A method of making a three-dimensionally crosslinked network silicone coating material

The preparation of a three-dimensional cross-linked network silicone coating by sol-gel technology and dip coating process solves the problem of poor applicability of coating materials in display touch screen and other fields, and achieves high transparency, fingerprint and stain resistance, while improving the wear resistance and UV aging resistance of the coating.

CN118580769BActive Publication Date: 2026-06-19ZHENGZHOU UNIV

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
ZHENGZHOU UNIV
Filing Date
2024-06-24
Publication Date
2026-06-19

AI Technical Summary

Technical Problem

In the existing technology, coating materials have poor applicability in fields such as display touch screens, especially in terms of fingerprint and stain resistance.

Method used

A three-dimensional cross-linked silicone coating was prepared using sol-gel technology and dip-coating process. A transparent, robust, fingerprint-resistant and stain-resistant silicone coating was prepared by using a Karstedt catalyst to catalyze a hydrosilylation reaction, combined with PVLE silicone sol and a blocked phosphate cationic initiator CTI-200.

Benefits of technology

The coating achieves high transparency, hydrophobicity, oleophobicity, excellent adhesion, abrasion resistance and UV aging resistance, significantly improving the coating's applicability in fields such as display touch screens.

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Abstract

This invention relates to the field of organosilicon coating technology, specifically to a method for preparing an organosilicon coating material with a three-dimensional cross-linked network. A stable, transparent sol system is formed in solution using a sol-gel method, followed by a dip-coating process to obtain an organosilicon coating with a three-dimensional cross-linked network. Under the action of the cationic thermal initiator CTI-200, the -OH groups formed after ring opening of the epoxy groups in the vinyl epoxy compound further react with the silanol groups on the substrate to generate Si-O-Si bonds, giving the coating good pencil hardness and abrasion resistance. Simultaneously, due to the synergistic effect of Si-CH3 and alkenyl long-chain compounds in polymethylhydrosiloxane, as well as the three-dimensional cage structure of cage-like polysilsesquioxane, a functional three-dimensional network structure is formed, giving the coating anti-fingerprint properties. This invention is simple, feasible, low-cost, and scalable, providing a novel transparent, robust, and fingerprint-resistant organosilicon coating, improving its applicability in fields such as display touchscreens.
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Description

Technical Field

[0001] This invention relates to the field of organosilicon coating technology, and more specifically to a method for preparing an organosilicon coating material with a three-dimensional cross-linked network. Background Technology

[0002] In recent years, with the development of information technology and the improvement of living standards, electronic smart devices have been rapidly popularized, accelerating the transformation of human-computer interaction. During use, fingerprints, dust, and other contaminants easily accumulate on their surfaces; fingerprints are a key factor affecting screen functionality, aesthetics, and hygiene. Simultaneously, the screen surface is susceptible to external environmental factors (such as scratches and ultraviolet radiation), thus reducing the overall lifespan of the touchscreen and even the device. Therefore, it is essential to modify the glass of human-computer interaction touchscreens with wear-resistant, stain-resistant, and fingerprint-resistant coatings. Organosilicon materials possess the characteristics of both inorganic and organic materials, and transparent, stain-resistant hard coatings can be synthesized through the sol-gel method. Hard coatings have high hardness and good wear resistance, making them an important approach for surface modification of electronic and optical devices. Therefore, developing organosilicon coatings that are transparent, robust, and fingerprint-resistant through functional modification has become a pressing technical problem to be solved.

[0003] It is well known that surfaces with good liquid repellency have broad application prospects in daily life and industrial production, including heat transfer, droplet collection, distillation, droplet transfer, self-cleaning, and antifouling. Generally, these antiwetting surfaces are created by combining low surface energy materials with engineered surface microstructures; however, superhydrophobic surfaces with micro / nano structures often have poor durability and reduce the transparency of optical materials or devices. While the sliding liquid-injected porous surface (SLIPS) prepared by Aizenberg et al., inspired by pitcher plants, exhibits good transparency and chemical inertness, its complex porous structure, lubricant secretion rate and loss, complex and time-consuming manufacturing process, and instability of its smoothing properties further shorten the coating's lifespan. Fluorocarbons (-CF) (such as perfluoropolyethers, polytetrafluoroethylene, and fluorosilanes) possess low surface energy and oleophobic properties. Although the -CF group is very effective in reducing the surface energy of coatings, its low degradability and persistence in ecosystems have led to its ban in many countries; at the same time, the production process of fluorosilanes is challenging, resulting in high prices for most fluorosilane raw materials on the market.

[0004] In view of this, the present invention prepares a transparent, robust and fingerprint-resistant silicone coating with a three-dimensional cross-linked network through a unique sol-gel technology and dip coating process, achieving wear resistance, fingerprint resistance and stain resistance, and greatly improving the applicability of the coating in display touch screen and other fields. Summary of the Invention

[0005] The purpose of this invention is to provide a method for preparing an organosilicon coating material with a three-dimensional cross-linked network, so as to solve the problem of poor applicability of existing coating materials in fields such as display touch screens.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: a method for preparing an organosilicon coating material with a three-dimensional cross-linked network, comprising the following steps:

[0007] Preparation of S1 and PVLE organosilicon sol

[0008] Polymethylhydrosiloxane, cage-type polysilsesquioxane, alkenyl long carbon chain compound and vinyl epoxy compound are mixed evenly in a solvent, and then Karstedt catalyst is added to react and obtain PVLE organosilicon sol.

[0009] Preparation of S2 and PVLE-I-200 organosilicon sol

[0010] Blocked phosphate cationic initiator CTI-200 was added to the PVLE organosilicon sol prepared in S1, and the PVLE-I-200 organosilicon sol was obtained after the reaction.

[0011] S3, PVLE-I-200 silicone coating application

[0012] The PVLE-I-200 silicone sol obtained in S2 is coated on a substrate to obtain a substrate coated with a silicone coating.

[0013] Curing of S4, PVLE-I-200 silicone coating

[0014] The substrate coated with the silicone coating obtained in S3 is cured to obtain the silicone coating material.

[0015] Furthermore, in S1, the cage-like polysilsesquioxane includes octavinylPOSS, octa(3-butenyl)POSS, and octa(4-pentenyl)POSS.

[0016] Furthermore, in S1, the alkenyl long-chain compound includes dodecyl acrylate; long-chain vinyl POSS, [(CH2=CH-(CH2)] n SiO 1.5 ]8, where n≥10; long-chain alkenylsilane, CH2=CH-(CH2) n -Si(OR)3, where R is a methoxy or ethoxy group, n≥7; long-chain vinyl polysiloxane, CH2=CH-(CH2). n -[Si(CH3)2O] m -Si(CH3)2-(CH2) n-CH=CH2, where m≥10, n≥1; long-chain olefins, CH2=CH-(CH2). n -CH3, where n≥7.

[0017] Furthermore, the long-chain alkenylsilane includes 1-decenyltrimethoxysilane; the long-chain vinyl polysiloxane includes vinyl-terminated polydimethylsiloxane; and the long-chain olefin includes 1-decene.

[0018] Furthermore, in S1, the vinyl epoxy compound includes vinylcyclohexane oxide and epoxy vinylsilane.

[0019] Furthermore, the vinylcyclohexane oxide includes 1,2-epoxy-4-vinylcyclohexane and 1,2-epoxy-4-(5-vinylpentyl)cyclohexane.

[0020] Furthermore, in S1, the solvent includes tetrahydrofuran, toluene, xylene, ethylbenzene, dichloromethane, chloroform, ethyl acetate, butyl acetate, dimethyl sulfoxide, chlorobenzene, dichlorobenzene, and N-methylpyrrolidone.

[0021] Furthermore, in S3, the substrate includes glass, polyvinyl alcohol, polymethyl methacrylate, polycarbonate, hydroxylated polyester film, silicone, and hydroxylated nanomaterial coating.

[0022] Furthermore, in step S3, before coating, the substrate is ultrasonically cleaned and dried, and then the silicone coating is applied using an immersion coating method.

[0023] Furthermore, in step S4, the substrate coated with the silicone coating is transferred to a vacuum oven and vacuum dried to remove volatile solvents.

[0024] The beneficial effects of this invention are:

[0025] In the presence of a Karstedt catalyst, PMHS, VPOSS, LA, and EVCH were rationally combined via hydrosilylation to obtain an environmentally friendly, transparent, hydrophobic, robust, UV-resistant, and stain-resistant silicone coating sol. After introducing the CTI-200 initiator, a multifunctional coating was prepared using a dip-coating method. The prepared silicone coating exhibits excellent visible light transparency, with an average transmittance of approximately 92%. Due to the abundant Si-CH3 in PMHS and the long carbon chains in LA, as well as the multiple crosslinking points provided by the three-dimensional cage structure of VPOSS, the PVLE-I-200 coating achieves hydrophobicity, oleophobicity, excellent adhesion, abrasion resistance, and UV aging resistance. Furthermore, the PVLE-I-200 coating also possesses anti-fingerprint and anti-stain properties, significantly improving the applicability of coated glass in practical applications. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the preparation process of the organosilicon coating in Example 1 of the present invention; wherein, (a) is the synthesis scheme of PVLE sol; and (b) is a schematic diagram of the preparation process of PVLE-I-200 organosilicon coating.

[0027] Figure 2 This is a schematic diagram of the three-dimensional network structure of the PVLE-I-200 organosilicon coating prepared in Example 1 of the present invention;

[0028] Figure 3 These are optical performance test diagrams of the silicone coatings obtained in Embodiment 1 and Comparative Examples 1-4 of the present invention; wherein, (a) optical photographs of different silicone coatings; (b) average visible light transmittance and haze of glass substrates and different silicone coatings; (c) visible light transmittance of glass substrates and different silicone coatings; and (d) visible light reflectance curves of glass substrates and different silicone coatings.

[0029] Figure 4 These are test diagrams of the waterproof and oleophobic properties of the silicone coatings obtained in Example 1 and Comparative Examples 1-4 of the present invention; wherein, (a) the contact angle of deionized water with different silicone coatings; and (b) the contact angle of diiodomethane with different silicone coatings.

[0030] Figure 5 These are test images of the antifouling performance of the silicone coatings obtained in Embodiment 1 and Comparative Examples 1-4 of the present invention; wherein, (a) are photographs of different silicone coatings after ink application, shrinkage and drying; and (b) are photographs of different silicone coatings after cleaning the ink with WIPERS paper towels.

[0031] Figure 6 These are adhesion test images of the silicone coatings obtained in Embodiment 1 and Comparative Examples 1-4 of the present invention; wherein, (a) is a surface morphology image of the PV silicone coating after adhesion test; (b) is a surface morphology image of the PL silicone coating after adhesion test; (c) is a surface morphology image of the PE silicone coating after adhesion test; (d) is a surface morphology image of the PVLE silicone coating after adhesion test; (e) is a surface morphology image of the PVLE-I-200 silicone coating after adhesion test; and (f) are images showing the adhesion grades and pencil hardness of different silicone coatings.

[0032] Figure 7 These are microscopic images of the surface morphology of the organosilicon coating obtained in Example 1 of the present invention after being rubbed with sandpaper; wherein, (a) 0 cycles; (b) 10 cycles; (c) 50 cycles; (d) 100 cycles; (e) 200 cycles; (f) 500 cycles;

[0033] Figure 8These are fingerprint test images of the silicone coating obtained in Example 1 of the present invention; wherein, (a) fingerprint image on blank glass; (b) fingerprint image on PVLE-I-200 coating; (c) fingerprint principle diagram of PVLE-I-200 coating;

[0034] Figure 9 These are test diagrams of the self-cleaning performance of the silicone coating obtained in Example 1 of the present invention; wherein, (a) the original, process and final self-cleaning performance of the PVLE-I-200 coating under the action of a simulant; and (b) the original, process and final self-cleaning performance of the vegetable blended oil on the surface of the PVLE-I-200 coating. Detailed Implementation

[0035] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.

[0036] Example 1

[0037] A method for preparing an organosilicon coating with a three-dimensional cross-linked network includes the following steps:

[0038] Preparation of S1 and PVLE sol

[0039] 8 g of polymethylhydrosiloxane (PMHS), 1.060 g of octavinylPOSS (VPOSS), 3.219 g of dodecyl acrylate (LA), and 9.978 g of 1,2-epoxy-4-vinylcyclohexane (EVCH) were sequentially added to 51.93 g of tetrahydrofuran (THF) and stirred at room temperature for 30 min. Then, 0.058 g of Karstedt catalyst was added, and stirring was continued for 10 h to complete the preparation of PVLE sol (transparent).

[0040] Preparation of S2 and PVLE-I-200 sol

[0041] Add 0.20 g of blocked phosphate cationic initiator CTI-200 to the PVLE sol prepared in S1 and stir at room temperature for 2-3 h; the solution gradually changes from turbid to transparent, and PVLE-I-200 organosilicon sol is obtained.

[0042] S3, PVLE-I-200 silicone coating application

[0043] Before coating, the glass substrate was thoroughly cleaned with alcohol and ultrasonically cleaned for 15 minutes and then dried; the silicone coating was applied using an immersion coating machine.

[0044] At room temperature, the prepared PVLE-I-200 silicone sol was transferred to a beaker, and a glass slide mounted on an immersion coater was slowly immersed in the sol and held for 40 seconds. The descent or lifting speed was the same and controlled at 1.8 mm / s.

[0045] Curing of S4, PVLE-I-200 silicone coating

[0046] The coated glass slides were transferred to a vacuum oven and dried at 100°C for 30 minutes to remove volatile solvents and accelerate the curing process.

[0047] During this process, the excess -Si-H bonds in PMHS undergo a dehydrogenation condensation reaction with the hydroxyl groups (-OH) on the glass surface; the CTI-200 initiator in the PVLE-I-200 coating causes the epoxy groups in EVCH to undergo a ring-opening reaction, thereby improving the adhesion of the coating.

[0048] The principle of this invention is as follows:

[0049] 1. Coating transparency mechanism

[0050] The addition of VPOSS helps maintain higher transmittance in the visible light range, which is not entirely the same phenomenon observed in coatings prepared by adding other types of nanoparticles (such as SiO2, TiO2, and ZnO). This is because VPOSS material has a nanocage structure, the size of which is much smaller than one-quarter of the wavelength of visible light; in addition, the three-dimensional cage structure of VPOSS helps reduce the absorption of light by the coating, thus the coating has stable transmittance and reflectance in the wavelength range of 380–780 nm.

[0051] 2. Principle of coating durability

[0052] Polymethylhydrosiloxane (PMHS) is a relatively soft and flexible silicon-based polymer. The active hydrogen on its side chains readily combines with monomers, oligomers, or polymers containing double bonds to form block, graft, or cross-linked polymers. Under the action of Karstedt catalysts, the silane (-Si-H) groups in PMHS exhibit strong reactivity with vinyl groups and -OH groups in other substances. Cage-type polysilsesquioxane (POSS) is a high-performance material with organic-inorganic bonding characteristics. Its inorganic core is composed of a silicon-oxygen skeleton with alternating -Si-O- bonds, giving it excellent thermal and mechanical properties. Introducing VPOSS with multiple cross-linking sites can enhance the hardness and toughness of the coating. Furthermore, the rigid structure of the epoxy cyclohexyl functional groups in the coating is beneficial for increasing the coating's hardness.

[0053] 3. Coating anti-fingerprint principle

[0054] Due to the synergistic effect of Si-CH3 and LA long carbon chains in PMHS and the three-dimensional cage structure of VPOSS forming a functional three-dimensional network structure, sweat and oil aggregate into beads on the surface (making them easier to carry away) and are difficult to adhere to the coating surface.

[0055] Comparative Example 1

[0056] Preparation of PV sol

[0057] In the preparation of PV sol, 8g of PMHS and 8.478g of VPOSS were first added to THF (38.45g) and stirred at room temperature for 30min. Then, Karstedt catalyst (0.058g) was added and stirring was continued for 10h to complete the preparation of PV sol (white).

[0058] Comparative Example 2

[0059] Preparation of PL sol

[0060] In the preparation of PL sol, 8g of PMHS and 25.754g of LA were first added sequentially to 78.76g of THF, and the mixture was stirred at room temperature for 30min. Then, 0.058g of Karstedt catalyst was added, and stirring was continued for 10h to complete the preparation of PL sol (transparent).

[0061] Comparative Example 3

[0062] Preparation of PE sol

[0063] In the preparation of PE sol, 8g of PMHS and 13.304g of EVCH were added to THF (49.71g) in sequence. After stirring at room temperature for 30min, Karstedt catalyst (0.058g) was added and stirring was continued for 10h to complete the preparation of PE sol (transparent).

[0064] Comparative Example 4

[0065] Preparation of PVLE sol

[0066] In the preparation of PVLE sol, 8g PMHS, 1.060g VPOSS, 3.219g LA and 9.978g EVCH were first added to THF (51.93g) and stirred at room temperature for 30min. Then, Karstedt catalyst (0.058g) was added and stirring was continued for 10h to complete the preparation of PVLE sol (transparent).

[0067] like Figure 3 As shown, all glass slides coated with different silicone coatings, except for the PV coating, exhibit high transparency and show no color change. Figure 3a) PV-coated glass slides exhibit opaque optical clarity due to the island-like structure formed on their surface.

[0068] From the visible light transmittance curve ( Figure 3 b) It can be seen that the transmittance of PL, PE, PVLE and PVLE-I-200 coatings all exceed that of the original glass, and they have stable transmittance in the wavelength range of 380 to 780 nm.

[0069] Visible light reflectance results ( Figure 3 c) shows that the visible light reflectance of the PL, PE, PVLE, and PVLE-I-200 coatings is lower than that of the original glass slide.

[0070] Statistical results of transmittance, reflectance, and absorptivity of different coatings are as follows: Figure 3 As shown in Figure d, the transmittance of PV, PL, PE, PVLE, and PVLE-I-200 coatings are 74.1%, 92.3%, 91.5%, 91.8%, and 91.6%, respectively, while the transmittance of glass is 90.2%. The reflectance of PV, PL, PE, PVLE, and PVLE-I-200 coatings are 19.2%, 6.3%, 6.4%, 7.3%, and 7.8%, respectively, while the reflectance of glass is 8.1%.

[0071] Therefore, the developed PL, PE, PVLE, and PVLE-I-200 coatings all exhibit antireflective properties on glass slides; the visible light absorption rates of the PV, PL, PE, PVLE, and PVLE-I-200 coatings are 6.7%, 1.3%, 2.1%, 0.9%, and 0.6%, respectively; the low visible light absorption of the PVLE and PVLE-I-200 coatings is due to the VPOSS nanocage structure being much smaller than one-quarter of the visible light wavelength; the PL and PE coatings without added VPOSS exhibit higher visible light absorption rates; the PV coating contains the highest proportion of VPOSS and exhibits the highest absorption rate, which is caused by light scattering from the rough surface of the PV coating.

[0072] like Figure 4 As shown, the PV coating exhibits the highest CA (WCA = 126.4°) for water and the highest CA (OCA = 73.4°) for diiodomethane, which is due to the "umbrella effect" caused by the rough surface of the PV coating; due to the low surface energy of the long carbon chain of the LA molecule, the PL coating exhibits hydrophobic and oleophilic surface properties, with WCA = 113.9° and OCA = 64.2°; the WCA and OCA of the PE, PVLE, and PVLE-I-200 coatings are relatively close.

[0073] The slightly higher WCA and OCA of the PVLE coating compared to the PE coating are attributed to the grafted carbon chains, while the slightly lower WCA and OCA of the PVLE-I-200 coating are due to the ring-opening reaction of the epoxy cyclohexyl group under the action of the initiator to generate hydroxyl groups. Nevertheless, the developed PE, PVLE, and PVLE-I-200 coating surfaces generally maintain hydrophobicity and slight oleophobicity.

[0074] like Figure 5 As shown, as a demonstration, ink from a Sharpie permanent marker was applied as a smudge simulation onto different coated glass slides. The ink exhibited good diffusion and spreadability on PV and PL coatings, but tended to shrink on PE, PVLE, and PVLE-I-200 coatings. On the PE coating, the ink formed large ink dots, while small black ink dots were observed on the PVLE and PVLE-I-200 coating surfaces. This is likely due to the presence of micron-sized protrusions on the PVLE and PVLE-I-200 coating surfaces.

[0075] After wiping ( Figure 5 (b) Ink residue on PE, PVLE, and PVLE-I-200 coatings was completely removed, demonstrating excellent stain resistance. The larger ink residue on the PV coating was due to the rough surface, while the ink residue on the PL coating was attributed to the surface's oleophilicity.

[0076] like Figure 6 As shown, a large proportion of the PV coating near the scratch was peeled off during the test. Figure 6 a) This may be due to the high VPOSS content, resulting in a three-dimensional cage-like structure in some areas, leading to weaker bonding with the substrate. The PL coating surface is relatively smooth, with only a small amount of coating peeling off, which is due to the flexibility of the grafted long carbon chains. Figure 6 b). The PE surface exhibits an adhesion morphology similar to that of the PL coating. Figure 6 c). The PVLE coating shows clear thin scratches with almost no peeling around the scratches, demonstrating excellent adhesion. Figure 6 d), while the PVLE-I-200 coating showed minor peeling around the scratches. Figure 6 e).

[0077] Adhesion rating and pencil hardness results ( Figure 6f) indicates that the adhesion grade of the PV coating is 3B, the adhesion grades of the PL, PE, and PVLE-I-200 coatings are 4B, and the adhesion grade of the PVLE coating is 5B. Pencil hardness results show that the PL coating has the lowest pencil hardness (5B), the PV and PVLE coatings have a pencil hardness of 2B, and the PE and PVLE-I-200 coatings have pencil hardnesses of H and 2H, respectively. Hardness may adversely affect coating adhesion, as rigid coating films are prone to peeling. The long carbon chains in LA contribute to the lower hardness of the PL coating. The VPOSS cage-like structure and epoxy cyclohexyl groups contribute to increased coating hardness. The higher epoxy cyclohexyl content in the PE coating is the main reason for its higher hardness, while the relatively lower epoxy cyclohexyl content results in a lower hardness and higher adhesion for the PVLE coating compared to the PE coating. For the PVLE-I-200 coating, the hardness significantly increases after the epoxy cyclohexyl groups undergo crosslinking under the action of the CTI-200 initiator; therefore, adhesion decreases with increasing coating hardness.

[0078] like Figure 7 As shown, the PVLE-I-200 coating showed no visible damage after 50 wear cycles. Therefore, it was subjected to 500 wear cycles. A few scratches appeared on the PVLE-I-200 coating after 100 and 200 wear cycles. After 500 wear cycles, although the number of scratches increased significantly, the coating remained relatively intact.

[0079] like Figure 8 As shown, fingerprints are clearly visible on bare glass, while they are almost invisible on PVLE-I-200 coated glass. When cleaned with WIPERS paper towels, fingerprints remaining on bare glass require more force to be completely removed than those remaining on PVLE-I-200 coated glass. This indicates that the PVLE-I-200 coating has excellent anti-fingerprint properties, which is attributed to the synergistic effect of Si-CH3 and long carbon chain low surface energy bonds, as well as the rigid 3D cage structure of VPOSS. The constructed functional 3D network structure makes it difficult for sweat and oil to accumulate into beads on the coating surface.

[0080] like Figure 9 As shown, when the slide is tilted at 14°, the graphite powder deposited on the PVLE-I-200 coated slide can be immediately carried away by water droplets, and no powder residue remains on the surface, indicating that the adhesion between the graphite powder and the PVLE-I-200 coating surface is low. Furthermore, due to its oleophobic properties, the PVLE-I-200 coated slide shows no oil residue when removed from the oil-red stained vegetable oil bath.

[0081] In summary, an environmentally friendly, transparent, hydrophobic, robust, UV-resistant, and anti-fouling silicone coating sol was obtained by rationally combining PMHS, VPOSS, LA, and EVCH via hydrosilylation reaction in the presence of a Karstedt catalyst. After introducing the CTI-200 initiator, a multifunctional coating was prepared using a dip-coating method. The prepared silicone coating exhibits excellent visible light transparency, with an average transmittance of approximately 92%. Due to the abundant Si-CH3 in PMHS and the long carbon chains in LA, as well as the multiple crosslinking points provided by the three-dimensional cage structure of VPOSS, the PVLE-I-200 coating achieves hydrophobicity, oleophobicity, excellent adhesion, abrasion resistance, and UV aging resistance. Furthermore, the PVLE-I-200 coating also possesses anti-fingerprint and anti-fouling properties, significantly improving the applicability of coated glass in practical applications.

[0082] This invention is not limited to the preferred embodiments described above. Anyone can derive other forms of products under the guidance of this invention. However, regardless of any changes made in their shape or structure, any technical solution that is the same as or similar to this application falls within the protection scope of this invention.

Claims

1. A method for producing a three-dimensionally crosslinked network silicone transparent coating material, characterized by, Includes the following steps: Preparation of S1 and PVLE organosilicon sol Polymethylhydrosiloxane, cage-type polysilsesquioxane, alkenyl long carbon chain compound and vinyl epoxy compound are mixed evenly in a solvent, and then Karstedt catalyst is added to react and obtain PVLE organosilicon sol. Cage-type polysilsesquioxanes include one or more combinations of octavinyl POSS, octa(3-butenyl) POSS and octa(4-pentenyl) POSS; Alkenyl long carbon chain compounds include dodecyl acrylate; long chain vinyl POSS, wherein ; long chain alkenyl silanes, wherein R is methoxy or ethoxy, ; long chain alkenyl silanes, wherein, , ; long chain alkenes, wherein ; one or several combinations thereof; Preparation of S2 and PVLE-I-200 organosilicon sol Blocked phosphate cationic initiator CTI-200 was added to the PVLE organosilicon sol prepared in S1, and the PVLE-I-200 organosilicon sol was obtained after the reaction. S3, PVLE-I-200 silicone coating application The PVLE-I-200 silicone sol obtained in S2 is coated on a substrate to obtain a substrate coated with a silicone coating. Curing of S4, PVLE-I-200 silicone coating The substrate coated with the silicone coating obtained in S3 is cured to obtain the silicone coating material.

2. The method for preparing a transparent organosilicon coating material with a three-dimensional cross-linked network according to claim 1, characterized in that: The long-chain alkenylsilanes include 1-decenyltrimethoxysilane; the long-chain vinyl polysiloxanes include vinyl-terminated polydimethylsiloxane; and the long-chain olefins include 1-decene.

3. The method of claim 1, wherein the method further comprises: In S1, the vinyl epoxy compound includes one or more combinations of vinyl cyclohexane oxide and vinyl silane oxide. ​ 4. The method of claim 3, wherein the method further comprises: The vinylcyclohexane oxide comprises one or more combinations of 1,2-epoxy-4-vinylcyclohexane and 1,2-epoxy-4-(5-vinylpentyl)cyclohexane. ​ 5. The method of claim 1, wherein the method further comprises: In S1, the solvent includes one or more of the following: tetrahydrofuran, toluene, xylene, ethylbenzene, dichloromethane, chloroform, ethyl acetate, butyl acetate, dimethyl sulfoxide, chlorobenzene, dichlorobenzene, and N-methylpyrrolidone. ​ 6. The method for preparing a transparent organosilicon coating material with a three-dimensional cross-linked network according to claim 1, characterized in that: In S3, the substrate includes one or more of the following: glass, polyvinyl alcohol, polymethyl methacrylate, polycarbonate, hydroxylated polyester film, silicone, and hydroxylated nanomaterial coating.

7. The method for preparing a transparent organosilicon coating material with a three-dimensional cross-linked network according to claim 1, characterized in that: In step S3, before coating, the substrate is ultrasonically cleaned and dried, and then the silicone coating is applied using an immersion coating method.

8. The method for preparing a transparent organosilicon coating material with a three-dimensional cross-linked network according to claim 1, characterized in that: In step S4, the substrate coated with an organosilicon coating is transferred to a vacuum oven and vacuum dried to remove volatile solvents.