Mirror anti-fouling and anti-fog high-adhesion coating and preparation method and application thereof
By leveraging the synergistic effect of nano-titanium oxide encapsulating hollow silica and chain-like tin-antimony oxide, the problem of easy aggregation of nano-TiO2 coatings on mirror surfaces was solved, achieving mirror coatings with high adhesion and anti-fog and anti-fog properties, while reducing costs and process complexity.
Patent Information
- Application Number
- CN202610625699.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Filing Date
- 2026-05-08
- Publication Date
- 2026-07-10
AI Technical Summary
In existing technologies, nano-TiO2 coatings tend to agglomerate on mirror surfaces, resulting in poor wear resistance, insufficient adhesion, and inadequate anti-fogging performance. Furthermore, multi-layer coatings increase costs and processing time.
The hollow silica encapsulated with nano-titanium oxide works synergistically with chain-like tin-antimony oxide, combined with ethanol/ethylene glycol propyl ether/deionized water solvent to enhance dispersibility, and forms a highly adhesive, anti-fog, and anti-fogging coating on the mirror surface through a spraying process.
It achieves high adhesion, anti-fog and anti-fog properties, and self-cleaning function of mirror coating, while reducing the number of coating layers, thus reducing costs and processing time.
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Figure CN122356848A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the technical field of mirror coatings, and relates to a mirror anti-fog and anti-fog high adhesion coating, its preparation method, and its application. Specifically, it relates to an anti-fog and anti-fog high adhesion coating based on nano-titanium oxide encapsulating hollow silica and chain-like antimony tin oxide, its preparation method, and a process method to enhance the adhesion of the coating when it is sprayed onto a mirror surface. Background Technology
[0002] Photocatalysis is the most attractive method for preparing self-cleaning coatings. TiO2 is considered an ideal photocatalyst due to its excellent properties, including high photocatalytic activity, chemical stability, non-toxicity, and good resistance to photocorrosion. Nano-TiO2 possesses the unique surface effects, volume effects, quantum size effects, and macroscopic quantum tunneling effects characteristic of nanoparticles, and exhibits unique properties such as strong photocatalytic activity, good thermal conductivity, and good dispersibility. As one of the main nanomaterials, it is widely used in the chemical industry. Its application and development as a novel coating component in the coating industry has become a research hotspot.
[0003] With the advancement of my country's coating industry and coating technology, the research, development, and application of mirror coatings have received widespread attention. Since its emergence in the 1980s, nano-TiO2 has been increasingly used in coating applications due to its unique photocatalytic properties, ultraviolet shielding, and angle-dependent color variation effect, leading to a growing demand for it.
[0004] Currently, in the field of vehicle rearview mirror coating technology, nano-TiO2 is mainly used in the construction of anti-reflective films and infrared anti-reflective films, and it has advantages such as high refractive index, wide spectrum control capability and photocatalytic self-cleaning effect.
[0005] For example, Chinese invention patent application "Multifunctional Reflective Film for Vehicle Exterior Mirror and Preparation Method Thereof" (CN106324731A) discloses a multifunctional reflective film for vehicle exterior mirrors and its preparation method. The reflective film includes a glass substrate, a first high-refractive-index layer, a first low-refractive-index layer, a second high-refractive-index layer, a second low-refractive-index layer, a metal material layer, a third low-refractive-index layer, and a conductive layer, stacked sequentially. The materials for the first and second high-refractive-index layers are Ta2O5, TiO2, and Nb2O5; the materials for the first, second, and third low-refractive-index layers are MgF2 and SiO2. x N y The materials used for the metal layer are Al and Ag; the materials used for the conductive layer are ITO and graphene.
[0006] However, in the aforementioned patent literature and prior art, nano-TiO2 is mostly used as a single coating layer. Therefore, to achieve multifunctionality, it is often necessary to combine it with other coatings for multi-layer coating. Furthermore, nano-TiO2 has drawbacks such as easy agglomeration during preparation, transportation, and storage. This leads to the formation of micron-sized pores during coating, reducing the wear resistance of the coating. Coatings primarily using nano-TiO2 also generally suffer from poor adhesion, insufficient mechanical properties, and inadequate anti-fogging performance. In addition, an excessive number of coating layers in mirror coating processes can significantly increase costs and processing time.
[0007] Therefore, there is an urgent need for a multifunctional coating material for mirror surfaces that can combine nano-TiO2, which has anti-fog and anti-fog properties as well as high adhesion, and has good application prospects while reducing the number of coating layers. Summary of the Invention
[0008] To address the problems in the prior art, this invention provides a high-adhesion, anti-fog, and anti-hazing coating for mirror surfaces, its preparation method, and its application. On one hand, it leverages the synergistic effect of nano-titanium oxide encapsulating hollow silica with a unique microstructure and chain-like antimony tin oxide to impart anti-fog and anti-hazing properties to the coating, while also providing antistatic and self-cleaning functions, as well as high adhesion to mirror materials. On the other hand, it provides a process method to enhance the adhesion of the above coating when sprayed onto mirror surfaces, especially chromium-containing inert mirror surfaces.
[0009] To achieve the above objectives, the present invention employs a technical solution consisting of the following technical measures.
[0010] On one hand, the present invention provides a mirror-finish anti-fog and high-adhesion coating, which, by weight, comprises the following raw material components:
[0011] 4-8 parts of nano-titanium oxide-encapsulated hollow silica dispersion
[0012] 0.1~0.5 parts of chain-like antimony tin oxide dispersion,
[0013] 50-60 parts of ethanol
[0014] 5-10 parts deionized water
[0015] 20-30 parts of ethylene glycol propyl ether
[0016] 1-2 parts of propylene glycol butyl ether
[0017] 2-4 parts of ethyl silicate adhesive;
[0018] The preparation method of the nano-titanium oxide-encapsulated hollow silica dispersion includes the following steps: 100-150 mL of a 5 wt% nano-hollow silica dispersion is added to 360-540 mL of deionized water and mixed. The pH value is adjusted to 2.0, and the mixture is homogeneous to prepare solution A. 34-51 mL of tetrabutyl titanate is dissolved in 100-150 mL of ethanol to prepare solution B. Solution B is added dropwise to solution A while stirring. After the addition is complete, stirring and mixing are continued for at least 48 h. The precipitate is then collected by centrifugation, washed with water, and calcined at 500 ℃ for 1 h. Finally, the obtained product is dispersed in deionized water to prepare a 5 wt% nano-titanium oxide-encapsulated hollow silica dispersion.
[0019] The preparation method of the chain-like antimony tin oxide dispersion includes the following steps: 28.2–56.4 g of SnCl·2H₂O is dissolved in 250–500 mL of ethanol to prepare solution C; 2.85–5.7 g of SbCl₃ is dissolved in 25–50 mL of ethanol to prepare solution D; solution D is added dropwise to solution C while stirring, and stirring is continued for 30 min after the addition is complete; 250–500 mL of deionized water is added dropwise while stirring, and stirring is continued for 1 h after the addition is complete; then the pH is adjusted to 9.0 and stirring is continued for 4 h; after the time is reached, the mixture is allowed to stand for at least 12 h to obtain a yellow intermediate gel product. After filtration and washing with water until neutral, the product is dried, ground into powder, and then calcined at 550 ℃ for 2 h. The obtained product is dispersed in deionized water to prepare an aqueous dispersion with a mass concentration of 5 wt%, and then ultrasonically treated and the pH is adjusted to 8.5, followed by hydrothermal treatment at 180 ℃ for 12 h. h, thus obtaining a chain-like antimony tin oxide dispersion.
[0020] The main inventive point of this invention lies in the synergistic effect of nano-titanium oxide encapsulating hollow silica and chain-like antimony tin oxide, which, while imparting antifogging and anti-fogging properties to the coating, also provides antistatic and self-cleaning functions, as well as high adhesion to mirror-like materials. The nano-titanium oxide encapsulating hollow silica structure ensures a high photocatalytic effect, promoting the coating's long-term maintenance of superhydrophilic properties while preserving high light transmittance. The chain-like antimony tin oxide nanostructure exhibits excellent antistatic effects, reducing the surface resistance of the coating and the adhesion of dust.
[0021] Based on the above-mentioned inventive points, this invention also employs a three-system solvent of ethanol / ethylene glycol propyl ether / deionized water to enhance the dispersibility of nano-titanium oxide-encapsulated hollow silica and chain-like antimony tin oxide. Furthermore, propylene glycol butyl ether is used as a dispersant.
[0022] In one technical solution, to facilitate adjustment of wetting properties during spraying, the raw material components may also include commonly known coating additives such as surfactants, defoamers, and leveling agents. Those skilled in the art can refer to the surfactants conventionally used in existing mirror coating technologies for selection and proportioning.
[0023] To better illustrate the present invention and provide a technical solution for reference, the raw material components further include 0.1 to 0.3 parts of surfactant; the surfactant includes, but is not limited to, any one or more of Triton X-100, Tween 20 and Tween 80.
[0024] In this article, the ethyl silicate adhesive is an adhesive with ethyl silicate as the main active component, which can be obtained directly from commercial sources or prepared in-house.
[0025] To better illustrate the present invention, a method for preparing a ethyl silicate adhesive is provided, which specifically includes the following steps. In the following examples, the ethyl silicate adhesive used was prepared in-house according to this method. However, it should be noted that this does not imply a limitation on the source of the ethyl silicate adhesive.
[0026] Mix 93-186 mL of ethyl silicate with 400-800 mL of ethanol to prepare solution E; mix 10-20 mL of 1 mol / L hydrochloric acid, 50-100 mL of deionized water with 47.4-94.8 mL of ethanol to prepare solution F; add solution F dropwise to solution E while stirring, and continue stirring for 12 h after the addition is complete to obtain ethyl silicate adhesive.
[0027] In this paper, the 5 wt% nano-hollow silica dispersion is prepared by hydrolysis of ethyl silicate to obtain nano-hollow silica. Those skilled in the art can refer to conventional preparation methods of nano-silica in the prior art.
[0028] To better illustrate the present invention and provide a technical solution for reference, the preparation method of the 5 wt% nano-hollow silica dispersion includes the following steps:
[0029] 104-208 g of tetraethyl orthosilicate, 25-50 g of ethanol, and 7.5-15 g of polyethylene glycol (average molecular weight 350) were mixed evenly. Then, 7.5-15 g of concentrated nitric acid and 5-10 g of deionized water were added and mixed evenly. After stirring for 5 min, the mixture was heated to 80 °C and reacted for 2 h. The solvent was removed by rotary distillation under reduced pressure to obtain the polyalkoxysiloxane precursor.
[0030] Take 50-100 g of polyalkoxysiloxane precursor and add it to 175-350 g of deionized water. After stirring and mixing, a dispersion is obtained. Add 12.5-25 g of concentrated ammonia and continue stirring for 5 h. Then adjust the pH to less than 10 and add ethanol to adjust the mass concentration to 5 wt%, thus obtaining a nano-hollow silica dispersion with a mass concentration of 5 wt%.
[0031] Typically, the preparation method of the anti-fog, anti-fog, high-adhesion coating for mirror surfaces provided by this invention follows the conventional coating preparation method, which simply involves mixing the raw material components evenly.
[0032] The anti-fog, anti-fog, and high-adhesion coating for mirrors provided by this invention can be directly applied to the coating process of mirrors.
[0033] To better illustrate the present invention, in another aspect, the present invention also provides a method for applying the above-mentioned anti-fog, anti-fog, high-adhesion coating for mirror surfaces, which mainly includes the following steps:
[0034] (1) Use a weak alkaline cleaning agent to perform ultrasonic cleaning on the conventional mirror surface; then spray and rinse the conventional mirror surface to remove residual cleaning agent and dry it.
[0035] (2) Perform surface plasma activation treatment on conventional mirror surfaces;
[0036] (3) Apply anti-fog and anti-fog high adhesion coating to conventional mirrors and control the final film thickness to be 110~130 nm.
[0037] (4) Curing the conventional mirror surface after spray coating at 100~150 ℃ for 3~5 min, and then cooling to room temperature.
[0038] It should be noted that the above application methods are mainly for conventional mirrors, such as ordinary white mirrors and blue mirrors, and can be directly applied to the mirror coating of vehicle rearview mirrors / exterior mirrors.
[0039] When a mirror coating is required on a chrome mirror (chrome-plated mirror), in order to improve the adhesion of the coating, this invention also provides a method for applying the above-mentioned anti-fog, anti-fog, high-adhesion coating for mirrors, which mainly includes the following steps:
[0040] (I) Use a weak alkaline cleaning agent to perform ultrasonic cleaning on the chrome mirror surface; then spray and rinse the chrome mirror surface to remove residual cleaning agent and dry it.
[0041] (II) Perform surface plasma activation treatment on the chromium mirror surface;
[0042] (III) Apply a zirconate coupling agent primer to the chromium mirror surface by spraying and coating, then cure at 100~120 ℃ for 3~5 min, and cool to room temperature;
[0043] (IV) Apply a high-adhesion anti-fog coating to the chromium mirror surface and control the final film thickness to be 110~130 nm; then cure at 100~150 ℃ for 3~5 min and cool to room temperature.
[0044] The zirconate coupling agent primer is a coating prepared by mixing a zirconate coupling agent with an organic solvent.
[0045] To better illustrate the present invention and provide a technical solution for reference, the zirconate coupling agent primer is prepared by mixing the following raw material components in parts by weight:
[0046] 5-20 parts of zirconate coupling agent
[0047] 80-95 parts of ethanol.
[0048] To facilitate adjustment of wettability during spraying, the raw material components of the zirconate coupling agent primer may also include commonly used coating additives such as surfactants, defoamers, and leveling agents. The specific selection is consistent with the aforementioned mirror-finish anti-fog, anti-fog, high-adhesion coating.
[0049] In this document, the mixing, washing, drying, and dripping processes all follow conventional principles in chemical processes, and those skilled in the art can perform the specific operations based on common knowledge. Attached Figure Description
[0050] Figure 1 This is a transmission electron microscope (TEM) image of hollow silica encapsulated in nano-titanium oxide prepared in Example 1 of this invention.
[0051] Figure 2 This is a transmission electron microscope (TEM) image of the chain-like antimony tin oxide prepared in Example 1 of the present invention.
[0052] Figure 3 This is a photograph showing the water contact angle test results of the coating formed on a regular white mirror by the coating prepared in Example 1 of the present invention. Detailed Implementation
[0053] The embodiments of this application will be described in detail below with reference to examples. However, those skilled in the art will understand that the following examples are for illustrative purposes only and should not be construed as limiting the scope of this application. Where specific conditions are not specified in the examples, conventional conditions or conditions recommended by the manufacturer shall apply. Where the manufacturers of reagents or instruments are not specified, they are all commercially available conventional products. This application should not be construed as being limited to the specific embodiments described.
[0054] Example 1
[0055] Example 1 provides a mirror-finish anti-fog and high-adhesion coating, which is obtained by uniformly mixing the following raw material components by weight:
[0056] Five parts of a nano-titanium oxide-encapsulated hollow silica dispersion were used.
[0057] 0.5 parts of chain-like antimony tin oxide dispersion,
[0058] 50 parts ethanol
[0059] 10 parts deionized water
[0060] 20 parts of ethylene glycol propyl ether
[0061] 2 parts of propylene glycol butyl ether
[0062] 3 parts of ethyl silicate adhesive
[0063] 0.25 copies of PPG100;
[0064] The preparation method of the nano-titanium oxide-encapsulated hollow silica dispersion includes the following steps: 100 mL of a 5 wt% nano-hollow silica dispersion is added to 360 mL of deionized water and mixed. The pH value is adjusted to 2.0, and the mixture is homogeneous to prepare solution A. 34 mL of tetrabutyl titanate is dissolved in 100 mL of ethanol to prepare solution B. Solution B is added dropwise to solution A while stirring. After the addition is complete, stirring and mixing are continued for 48 h. The precipitate is then collected by centrifugation, washed with water, and calcined at 500℃ for 1 h. Finally, the obtained product is dispersed in deionized water to prepare a 5 wt% nano-titanium oxide-encapsulated hollow silica dispersion.
[0065] The preparation method of the chain-like antimony tin oxide dispersion includes the following steps: 56.4 g SnCl·2H2O is dissolved in 500 mL ethanol to prepare solution C; 5.7 g SbCl3 is dissolved in 50 mL ethanol to prepare solution D; solution D is added dropwise to solution C while stirring, and stirring is continued for 30 min after the addition is complete; 500 mL deionized water is added dropwise while stirring, and stirring is continued for 1 h after the addition is complete; then the pH value is adjusted to 9.0 and stirring is continued for 4 h; after the time is reached, the mixture is allowed to stand for 12 h to obtain a yellow intermediate gel product; after filtration and washing with water until neutral, the product is dried and ground into powder; then calcined at 550 ℃ for 2 h; the obtained product is dispersed in deionized water to prepare an aqueous dispersion with a mass concentration of 5 wt%; then ultrasonically treated for 30 min and the pH value is adjusted to 8.5; and then hydrothermally treated at 180 ℃ for 12 h to obtain the chain-like antimony tin oxide dispersion.
[0066] The preparation method of the 5 wt% nano-hollow silica dispersion includes the following steps:
[0067] 10.4 g tetraethyl orthosilicate, 2.5 g ethanol, and 0.75 g polyethylene glycol (average molecular weight 350) were mixed evenly. Then, 0.75 g concentrated nitric acid and 0.5 g deionized water were added and mixed evenly. After stirring for 5 min, the temperature was raised to 80 °C and the reaction was continued for 2 h. The solvent was removed by rotary distillation under reduced pressure to obtain the polyalkoxysiloxane precursor.
[0068] 5.0 g of polyalkoxysiloxane precursor was added to 17.5 g of deionized water and stirred to obtain a dispersion. 1.25 g of concentrated ammonia was added and stirring was continued for 5 h. Then, the pH was adjusted to less than 10 and ethanol was added to adjust the mass concentration to 5 wt%, thus obtaining a nano-hollow silica dispersion with a mass concentration of 5 wt%.
[0069] The preparation method of the ethyl silicate adhesive includes the following steps:
[0070] Mix 93 mL of ethyl silicate with 400 mL of ethanol to prepare solution E; mix 10 mL of 1 mol / L hydrochloric acid, 50 mL of deionized water and 47.4 mL of ethanol to prepare solution F; add solution F dropwise to solution E while stirring, and continue stirring for 12 h after the addition is complete to obtain ethyl silicate adhesive.
[0071] Comparative Example 1
[0072] Comparative Example 1 coating was prepared according to the raw material composition and ratio of Example 1, but the nano-titanium oxide-encapsulated hollow silica dispersion was replaced with a nano-hollow silica dispersion with a mass concentration of 5 wt%, and no chain-like antimony oxide dispersion was added. All raw material components were mixed evenly to obtain the coating.
[0073] Comparative Example 2
[0074] Comparative Example 2 coating was prepared according to the raw material composition and proportion of Example 1, but without the addition of chain-like antimony tin oxide dispersion, by mixing all raw material components evenly.
[0075] Comparative Example 3
[0076] Comparative Example 3 coating was prepared according to the raw material composition and ratio of Example 1, but the nano-titanium oxide-encapsulated hollow silica dispersion was replaced with a 5 wt% nano-hollow silica dispersion, and the chain-like tin-antimony oxide dispersion was replaced with non-chain-like tin-antimony oxide nanoparticles. All raw material components were mixed evenly to obtain the coating.
[0077] The preparation method of the non-chain antimony tin oxide nanoparticles includes the following steps:
[0078] Take 1 mol / L SnCl4·5H2O and add it to SbCl3 at a Sb:Sn molar ratio of 10% and mix well. Adjust the pH value to 9 with ammonia water, and disperse it by ultrasonication for 2 h. Take 80 mL and stir the reaction at 180 ℃ for 2 h at a reaction pressure of 1 MPa. The resulting product is dispersed in deionized water under ultrasonic action and separated by centrifugation to obtain non-chain tin-antimony oxide nanoparticles.
[0079] Comparative Example 4
[0080] Comparative Example 4 coating was prepared according to the raw material composition and ratio of Example 1, but the nano-titanium oxide-encapsulated hollow silica dispersion was replaced with a nano-hollow silica dispersion with a mass concentration of 5 wt%, and the raw material components were mixed evenly to obtain the coating.
[0081] Comparative Example 5
[0082] Comparative Example 5 coating was prepared according to the raw material composition and ratio of Example 1, but the chain-like tin-antimony oxide dispersion was replaced with non-chain-like tin-antimony oxide nanoparticles, and the raw material components were mixed evenly to obtain the coating.
[0083] Application Example 1
[0084] Based on the coatings obtained in Example 1 and Comparative Examples 1-5 above, they were applied to the surface of a regular white mirror according to the following application method, and cured to form a coating for subsequent testing:
[0085] (1) Use a commercially available weak alkaline cleaning agent (pH value 7~9) to perform ultrasonic cleaning on the white mirror; then spray and rinse the white mirror to remove residual cleaning agent on the surface and then dry it.
[0086] (2) Use a vacuum plasma cleaner to perform surface plasma activation treatment on the white mirror for about 15 to 30 seconds;
[0087] (3) The coating samples obtained in Example 1 and Comparative Examples 1 to 5 were used to spray and coat the white mirror, and the final film thickness was controlled to be 110 to 130 nm.
[0088] (4) The white mirror that has been coated with the spray coating is cured at 100 °C for 5 min and then cooled to room temperature.
[0089] Among them, the coatings obtained by comparative examples 1 to 5 are designated as groups 1 to 5 in sequence, and the coating obtained by example 1 is designated as group 6.
[0090] like Figure 1 , 2 As shown, the morphology and size of nano-titanium oxide encapsulating hollow silica and chain-like antimony tin oxide were observed using transmission electron microscopy (TEM).
[0091] like Figure 3 As shown, the water contact angle of the coating formed by the paint sample of Example 1 was tested using a contact meter.
[0092] Coating adhesion was tested using the cross-cut adhesion test (GB / T 9286); coating hardness was tested using the pencil hardness test (GB / T6739); surface resistivity was tested using an electrostatic tester (Model: MODEL 800); photolysis index was tested using the fluorescence catalysis method (GB / T 30452-2013); aging performance was tested using the pressure cooker test (PCT); and UV resistance was tested using a xenon lamp.
[0093] The test results are shown in Table 1 below:
[0094] Table 1 Summary of coating tests on the surface of white mirrors in Examples 1 and Comparative Examples 1-5
[0095]
[0096] Application Example 2
[0097] Using the coating obtained in Example 1 as a sample, it was applied to the surface of a chromium mirror according to the following application method, and cured to form a coating for subsequent testing:
[0098] (I) Use a commercially available weak alkaline cleaning agent (pH value 7~9) to perform ultrasonic cleaning on the chromium mirror, remove the residual cleaning agent on the surface and then dry it;
[0099] (II) Perform surface plasma activation treatment on the chromium mirror using a vacuum plasma cleaner for approximately 15-30 seconds;
[0100] (III) A zirconate coupling agent primer was sprayed onto the chromium mirror, and then cured at 100 °C for 5 min, and cooled to room temperature.
[0101] The zirconate coupling agent primer is prepared by mixing the following raw material components in parts by weight:
[0102] 15 parts of zirconate coupling agent,
[0103] 85 parts of ethanol;
[0104] (IV) The coating sample obtained in Example 1 was used to spray and coat the chromium mirror, and the final film thickness was controlled to be 110~130 nm; then it was cured at 100 °C for 5 min and cooled to room temperature.
[0105] The adhesion of the coating obtained in Example 1 to the chrome mirror surface was found to be grade 0 by cross-cut adhesion test (GB / T 9286).
[0106] Based on the steps in Application Example 2, but without using a vacuum plasma cleaner to perform surface plasma activation treatment on the chromium mirror (i.e., step (II) was not performed), the adhesion level was found to be higher than level 2 after testing.
[0107] Based on the steps of Application Example 2, but without using zirconate coupling agent primer to spray coating the chromium mirror (i.e. step (Ⅲ) was not performed), the adhesion level was found to be higher than level 2 after testing.
[0108] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.
Claims
1. A mirror-finish anti-fog, high-adhesion coating, characterized in that... By weight, it includes the following raw material components: 4-8 parts of nano-titanium oxide-encapsulated hollow silica dispersion 0.1~0.5 parts of chain-like antimony tin oxide dispersion, 50-60 parts of ethanol 5-10 parts deionized water 20-30 parts of ethylene glycol propyl ether 1-2 parts of propylene glycol butyl ether 2-4 parts of ethyl silicate adhesive; The preparation method of the nano-titanium oxide-encapsulated hollow silica dispersion includes the following steps: 100-150 mL of a 5 wt% nano-hollow silica dispersion is added to 360-540 mL of deionized water and mixed. The pH value is adjusted to 2.0, and the mixture is homogeneous to prepare solution A. 34-51 mL of tetrabutyl titanate is dissolved in 100-150 mL of ethanol to prepare solution B. Solution B is added dropwise to solution A while stirring. After the addition is complete, stirring and mixing are continued for at least 48 h. The precipitate is then collected by centrifugation, washed with water, and calcined at 500 ℃ for 1 h. Finally, the obtained product is dispersed in deionized water to prepare a 5 wt% nano-titanium oxide-encapsulated hollow silica dispersion. The preparation method of the chain-like antimony tin oxide dispersion includes the following steps: 28.2–56.4 g of SnCl·2H₂O is dissolved in 250–500 mL of ethanol to prepare solution C; 2.85–5.7 g of SbCl₃ is dissolved in 25–50 mL of ethanol to prepare solution D; solution D is added dropwise to solution C while stirring, and stirring is continued for 30 min after the addition is complete; 250–500 mL of deionized water is added dropwise while stirring, and stirring is continued for 1 h after the addition is complete; then the pH is adjusted to 9.0 and stirring is continued for 4 h; after the time is reached, the mixture is allowed to stand for at least 12 h to obtain a yellow intermediate gel product. After filtration and washing with water until neutral, the product is dried, ground into powder, and then calcined at 550 ℃ for 2 h. The obtained product is dispersed in deionized water to prepare an aqueous dispersion with a mass concentration of 5 wt%, which is then ultrasonically treated and the pH is adjusted to 8.5, followed by hydrothermal treatment at 180 ℃ for 12 h. h, thus obtaining a chain-like antimony tin oxide dispersion.
2. The anti-fog, anti-fog, high-adhesion coating for mirror surfaces according to claim 1, characterized in that: The raw material components also include at least one of surfactants, defoamers, and leveling agents.
3. The anti-fog, anti-fog, high-adhesion coating for mirror surfaces according to claim 1, characterized in that: The raw material components also include 0.1 to 0.3 parts of surfactant; the surfactant includes any one or more of Triton X-100, Tween 20 and Tween 80.
4. The anti-fog, anti-fog, high-adhesion coating for mirror surfaces according to claim 1, characterized in that... The preparation method of the ethyl silicate adhesive includes the following steps: Mix 93-186 mL of ethyl silicate with 400-800 mL of ethanol to prepare solution E; mix 10-20 mL of 1 mol / L hydrochloric acid, 50-100 mL of deionized water with 47.4-94.8 mL of ethanol to prepare solution F; add solution F dropwise to solution E while stirring, and continue stirring for 12 h after the addition is complete to obtain ethyl silicate adhesive.
5. The anti-fog, anti-fog, high-adhesion coating for mirror surfaces according to claim 1, characterized in that... The preparation method of the 5 wt% nano-hollow silica dispersion includes the following steps: Mix 104-208 g of tetraethyl orthosilicate, 25-50 g of ethanol, and 7.5-15 g of polyethylene glycol evenly. Then add 7.5-15 g of concentrated nitric acid and 5-10 g of deionized water and mix evenly. After stirring for 5 min, heat to 80 ℃ and continue the reaction for 2 h. Remove the solvent by rotary distillation under reduced pressure to obtain the polyalkoxysiloxane precursor. Take 50-100 g of polyalkoxysiloxane precursor and add it to 175-350 g of deionized water. After stirring and mixing, a dispersion is obtained. Add 12.5-25 g of concentrated ammonia and continue stirring for 5 h. Then adjust the pH to less than 10 and add ethanol to adjust the mass concentration to 5 wt%, thus obtaining a nano-hollow silica dispersion with a mass concentration of 5 wt%.
6. The application of the anti-fog, anti-fog, high-adhesion coating for mirror surfaces as described in claim 1 in the mirror coating process.
7. The application according to claim 6, characterized in that... The application method mainly includes the following steps: (1) Use a weak alkaline cleaning agent to perform ultrasonic cleaning on the conventional mirror surface; then spray and rinse the conventional mirror surface to remove residual cleaning agent and dry it. (2) Perform surface plasma activation treatment on conventional mirror surfaces; (3) Apply the anti-fog and anti-fog high adhesion coating of the mirror surface as described in claim 1 to the conventional mirror surface and control the final film thickness to be 110~130 nm. (4) Curing the conventional mirror surface after spray coating at 100~150 ℃ for 3~5 min, and then cooling to room temperature.
8. The application according to claim 6, characterized in that... The application method mainly includes the following steps: (I) Use a weak alkaline cleaning agent to perform ultrasonic cleaning on the chrome mirror surface; then spray and rinse the chrome mirror surface to remove residual cleaning agent and dry it. (II) Perform surface plasma activation treatment on the chromium mirror surface; (III) Apply a zirconate coupling agent primer to the chromium mirror surface by spraying and coating, then cure at 100~120 ℃ for 3~5 min, and cool to room temperature; (IV) Apply a high-adhesion anti-fog coating to the chromium mirror surface and control the final film thickness to be 110~130 nm; then cure at 100~150 ℃ for 3~5 min and cool to room temperature.
9. The application according to claim 8, characterized in that... The zirconate coupling agent primer is prepared by mixing the following raw material components in parts by weight: 5-20 parts of zirconate coupling agent 80-95 parts of ethanol.
10. The application according to claim 9, characterized in that: The raw material components also include at least one of surfactants, defoamers, and leveling agents.
Citation Information
Patent Citations
Multi-functional reflective film of on-board exterior mirror and preparation method
CN106324731A
