microorganisms in a mass ratio of 50:1.5 and fermenting for 12-13 hours to produce lactic acid;

[0013] c. Adding polyacrylic acid to the prepared lactic acid, performing ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then precipitating and washing the primary polylactic acid with a purification solvent, and obtaining the desired polylactic acid after drying.

[0014] By adopting the above technical solution, polylactic acid and polyhydroxyalkanoates can be completely degraded by microorganisms in nature without causing pollution to the environment. During the production or use of the coating, the content of volatile organic compounds is reduced, thereby improving the environmental performance of the coating material.

[0015] Preferably, the mass ratio of the corn to glutinous rice is 10:3, and the mass ratio of the lactic acid to polyacrylic acid to dichloromethane is 1:0.1-0.2:0.2-0.5.

[0016] Preferably, the heating temperature is 150-190°C, and the drying temperature is 50-70°C.

[0017] Preferably, the purification solvent is prepared by mixing dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:2-4, and the volume fraction of the ethanol solution is 60%-80%.

[0018] In a second aspect, the present application provides a method for preparing an environmentally friendly optical anti-reflection coating material, comprising the following preparation steps:

[0019] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0020] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0021] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0022] Compared with the prior art, the advantages of the present application are as follows: the present application uses tetraethoxysilane, trichlorofluorosilane, acrylate, and polyurethane as the main base materials of the coating, which can enhance the hardness and wear resistance of the coating, and can exhibit a high light transmittance even at a lower silicon content, thereby reducing the adhesion of dirt and microorganisms on the coating surface and maintaining the cleanliness and functionality of the coating; reducing the curing time, and by adding polymers of polylactic acid and polyhydroxyalkanoate, the environmental performance of the coating can be further improved. DETAILED DESCRIPTION

[0023] The present application is further described in detail below with reference to the embodiments.

[0024] Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without making any creative work shall fall within the scope of protection of this application.

[0025] Embodiment 1:

[0026] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 60 parts of a mixed substrate, 15 parts of a fluoride additive, 1 part of a polymer, 1 part of a surfactant, and 5 parts of water;

[0027] The mixed substrate is prepared by the following method:

[0028] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were mixed evenly in a mass ratio of 10:20:3:2:1, and deionized water and ammonia water in a mass ratio of 5:1 were added to adjust the true pH value, and the pH value range was adjusted to 5, the stirring speed was 500r / min, and the mixed substrate was formed and stored for use at a storage temperature of 5°C.

[0029] The polymer comprises polylactic acid and polyhydroxyalkanoate in a mass ratio of 5:3; the polylactic acid is prepared by the following method:

[0030] a. Mix the collected corn and glutinous rice, wash, soak, grind, and filter through a fine mesh to extract the precipitated starch;

[0031] b. Mix starch and Lactobacillus microorganisms in a mass ratio of 50:1.5 and ferment for 12 hours to prepare lactic acid;

[0032] c. Add polyacrylic acid to the prepared lactic acid, carry out ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then use a purification solvent to precipitate and wash the primary polylactic acid, the heating temperature is 150°C, and the required polylactic acid is obtained after drying, and the drying temperature is 50°C.

[0033] The mass ratio of corn and glutinous rice is 10:3, the mass ratio of lactic acid, polyacrylic acid and dichloromethane is 1:0.1:0.2, and the purification solvent is prepared by compounding dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:2, and the volume fraction of the ethanol solution is 60%.

[0034] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0035] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0036] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0037] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0038] Embodiment 2:

[0039] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 70 parts of a mixed substrate, 20 parts of a fluoride additive, 4 parts of a polymer, 3 parts of a surfactant, and 10 parts of water;

[0040] The mixed substrate is prepared by the following method:

[0041] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were mixed evenly in a mass ratio of 13:20:5:2:1, and deionized water and ammonia water in a mass ratio of 10:1 were added to adjust the true pH value, and the pH value range was adjusted to 6. The stirring speed was 600r / min. After forming a mixed substrate, it was stored for use at a storage temperature of 13°C.

[0042] The polymer comprises polylactic acid and polyhydroxyalkanoate in a mass ratio of 7:3; the polylactic acid is prepared by the following method:

[0043] a. Mix the collected corn and glutinous rice, wash, soak, grind, and filter through a fine mesh to extract the precipitated starch;

[0044] b. Mix starch and Lactobacillus microorganisms in a mass ratio of 50:1.5 and ferment for 12 hours to prepare lactic acid;

[0045] c. Add polyacrylic acid to the prepared lactic acid, carry out ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then use a purification solvent to precipitate and wash the primary polylactic acid, the heating temperature is 170°C, and the required polylactic acid is obtained after drying, and the drying temperature is 60°C.

[0046] The mass ratio of corn and glutinous rice is 10:3, the mass ratio of lactic acid, polyacrylic acid and dichloromethane is 1:0.1:0.3, the purification solvent is prepared by compounding dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:3, and the volume fraction of the ethanol solution is 70%.

[0047] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0048] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0049] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0050] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0051] Embodiment 3:

[0052] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 95 parts of a mixed substrate, 25 parts of a fluoride additive, 5 parts of a polymer, 5 parts of a surfactant, and 15 parts of water;

[0053] The mixed substrate is prepared by the following method:

[0054] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were uniformly mixed in a mass ratio of 15:25:9:2:1, and deionized water and ammonia water in a mass ratio of 15:2 were added for vacuum stirring, and the pH value was adjusted to 8 and the stirring speed was 700 r / min. After the mixed substrate was formed, it was stored for use at a storage temperature of 15°C.

[0055] The polymer comprises polylactic acid and polyhydroxyalkanoate in a mass ratio of 8:3; the polylactic acid is prepared by the following method:

[0056] a. The collected corn and glutinous rice are mixed, washed, soaked, ground, and filtered through a fine mesh to extract the precipitated starch at the bottom;

[0057] b. Mixing starch with Lactobacillus microorganisms in a mass ratio of 50:1.5 and fermenting for 13 hours to produce lactic acid;

[0058] c. Add polyacrylic acid to the prepared lactic acid, carry out ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then precipitate and wash the primary polylactic acid with a purification solvent, the heating temperature is 190°C, and the desired polylactic acid is obtained after drying at 70°C.

[0059] The mass ratio of corn and glutinous rice is 10:3, the mass ratio of lactic acid, polyacrylic acid and dichloromethane is 1:0.2:0.5, and the purification solvent is prepared by compounding dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:4, and the volume fraction of the ethanol solution is 80%.

[0060] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0061] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0062] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0063] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0064] Comparative Example 1:

[0065] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 60 parts of a mixed substrate, 15 parts of a fluoride additive, 1 part of a polymer, 1 part of a surfactant, and 5 parts of water;

[0066] The mixed substrate is prepared by the following method:

[0067] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were mixed evenly in a mass ratio of 10:20:3:2:1, and then deionized water and ammonia water in a mass ratio of 5:1 were added for vacuum stirring. The pH value was adjusted to 5 and the stirring speed was 500 r / min. After the mixed substrate was formed, it was stored for use at a storage temperature of 5°C.

[0068] The polymer includes polylactic acid; the polylactic acid is prepared by the following method:

[0069] a. The collected corn and glutinous rice are mixed, washed, soaked, ground, and filtered through a fine mesh to extract the precipitated starch at the bottom;

[0070] b. Mixing starch and Lactobacillus microorganisms in a mass ratio of 50:1.5 and fermenting for 12 hours to produce lactic acid;

[0071] c. Add polyacrylic acid to the prepared lactic acid, carry out ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then precipitate and wash the primary polylactic acid with a purification solvent, the heating temperature is 150°C, and the desired polylactic acid is obtained after drying, and the drying temperature is 50°C.

[0072] The mass ratio of corn and glutinous rice is 10:3, the mass ratio of lactic acid, polyacrylic acid and dichloromethane is 1:0.1:0.2, and the purification solvent is prepared by compounding dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:2, and the volume fraction of the ethanol solution is 60%.

[0073] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0074] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0075] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0076] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0077] Comparative Example 2:

[0078] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 60 parts of a mixed substrate, 15 parts of a fluoride additive, 1 part of a polymer, 1 part of a surfactant, and 5 parts of water;

[0079] The mixed substrate is prepared by the following method:

[0080] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were mixed evenly in a mass ratio of 10:20:3:2:1, and then deionized water and ammonia water in a mass ratio of 5:1 were added for vacuum stirring. The pH value was adjusted to 5 and the stirring speed was 500 r / min. After the mixed substrate was formed, it was stored for use at a storage temperature of 5°C.

[0081] Polymers include polyhydroxyalkanoates;

[0082] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0083] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0084] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0085] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0086] Comparative Example 3:

[0087] The present invention provides an environmentally friendly optical anti-reflection coating material, comprising the following raw materials in parts by weight: 60 parts of a mixed substrate, 15 parts of a fluoride additive, 1 part of a polymer, 1 part of a surfactant, and 5 parts of water;

[0088] The mixed substrate is prepared by the following method:

[0089] Tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol were mixed evenly in a mass ratio of 10:20:3:2:1, and then deionized water and ammonia water in a mass ratio of 5:1 were added for vacuum stirring. The pH value was adjusted to 5 and the stirring speed was 500 r / min. After the mixed substrate was formed, it was stored for use at a storage temperature of 5°C.

[0090] The polymer includes polymethyl methacrylate.

[0091] A method for preparing an environmentally friendly optical anti-reflection coating material comprises the following preparation steps:

[0092] S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution;

[0093] S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion;

[0094] S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

[0095] Performance testing:

[0096] According to the test standards, the environmentally friendly optical anti-reflection coating materials prepared in Examples 1-3 of the present application and Comparative Examples 1-3 were coated on the glass surface to prepare test samples, and the sample performances were tested after being placed in a test room at a temperature of 25°C and a relative humidity of 55% for 2 hours.

[0097] According to GB / T 23986-2009 “Determination of Volatile Organic Compound (VOC) Content of Paints and Varnishes - Gas Chromatography”, the air quality in the indoor environment after the sample is coated is tested. The coating range of the test piece is 40cmx40cm and the coating thickness is 100nm.

[0098] According to ISO 4040 "Determination of light transmittance and reflectance of optical coatings", the light transmittance of the sample was tested. The specimen size was 40cmx40cm, the glass thickness was 0.5cm, and the coating thickness was 100nm.

[0099] The test results are shown in Table 1 below:

[0100]

[0101] It can be seen from the data shown in Table 1 above that the environmentally friendly optical anti-reflection coating materials prepared in Examples 1-3 of the present application have high light transmittance, low organic volatiles, and excellent comprehensive performance.

[0102] From the data shown in Example 1 and Comparative Example 1, it can be seen that Example 1 of the present application can significantly improve the light transmittance of the coating by pre-preparing polylactic acid and polyhydroxyalkanoate as polymers, compared with directly adding the polymer made of polylactic acid, and the volatility of volatile organic compounds is also reduced.

[0103] It can be seen from the data shown in Example 1 and Comparative Examples 2-3 that Example 1 of the present application can promote the combination of the mixed substrate and further improve the light transmittance and environmental protection performance of the coating by pre-preparing polylactic acid and polyhydroxyalkanoate as polymers.

[0104] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. An environmentally friendly optical anti-reflection coating material, characterized in that: The invention comprises the following raw materials in parts by weight: 60-95 parts of a mixed base material, 15-25 parts of a fluoride additive, 1-5 parts of a polymer, 1-5 parts of a surfactant, and 5-15 parts of water; The mixed substrate is prepared by the following method: After tetraethoxysilane, trichlorofluorosilane, acrylate, polyurethane and anhydrous ethanol are uniformly mixed in a mass ratio of 10-15:20-25:3-9:2:1, deionized water and ammonia water in a mass ratio of 5-15:1-2 are added for vacuum stirring, and the pH value is adjusted to 5-8, the stirring speed is 500-700r / min, and after the mixed base material is formed, it is stored for standby use at a storage temperature of 5-15°C.

2. The environmentally friendly optical antireflection coating material according to claim 1, characterized in that: The polymer comprises polylactic acid and polyhydroxyalkanoate in a mass ratio of 5-8:

3.

3. The environmentally friendly optical anti-reflection coating material according to claim 2, characterized in that: The polylactic acid is prepared by the following method: a. The collected corn and glutinous rice are mixed, washed, soaked, ground, and filtered through a fine mesh to extract the precipitated starch at the bottom; b. Mixing starch and Lactobacillus microorganisms in a mass ratio of 50:1.5 and fermenting for 12-13 hours to produce lactic acid; c. Adding polyacrylic acid to the prepared lactic acid, performing ring-opening polymerization under heating and vacuum conditions to prepare primary polylactic acid, then precipitating and washing the primary polylactic acid with a purification solvent, and obtaining the desired polylactic acid after drying.

4. The environmentally friendly optical antireflection coating material according to claim 3, characterized in that: The mass ratio of the corn to the glutinous rice is 10:3, and the mass ratio of the lactic acid, the polyacrylic acid and the dichloromethane is 1:0.1-0.2:0.2-0.

5.

5. The environmentally friendly optical anti-reflection coating material and the preparation method thereof according to claim 3, characterized in that: The heating temperature is 150-190°C, and the drying temperature is 50-70°C.

6. The environmentally friendly optical anti-reflection coating material according to claim 3, characterized in that: The purification solvent is prepared by compounding dichloromethane, ethyl acetate and ethanol solution in a mass ratio of 1:1:2-4, and the volume fraction of the ethanol solution is 60%-80%.

7. A method for preparing an environmentally friendly optical anti-reflection coating material according to any one of claims 1 to 6, characterized in that: The method comprises the following preparation steps: S1. Weighing the mixed base material, the fluoride additive, the polymer, the surfactant and water in parts by weight to prepare a mixed solution; S2, emulsifying the mixed solution through a high shear mixer to prepare an emulsion; S3, filtering the emulsion through a filter cloth and evacuating the filter cloth to obtain the desired environmentally friendly optical anti-reflection coating material.

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