Anti-fog glass and preparation method thereof
By designing a double-layer structure for anti-fog glass on automotive glass, and utilizing hydrophilic and hydrophobic monomers to construct a three-dimensional heterogeneous network and an organic-inorganic hybrid bonding layer, the problems of high energy consumption and insufficient performance of existing defogging methods are solved, achieving a highly efficient and energy-saving anti-fog effect.
Patent Information
- Application Number
- CN202510923461.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-04
- Publication Date
- 2025-11-07
AI Technical Summary
Existing methods for defogging automotive glass, such as heated defogging and air conditioning system defogging, suffer from high energy consumption, low efficiency, and significant delays. Existing antifogging coatings also face challenges in balancing antifogging performance, moisture resistance, salt spray resistance, and abrasion resistance.
The anti-fog glass adopts a double-layer structure, including a glass substrate, an adhesive layer, and an anti-fog layer. The anti-fog layer coating is composed of hydrophilic and hydrophobic monomers, and water vapor transmission is regulated through a three-dimensional heterogeneous network structure. Combined with an organic-inorganic hybrid adhesive layer, it can improve adhesion and resistance to environmental aging.
It achieves improved wear resistance, moisture resistance and salt spray resistance while ensuring anti-fog performance, reduces energy consumption and enhances driving safety, which is in line with the development trend of energy conservation and environmental protection.
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Figure BDA0005483880270000151
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to a kind of anti-fog glass and its preparation method, belong to glass coating technical field. BACKGROUND
[0002] When the temperature difference between the inside and outside of the car is large during driving, the water molecules in the air inside the car will quickly condense on the surface of the car glass with lower temperature and form a layer of fog. This fogging phenomenon seriously hinders the driver's vision and greatly increases the driving safety hazard.
[0003] Currently, the common defogging methods for automobile glass mainly include heating defogging and air conditioning system defogging. Among them, heating defogging is to heat the glass to increase the surface temperature of the glass, so that the condensed water droplets evaporate. Air conditioning system defogging is to use dry cold air or hot air blown by the air conditioner to reduce air humidity or increase glass temperature to achieve the purpose of defogging. However, both methods have obvious drawbacks. Heating defogging continuously consumes electrical energy, and air conditioning system defogging increases fuel consumption or electrical consumption whether in cooling or heating mode. Moreover, they have a certain hysteresis after being turned on, and it is difficult to quickly eliminate the fog.
[0004] Surface coating technology, as a new anti-fogging method, has gradually entered people's field of vision. It is to uniformly coat anti-fogging paint on the surface of the substrate, and form an anti-fogging coating through a series of physical or chemical changes, so as to achieve the purpose of active anti-fogging. This method does not need to consume a large amount of energy for heating or cooling, and has the advantages of green, environmental protection, energy saving, etc. For example, CN108025542A discloses an epoxy resin cured product anti-fogging coating, which not only can exhibit good anti-fogging performance, but also has excellent peel resistance, and provides an anti-fogging article with good appearance. However, compared with the epoxy resin system, it is more susceptible to environmental aging and yellowing, appearance, etc. In practical applications, the existing anti-fogging coating still faces many challenges. It is difficult to balance anti-fogging performance and environmental aging resistance (moisture resistance, salt spray resistance, etc.) at the same time.
[0005] Therefore, the present application provides an anti-fogging coating technology with good comprehensive performance, which is of great significance to balance anti-fogging performance, moisture resistance, salt spray resistance, wear resistance, adhesion, etc. It not only can improve driving safety, but also meets the development trend of energy saving and environmental protection. SUMMARY
[0006] To solve the above problems, the present application provides an anti-fogging glass and its preparation method, which has anti-fogging performance, moisture resistance, salt spray resistance, wear resistance, adhesion, etc.
[0007] To achieve the above object, in a first aspect, the present application provides an anti-fog glass, wherein the anti-fog glass comprises a glass substrate, a bonding layer, and an anti-fog layer, the bonding layer is arranged between the anti-fog layer and the glass substrate;
[0008] The anti-fog layer is prepared from an anti-fog layer coating; the anti-fog layer coating comprises, in terms of mass fraction, 70-90 parts of a first monomer, 5-15 parts of a second monomer, 3-6 parts of a cross-linking agent, and 5-10 parts of a photoinitiator.
[0009] The first monomer comprises one or more than two combinations of hydroxyethyl methacrylate, polyethylene glycol diacrylate, N-hydroxymethyl acrylamide, methacrylamide, N-isopropyl acrylamide, and N,N-dimethyl acrylamide.
[0010] The second monomer comprises one or more than two combinations of trifluoroethyl methacrylate, methyl methacrylate, butyl acrylate, ethylene glycol dimethacrylate, glycidyl methacrylate, benzyl methacrylate, and 2-hydroxy-3-phenoxypropyl acrylate.
[0011] According to a specific embodiment of the present application, preferably, the anti-fog layer coating comprises, in terms of mass fraction, 75-88 parts of the first monomer, 7-12 parts of the second monomer, 4-6 parts of the cross-linking agent, and 5-8 parts of the photoinitiator. The first monomer used in the present application is a hydrophilic monomer, and the hydrophilic group in the hydrophilic monomer can strongly adsorb water vapor by hydrogen bonding with water molecules and the like, and can capture and retain water vapor inside the polymer network of the coating. The second monomer used in the present application is a hydrophobic monomer, which can adjust the hydrophobicity of the coating. The hydrophilic monomer, the hydrophobic monomer, and the multi-functional cross-linking agent can form a three-dimensional heterogeneous network structure, which skillfully regulates the transmission path of water vapor in the coating, ensuring efficient and stable water absorption process. Through the construction of the hydrophilic-hydrophobic three-dimensional network, the anti-fog performance can be ensured while preventing the coating from swelling and deforming due to water absorption.
[0012] According to a specific embodiment of the present application, preferably, the first monomer comprises 30-40 parts of polyethylene glycol diacrylate and 40-50 parts of N-hydroxy acrylamide; or the first monomer comprises 35-45 parts of hydroxyethyl methacrylate and 35-45 parts of N,N-dimethyl acrylamide.
[0013] According to a specific embodiment of the present application, preferably, the second monomer comprises 5-10 parts of glycidyl methacrylate and 1-5 parts of 2-hydroxy-3-phenoxypropyl acrylate.
[0014] According to a specific embodiment of the present application, preferably, the first monomer comprises 30-40 parts of polyethylene glycol diacrylate and 40-50 parts of N-hydroxy acrylamide, and the second monomer comprises 5-10 parts of glycidyl methacrylate and 1-5 parts of 2-hydroxy-3-phenoxypropyl acrylate.
[0015] Alternatively, the first monomer comprises 35-45 parts of hydroxyethyl methacrylate and 35-45 parts of N,N-dimethyl acrylamide, and the second monomer comprises 5-15 parts of benzyl methacrylate.
[0016] Alternatively, the first monomer comprises 70-90 parts of N-hydroxymethyl acrylamide, and the second monomer comprises 5-15 parts of methyl methacrylate.
[0017] Alternatively, the first monomer comprises 30-40 parts of polyethylene glycol diacrylate and 40-50 parts of N-hydroxy acrylamide, and the second monomer comprises 5-10 parts of glycidyl methacrylate and 1-5 parts of 2-hydroxy-3-phenoxypropyl acrylate.
[0018] According to a specific embodiment of the present application, preferably, the sum of the mass of each component of the anti-fog coating is 100 parts by mass.
[0019] According to a specific embodiment of the present application, preferably, the thickness of the anti-fog layer is 10-100 μm, more preferably 20-80 μm. If the thickness of the anti-fog layer is too thin, the anti-fog effect will be poor; if the thickness of the anti-fog layer is too thick, the adhesion of the coating and the glass will be reduced.
[0020] According to a specific embodiment of the present application, preferably, the cross-linking agent comprises one of pentaerythritol triacrylate, pentaerythritol tetraacrylate, trimethylolpropane triacrylate, and dipentaerythritol pentaacrylate. The cross-linking agent of the present application can react with the first monomer and the second monomer during polymerization to form a three-dimensional heterogeneous cross-linking network structure, thereby improving the wear resistance, moisture resistance, neutral salt spray resistance, and other properties of the anti-fog layer, and preventing the anti-fog layer from deforming or dissolving during use.
[0021] According to a specific embodiment of the present application, preferably, the photoinitiator comprises one or two or more combinations of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, methyl phenylglyoxylate, 2-hydroxy-2-methyl-1-phenyl-1-propanone, (2,4,6-trimethylbenzoyl)diphenyl phosphine oxide, ethyl (2,4,6-trimethylbenzoyl) phenyl phosphine, 1-hydroxycyclohexyl phenyl ketone, and 2,4-diethylthioxanthone. The photoinitiator of the present application generates free radicals to initiate the polymerization of the monomers and the cross-linking agent, allowing the anti-fog layer coating to be quickly cured into a film.
[0022] According to the specific embodiment of the present application, preferably, the anti-fog layer coating further contains 0.05%-0.2% of an auxiliary agent; the auxiliary agent is a leveling agent. More preferably, 0.07%-0.15%; the leveling agent can be selected from one or a combination of more than two of BYK333, BYK307, EFKA3580, and EFKA3522. The leveling agent of the present application can improve the leveling property of the anti-fog coating, so that the coating can spread uniformly during the coating process, forming a flat and smooth anti-fog layer, and reducing the defects on the surface of the anti-fog layer.
[0023] According to the specific embodiment of the present application, preferably, the anti-fog layer coating is prepared by mixing the first monomer, the second monomer, the crosslinking agent, the photoinitiator, and the auxiliary agent, and stirring in the dark for 0.5-3h. More preferably, the stirring is carried out at room temperature (20-30℃).
[0024] The anti-fog glass of the present application preferably connects the glass substrate and the anti-fog layer through the adhesive layer as a bridge. In addition, the adhesive layer also plays an important role in the environmental aging process. The elements of the glass substrate can migrate into the anti-fog layer, destroy its structure, and affect its performance. By providing the adhesive layer, the migration of these elements into the anti-fog layer can be prevented, and the anti-fog performance can be affected. Secondly, the adhesive layer is preferably an organic-inorganic hybrid silica sol layer, and its thermal expansion coefficient is close to that of glass. The thermal expansion coefficients of the anti-fog layer and glass are quite different. By providing the adhesive layer, the stress can be buffered, and the overall environmental aging resistance of the anti-fog layer can be improved.
[0025] According to the specific embodiment of the present application, preferably, the adhesive layer is prepared from an adhesive layer coating; the adhesive layer coating contains silicate, coupling agent, acid solution, and solvent in a mass ratio of 10-15:2-15:15-25:50-65.
[0026] According to the specific embodiment of the present application, preferably, the adhesive layer coating contains, in terms of mass percentage: silicate 10%-15%, coupling agent 2%-15%, acid solution 15%-25%, and solvent 50%-65%. More preferably, the adhesive layer coating contains: silicate 12%-15%, coupling agent 5%-12%, acid solution 18%-23%, and solvent 52%-62%. The silicate used in the adhesive layer of the present application can form silanol groups after hydrolysis, can undergo polycondensation reaction with the hydroxyl groups on the surface of the glass substrate to form a firm chemical bond, and can further form a siloxane network structure during the drying process to improve the heat resistance of the adhesive layer.
[0027] According to the specific embodiment of the present application, preferably, the thickness of the adhesive layer is 0.3-6μm, more preferably 0.5-3μm.
[0028] According to the specific embodiment of the present application, preferably, the adhesive layer coating is prepared by mixing solvent, silicate, coupling agent, acid solution under stirring, and stirring for 2-8 hours.
[0029] According to the specific embodiment of the present application, preferably, in the adhesive layer coating, the silicate comprises one or more than two combinations of ethyl silicate, methyl silicate, propyl silicate.
[0030] According to the specific embodiment of the present application, preferably, the coupling agent comprises one or more than two combinations of vinyl silane and / or propylene silane, such as vinyl trimethoxysilane, vinyl tri(2-methoxyethoxy)silane, γ-methacryloyloxypropyl trimethoxysilane. The coupling agent used in the present application has Si-O and C=C double bond. The surface of the glass substrate is rich in hydroxyl. The Si-O bond in the coupling agent molecule is hydrolyzed in water to generate silanol (Si-OH) group. The silanol group and the hydroxyl on the surface of the glass form Si-O-Si bond through condensation reaction. During the polymerization process, the C=C double bond of the coupling agent can add to the unsaturated bond in the monomer molecule to connect the adhesive layer and the anti-fog layer together, increase the cross-linking density of the adhesive layer, and thus improve the adhesion of the anti-fog layer, adhesive layer and glass substrate, and the environmental aging resistance and other abilities.
[0031] According to the specific embodiment of the present application, preferably, the solvent comprises one or more than two combinations of ethanol, methanol, isopropyl alcohol, propylene glycol ethyl ether, propylene glycol methyl ether, ethylene glycol butyl ether.
[0032] According to the specific embodiment of the present application, preferably, the acid solution is hydrochloric acid and / or nitric acid solution. More preferably, the pH of the acid solution is 1.00-6.00. The acid solution in the present application acts as a catalyst for the adhesive layer reaction, and plays a role in regulating the hydrolysis and condensation polymerization rate of the adhesive layer, which is conducive to forming a more uniform Si-O-Si network structure. The amount of the acid solution is controlled within the range of the present application, which can avoid excessive cross-linking or gelation. If the pH of the acid solution is too high, the reaction rate will be reduced, and the network structure will not be dense enough.
[0033] According to the specific embodiment of the present application, preferably, in the anti-fog glass of the present application, the anti-fog layer and the adhesive layer are arranged on the surface of the glass substrate facing the inside of the vehicle.
[0034] According to the specific embodiment of the present application, preferably, the haze change value of the anti-fog glass before and after the abrasion resistance test is less than or equal to 3. The haze change value before and after the abrasion resistance test is confirmed in the following manner:
[0035] The haze of the anti-fog glass is tested to obtain the haze value before the abrasion resistance test;
[0036] The anti-abrasion test is performed on the anti-fog glass, and then the haze test is performed to obtain the haze value after the anti-abrasion test;
[0037] Then the haze change value before and after the anti-abrasion test is calculated in the following manner:
[0038] The haze change value before and after the anti-abrasion test = the haze value after the anti-abrasion test - the haze value before the anti-abrasion test.
[0039] The anti-abrasion test is performed according to the anti-abrasion test of GB / T 5137.1 "Automotive Safety Glass Test Methods Part 1: Mechanical Property Test", wherein the test conditions are: load 2.45N, 100 revolutions.
[0040] In the above anti-fog glass, preferably, the glass substrate is a single piece of glass or a laminated glass.
[0041] In a second aspect, the present application also provides a preparation method of the above anti-fog glass, wherein the preparation method comprises the following steps:
[0042] Step one: coating the adhesive layer coating on the pretreated glass substrate, leveling and heat curing to form an adhesive layer;
[0043] Step two: coating the anti-fog layer coating on the adhesive layer, leveling and UV light curing to form an anti-fog layer, thereby obtaining an anti-fog glass.
[0044] In the above preparation method of the anti-fog glass, preferably, in step one, the temperature of the heat curing is 60-180℃, more preferably 70-150℃.
[0045] In the above preparation method of the anti-fog glass, preferably, in step one, the time of the heat curing is 30-120min.
[0046] In the above preparation method of the anti-fog glass, preferably, in step one, the time of the leveling is 3-5min.
[0047] In the above preparation method of the anti-fog glass, preferably, in step one, the surface energy of the glass substrate is 65mN / m or more. When the surface energy of the glass substrate does not meet the above requirement, it can be made to meet the requirement by pretreatment; the pretreatment is preferably polishing treatment.
[0048] In the above preparation method of the anti-fog glass, preferably, in step two, the irradiation intensity of the UV light curing is 500-1500W / cm 2 , more preferably 700-1200W / cm 2If the irradiation intensity of the UV light curing of the present application is too low, the wear resistance of the anti-fog layer is poor; if the irradiation intensity of the UV light curing of the present application is too high, it will accelerate the initial reaction rate, accelerate the curing speed, and cause the anti-fog layer to be cured unevenly.
[0049] In the above method for preparing the anti-fog glass, preferably, in step two, the energy density of the UV light curing is 3000-8000 mJ / cm 2 , more preferably 4500-6500 mJ / cm 2 If the energy density of the UV light curing of the present application is too low, the anti-fog layer is not fully cured, and the low curing rate will cause the anti-fog performance, wear resistance, moisture resistance, and salt mist resistance of the anti-fog layer to decrease; if the energy density of the UV light curing of the present application is too high, it will cause the anti-fog layer to be over-cured, and even cause yellowing and other aging behaviors.
[0050] In the above method for preparing the anti-fog glass, preferably, in step two, the wavelength of the light source of the UV light curing is 365 nm or 385 nm.
[0051] In the above method for preparing the anti-fog glass, preferably, in step two, the oxygen volume concentration of the UV light curing is less than 8%. If the oxygen concentration of the UV light curing of the present application is too high, it will affect the free radical polymerization reaction, cause the structure of the anti-fog layer to be not dense enough, and thus affect the wear resistance, moisture resistance, and salt mist resistance.
[0052] In the above method for preparing the anti-fog glass, preferably, in step two, the leveling time is 3-5 min.
[0053] In the above method for preparing the anti-fog glass, preferably, in steps one and two, the coating method is selected from spin coating, spraying, shower coating, blade coating, and printing, which can be selected according to actual experimental conditions to achieve the required film thickness. For example, when the coating method is spin coating, the rotation speed of spin coating is 100-800 revolutions, the acceleration is 40-60 revolutions / s, and the spin coating time is 10-40 s.
[0054] Compared with the prior art, the present application has the following beneficial effects:
[0055] The anti-fog glass of the present application comprises a double-layer structure of an anti-fog layer and a bonding layer, the organic-inorganic hybrid bonding layer can realize good interfacial bonding of the glass substrate and the anti-fog layer, the double-layer structure coating has the abilities of anti-fogging, moisture resistance, salt mist resistance, wear resistance, and adhesion, and is more suitable for automobile driving scenarios. The anti-fog glass provided by the present application not only can improve driving safety, but also meets the development trend of energy saving and environmental protection. DETAILED DESCRIPTION
[0056] In order to have a clearer understanding of the technical features, objectives and beneficial effects of the present application, the technical solutions of the present application are described in detail as follows, but cannot be understood as limiting the implementable scope of the present application.
[0057] Example 1
[0058] The present embodiment provides a preparation method of anti-fog glass, specifically comprising the following steps:
[0059] The adhesive layer coating: in a reaction bottle, 50g of propylene glycol methyl ether, 12g of tetraethyl orthosilicate and 8g of vinyl trimethoxysilane were sequentially added and stirred, 20g of hydrochloric acid solution with pH = 1.59 was slowly added, and after mixing, the mixture was stirred at room temperature for 2h.
[0060] The anti-fog layer coating: 25g of polyethylene glycol diacrylate, 30g of N-hydroxy acrylamide, 5g of glycidyl methacrylate, 1g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 3g of dipentaerythritol pentaacrylate, 4g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2g of 2,4-diethylthiazolone and 0.56g of BYK333 were mixed and stirred at room temperature for 0.5h in the dark.
[0061] Preparation of anti-fog glass A1: first polish the single glass substrate, the surface energy is 70mN / m, then clean and dry for standby use;
[0062] The rotation speed of the spin coater was set to 600r / min, the acceleration was 50r / s, and the rotation time was 30s, then the pretreated, cleaned and dried glass substrate was placed on the vacuum chuck of the spin coater, the adhesive layer coating was added dropwise on the surface of the glass, the vacuum pump was started, and coating was carried out; after coating was completed, leveling was carried out for 3min, and then the glass was placed in an oven at 80℃ for heat curing for 120min, after curing was completed, the glass was taken out after it was cooled to room temperature;
[0063] Then, the rotation speed of the spin coater was set to 250r / min, the acceleration was 50r / s, and the rotation time was 30s, the glass with the adhesive layer was placed on the vacuum chuck, the anti-fog layer coating was added dropwise, the vacuum pump was started, and coating was carried out; after coating was completed, leveling was carried out for 3min, and then the glass was placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions were as follows: the wavelength of the light source was 385nm, the irradiation intensity was 1000mW / cm 2 , the energy density was 5000mJ / cm 2 , and the oxygen concentration was 7%(volume fraction).
[0064] Example 2:
[0065] The present embodiment provides a preparation method of anti-fog glass, specifically comprising the following steps:
[0066] Binder layer coating: 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyltrimethoxysilane were sequentially added to a reaction bottle and stirred, and 20 g of a hydrochloric acid solution having a pH of 1.59 was slowly added. After mixing, stirring was performed at room temperature for 2 h.
[0067] Anti-fog layer coating: 35 g of hydroxyethyl methacrylate, 35 g of N,N-dimethylacrylamide, 8 g of benzyl methacrylate, 4 g of pentaerythritol triacrylate, 6 g of (2,4,6-trimethylbenzoyl) diphenylphosphine oxide, and 0.8 g of BYK333 were mixed and stirred at room temperature for 1 h in the dark.
[0068] Preparation of anti-fog glass A2: a single glass substrate was polished and polished to have a surface energy of 68 mN / m, and then washed and dried for standby use;
[0069] The rotation speed of the spin coater was set to 600 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. Then, the pretreated, washed, and dried glass substrate was placed on the vacuum chuck of the spin coater, the binder layer coating was added dropwise to the surface of the glass, the vacuum pump was started, and coating was performed. After leveling for 3 min, it was placed in an oven at 100°C for heat curing for 60 min. After curing was completed, it was taken out after being reduced to room temperature;
[0070] Then, the rotation speed of the spin coater was set to 200 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. The glass with the binder layer was placed on the vacuum chuck, the anti-fog layer coating was added dropwise, the vacuum pump was started, and coating was performed. After leveling for 4 min, it was placed in a UV curing box to form an anti-fog layer, thereby obtaining an anti-fog glass. The conditions for UV curing were as follows: the wavelength of the light source was 385 nm, the irradiation intensity was 1000 mW / cm 2 , the energy density was 4000 mJ / cm 2 , and the oxygen concentration was 4% (volume fraction).
[0071] Example 3:
[0072] The present embodiment provides a method for preparing an anti-fog glass, which specifically comprises the following steps:
[0073] Binder layer coating: 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyltrimethoxysilane were sequentially added to a reaction bottle and stirred, and 20 g of a hydrochloric acid solution having a pH of 1.59 was slowly added. After mixing, stirring was performed at room temperature for 4 h.
[0074] Anti-fog layer coating: 85 g of N-hydroxymethyl acrylamide, 12 g of methyl methacrylate, 6 g of dipentaerythritol pentaacrylate, 5 g of 1-hydroxycyclohexyl phenyl ketone, 3 g of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylbenzophenone, 0.8 g of BYK333 are mixed, and stirred at room temperature for 1 h in the dark.
[0075] Preparation of anti-fog glass A3: first polish the single glass substrate, and the surface energy is 65 mN / m, then clean and dry for standby use;
[0076] The rotation speed of the spin coater is set to 600 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. Then, the pretreated, cleaned and dried glass substrate is placed on the vacuum chuck of the spin coater, the adhesive layer coating is added dropwise on the surface of the glass, the vacuum pump is started, and the coating is carried out. After leveling for 5 min, it is placed in an oven at 120°C for heat curing for 30 min. After curing, it is taken out after cooling to room temperature.
[0077] Then, the rotation speed of the spin coater is set to 150 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. The glass with the adhesive layer is placed on the vacuum chuck, the anti-fog layer coating is added dropwise, the vacuum pump is started, and the coating is carried out. After leveling for 3 min, it is placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions are: light source wavelength is 385 nm, irradiation intensity is 1100 mW / cm 2 , energy density is 5000 mJ / cm 2 , and oxygen concentration is 3% (volume fraction).
[0078] Example 4:
[0079] The present embodiment provides a method for preparing an anti-fog glass, which specifically comprises the following steps:
[0080] Adhesive layer coating: 40 g of propylene glycol methyl ether, 30 g of isopropyl alcohol, 15 g of tetraethyl orthosilicate, and 10 g of vinyltrimethoxysilane are sequentially added to a reaction bottle and stirred. Then, 24 g of hydrochloric acid solution with pH = 4.00 is slowly added, and after mixing, the mixture is stirred at room temperature for 4 h.
[0081] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl acrylate, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 are mixed, and stirred at room temperature for 0.5 h in the dark.
[0082] Preparation of anti-fog glass A4: polish the single glass substrate first, and the surface energy is 70 mN / m, then clean and dry for standby;
[0083] The rotation speed of the spin coater is set to 600 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. Then, the pretreated, cleaned, and dried glass substrate is placed on the vacuum chuck of the spin coater, and the adhesive layer coating is added dropwise on the glass surface. The vacuum pump is started, and coating is performed. After coating, leveling is performed for 3 min, and then the glass is placed in an oven at 80°C for heat curing for 100 min. After curing, the glass is taken out after cooling to room temperature.
[0084] Then, the rotation speed of the spin coater is set to 100 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. The glass with the adhesive layer is placed on the vacuum chuck, and the anti-fog layer coating is added dropwise. The vacuum pump is started, and coating is performed. After leveling for 3 min, the glass is placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining anti-fog glass. The UV curing conditions are as follows: light source wavelength is 385 nm, irradiation intensity is 1100 mW / cm 2 , energy density is 5000 mJ / cm 2 , and oxygen concentration is 5% (volume fraction).
[0085] Example 5
[0086] The preparation method of the anti-fog glass provided in this embodiment is different from that of Example 1 in that:
[0087] The first monomer is 25 g of polyethylene glycol dipropylate and 30 g of N,N-dimethyl acrylamide.
[0088] Example 6
[0089] The preparation method of the anti-fog glass provided in this embodiment is different from that of Example 1 in that:
[0090] The second monomer is 6 g of ethylene glycol dimethyl acrylate and 2 g of butyl acrylate.
[0091] Comparative Example 1
[0092] The preparation method of the anti-fog glass provided in this comparative example specifically includes the following steps:
[0093] The adhesive layer coating: in a reaction bottle, 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyl trimethoxysilane are sequentially added and stirred. Then, 20 g of hydrochloric acid solution with pH = 1.59 is slowly added. After mixing, stirring is performed at room temperature for 4 h.
[0094] Anti-fog layer coating: 40 g of N-methylol acrylamide, 20 g of methyl methacrylate, 4 g of dipentaerythritol pentaacrylate, 3 g of 1-hydroxycyclohexyl phenyl ketone, 3 g of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylbenzophenone, and 0.8 g of BYK333 are mixed, and stirred at room temperature for 1 h in the dark.
[0095] Preparation of anti-fog glass B1: polish and polish the single glass substrate first, and the surface energy is 65 mN / m, then clean and dry for standby;
[0096] The rotation speed of the spin coater is set to 600 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. Then, the pretreated, cleaned and dried glass substrate is placed on the vacuum chuck of the spin coater, the adhesive layer coating is added dropwise on the surface of the glass, the vacuum pump is started, and the coating is carried out. After leveling for 5 min, it is placed in a 120°C oven for heat curing for 30 min. After curing, it is taken out after cooling to room temperature.
[0097] Then, the rotation speed of the spin coater is set to 150 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. The glass with the adhesive layer is placed on the vacuum chuck, the anti-fog layer coating is added dropwise, the vacuum pump is started, and the coating is carried out. After leveling for 3 min, it is placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions are: light source wavelength is 385 nm, irradiation intensity is 1100 mW / cm 2 , energy density is 5000 mJ / cm 2 , and oxygen concentration is 3% (volume fraction).
[0098] Comparative Example 2
[0099] The present comparative example provides a preparation method of an anti-fog glass, which specifically comprises the following steps:
[0100] Adhesive layer coating: 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyltrimethoxysilane are sequentially added to a reaction bottle and stirred, and 20 g of hydrochloric acid solution with pH = 1.59 is slowly added. After mixing, stirring is carried out at room temperature for 2 h.
[0101] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 are mixed, and stirred at room temperature for 0.5 h in the dark.
[0102] Preparation of anti-fog glass B2: polish and polish the single glass substrate first, and the surface energy is 70 mN / m, then clean and dry for standby;
[0103] The rotation speed of the spin coater was set to 600 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. Then, the pretreated, cleaned, and dried glass substrate was placed on the vacuum chuck of the spin coater, and the adhesive layer coating was added dropwise on the glass surface. The vacuum pump was started, and coating was performed. After coating was completed, leveling was performed for 3 min, and the glass was placed in an oven at 80°C for heat curing for 120 min. After curing was completed, the glass was removed after it cooled to room temperature.
[0104] Then, the rotation speed of the spin coater was set to 250 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. The glass with the adhesive layer was placed on the vacuum chuck, and the anti-fog layer coating was added dropwise. The vacuum pump was started, and coating was performed. After coating was completed, leveling was performed for 3 min, and the glass was placed in a UV curing box to form an anti-fog layer, thereby obtaining anti-fog glass. The UV curing conditions were as follows: a light source with a wavelength of 385 nm, an irradiation intensity of 1000 mW / cm 2 , an energy density of 5000 mJ / cm 2 , and an oxygen concentration of 7% (volume fraction).
[0105] Comparative Example 3
[0106] The present comparative example provides a method for preparing anti-fog glass, which specifically comprises the following steps:
[0107] Adhesive layer coating: 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyltrimethoxysilane were sequentially added to a reaction bottle and stirred. Then, 20 g of hydrochloric acid solution with a pH of 1.59 was slowly added. After mixing, stirring was performed at room temperature for 2 h.
[0108] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 7 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 were mixed and stirred at room temperature for 0.5 h in the dark.
[0109] Preparation of anti-fog glass B3: A single glass substrate was polished and polished to have a surface energy of 70 mN / m, and then cleaned and dried for standby use.
[0110] The rotation speed of the spin coater was set to 600 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. Then, the pretreated, cleaned, and dried glass substrate was placed on the vacuum chuck of the spin coater, and the adhesive layer coating was added dropwise on the glass surface. The vacuum pump was started, and coating was performed. After coating was completed, leveling was performed for 3 min, and the glass was placed in an oven at 80°C for heat curing for 120 min. After curing was completed, the glass was removed after it cooled to room temperature.
[0111] Then, the spin coater speed is set to 250 rpm, the acceleration is 50 rpm / s, the rotation time is 30 s, the glass with the adhesive layer is placed on the vacuum chuck, the anti-fog layer coating is added dropwise, the vacuum pump is started, and coating is performed; after leveling for 3 min, it is placed in a UV curing box to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions are: a light source with a wavelength of 385 nm, an irradiation intensity of 1000 mW / cm 2 , an energy density of 5000 mJ / cm 2 , and an oxygen concentration of 7% (volume fraction).
[0112] Comparative Example 4
[0113] The present comparative example provides a method for preparing an anti-fog glass, specifically comprising the following steps:
[0114] Adhesive layer coating: in a reaction bottle, 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of γ-glycidoxypropyltrimethoxysilane are sequentially added and stirred, 20 g of hydrochloric acid solution with pH = 1.59 is slowly added, and after mixing, stirring is performed at room temperature for 2 h.
[0115] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 are mixed and stirred at room temperature for 0.5 h in the dark.
[0116] Preparation of anti-fog glass B4: first polish the single glass substrate, and the surface energy is 70 mN / m, then clean and dry for standby use;
[0117] The spin coater speed is set to 600 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s, then the pretreated, cleaned, and dried glass substrate is placed on the vacuum chuck of the spin coater, the adhesive layer coating is added dropwise on the glass surface, the vacuum pump is started, and coating is performed; after leveling for 3 min, it is placed in an oven at 80°C for heat curing for 120 min, and after curing, it is taken out after cooling to room temperature;
[0118] Then, the spin coater speed is set to 250 rpm, the acceleration is 50 rpm / s, the rotation time is 30 s, the glass with the adhesive layer is placed on the vacuum chuck, the anti-fog layer coating is added dropwise, the vacuum pump is started, and coating is performed; after leveling for 3 min, it is placed in a UV curing box to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions are: a light source with a wavelength of 385 nm, an irradiation intensity of 1000 mW / cm 2 , an energy density of 5000 mJ / cm2 oxygen concentration of 7% (volume fraction).
[0119] Comparative Example 5
[0120] The present comparative example provides a method for preparing an anti-fog glass, specifically comprising the following steps:
[0121] The adhesive layer coating: in a reaction bottle, 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyl trimethoxysilane were sequentially added and stirred, 20 g of hydrochloric acid solution with pH = 1.59 was slowly added, and after mixing, it was stirred at room temperature for 2 h.
[0122] The anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 were mixed and stirred at room temperature for 0.5 h in the dark.
[0123] Preparation of anti-fog glass B5: the single glass substrate was polished and polished first, and the surface energy was 70 mN / m, and then it was cleaned and dried for standby use;
[0124] The rotation speed of the spin coater was set to 600 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. Then the pretreated, cleaned, and dried glass substrate was placed on the vacuum chuck of the spin coater, the adhesive layer coating was added dropwise on the surface of the glass, the vacuum pump was started, and the coating was carried out. After leveling for 3 min, it was placed in an oven at 80°C for heat curing for 120 min. After curing, it was taken out after cooling to room temperature.
[0125] Then, the rotation speed of the spin coater was set to 250 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. The glass with the adhesive layer was placed on the vacuum chuck, the anti-fog layer coating was added dropwise, the vacuum pump was started, and the coating was carried out. After leveling for 3 min, it was placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions were: light source wavelength of 385 nm, irradiation intensity of 1000 mW / cm 2 , energy density of 5000 mJ / cm 2 oxygen concentration of 20.9% (volume fraction).
[0126] Comparative Example 6
[0127] The present comparative example provides a method for preparing an anti-fog glass, specifically comprising the following steps:
[0128] Binder layer coating: In a reaction bottle, 50 g of propylene glycol methyl ether, 12 g of tetraethyl orthosilicate, and 8 g of vinyltrimethoxysilane were sequentially added and stirred, 20 g of a hydrochloric acid solution with pH = 1.59 was slowly added, and after mixing, stirring was performed at room temperature for 2 h.
[0129] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 were mixed and stirred at room temperature for 0.5 h in the dark.
[0130] Preparation of anti-fog glass B6: The single glass substrate was polished and polished first, and the surface energy was 70 mN / m, and then cleaned, dried and ready for use;
[0131] The rotation speed of the spin coater was set to 600 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. Then, the pretreated, cleaned, and dried glass substrate was placed on the vacuum chuck of the spin coater, the binder layer coating was added dropwise on the surface of the glass, the vacuum pump was started, and coating was performed. After leveling for 3 min, it was placed in an oven at 80°C for heat curing for 120 min. After curing, it was taken out after cooling to room temperature.
[0132] Then, the rotation speed of the spin coater was set to 250 rpm, the acceleration was 50 rpm / s, and the rotation time was 30 s. The glass with the binder layer was placed on the vacuum chuck, the anti-fog layer coating was added dropwise, the vacuum pump was started, and coating was performed. After leveling for 3 min, it was placed in a UV curing box for curing to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions were: a light source with a wavelength of 385 nm, an irradiation intensity of 1000 mW / cm 2 , an energy density of 1500 mJ / cm 2 , and an oxygen concentration of 7% (volume fraction).
[0133] Comparative Example 7
[0134] This comparative example provides a method for preparing an anti-fog glass, which specifically comprises the following steps:
[0135] Anti-fog layer coating: 25 g of polyethylene glycol diacrylate, 30 g of N-hydroxy acrylamide, 5 g of glycidyl methacrylate, 1 g of 2-hydroxy-3-phenoxypropyl 2-acrylate, 3 g of dipentaerythritol pentaacrylate, 4 g of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, 2 g of 2,4-diethylthiazolone, and 0.56 g of BYK333 were mixed and stirred at room temperature for 0.5 h in the dark.
[0136] Preparation of anti-fog glass B7: polish the single glass substrate first, and the surface energy is 70 mN / m, then clean and dry for standby;
[0137] The spin coater speed is set to 250 rpm, the acceleration is 50 rpm / s, and the rotation time is 30 s. The glass is placed on the vacuum chuck, the anti-fog layer coating is added dropwise, the vacuum pump is started, and the coating is performed. After leveling for 3 min, it is placed in a UV curing box to form an anti-fog layer, thereby obtaining an anti-fog glass. The UV curing conditions are: light source wavelength of 385 nm, irradiation intensity of 1000 mW / cm 2 , energy density of 5000 mJ / cm 2 , and oxygen concentration of 7% (volume fraction).
[0138] The anti-fog glass provided in the above examples and comparative examples is tested, and the test method is as follows:
[0139] (1) Film thickness test
[0140] The coating thickness is tested by MCPD film thickness meter.
[0141] (2) Anti-fog performance test
[0142] The anti-fog glass is placed in a constant temperature water bath with a distance of 70 mm from the water surface in a sealed state, and the constant temperature water bath temperature is 35℃. The time from the start to the visual confirmation of fogging is the anti-fog time T (s).
[0143] (3) Humidity resistance test
[0144] According to the humidity resistance test of standard GB / T 5137.3 "Automobile safety glass test method part 3: resistance to radiation, high temperature, humidity, combustion and resistance to simulated climate test", the sample is placed in a 50℃, 95% RH environmental chamber for 1000h. After the test, the appearance of the anti-fog glass has no obvious change, and the coating has no cracking and falling off, which is considered to be qualified.
[0145] (4) Neutral salt spray test
[0146] According to the neutral salt spray test of standard GB / T 10125 "Artificial atmosphere corrosion test salt spray test", the test period is 720h. After the test, the appearance of the anti-fog glass has no obvious change, and the coating has no cracking and falling off, which is considered to be qualified.
[0147] (5) Abrasion resistance test
[0148] The abrasion resistance test is carried out according to the abrasion resistance test of standard GB / T 5137.1 "Automobile safety glass test methods Part 1: Mechanical property test", the load is 2.45N, 100 revolutions, the haze change value ΔH before and after the test is used as the evaluation index, the greater the haze change value ΔH, the worse the abrasion resistance, and the haze change value ΔH≤3 meets the requirements.
[0149] (6) Haze test
[0150] The haze value of the anti-fog glass is tested by using a BYK haze meter.
[0151] (7) Cross-cut test
[0152] The cross-cut test is carried out on the anti-fog glass according to standard GB / T 9286-1998 "Cross-cut test of paint film of pigmented and clear coatings", and the grade evaluation is carried out, and 0-1 grade meets the requirements.
[0153] When the glass substrate is a laminated glass, the anti-fog glass comprises a second glass and a bonding layer and an anti-fog layer coated on the second glass, the anti-fog layer is arranged on the surface of the second glass facing the inside of the vehicle; the anti-fog glass further comprises a connecting layer connected to the surface of the second glass facing the outside of the vehicle, and the other side of the connecting layer is connected to the surface of the first glass facing the inside of the vehicle. The connecting layer can be one or a combination of two or more of polyvinyl butyral, ethylene vinyl acetate, polyurethane or a copolymer or derivative thereof.
[0154] Table 1 is the test results of the anti-fog glass of examples 1-6 and comparative examples 1-7.
[0155] Table 1
[0156]
[0157] As can be seen from Table 1, the anti-fog glass of examples 1-6 is qualified in terms of moisture resistance, neutral salt spray resistance, abrasion resistance and cross-cut test, the anti-fog glass in the present application does not stick and does not fog after moisture aging, and it has a dense spatial network structure and can resist harsh environmental aging tests.
[0158] Compared with example 3, when the content of the hydrophilic monomer in the anti-fog layer coating is too low, the anti-fog performance and the cross-cut performance of the coating are obviously decreased.
[0159] Compared with example 1, when the second monomer is not added in the anti-fog layer coating, the moisture resistance, neutral salt spray resistance and abrasion resistance are obviously decreased, because the second monomer has a certain hydrophobicity or rigidity, and when the second monomer is not added, the water resistance and mechanical properties of the anti-fog glass will be poor.
[0160] Comparative Example 3 compared with Example 1, when the amount of crosslinking agent in the anti-fog layer coating is too much, the crosslinking density of the coating will rise, and its brittleness will also rise, resulting in the abrasion resistance and adhesion of the anti-fog glass to decline.
[0161] Comparative Example 4 compared with Example 1, when a coupling agent without double bond group (γ-glycidoxypropyltrimethoxysilane) is used in the bonding layer coating, the moisture resistance, neutral salt spray resistance, and crosshatch knife test of the anti-fog glass are all unqualified, because the bonding layer only combines with the glass substrate, and fails to form an interface combination with the anti-fog layer.
[0162] Comparative Example 5 and Comparative Example 6 compared with Example 1, the moisture resistance, neutral salt spray resistance, abrasion resistance, and crosshatch knife test of the anti-fog glass have a great relationship with the oxygen concentration and the irradiation energy density of the curing. This is because when the oxygen concentration or the irradiation energy density of the present application does not meet the requirements, it will lead to incomplete reaction or not enough dense surface of the anti-fog glass, thus resulting in the performance of the anti-fog glass to decline.
[0163] Comparative Example 7 compared with Example 1, when there is only one anti-fog layer without the bonding layer of the present application, the moisture resistance, neutral salt spray resistance, and crosshatch knife test of the anti-fog glass are all unqualified, because the anti-fog layer cannot directly interface combine with the glass substrate, thus the bonding layer of the present application is needed to connect the anti-fog layer and the glass substrate.
Claims
1. Anti-fog glass, wherein, The anti-fog glass comprises a glass substrate, a bonding layer and an anti-fog layer, the bonding layer is arranged between the anti-fog layer and the glass substrate; The thickness of the bonding layer is 0.3-6 μm, and the thickness of the anti-fog layer is 10-100 μm; The anti-fog glass has a haze change value less than or equal to 3 before and after the abrasion resistance test; The anti-fog time of the anti-fog glass is greater than 120 s; The anti-fog glass has a cross-cut knife test less than or equal to 1 level.
2. The anti-fog glass according to claim 1, wherein, The anti-fog layer is prepared from an anti-fog layer coating; the anti-fog layer coating contains, in terms of mass fraction, 70-90 parts of a first monomer, 5-15 parts of a second monomer, 3-6 parts of a cross-linking agent and 5-10 parts of a photoinitiator; The first monomer includes one or more than two combinations of hydroxyethyl methacrylate, polyethylene glycol diacrylate, N-hydroxymethyl acrylamide, methyl acrylamide, N-isopropyl acrylamide and N,N-dimethyl acrylamide. The second monomer includes one or more than two combinations of trifluoroethyl methacrylate, methyl methacrylate, butyl acrylate, ethylene glycol dimethyl acrylate, glycidyl methacrylate, benzyl methacrylate and 2-hydroxy-3-phenoxypropyl acrylate.
3. The anti-fog glass according to claim 2, wherein, The first monomer includes 30-40 parts of polyethylene glycol diacrylate and 40-50 parts of N-hydroxy acrylamide. Alternatively, the first monomer includes 35-45 parts of hydroxyethyl methacrylate and 35-45 parts of N,N-dimethyl acrylamide.
4. The anti-fog glass according to claim 2, wherein, The second monomer includes 5-10 parts of glycidyl methacrylate and 1-5 parts of 2-hydroxy-3-phenoxypropyl acrylate.
5. The anti-fog glass according to claim 1, wherein, The thickness of the anti-fog layer is 10-100 μm.
6. The anti-fog glass according to claim 2, wherein, The cross-linking agent includes one or more than two combinations of pentaerythritol triacrylate, pentaerythritol tetraacrylate, trimethylolpropane triacrylate and dipentaerythritol pentaacrylate. The photoinitiator includes one or more than two combinations of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, methyl phenylacetate, 2-hydroxy-2-methyl-1-phenyl-1-propanone, (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide, ethyl (2,4,6-trimethylbenzoyl) phenyl phosphine and 1-hydroxycyclohexyl phenyl ketone.
7. The anti-fog glass according to claim 2, wherein, The anti-fog layer coating further contains 0.05%-0.2% of an auxiliary agent; the auxiliary agent is a leveling agent.
8. The anti-fog glass according to claim 1, wherein, The bonding layer is prepared from a bonding layer coating; The bonding layer coating contains silicate, coupling agent, acid solution and solvent in a mass ratio of 10-15:2-15:15-25:50-65.
9. The anti-fog glass according to claim 8, wherein, The bonding layer coating contains silicate 10%-15%, coupling agent 2%-15%, acid solution 15%-25% and solvent 50%-65% in terms of mass percentage.
10. The anti-fog glass according to claim 1 or 8, wherein, The thickness of the bonding layer is 0.3-6 μm.
11. The anti-fog glass according to claim 8, wherein, The silicate includes one or more than two combinations of ethyl silicate, methyl silicate and propyl silicate.
12. The anti-fog glass according to claim 8, wherein, The coupling agent includes vinyl silane and / or propylene silane; and / or The solvent includes one or more than two combinations of ethanol, methanol, isopropyl alcohol, propylene glycol ethyl ether, propylene glycol methyl ether, ethylene glycol butyl ether.
13. The anti-fog glass according to claim 12, wherein, The coupling agent includes one or more than two combinations of vinyl trimethoxysilane, vinyl tri(2-methoxyethoxy)silane, gamma-methacryloyloxypropyl trimethoxysilane.
14. The anti-fog glass according to claim 1, wherein, The anti-fog layer and the adhesive layer are arranged on the surface of the glass substrate facing the vehicle interior.
15. A method of producing the anti-fog glass according to any one of claims 1 to 14, wherein, The preparation method comprises the following steps: Step one: coating the adhesive layer coating on the glass substrate, leveling, and heat curing to form the adhesive layer; Step two: coating the anti-fog layer coating on the adhesive layer, leveling, and UV light curing to form the anti-fog layer, thereby obtaining the anti-fog layer and the anti-fog glass.
16. The method of claim 15, wherein the anti-fog glass is prepared by the steps of: In step one, the temperature of the heat curing is 60-180℃, and the time is 30-120min. And / or, the leveling time is 3-5min.
17. The method of claim 16, wherein the anti-fog glass is prepared by the steps of: In step one, the surface energy of the glass substrate is 65mN / m or more.
18. The method of claim 16, wherein the anti-fog glass is prepared by the steps of: In step two, the irradiation intensity of the UV light curing is 500-1500 W / cm 2 , and the energy density is 3000-8000 mJ / cm 2 . And / or, the wavelength of the UV light source for curing is 365nm or 385nm.
19. The method of claim 16, wherein the anti-fog glass is prepared by the steps of: In step two, the oxygen volume concentration for UV light curing is less than 8%; And / or, the leveling time is 3-5min.
20. The method of claim 16, wherein the anti-fog glass is prepared by the steps of: The coating method is selected from spin coating, spraying, showering, scraping, and printing.
21. The method of claim 20, wherein the anti-fog glass is prepared by the steps of: The rotation speed of the spin coating is 100-800rpm, the acceleration is 40-60rpm / s, and the spin coating time is 10-40s.
Citation Information
Patent Citations
Antifogging product and vehicle glass
CN108025542A
