Anti-glare coating liquid, preparation method and application thereof

Abstract

This invention relates to an anti-glare coating liquid, its preparation method, and its application. The preparation method includes the following steps: mixing 30-40 parts by weight of a main resin, 10-20 parts by weight of a high-functionality acrylate monomer, 10-20 parts by weight of a low-functionality acrylate monomer, 10-30 parts by weight of solvent A, 10-30 parts by weight of solvent B, 0.5-1.5 parts by weight of organic anti-glare particles, 0.1-0.5 parts by weight of inorganic anti-glare particles, 1-3 parts by weight of a photoinitiator, and 3-5 parts by weight of a leveling agent by stirring and ultrasonication to obtain the anti-glare coating liquid; the boiling point of solvent A is greater than that of solvent B. The anti-glare layer formed by the anti-glare coating liquid provided by this invention has a raised peak structure, a valley structure adjacent to the peak structure, and an islet structure raised within the valley structure; the height of the peak structure is greater than the height of the islet structure. The anti-glare layer has anti-glare properties, excellent hardness and wear resistance, and can suppress the generation of rainbow-like halos.

Description

Technical Field

[0001] This invention relates to the field of optical materials technology, and in particular to an anti-glare coating liquid, its preparation method, and its application. Background Technology

[0002] Glare is primarily caused by extremely bright light sources in the environment, which, upon reflection, create a strong contrast in brightness, ultimately resulting in glare for the human eye. Liquid crystal displays (LCDs) were initially used mainly in home televisions, but are now widely used in outdoor applications such as mobile phones, car dashboards, in-vehicle navigation systems, and digital signage. The visibility of an LCD panel is easily impaired when external light shines on it. For example, while driving, glare from sunlight can obscure the view of displays on navigation systems or dashboards, posing a serious safety hazard. Therefore, materials such as anti-glare films are typically used on LCDs to reduce glare and reflection.

[0003] Most existing anti-glare films achieve their anti-glare effect by either embossing resin to create an uneven structure or by adding micron-sized particles to create a textured surface on the resin. However, anti-glare films made by embossing resin to create an uneven structure have relatively low surface hardness, making them easily scratched or worn by hard objects. Their poor mechanical properties can lead to microstructural deformation or damage, thus reducing their anti-glare effect. Adding micron-sized particles to create an uneven structure on the resin surface can result in uneven anti-glare layer thickness due to particle aggregation. This leads to uneven refractive index, spatial optical path differences in reflected light at different locations, and rainbow-like halos when inspected under fluorescent light. Significant color differences at different angles also negatively impact the visual appearance of subsequent products.

[0004] Therefore, there is a need to develop an anti-glare film with excellent optical, mechanical, and anti-glare properties, while also effectively suppressing the generation of rainbow-like halos. Summary of the Invention

[0005] To solve the above-mentioned technical problems, the present invention provides an anti-glare coating liquid, its preparation method and application. The anti-glare film prepared by coating with the anti-glare coating liquid has excellent optical properties, mechanical properties and anti-glare properties, and can effectively suppress the generation of rainbow halo.

[0006] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a method for preparing an anti-glare coating liquid, the method comprising the following steps: 30-40 parts by weight of a main resin (e.g., 31 parts by weight, 32 parts by weight, 33 parts by weight, 34 parts by weight, 35 parts by weight, 36 parts by weight, 37 parts by weight, 38 parts by weight, or 39 parts by weight, etc.), 10-20 parts by weight of a high-functionality acrylate monomer (e.g., 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight, 16 parts by weight, 17 parts by weight, 18 parts by weight, or 19 parts by weight, etc.), 10-20 parts by weight of a low-functionality acrylate monomer (e.g., 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight, 16 parts by weight, 17 parts by weight, 18 parts by weight, or 19 parts by weight, etc.), and solvent A. 10-30 parts by weight (e.g., 12 parts by weight, 14 parts by weight, 16 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 24 parts by weight, 26 parts by weight, or 28 parts by weight, etc.), Solvent B 10-30 parts by weight (e.g., 12 parts by weight, 14 parts by weight, 16 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 24 parts by weight, 26 parts by weight, or 28 parts by weight, etc.), Organic anti-glare particles 0.5-1.5 parts by weight (e.g., 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, 1.0 parts by weight, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, or 1.4 parts by weight, etc.), Inorganic anti-glare particles 0.1-0.5 parts by weight (e.g., 0.15 parts by weight, 0.2 parts by weight, 0.25 parts by weight, 0.3 parts by weight, 0.35 parts by weight, etc.), The anti-glare coating liquid is obtained by mixing 0.4 parts by weight or 0.45 parts by weight, 1-3 parts by weight of photoinitiator (e.g., 1.2 parts by weight, 1.4 parts by weight, 1.6 parts by weight, 1.8 parts by weight, 2.0 parts by weight, 2.2 parts by weight, 2.4 parts by weight, 2.6 parts by weight or 2.8 parts by weight, etc.) and 3-5 parts by weight of leveling agent (e.g., 3.2 parts by weight, 3.4 parts by weight, 3.6 parts by weight, 3.8 parts by weight, 4.0 parts by weight, 4.2 parts by weight, 4.4 parts by weight, 4.6 parts by weight or 4.8 parts by weight, etc.) by stirring and ultrasonication; the boiling point of solvent A is greater than that of solvent B.

[0007] In this invention, the combination of solvent A and solvent B makes the system more stable. The surface of the anti-glare coating formed by the anti-glare coating liquid has a raised peak structure, a valley structure adjacent to the peak structure, and an island structure raised in the valley structure. The height of the peak structure is greater than the height of the island structure, which makes the anti-glare layer have excellent anti-glare performance, excellent hardness and wear resistance, while also suppressing the generation of rainbow halo.

[0008] Preferably, the main resin includes a photosensitive resin.

[0009] Preferably, the photosensitive resin comprises polyurethane acrylate.

[0010] Preferably, the high-functionality acrylate monomer includes any one or a combination of at least two of trimethylolpropane triacrylate (TMPTA), pentaerythritol triacrylate (PETA), dipentaerythritol pentaacrylate, or dipentaerythritol hexaacrylate (DPHA).

[0011] Preferably, the low-functionality acrylate monomer includes any one or a combination of at least two of 2-hydroxyethyl acrylate (HEA), 2-hydroxyethyl methacrylate (HEMA), 1,6-hexanediol diacrylate (HDDA), or hydroxybutyl acrylate (4-HBA).

[0012] In this invention, the high-functionality acrylate monomer refers to an acrylate monomer with a functionality greater than 2; the low-functionality acrylate monomer refers to an acrylate monomer with a functionality less than or equal to 2.

[0013] Preferably, solvent A and solvent B each independently comprise any one or a combination of at least two of diacetone alcohol (DAA), propylene glycol methyl ether acetate (PGMEA), methyl isobutyl ketone (MIBK), propylene glycol methyl ether (PGME), methyl ethyl ketone (MEK), isopropanol (IPA), n-propanol (NPA), or ethanol (EtOH), and solvent A and solvent B are not the same.

[0014] Preferably, the solvent A has a boiling point ≥100℃, such as 110℃, 120℃, 130℃, 140℃ or 150℃.

[0015] Preferably, the boiling point of solvent B is <100°C, for example 50°C, 60°C, 70°C, 80°C or 90°C.

[0016] Preferably, the boiling point of solvent A is 30-100°C higher than that of solvent B, for example, 40°C, 50°C, 60°C, 70°C, 80°C, or 90°C.

[0017] Preferably, solvent A comprises any one or a combination of at least two of diacetone alcohol, propylene glycol methyl ether acetate, methyl isobutyl ketone, or propylene glycol methyl ether.

[0018] Preferably, solvent B comprises any one or a combination of at least two of methyl ethyl ketone, isopropanol, n-propanol, or ethanol.

[0019] Preferably, the organic anti-glare particles include acrylic polymer particles.

[0020] Preferably, the acrylic polymer particles include acrylic particles.

[0021] Preferably, the average particle size of the organic anti-glare particles is 0.5~5 µm, such as 1.0 µm, 1.5 µm, 2.0 µm, 2.5 µm, 3.0 µm, 3.5 µm, 4.0 µm or 4.5 µm.

[0022] Preferably, the inorganic anti-glare particles include silicon dioxide particles.

[0023] Preferably, the average particle size of the inorganic anti-glare particles is 5~30 nm, such as 8 nm, 11 nm, 14 nm, 17 nm, 20 nm, 23 nm, 26 nm or 29 nm.

[0024] Preferably, the photoinitiator comprises any one or a combination of at least two of 2-hydroxy-2-methylphenylacetone (e.g., Darocur 1173), 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone (e.g., Irgacure 907), 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butanone (e.g., Irgacure 369), or hydroxycyclohexylphenyl methyl ketone (e.g., Irgacure 184).

[0025] Preferably, the mixing via stirring and ultrasound includes the following steps: mixing organic anti-glare particles and solvent A via first stirring and first ultrasound treatment; adding inorganic anti-glare particles via second stirring and second ultrasound treatment; adding solvent B, main resin, high-functionality acrylate monomer, low-functionality acrylate monomer, photoinitiator, and leveling agent via third stirring and third ultrasound treatment to obtain the anti-glare coating liquid.

[0026] Preferably, the first stirring, the second stirring, and the third stirring each independently include stirring using a magnetic stirrer.

[0027] Preferably, the rotation speeds of the first, second, and third stirring are each ≥500 r / min, for example, 550 r / min, 600 r / min, 650 r / min, 700 r / min, 750 r / min, or 800 r / min.

[0028] Preferably, the stirring time of the first stirring, the second stirring and the third stirring is each ≥20 min independently, such as 25 min, 30 min, 35 min, 40 min, 45 min or 50 min.

[0029] Preferably, the power of the first ultrasonic treatment, the second ultrasonic treatment, and the third ultrasonic treatment is independently 500~700 W, such as 520 W, 540 W, 560 W, 580 W, 600 W, 620 W, 640 W, 660 W, or 680 W.

[0030] Preferably, the duration of the first, second, and third ultrasonic treatments is independently ≥10 min, for example, 12 min, 14 min, 16 min, 18 min, or 20 min.

[0031] In a second aspect, the present invention provides an anti-glare coating liquid, which is prepared by the preparation method described in the first aspect.

[0032] Thirdly, the present invention provides an anti-glare film, the anti-glare film comprising a substrate layer and an anti-glare layer located on the substrate layer, the anti-glare layer being prepared using the anti-glare coating liquid as described in the second aspect.

[0033] In this invention, the anti-glare film has the characteristics of excellent optical performance, excellent mechanical performance, excellent anti-glare performance, and can effectively suppress the generation of rainbow-like halos.

[0034] Preferably, the side of the substrate layer away from the anti-glare layer also includes a primer layer.

[0035] In this invention, the primer layer enables the anti-glare film to have good adhesion to the polarizing unit of the polarizer, thereby playing the role of a "protective film".

[0036] Preferably, the substrate layer comprises a polymethyl methacrylate (PMMA) film.

[0037] Preferably, the surface of one side of the anti-glare layer has a raised peak structure, a valley structure adjacent to the peak structure, and an island structure raised in the valley structure; the height of the peak structure is greater than the height of the island structure.

[0038] In this invention, protrusions with a height greater than 0.2 μm on one side of the anti-glare layer are called peak structures, and protrusions with a height less than or equal to 0.2 μm are called island structures. The peak and island structures are formed by the aggregation of organic and inorganic anti-glare particles, respectively. The height of the peak structures is greater than the height of the island structures, forming a surface structure state of "peaks surrounding valleys, with islands embedded in the valleys."

[0039] Preferably, the average height of the peak structure is >0.2 μm and ≤1 μm (e.g., 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm or 0.9 μm, etc.), and more preferably 0.3~0.5 μm.

[0040] Preferably, the average surface area of ​​the peak structure is 300~1500 μm. 2 (e.g., 500 μm) 2 700 μm 2 900 μm 2 1100 μm 2 Or 1300 μm 2 (etc.), and more preferably 500~800 μm. 2 .

[0041] Preferably, the average bottom area of ​​the valley structure is 1000~3000 μm. 2 (e.g., 1200 μm) 2 1400 μm 2 1600 μm 2 1800 μm 2 2000 μm 2 2200 μm 2 2400 μm 2 2600 μm 2 or 2800 μm 2 (etc.), and more preferably 1000~2000 μm. 2 .

[0042] Preferably, the average height of the islet structure is ≥0.05 μm and ≤0.2 μm (e.g., 0.07 μm, 0.09 μm, 0.11 μm, 0.13 μm, 0.15 μm, 0.17 μm or 0.19 μm, etc.), and more preferably 0.1~0.15 μm.

[0043] Preferably, the average surface area of ​​the islet structure is 10~100 μm. 2 (e.g., 20 μm) 2 30 μm 2 40 μm 2 50μm 2 60 μm 2 70 μm 2 80 μm 2 or 90 μm 2 (etc.), and more preferably 20~50 μm. 2 .

[0044] Preferably, the average number of islet structures in the valley structure is 5 to 50 (e.g., 10, 15, 20, 25, 30, 35, 40 or 45, etc.), and more preferably 10 to 20.

[0045] In this invention, the average height, average surface area, average bottom area of ​​the peak structure, valley structure, and islet structure, as well as the average number of islet structures in the valley structure, are obtained by profilometry microscopy.

[0046] Fourthly, the present invention provides a method for preparing an anti-glare film, the method comprising the following steps: coating an anti-glare coating liquid as described in the second aspect onto a substrate layer, curing it, and obtaining the anti-glare film.

[0047] Preferably, the coating amount is 24~50 mL / m 2 For example, 27 mL / m 2 30 mL / m 2 33 mL / m 2 36 mL / m 2 39 mL / m 2 42 mL / m 2 45 mL / m 2 Or 48 mL / m 2 wait.

[0048] Preferably, the coating process includes coating with a coating rod.

[0049] Preferably, the coating rod includes a coating rod prepared by an extrusion process (OSP series coating rod) or a coating rod prepared by a wire winding process (RDS series coating rod).

[0050] Preferably, the curing process includes sequential thermal curing and photocuring.

[0051] Preferably, the thermosetting temperature is 70~90℃ (e.g., 72℃, 74℃, 76℃, 78℃, 80℃, 82℃, 84℃, 86℃ or 88℃, etc.), and the time is 1~5 min (e.g., 1.5 min, 2 min, 2.5 min, 3 min, 3.5 min, 4 min or 4.5 min, etc.).

[0052] Preferably, the photocuring includes photocuring using a mercury lamp.

[0053] Preferably, the power of the photocuring is 1~5 kW, such as 1.5 kW, 2 kW, 2.5 kW, 3 kW, 3.5 kW, 4 kW or 4.5 kW, etc.

[0054] Preferably, the photocuring time is 3 to 10 seconds, such as 4 seconds, 5 seconds, 6 seconds, 7 seconds, 8 seconds, or 9 seconds.

[0055] Compared with the prior art, the present invention has at least the following beneficial effects: The anti-glare coating liquid of the present invention has good dispersion stability. The anti-glare film prepared using it has a raised peak structure on one side of the anti-glare layer, a valley structure adjacent to the peak structure, and an island structure raised in the valley structure. The height of the peak structure is greater than the height of the island structure. The anti-glare film prepared has anti-glare performance, excellent hardness and wear resistance, high gloss, and can suppress the generation of rainbow halo. The gloss is ≥88%, and more preferably ≥90%. Attached Figure Description

[0056] Figure 1 This is a schematic diagram of the structure of the anti-glare film provided in Example 1; Among them, 1-anti-glare layer, 2-substrate layer, 3-primer layer; Figure 2 Microscopic morphology of one side of the anti-glare layer in the anti-glare film provided in Example 1; Among them, 1-peak structure, 2-valley structure, 3-island structure; Figure 3 Microscopic morphology of the surface of the anti-glare layer on one side of the anti-glare film provided in Comparative Example 1; Figure 4 Microscopic morphology of the surface of the anti-glare layer on one side of the anti-glare film provided in Comparative Example 4; Figure 5 A diagram showing the effect of detecting rainbow-shaped halo in the anti-glare film provided in Comparative Example 1; Figure 6 The rendering shows the effect of superior anti-glare performance; Figure 7 and Figure 8 The image shows a good anti-glare performance. Detailed Implementation

[0057] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0058] Unless otherwise specified, the materials and equipment involved in the following detailed embodiments are all conventional materials and equipment in the art and will not affect the technical effects of the present invention.

[0059] Unless otherwise specified, all reagents and raw materials used in the following examples and comparative examples are commercially available products. Some raw material information is as follows: Main resin: polyurethane acrylate, model UA-122P, manufactured by Shin-Nakamura Chemical Industry Co., Ltd.

[0060] Example 1 This embodiment provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The anti-glare coating liquid is prepared by the following method: 1 part by weight of organic anti-glare particles (acrylic particles, average particle size of 3 μm) is placed in a brown glass bottle, and 15 parts by weight of solvent A (propylene glycol methyl ether acetate) is added. Then, a magnetic stirrer is placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a first stirring operation at 500 r / min for 20 min. Next, it is placed in an ultrasonic cleaner (model JPS-100AH, 30L capacity) for a first ultrasonic treatment at 600W for 10 min. Then, 0.5 parts by weight of inorganic anti-glare particles (silica particles, average particle size of 15 nm) are added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a second stirring operation at 500 r / min. The mixture was stirred at 500 r / min for 20 min, then placed in an ultrasonic cleaner (model JPS-100AH, 30L capacity) for a second ultrasonic treatment at 600W for 10 min. Finally, 20 parts by weight of solvent B (methyl ethyl ketone), 30 parts by weight of main resin (polyurethane acrylate), 15 parts by weight of high-functionality acrylate monomer (pentaerythritol triacrylate), 15 parts by weight of low-functionality acrylate monomer (hydroxybutyl acrylate), 1.5 parts by weight of photoinitiator (Irgacure 907, BASF), and 3 parts by weight of leveling agent (PC4100, DIC Corporation) were added. The mixture was then placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a third stirring operation at 500 r / min for 20 min. The mixture was then placed in an ultrasonic cleaner (model JPS-100AH, 30L capacity) for a third ultrasonic treatment at 600W for 10 min. min, the anti-glare coating liquid is obtained.

[0061] The anti-glare film, such as Figure 1The image shows an anti-glare layer 1, a substrate layer 2, and a primer layer 3 stacked sequentially. The substrate was prepared using the following method: A light-transmitting substrate (composed of a PMMA film and a primer layer on one side of the PMMA film, with a thickness of 40µm, model KU164, manufactured by Anhui Hemei Materials Co., Ltd.) was cut to a size of 210 mm × 297 mm and fixed on a coating table. 2 mL of the anti-glare coating liquid was then drawn up with a pipette and squeezed onto one side of the PMMA film in the light-transmitting substrate. The coating was then applied using an OSP#20 coating rod. The substrate was then dried in an 80°C controlled atmosphere heat treatment oven (model OF-02GW) for 2 minutes. Finally, it was removed and photocured under nitrogen atmosphere using a mercury lamp at a power of 2 kW for 5 seconds to obtain the anti-glare film.

[0062] Example 2 This embodiment provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The anti-glare coating liquid is prepared by the following method: 0.7 parts by weight of organic anti-glare particles (acrylic particles, average particle size of 1 µm) are placed in a brown glass bottle, and 25 parts by weight of solvent A (propylene glycol methyl ether acetate) are added. Then, a magnetic stirrer is placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a first stirring operation at 500 r / min for 20 min. Next, the mixture is placed in an ultrasonic cleaner (model JPS-100AH, 30L capacity) for a first ultrasonic treatment at 600W for 10 min. Then, 0.5 parts by weight of inorganic anti-glare particles (silica particles, average particle size of 15 nm) are added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a second stirring operation at 500 r / min for 20 min. After 10 minutes, the mixture is placed in an ultrasonic cleaner (model JPS-100AH, volume 30L) for a second ultrasonic treatment at a power of 600W for 10 minutes. Finally, 10 parts by weight of solvent B (methyl ethyl ketone), 40 parts by weight of main resin (polyurethane acrylate), 10 parts by weight of high-functionality acrylate monomer (pentaerythritol triacrylate), 20 parts by weight of low-functionality acrylate monomer (hydroxybutyl acrylate), 3 parts by weight of photoinitiator (Irgacure 907, manufacturer: BASF) and 4 parts by weight of leveling agent (PC4100, manufacturer: DIC Corporation) are added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a third stirring operation at a speed of 500 r / min for 20 minutes. Then, the mixture is placed in an ultrasonic cleaner (model JPS-100AH, volume 30L) for a third ultrasonic treatment at a power of 600W for 10 minutes to obtain the anti-glare coating liquid.

[0063] The anti-glare film comprises an anti-glare layer, a substrate layer, and a primer layer stacked sequentially, and is prepared by the following method: A light-transmitting substrate (composed of a PMMA film and a Primer layer located on one side of the PMMA film, with a thickness of 40 µm, model KU164, manufactured by Anhui Hemei Materials Co., Ltd.) is cut into a size of 210 mm × 297 mm, then fixed on a coating table. 1.5 mL of the above-mentioned anti-glare coating liquid is then drawn up with a pipette and squeezed onto one side of the PMMA film in the light-transmitting substrate, and then coated with an OSP#20 coating rod. After drying in an 80°C controlled atmosphere heat treatment oven (model OF-02GW) for 3 min, it is then removed and photocured in a nitrogen environment using a mercury lamp with a power of 2 kW for 5 s to obtain the anti-glare film.

[0064] Example 3 This embodiment provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The anti-glare coating liquid is prepared by the following method: 1.5 parts by weight of organic anti-glare particles (acrylic particles, average particle size of 5 μm) are placed in a brown glass bottle, and 10 parts by weight of solvent A (propylene glycol methyl ether acetate) are added. Then, a magnetic rotor is added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for the first stirring operation at a speed of 500 r / min for 20 min. Next, it is placed in an ultrasonic cleaner (model JPS-100AH, volume 30L) for the first ultrasonic treatment at a power of 600W for 10 min. Then, 0.2 parts by weight of inorganic anti-glare particles (silica particles, average particle size of 15 nm) are added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for the second stirring operation at a speed of 500 r / min for 20 min. After 10 minutes, the mixture is placed in an ultrasonic cleaner (model JPS-100AH, volume 30L) for a second ultrasonic treatment at 600W for 10 minutes. Finally, 30 parts by weight of solvent B (methyl ethyl ketone), 35 parts by weight of main resin (polyurethane acrylate), 20 parts by weight of high-functionality acrylate monomer (pentaerythritol triacrylate), 10 parts by weight of low-functionality acrylate monomer (hydroxybutyl acrylate), 1 part by weight of photoinitiator (Irgacure 907, manufacturer: BASF) and 5 parts by weight of leveling agent (PC4100, manufacturer: DIC Corporation) are added and placed on a 15-station laboratory magnetic stirrer (model MS-T-S15) for a third stirring operation at 500 r / min for 20 minutes. Then, the mixture is placed in an ultrasonic cleaner (model JPS-100AH, volume 30L) for a third ultrasonic treatment at 600W for 10 minutes to obtain the anti-glare coating liquid.

[0065] The anti-glare film comprises an anti-glare layer, a substrate layer, and a primer layer stacked sequentially, and is prepared by the following method: A light-transmitting substrate (composed of a PMMA film and a Primer layer located on one side of the PMMA film, with a thickness of 40 µm, model KU164, manufactured by Anhui Hemei Materials Co., Ltd.) is cut into a size of 210 mm × 297 mm, then fixed on a coating table. 1.5 mL of the above-mentioned anti-glare coating liquid is then drawn up with a pipette and squeezed onto one side of the PMMA film in the light-transmitting substrate, and then coated with an OSP#20 coating rod. After drying in an 80°C controlled atmosphere heat treatment oven (model OF-02GW) for 2 min, it is then removed and photocured in a nitrogen environment using a mercury lamp with a power of 2kW for 5 s to obtain the anti-glare film.

[0066] Example 4 This embodiment provides an anti-glare coating liquid and its preparation method, as well as an anti-glare film. The difference between this embodiment and Example 1 is that solvent B (methyl ethyl ketone) is replaced with the same mass of solvent B (ethanol), while other conditions are the same as in Example 1.

[0067] Example 5 This embodiment provides an anti-glare coating liquid and its preparation method, as well as an anti-glare film. The difference between this embodiment and Example 1 is that solvent A (propylene glycol methyl ether acetate) is replaced with the same mass of solvent A (diacetone alcohol), while other conditions are the same as in Example 1.

[0068] Example 6 This embodiment provides an anti-glare coating liquid and its preparation method, as well as an anti-glare film. The difference between this embodiment and Example 1 is that solvent A (propylene glycol methyl ether acetate) is replaced with the same mass of solvent A (methyl isobutyl ketone), while other conditions are the same as in Example 1.

[0069] Example 7 This embodiment provides an anti-glare coating liquid and its preparation method, as well as an anti-glare film. The difference between this embodiment and Example 1 is that solvent A (propylene glycol methyl ether acetate) is replaced with the same mass of solvent A (propylene glycol methyl ether), while other conditions are the same as in Example 1.

[0070] Example 8 This embodiment provides an anti-glare coating liquid and its preparation method, as well as an anti-glare film. The difference between this embodiment and Example 1 is that solvent A (propylene glycol methyl ether acetate) is replaced with the same mass of solvent B (n-propanol), while other conditions are the same as in Example 1.

[0071] Comparative Example 1 This comparative example provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The difference between this example and Example 1 is that the first, second, and third stirring operations performed by placing a magnetic rotor on a 15-station laboratory magnetic stirrer (model MS-T-S15) in the preparation of the anti-glare coating liquid are replaced by stirring with a homogenizer (model M2-2.5). The rotation speed in the first, second, and third stirring operations is adjusted to 2500 r / min, and the time is adjusted to 20 min. Furthermore, the first, second, and third ultrasonic treatments performed in an ultrasonic cleaner (model JPS-100AH, volume 30L) are not included. Other conditions are the same as in Example 1.

[0072] Comparative Example 2 This comparative example provides an anti-glare coating liquid and its preparation method. The difference between this example and Example 1 is that the preparation of the anti-glare coating liquid does not include the first, second, and third ultrasonic treatments performed by placing it in an ultrasonic cleaner (model JPS-100AH, volume 30L). Other conditions are the same as in Example 1.

[0073] Comparative Example 3 This comparative example provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The difference between this example and Example 1 is that 20 parts by weight of solvent B (methyl ethyl ketone) are replaced with 20 parts by weight of solvent A (propylene glycol methyl ether acetate) in the preparation of the anti-glare coating liquid. Other conditions are the same as in Example 1.

[0074] Comparative Example 4 This comparative example provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The difference between this example and Example 1 is that in the preparation of the anti-glare coating liquid, 15 parts by weight of solvent A (propylene glycol methyl ether acetate) are replaced with 15 parts by weight of ethanol, and 20 parts by weight of solvent B (methyl ethyl ketone) are replaced with 20 parts by weight of ethanol. Other conditions are the same as in Example 1.

[0075] Comparative Example 5 This comparative example provides an anti-glare coating liquid, its preparation method, and an anti-glare film. The difference between this example and Example 1 is that 15 parts by weight of solvent A (propylene glycol methyl ether acetate) is replaced with 15 parts by weight of solvent B (methyl ethyl ketone) in the preparation of the anti-glare coating liquid, while other conditions are the same as in Example 1.

[0076] The anti-glare coating liquids and anti-glare films provided in Examples 1-8 and Comparative Examples 1-5 were subjected to the following performance tests.

[0077] (1) Dispersion status: The anti-glare coating liquid was placed at room temperature of 25°C for 10 min to observe whether precipitation would occur, and the dispersion stability of the anti-glare coating liquid was judged.

[0078] (2) Pencil hardness: The test was conducted using an electric pencil hardness tester (model ASR-5608-D2) with a load weight of 500g. Five parallel tests were performed. If scratches appeared in two or more tests, the test was considered unqualified and recorded as NG. If no scratches appeared in any test or only one test showed scratches, the test was considered qualified and recorded as OK.

[0079] (3) Abrasion resistance: The abrasion resistance tester (model ZJ-339-GSR) was used for testing. The load weight was 500g. If scratches appeared, it was considered unqualified and recorded as NG; if no scratches appeared, it was considered qualified and recorded as OK.

[0080] (4) Gloss: The gloss was tested using a gloss meter (model VG8000).

[0081] (5) Surface morphology: Observation and measurement were performed using a profile measuring microscope (model VK-X3000).

[0082] (6) Rainbow halo detection: The light source (fluorescent lamp) is placed on one side of the primer layer in the anti-glare film, and the light source (fluorescent lamp) is observed through the anti-glare film from the other side to see if a rainbow halo appears.

[0083] (7) Anti-glare performance: Visually observed, the anti-glare effect increases from low to high as follows: Figures 6-8 As shown, it appears Figure 7 The anti-glare effect shown is rated as excellent; any glare is detected. Figure 6 and Figure 8 The anti-glare effect shown is rated as good; if it is lower than that, the anti-glare performance is rated as good. Figure 6 The anti-glare effect is higher than Figure 8 The anti-glare effect is poor, and the anti-glare performance is rated as poor.

[0084] The test results are shown in Tables 1 and 2 below.

[0085] Table 1 In Table 1, " / " indicates that the test was not performed.

[0086] Table 2 In Table 2, " / " indicates that the test was not performed.

[0087] According to the test results in Tables 1 and 2, the anti-glare coating liquids prepared in Examples 1-8 exhibit good dispersion stability. The anti-glare films formed have raised peak structures, adjacent valley structures, and raised islet structures within the valley structures on one side of the anti-glare layer. The resulting anti-glare films possess anti-glare properties, good abrasion resistance, and effectively suppress the generation of rainbow-like halos. The average height of the peak structures in Examples 1-8 ranges from 0.33 to 0.45 μm, and the average surface area ranges from 565 to 653 μm². 2 The average base area of ​​the valley structure is 1109~1145 μm. 2 The average height of the islet structure is 0.13–0.14 μm, and the average surface area is 34–36 μm². 2 The average number of islet structures in the valley structure is 15-20. This is a "mild and effective" microstructure, corresponding to the good overall performance shown in Table 1.

[0088] The surface of the anti-glare layer of the anti-glare film prepared in Example 1, as shown... Figure 2 As shown, there is a peak structure 1 with a protrusion, a valley structure 2 adjacent to the peak structure, and an islet structure 3 with a protrusion located in the valley structure.

[0089] Compared to Example 1, replacing solvent A (propylene glycol methyl ether acetate) with the same mass of solvent B (n-propanol) (Example 8) results in faster solvent evaporation, causing some organic and / or inorganic anti-glare particles to rapidly aggregate and solidify. This leads to a larger peak height, a smaller base area, a larger average base area of ​​the valley structure, and a greater average number of islet structures within the valley structure. Consequently, the anti-glare effect becomes foggy, excessively high, resulting in excessive light loss, limited visual effects, and a decline in overall anti-glare performance.

[0090] Compared to Example 1, if the magnetic rotor is replaced with a homogenizer and ultrasonic treatment is not performed (Comparative Example 1), the dispersion effect of the anti-glare coating liquid is poor, and the surface of the anti-glare layer of the prepared anti-glare film is as follows: Figure 3 As shown, island structures are relatively few, and there are almost no islands, such as... Figure 5 As shown, the anti-glare film exhibits a heavier rainbow-like halo; the average height and average surface area of ​​the peak structure are larger, resulting in decreased abrasion resistance and mechanical properties. Comparative Example 1 shows a peak structure with an average height (0.93 μm) and an average surface area (3573 μm). 2 The sharp increase corresponds to the effects of "heavy rainbow halo" and "NG abrasion resistance" in Table 1. This indicates that excessive mechanical dispersion (homogenizer) and the lack of ultrasonic treatment have damaged the uniformity of the particles, resulting in coarse protrusions.

[0091] Compared with Example 1, the anti-glare coating liquid prepared without ultrasonic treatment (Comparative Example 2) has poor dispersion stability and particles precipitate rapidly after preparation.

[0092] As can be seen from the comparison of Example 1, Comparative Examples 1 and 2, the mixing method affects the dispersion, and thus affects the surface morphology after coating. In Comparative Example 2, the dispersion effect of magnetic stirring alone is very poor, resulting in the rapid sedimentation of organic and inorganic anti-glare particles, which affects the coating.

[0093] Compared to Example 1, if only propylene glycol methyl ether acetate is used as a solvent (Comparative Example 3), the solvent evaporation rate in the system is uniform, but the dispersion stability of the prepared anti-glare coating liquid decreases. Island structures form on one side of the anti-glare layer of the prepared anti-glare film, but the height of the island structures is relatively small. The anti-glare film test shows a rainbow-like halo, which is less pronounced than in Comparative Example 1. Peak structures are formed, with increased average height and average surface area, resulting in decreased abrasion resistance and mechanical properties. The average height (0.80 μm) and average surface area (2566 μm) of the peak structures in Comparative Example 3 are... 2 The concentration of the chromatic aura also increased significantly, and the "islet structure height was extremely small," corresponding to the effects of "lighter rainbow halo" (lighter than Comparative Example 1) and "decreased abrasion resistance" in Table 1. This indicates that although a single solvent can form peaks, it cannot finely control the secondary structure (islets), leading to a decrease in performance.

[0094] Compared to Example 1, if only ethanol is used as a solvent (Comparative Example 4) or only methyl ethyl ketone is used as a solvent (Comparative Example 5), the dispersion stability of the anti-glare coating liquid decreases, and the surface of the anti-glare layer of the prepared anti-glare film is as follows: Figure 4 As shown, under the same magnification view, only two peak structures were observed, which could not form valley structures and were mostly island structures, indicating poor anti-glare performance.

[0095] As can be seen from the comparison between Example 1 and Comparative Examples 3, 4 and 5, the choice of solvent affects the dispersion effect, and thus affects the distribution of organic and inorganic anti-glare particles on the surface after coating. When solvents A and B with different boiling points are combined, the dispersion stability of the prepared anti-glare coating liquid is better, and the performance of the prepared anti-glare film is better.

[0096] Regarding Comparative Examples 2, 4, and 5: Table 2 shows " / " or "few peak structures", which corresponds exactly to the descriptions in Table 1 of "rapid precipitation, difficult to disperse" or "flocculated precipitation occurs", because the dispersion stage failed, and naturally no effective surface structure could be formed after coating.

[0097] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing an anti-glare coating liquid, characterized in that, The preparation method includes the following steps: mixing 30-40 parts by weight of main resin, 10-20 parts by weight of high-functionality acrylate monomer, 10-20 parts by weight of low-functionality acrylate monomer, 10-30 parts by weight of solvent A, 10-30 parts by weight of solvent B, 0.5-1.5 parts by weight of organic anti-glare particles, 0.1-0.5 parts by weight of inorganic anti-glare particles, 1-3 parts by weight of photoinitiator, and 3-5 parts by weight of leveling agent by stirring and sonication to obtain the anti-glare coating liquid; The boiling point of solvent A is greater than that of solvent B.

2. The preparation method according to claim 1, characterized in that, The main resin includes a photosensitive resin; Preferably, the photosensitive resin comprises polyurethane acrylate; Preferably, the high-functionality acrylate monomer includes any one or a combination of at least two of trimethylolpropane triacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate, or dipentaerythritol hexaacrylate. Preferably, the low-functionality acrylate monomer includes any one or a combination of at least two of 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, 1,6-hexanediol diacrylate or hydroxybutyl acrylate.

3. The preparation method according to claim 1 or 2, characterized in that, Solvent A and solvent B each independently comprise any one or a combination of at least two of diacetone alcohol, propylene glycol methyl ether acetate, methyl isobutyl ketone, propylene glycol methyl ether, methyl ethyl ketone, isopropanol, n-propanol, or ethanol, and solvent A and solvent B are not the same.

4. The preparation method according to any one of claims 1 to 3, characterized in that, The boiling point of solvent A is ≥100℃; Preferably, the boiling point of solvent B is <100°C; Preferably, the boiling point of solvent A is 30-100°C higher than that of solvent B.

5. The preparation method according to any one of claims 1 to 4, characterized in that, The organic anti-glare particles include acrylic polymer particles; Preferably, the acrylic polymer particles include acrylic particles; Preferably, the average particle size of the organic anti-glare particles is 0.5~5 µm; Preferably, the inorganic anti-glare particles include silicon dioxide particles; Preferably, the average particle size of the inorganic anti-glare particles is 5~30 nm; Preferably, the photoinitiator comprises any one or a combination of at least two of 2-hydroxy-2-methylphenylacetone, 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butanone, or hydroxycyclohexylphenyl methyl ketone.

6. The preparation method according to any one of claims 1 to 5, characterized in that, The mixing process via stirring and ultrasound includes the following steps: mixing organic anti-glare particles and solvent A through a first stirring and a first ultrasound treatment; adding inorganic anti-glare particles and mixing through a second stirring and a second ultrasound treatment; adding solvent B, main resin, high-functionality acrylate monomers, low-functionality acrylate monomers, photoinitiator, and leveling agent and mixing through a third stirring and a third ultrasound treatment to obtain the anti-glare coating liquid. Preferably, the first stirring, the second stirring, and the third stirring each independently include stirring using a magnetic stirrer; Preferably, the rotation speeds of the first stirring, the second stirring, and the third stirring are each ≥500 r / min independently; Preferably, the stirring time of the first stirring, the second stirring, and the third stirring is each ≥20 min independently; Preferably, the power of the first ultrasonic treatment, the second ultrasonic treatment, and the third ultrasonic treatment is each independently 500~700 W; Preferably, the duration of the first, second, and third ultrasonic treatments is ≥10 min each independently.

7. An anti-glare coating liquid, characterized in that, The anti-glare coating liquid is prepared using the preparation method described in any one of claims 1 to 6.

8. An anti-glare film, characterized in that, The anti-glare film includes a substrate layer and an anti-glare layer located on the substrate layer, wherein the anti-glare layer is prepared using the anti-glare coating liquid as described in claim 7.

9. The anti-glare film according to claim 8, characterized in that, The side of the substrate layer away from the anti-glare layer also includes a primer layer; Preferably, the substrate layer comprises a polymethyl methacrylate film; Preferably, the surface of one side of the anti-glare layer has a raised peak structure, a valley structure adjacent to the peak structure, and an island structure raised in the valley structure; the height of the peak structure is greater than the height of the island structure. Preferably, the average height of the peak structure is >0.2 μm and ≤1 μm; Preferably, the average surface area of ​​the peak structure is 300~1500 μm. 2 ; Preferably, the average bottom area of ​​the valley structure is 1000~3000 μm. 2 ; Preferably, the average height of the islet structure is ≥0.05 μm and ≤0.2 μm; Preferably, the average surface area of ​​the islet structure is 10~100 μm. 2 ; Preferably, the average number of islet structures in the valley structure is 5 to 50.

10. A method for preparing an anti-glare film, characterized in that, The preparation method includes the following steps: coating the anti-glare coating liquid as described in claim 7 onto the substrate layer, curing it, and obtaining the anti-glare film.

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