Preparation method of high-strength glass product

Abstract

The invention relates to a preparation method of a high-strength glass product, and belongs to the technical field of glass products. Sequentially adding the pretreated material, sodium carbonate, boric acid, a clarifying agent and a lithium-selenium doped silane coupling agent into a mixing machine, and stirring to obtain a mixed material; sequentially carrying out melting clarification, compression molding, annealing treatment, toughening treatment and high-pressure cold air rapid cooling on the mixed material to obtain the high-strength glass product. The lithium selenium doped silane coupling agent is prepared from allyl glycidyl ether, trimethoxysilane, lithium methacrylate, diallyl diselenide, tetrahydrofuran and a chloroplatinic acid isopropanol solution; the glass product prepared by the invention is high in impact strength, and the crushing resistance is remarkably enhanced; the high-temperature-resistant temperature is high, deformation and cracking are not prone to occurring, and the service life of a product is prolonged.

Description

Technical Field

[0001] This invention relates to the field of glass product technology, and in particular to a method for preparing high-strength glass products. Background Technology

[0002] Glass products are widely used in construction, automobiles, electronic equipment, medical devices, and many other fields due to their transparency, aesthetics, and corrosion resistance. With the rapid development of various industries, the performance requirements for glass products are becoming increasingly stringent, especially in terms of mechanical strength, impact resistance, and high-temperature resistance. Traditional glass products are no longer sufficient to meet the demands of high-end applications.

[0003] Chinese Patent CN108698909B discloses embodiments of glass compositions, glass articles, and chemically strengthened glass articles. In one or more embodiments, the glass composition comprises: Li2O, more than about 0.9 mol% B2O3, more than or equal to 10 mol% Al2O3, and about 60-80 mol% SiO2.

[0004] Chinese Patent CN112079574A relates to the field of glass products, specifically disclosing a manufacturing process for wear-resistant and scratch-resistant glass products. The wear-resistant and scratch-resistant glass products include a glass substrate and a wear-resistant and scratch-resistant coating applied to the outer wall of the glass substrate. The manufacturing process includes preparing the glass substrate and a wear-resistant treatment, specifically comprising the following steps: adding the raw materials required for preparing the glass substrate to a reaction vessel, closing the reaction vessel, and thoroughly stirring and mixing the raw materials using a mixing mechanism inside the reaction vessel to obtain a mixed raw material; liquefying the mixed raw material in a furnace to obtain molten glass, clarifying it, and then subjecting it to venting and ultrasonic treatment; introducing the molten glass into a mold, cooling and shaping it to obtain a glass substrate; placing the glass substrate in an annealing furnace for annealing; and applying and curing a wear-resistant coating to the working surface of the glass substrate using a wear-resistant treatment module to obtain the finished glass product.

[0005] To improve glass strength, existing technologies typically employ methods such as adding a single reinforcing agent or tempering. However, the reinforcing effect of a single reinforcing agent is limited and can easily lead to increased difficulty in glass melting and deterioration in formability. While conventional tempering can improve the surface strength of glass, the uneven distribution of internal stress makes it prone to spontaneous breakage after long-term use, and the improvement in high-temperature resistance is not significant. Summary of the Invention

[0006] To address the above problems, this invention provides a method for preparing high-strength glass products, the operation steps of which are as follows, in parts by weight: S1: Crush 50-70 parts of quartz sand, 7-15 parts of feldspar, and 3-8 parts of limestone separately, place them in a drying oven, and dry them at 110-120℃ for 2-3 hours to remove moisture; calcine 1-5 parts of nano-alumina and 0.5-3 parts of zirconium oxide at 800-900℃ for 1-2 hours, and cool to room temperature; soak 0.5-2 parts of silicon carbide fiber in an ethanol solution of 20-40 parts of lithium selenide-doped silane coupling agent for 60-120 minutes, remove it, and dry it at 100-110℃ for 30-60 minutes to complete surface modification and obtain the pretreated material; S2: Add the pretreated material, 2-6 parts of soda ash, 0.5-2 parts of boric acid, 0.3-0.8 parts of clarifying agent, and 0.1-0.5 parts of lithium selenide doped silane coupling agent into the mixer in sequence. Stir at low speed for 15-20 minutes, then stir at high speed for 10-15 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500-600℃ and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0007] In a specific embodiment, the mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent in S1 is 5-10%.

[0008] In a specific embodiment, the S2 clarifying agent is a compound of sodium nitrate and sodium sulfate, with a mass ratio of 1:1-2.

[0009] In a specific implementation, the low-speed stirring rate of S2 is 200-300 r / min, and the high-speed stirring rate is 500-600 r / min.

[0010] In a specific implementation, the S3 melting and clarification step is as follows: first, heat to 1450-1500℃ and keep at that temperature for melting for 2-3 hours, stirring once every 30 minutes for 5-10 minutes each time; then heat to 1550-1600℃ and keep at that temperature for clarification for 60-90 minutes.

[0011] In a specific implementation, the pressure of the S4 pressing molding is 10-15 MPa, and the temperature is 1200-1300℃.

[0012] In a specific implementation, the S5 annealing process is as follows: first, the temperature is lowered to 800-850℃ at a rate of 5-8℃ / min and held for 2-3 hours; then, the temperature is lowered to 400-450℃ at a rate of 2-3℃ / min and held for 1-2 hours; finally, the temperature is allowed to cool naturally to room temperature.

[0013] In a specific implementation, the S6 tempering treatment is carried out at a temperature of 650-700℃ for 20-40 minutes.

[0014] In a specific implementation, the pressure of the S6 high-pressure cooling air is 0.6-0.8 MPa, and the cooling rate is 20-30℃ / s.

[0015] In a specific embodiment, the preparation method of the lithium selenide-doped silane coupling agent is as follows: By weight, 11-22 parts of allyl glycidyl ether, 16-32 parts of trimethoxysilane, 0.9-2.8 parts of lithium methacrylate, 0.11-0.42 parts of diallyl diselenide, and 150-250 parts of tetrahydrofuran are mixed. Then, 0.2-0.5 parts of 0.5-2 wt% isopropanol chloroplatinate solution are added. Nitrogen gas is introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature is controlled at 40-50℃, the stirring rate at 300-400 r / min, and the reaction time at 2-4 h. After the reaction is completed, the temperature is raised to 120-130℃ and the vacuum degree is -0.095 MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5-10 parts of anhydrous magnesium sulfate are added and dried for 1-3 h. After filtration, lithium selenide-doped silane coupling agent is obtained.

[0016] Reaction mechanism A three-dimensional composite reinforcement network is constructed from nano-alumina, zirconium oxide, and silicon carbide fibers. Trimethoxysilane, lithium methacrylate, and diallyl diselenyl ether undergo hydrosilylation reactions with allyl glycidyl ether. Lithium ions, with their small ionic radius, form stable ionic bonds, participating in interfacial bonding and refining the glass microstructure. Selenium elements construct a stable cross-linked structure, strengthening the chemical bond strength. Silane coupling agents further optimize the interfacial bonding between the inorganic reinforcement phase and the glass matrix, reducing stress concentration. The synergistic and complementary effects of these components reduce the difficulty of glass melting while improving the density and overall stability of the matrix structure.

[0017] Technical effect The present invention provides a method for preparing high-strength glass products. Compared with the prior art, the present invention has the following significant advantages: 1. The composite reinforcement system and hydrosilylation reaction (including lithium and selenium) work synergistically to refine the structure of lithium and inhibit crack initiation and propagation, while selenium strengthens the bonding of components, significantly improving the impact resistance and shatter resistance of glass products, making them suitable for high-stress applications in high-end scenarios such as building curtain walls and automotive windshields.

[0018] 2. The thermal stability of zirconium oxide, combined with the chemical stability of selenium and the stable structure formed by lithium, significantly optimizes the thermal stability of glass, improves its high-temperature resistance, effectively avoids deformation and cracking during use, and extends the service life of products.

[0019] 3. By innovatively introducing lithium methacrylate and diallyl diselenide to participate in the hydrosilylation reaction, combined with the composite reinforcement system and optimized process, we can not only strengthen the interfacial bonding force and improve the internal stress distribution, but also solve the pain points of poor molding performance and easy self-explosion of traditional reinforcement methods, thus achieving a simultaneous leap in mechanical strength and high temperature resistance. Detailed Implementation

[0020] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features and effects of the present invention, in conjunction with embodiments, is provided below.

[0021] 1. Impact resistance: Tested according to GB / T6552-2015, using a falling ball impact test with a steel ball mass of 500g.

[0022] 2. High temperature resistance test: Place the sample in a muffle furnace and heat it at a rate of 10℃ / min. Observe whether the sample shows defects such as cracks or deformation. The highest temperature at which the sample can remain intact without defects is the high temperature resistance temperature.

[0023] Example 1

[0024] A method for preparing a high-strength glass product, comprising the following steps: S1: Crush 50g of quartz sand, 7g of feldspar, and 3g of limestone separately, place them in a drying oven, and dry them at 110℃ for 2 hours to remove moisture; calcine 1g of nano-alumina and 0.5g of zirconium oxide at 800℃ for 1 hour, and cool to room temperature; soak 0.5g of silicon carbide fiber in an ethanol solution of 20g of lithium selenide-doped silane coupling agent for 60 minutes, take it out, and dry it at 100℃ for 30 minutes to complete surface modification and obtain the pretreated material; S2: Add the pretreated material, 2g soda ash, 0.5g boric acid, 0.3g clarifying agent, and 0.1g lithium selenide doped silane coupling agent into the mixer in sequence, stir at low speed for 15 minutes, and then stir at high speed for 10 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0025] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 5%.

[0026] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate in a mass ratio of 1:1.

[0027] The low-speed stirring rate of S2 is 200 r / min, and the high-speed stirring rate is 500 r / min.

[0028] The steps for S3 melting and clarifying are as follows: first, heat to 1450℃ and keep at that temperature for 2 hours, stirring once every 30 minutes for 5 minutes each time; then heat to 1550℃ and keep at that temperature for 60 minutes to clarify.

[0029] The pressure for S4 pressing is 10 MPa and the temperature is 1200℃.

[0030] The S5 annealing process is as follows: first, the temperature is lowered to 800℃ at a rate of 5℃ / min and held for 2 hours; then, the temperature is lowered to 400℃ at a rate of 2℃ / min and held for 1 hour; finally, the temperature is allowed to cool naturally to room temperature.

[0031] The S6 tempering process is carried out at a temperature of 650°C for 20 minutes.

[0032] The pressure of the S6 high-pressure cold air is 0.6 MPa, and the cooling rate is 20℃ / s.

[0033] The preparation method of the lithium selenide-doped silane coupling agent is as follows: 11g allyl glycidyl ether, 16g trimethoxysilane, 0.9g lithium methacrylate, 0.11g diallyl diselenide, and 150g tetrahydrofuran were mixed and then 0.2g of 0.5wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 40℃, the stirring rate at 300r / min, and the reaction time at 2h. After the reaction was completed, the temperature was raised to 120℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5g of anhydrous magnesium sulfate was added and dried for 1h. After filtration, lithium selenide-doped silane coupling agent was obtained.

[0034] Example 2

[0035] A method for preparing a high-strength glass product, comprising the following steps: S1: 55g of quartz sand, 9g of feldspar, and 4g of limestone were crushed separately and placed in a drying oven and dried at 115℃ for 2.5h to remove moisture; 2g of nano-alumina and 1g of zirconium oxide were calcined at 840℃ for 1.5h and cooled to room temperature; 1g of silicon carbide fiber was soaked in an ethanol solution of 25g of lithium selenide-doped silane coupling agent for 80min, and then dried at 105℃ for 40min to complete surface modification and obtain the pretreated material. S2: Add the pretreated material, 3g soda ash, 1g boric acid, 0.4g clarifying agent, and 0.2g lithium selenide doped silane coupling agent into the mixer in sequence, stir at low speed for 15 minutes, and then stir at high speed for 10 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 540°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0036] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 6%.

[0037] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate, with a mass ratio of 1:1.5.

[0038] The low-speed stirring rate of S2 is 250 r / min, and the high-speed stirring rate is 550 r / min.

[0039] The steps for S3 melting and clarifying are as follows: first, heat to 1460℃ and keep at that temperature for 2.5 hours, stirring once every 30 minutes for 5 minutes each time; then heat to 1560℃ and keep at that temperature for 70 minutes.

[0040] The pressure for S4 pressing is 12 MPa and the temperature is 1240℃.

[0041] The S5 annealing process is as follows: first, the temperature is lowered to 810℃ at a rate of 6℃ / min and held for 2.5h; then, the temperature is lowered to 410℃ at a rate of 2℃ / min and held for 1.5h; finally, the temperature is allowed to cool naturally to room temperature.

[0042] The S6 tempering process is carried out at a temperature of 660°C for 25 minutes.

[0043] The pressure of the S6 high-pressure cold air is 0.7 MPa, and the cooling rate is 25℃ / s.

[0044] The preparation method of the lithium selenide-doped silane coupling agent is as follows: 15g allyl glycidyl ether, 20g trimethoxysilane, 1.5g lithium methacrylate, 0.2g diallyl diselenide, and 180g tetrahydrofuran were mixed and then 0.3g of 1wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 45℃, the stirring rate at 350r / min, and the reaction time at 3h. After the reaction was completed, the temperature was raised to 125℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 6g of anhydrous magnesium sulfate was added and dried for 2h. After filtration, lithium selenide-doped silane coupling agent was obtained.

[0045] Example 3

[0046] A method for preparing a high-strength glass product, comprising the following steps: S1: 65g of quartz sand, 13g of feldspar, and 7g of limestone were crushed separately and placed in a drying oven at 115℃ for 2.5h to remove moisture; 4g of nano-alumina and 2g of zirconium oxide were calcined at 880℃ for 1.5h and cooled to room temperature; 1.5g of silicon carbide fiber was soaked in an ethanol solution of 35g of lithium selenide-doped silane coupling agent for 100min, and then dried at 105℃ for 50min to complete surface modification and obtain the pretreated material. S2: Add the pretreated material, 5g soda ash, 1.5g boric acid, 0.7g clarifying agent, and 0.4g lithium selenide doped silane coupling agent into the mixer in sequence, stir at low speed for 20 minutes, and then stir at high speed for 15 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 580°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0047] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 8%.

[0048] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate, with a mass ratio of 1:1.5.

[0049] The low-speed stirring rate of S2 is 250 r / min, and the high-speed stirring rate is 550 r / min.

[0050] The steps for S3 melting and clarifying are as follows: first, heat to 1480℃ and keep at that temperature for 2.5 hours, stirring once every 30 minutes for 10 minutes each time; then heat to 1580℃ and keep at that temperature for 80 minutes to clarify.

[0051] The pressure for S4 pressing is 14 MPa and the temperature is 1280℃.

[0052] The S5 annealing process is as follows: first, the temperature is lowered to 840℃ at a rate of 7℃ / min and held for 2.5h; then, the temperature is lowered to 440℃ at a rate of 3℃ / min and held for 1.5h; finally, the temperature is allowed to cool naturally to room temperature.

[0053] The S6 tempering process is carried out at a temperature of 680°C for 35 minutes.

[0054] The pressure of the S6 high-pressure cold air is 0.7 MPa, and the cooling rate is 25℃ / s.

[0055] The preparation method of the lithium selenide-doped silane coupling agent is as follows: 20g allyl glycidyl ether, 30g trimethoxysilane, 2.5g lithium methacrylate, 0.4g diallyl diselenide, and 230g tetrahydrofuran were mixed and then 0.4g of 1.5wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 45℃, the stirring rate at 350r / min, and the reaction time at 3h. After the reaction was completed, the temperature was raised to 125℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 8g of anhydrous magnesium sulfate was added and dried for 2h. After filtration, lithium selenide-doped silane coupling agent was obtained.

[0056] Example 4

[0057] A method for preparing a high-strength glass product, comprising the following steps: S1: Crush 70g of quartz sand, 15g of feldspar, and 8g of limestone separately, place them in a drying oven, and dry them at 120℃ for 3 hours to remove moisture; calcine 5g of nano-alumina and 3g of zirconium oxide at 900℃ for 2 hours and cool to room temperature; soak 2g of silicon carbide fiber in an ethanol solution of 40g of lithium selenide-doped silane coupling agent for 120 minutes, take it out, and dry it at 110℃ for 60 minutes to complete the surface modification and obtain the pretreated material; S2: Add the pretreated material, 6g soda ash, 2g boric acid, 0.8g clarifying agent, and 0.5g lithium selenide doped silane coupling agent into the mixer in sequence, stir at low speed for 20 minutes, and then stir at high speed for 15 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 600°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0058] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 10%.

[0059] The S2 clarifying agent is a compound of sodium nitrate and sodium sulfate, with a mass ratio of 1:2.

[0060] The low-speed stirring rate of S2 is 300 r / min, and the high-speed stirring rate is 600 r / min.

[0061] The steps for S3 melting and clarifying are as follows: first, heat to 1500℃ and keep at that temperature for 3 hours, stirring once every 30 minutes for 10 minutes each time; then heat to 1600℃ and keep at that temperature for 90 minutes to clarify.

[0062] The pressure for S4 pressing is 15 MPa, and the temperature is 1300℃.

[0063] The S5 annealing process is as follows: first, the temperature is lowered to 850℃ at a rate of 8℃ / min and held for 3 hours; then, the temperature is lowered to 450℃ at a rate of 3℃ / min and held for 2 hours; finally, the temperature is allowed to cool naturally to room temperature.

[0064] The S6 tempering process is carried out at a temperature of 700°C for 40 minutes.

[0065] The pressure of the S6 high-pressure cold air is 0.8 MPa, and the cooling rate is 30℃ / s.

[0066] The preparation method of the lithium selenide-doped silane coupling agent is as follows: 22g allyl glycidyl ether, 32g trimethoxysilane, 2.8g lithium methacrylate, 0.42g diallyl diselenide, and 250g tetrahydrofuran were mixed and then 0.5g of 2wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 50℃, the stirring rate at 400r / min, and the reaction time at 4h. After the reaction was completed, the temperature was raised to 130℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. After adding 10g of anhydrous magnesium sulfate and drying for 3h, the mixture was filtered to obtain lithium selenide-doped silane coupling agent.

[0067] Comparative Example 1 A method for preparing a high-strength glass product, comprising the following steps: S1: Crush 50g of quartz sand, 7g of feldspar, and 3g of limestone separately, place them in a drying oven, and dry them at 110℃ for 2 hours to remove moisture; calcine 1g of nano-alumina and 0.5g of zirconium oxide at 800℃ for 1 hour, and cool to room temperature; soak 0.5g of silicon carbide fiber in an ethanol solution of 20g of silane coupling agent for 60 minutes, take it out, and dry it at 100℃ for 30 minutes to complete the surface modification and obtain the pretreated material; S2: Add the pretreated material, 2g soda ash, 0.5g boric acid, 0.3g clarifying agent, and 0.1g silane coupling agent into the mixer in sequence, stir at low speed for 15 minutes, and then stir at high speed for 10 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0068] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 5%.

[0069] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate in a mass ratio of 1:1.

[0070] The low-speed stirring rate of S2 is 200 r / min, and the high-speed stirring rate is 500 r / min.

[0071] The steps for S3 melting and clarifying are as follows: first, heat to 1450℃ and keep at that temperature for 2 hours, stirring once every 30 minutes for 5 minutes each time; then heat to 1550℃ and keep at that temperature for 60 minutes to clarify.

[0072] The pressure for S4 pressing is 10 MPa and the temperature is 1200℃.

[0073] The S5 annealing process is as follows: first, the temperature is lowered to 800℃ at a rate of 5℃ / min and held for 2 hours; then, the temperature is lowered to 400℃ at a rate of 2℃ / min and held for 1 hour; finally, the temperature is allowed to cool naturally to room temperature.

[0074] The S6 tempering process is carried out at a temperature of 650°C for 20 minutes.

[0075] The pressure of the S6 high-pressure cold air is 0.6 MPa, and the cooling rate is 20℃ / s.

[0076] The preparation method of the silane coupling agent is as follows: 11g of allyl glycidyl ether, 16g of trimethoxysilane, and 150g of tetrahydrofuran were mixed and then 0.2g of 0.5wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 40℃, the stirring rate at 300r / min, and the reaction time at 2h. After the reaction was completed, the temperature was raised to 120℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5g of anhydrous magnesium sulfate was added and dried for 1h. After filtration, the silane coupling agent was obtained.

[0077] Comparative Example 2 A method for preparing a high-strength glass product, comprising the following steps: S1: Crush 50g of quartz sand, 7g of feldspar, and 3g of limestone separately, place them in a drying oven, and dry them at 110℃ for 2 hours to remove moisture; calcine 1g of nano-alumina and 0.5g of zirconium oxide at 800℃ for 1 hour, and cool to room temperature; soak 0.5g of silicon carbide fiber in an ethanol solution of 20g of lithium-doped silane coupling agent for 60 minutes, take it out, and dry it at 100℃ for 30 minutes to complete the surface modification and obtain the pretreated material; S2: Add the pretreated material, 2g soda ash, 0.5g boric acid, 0.3g clarifying agent, and 0.1g lithium-doped silane coupling agent into the mixer in sequence, stir at low speed for 15 minutes, and then stir at high speed for 10 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0078] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 5%.

[0079] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate in a mass ratio of 1:1.

[0080] The low-speed stirring rate of S2 is 200 r / min, and the high-speed stirring rate is 500 r / min.

[0081] The steps for S3 melting and clarifying are as follows: first, heat to 1450℃ and keep at that temperature for 2 hours, stirring once every 30 minutes for 5 minutes each time; then heat to 1550℃ and keep at that temperature for 60 minutes to clarify.

[0082] The pressure for S4 pressing is 10 MPa and the temperature is 1200℃.

[0083] The S5 annealing process is as follows: first, the temperature is lowered to 800℃ at a rate of 5℃ / min and held for 2 hours; then, the temperature is lowered to 400℃ at a rate of 2℃ / min and held for 1 hour; finally, the temperature is allowed to cool naturally to room temperature.

[0084] The S6 tempering process is carried out at a temperature of 650°C for 20 minutes.

[0085] The pressure of the S6 high-pressure cold air is 0.6 MPa, and the cooling rate is 20℃ / s.

[0086] The preparation method of the lithium-doped silane coupling agent is as follows: 11g allyl glycidyl ether, 16g trimethoxysilane, 0.9g lithium methacrylate, and 150g tetrahydrofuran were mixed and then 0.2g of 0.5wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 40℃, the stirring rate at 300r / min, and the reaction time at 2h. After the reaction was completed, the temperature was raised to 120℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5g of anhydrous magnesium sulfate was added and dried for 1h. After filtration, lithium-doped silane coupling agent was obtained.

[0087] Comparative Example 3 A method for preparing a high-strength glass product, comprising the following steps: S1: Crush 50g of quartz sand, 7g of feldspar, and 3g of limestone separately, place them in a drying oven, and dry them at 110℃ for 2 hours to remove moisture; calcine 1g of nano-alumina and 0.5g of zirconium oxide at 800℃ for 1 hour, and cool to room temperature; soak 0.5g of silicon carbide fiber in an ethanol solution of 20g of selenium-doped silane coupling agent for 60 minutes, take it out, and dry it at 100℃ for 30 minutes to complete the surface modification and obtain the pretreated material; S2: Add the pretreated material, 2g soda ash, 0.5g boric acid, 0.3g clarifying agent, and 0.1g selenium-doped silane coupling agent to the mixer in sequence, stir at low speed for 15 minutes, and then stir at high speed for 10 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500°C and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products.

[0088] The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 5%.

[0089] The S2 clarifying agent is a mixture of sodium nitrate and sodium sulfate in a mass ratio of 1:1.

[0090] The low-speed stirring rate of S2 is 200 r / min, and the high-speed stirring rate is 500 r / min.

[0091] The steps for S3 melting and clarifying are as follows: first, heat to 1450℃ and keep at that temperature for 2 hours, stirring once every 30 minutes for 5 minutes each time; then heat to 1550℃ and keep at that temperature for 60 minutes to clarify.

[0092] The pressure for S4 pressing is 10 MPa and the temperature is 1200℃.

[0093] The S5 annealing process is as follows: first, the temperature is lowered to 800℃ at a rate of 5℃ / min and held for 2 hours; then, the temperature is lowered to 400℃ at a rate of 2℃ / min and held for 1 hour; finally, the temperature is allowed to cool naturally to room temperature.

[0094] The S6 tempering process is carried out at a temperature of 650°C for 20 minutes.

[0095] The pressure of the S6 high-pressure cold air is 0.6 MPa, and the cooling rate is 20℃ / s.

[0096] The preparation method of the selenium-doped silane coupling agent is as follows: 11g allyl glycidyl ether, 16g trimethoxysilane, 0.11g diallyl diselenyl ether, and 150g tetrahydrofuran were mixed and then 0.2g of 0.5wt% isopropanol chloroplatinate solution was added. Nitrogen gas was introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature was initially controlled at 40℃, the stirring rate at 300r / min, and the reaction time at 2h. After the reaction was completed, the temperature was raised to 120℃ and the vacuum degree was -0.095MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5g of anhydrous magnesium sulfate was added and dried for 1h. After filtration, selenium-doped silane coupling agent was obtained.

[0097] Table 1 shows the test results of impact strength and high temperature resistance of the glass products in the examples and comparative examples. Impact resistance (kJ / m²) High temperature resistance (°C) Example 1 21.3 600 Example 2 21.5 610 Example 3 21.9 640 Example 4 22.1 660 Comparative Example 1 9.6 450 Comparative Example 2 15.7 540 Comparative Example 3 16.2 560 The data shows that the glass products of this invention are significantly superior to the comparative examples in terms of impact resistance and high-temperature resistance. The core innovation lies in introducing lithium and selenium-related components into the hydrosilylation reaction, combined with a composite reinforcement system of nano-alumina, zirconium oxide, and silicon carbide fibers, constructing a triple strengthening mechanism of "composite reinforcement + chemical bonding + ion optimization," which significantly improves the compatibility and interfacial bonding stability of each component. Simultaneously, with precise melting and clarifying processes and gradient annealing, the core performance of the products achieves a breakthrough improvement, better meeting the stringent requirements of high-end applications.

[0098] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a high-strength glass product, comprising the following steps, in parts by weight: S1: Crush 50-70 parts of quartz sand, 7-15 parts of feldspar, and 3-8 parts of limestone separately, place them in a drying oven, and dry them at 110-120℃ for 2-3 hours to remove moisture; calcine 1-5 parts of nano-alumina and 0.5-3 parts of zirconium oxide at 800-900℃ for 1-2 hours, and cool to room temperature; soak 0.5-2 parts of silicon carbide fiber in an ethanol solution of 20-40 parts of lithium selenide-doped silane coupling agent for 60-120 minutes, remove it, and dry it at 100-110℃ for 30-60 minutes to complete surface modification and obtain the pretreated material; S2: Add the pretreated material, 2-6 parts of soda ash, 0.5-2 parts of boric acid, 0.3-0.8 parts of clarifying agent, and 0.1-0.5 parts of lithium selenide doped silane coupling agent into the mixer in sequence. Stir at low speed for 15-20 minutes, then stir at high speed for 10-15 minutes to obtain a uniform mixture. S3: The mixture is fed into a glass furnace for melting and clarification to remove air bubbles and impurities; S4: Pour the clarified molten glass into a mold preheated to 500-600℃ and press it into shape; S5: The formed glass product is sent into an annealing furnace for annealing treatment to obtain the glass product; S6: After annealing, the glass products are placed in a tempering furnace for tempering treatment. Then, they are rapidly cooled to room temperature using high-pressure cold air to obtain high-strength glass products. The lithium selenide-doped silane coupling agent is prepared by reacting allyl glycidyl ether, trimethoxysilane, lithium methacrylate, diallyl diselenyl ether, and isopropanol chloroplatinate solution.

2. The method for preparing a high-strength glass product according to claim 1, characterized in that: The mass percentage of the ethanol solution of the lithium selenide-doped silane coupling agent S1 is 5-10%.

3. The method for preparing a high-strength glass product according to claim 1, characterized in that: The S2 clarifying agent is a compound of sodium nitrate and sodium sulfate, with a mass ratio of 1:1-2.

4. The method for preparing a high-strength glass product according to claim 1, characterized in that: The low-speed stirring rate of S2 is 200-300 r / min, and the high-speed stirring rate is 500-600 r / min.

5. The method for preparing a high-strength glass product according to claim 1, characterized in that: The steps for S3 melting and clarifying are as follows: first, heat to 1450-1500℃ and keep at that temperature for melting for 2-3 hours, stirring once every 30 minutes for 5-10 minutes each time; then heat to 1550-1600℃ and keep at that temperature for clarification for 60-90 minutes.

6. The method for preparing a high-strength glass product according to claim 1, characterized in that: The pressure for S4 pressing is 10-15 MPa, and the temperature is 1200-1300℃.

7. The method for preparing a high-strength glass product according to claim 1, characterized in that: The S5 annealing process is as follows: first, the temperature is lowered to 800-850℃ at a rate of 5-8℃ / min and held for 2-3 hours; then, the temperature is lowered to 400-450℃ at a rate of 2-3℃ / min and held for 1-2 hours; finally, the temperature is allowed to cool naturally to room temperature.

8. The method for preparing a high-strength glass product according to claim 1, characterized in that: The S6 tempering process is carried out at a temperature of 650-700℃ for 20-40 minutes.

9. The method for preparing a high-strength glass product according to claim 1, characterized in that: The pressure of the S6 high-pressure cooling air is 0.6-0.8MPa, and the cooling rate is 20-30℃ / s.

10. The method for preparing a high-strength glass article according to claim 1, characterized in that: The preparation method of the lithium selenide-doped silane coupling agent is as follows: By weight, 11-22 parts of allyl glycidyl ether, 16-32 parts of trimethoxysilane, 0.9-2.8 parts of lithium methacrylate, 0.11-0.42 parts of diallyl diselenide, and 150-250 parts of tetrahydrofuran are mixed. Then, 0.2-0.5 parts of 0.5-2 wt% isopropanol chloroplatinate solution are added. Nitrogen gas is introduced to replace the air in the reaction system to maintain an anhydrous and oxygen-free environment. The reaction temperature is controlled at 40-50℃, the stirring rate at 300-400 r / min, and the reaction time at 2-4 h. After the reaction is completed, the temperature is raised to 120-130℃ and the vacuum degree is -0.095 MPa to remove unreacted trimethoxysilane and tetrahydrofuran. 5-10 parts of anhydrous magnesium sulfate are added and dried for 1-3 h. After filtration, lithium selenide-doped silane coupling agent is obtained.