Explosion-proof high-temperature-resistant tempered glass and preparation method thereof

CN120398434BActive Publication Date: 2026-08-21济南嘉益建材有限公司
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Patent Information

Application Number
CN202510532203.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-25
Publication Date
2026-08-21
Estimated Expiration
2045-04-25

AI Technical Summary

Technical Problem

[0003]但是,钢化玻璃内部应力分布不均,长期使用后应力释放导致破裂,在无直接外力作用下可能发生自爆;而且钢化玻璃也会因热应力过大而破裂

Benefits of technology

[0019]本发明在制备防爆耐高温钢化玻璃时,先将葡萄糖酸钙和正硅酸乙酯组成的混合液涂覆在玻璃基体表面,然后通过逐渐升温进行钢化处理,得到含有多孔夹层的钢化玻璃;再将含有有机阳离子的改性蛭石和六氟合硅酸盐按照一定比例混合涂覆于钢化玻璃表面,以实现耐高温防爆的效果。

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses an explosion-proof high-temperature-resistant tempered glass and a preparation method thereof, and relates to the field of glass manufacturing. The explosion-proof high-temperature-resistant tempered glass comprises tempered glass, a porous interlayer and a coating. The porous interlayer is obtained by gradually increasing the temperature from room temperature to high temperature and solidifying a mixed solution obtained by mixing a calcium gluconate solution and tetraethyl orthosilicate at a mass ratio of 1:3-5; and the coating is obtained by solidifying a slurry obtained by mixing modified vermiculite containing organic cations and hexafluorosilicate at a mass ratio of 1:1-3 at 150-200 DEG C. The mixed solution composed of calcium gluconate and tetraethyl orthosilicate is gradually heated for tempering treatment to form a more compact silicon dioxide network structure, thereby improving the bonding force of the porous interlayer with ordinary glass and the high-temperature resistance; the hexafluorosilicate can form a compact protective film, delay the heat transfer to the tempered glass, effectively prevent the tempered glass from being overheated and broken, and significantly improve the explosion-proof performance.
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Description

Technical Field

[0001] This invention relates to the field of glass manufacturing technology, specifically to an explosion-proof, high-temperature resistant tempered glass and its preparation method. Background Technology

[0002] With technological advancements, tempered glass has expanded from its early application in construction to high-end scenarios such as electronic products (e.g., mobile phone screens) and aerospace (aircraft cabin glass), becoming an indispensable material in modern society. Through nanotechnology and coating processes, tempered glass is evolving towards multi-functional properties such as self-cleaning, heat insulation, and UV protection, meeting the personalized needs of smart homes and green buildings. New products such as smart dimming glass and optoelectronic glass are also under development, leading the industry towards intelligent and integrated development.

[0003] However, tempered glass has uneven internal stress distribution, which can lead to breakage after prolonged use due to stress release, and it may spontaneously shatter even without direct external force. Furthermore, tempered glass can also crack due to excessive thermal stress. For example, sudden localized cooling or heating can cause stress concentration, reducing its lifespan. Therefore, there is an urgent need to develop explosion-proof and high-temperature-resistant tempered glass. Summary of the Invention

[0004] The purpose of this invention is to provide an explosion-proof, high-temperature resistant tempered glass and its preparation method, so as to solve the problems existing in the prior art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: an explosion-proof and high-temperature resistant tempered glass, the explosion-proof and high-temperature resistant tempered glass comprising a porous interlayer and a coating, wherein the porous interlayer is obtained by gradually heating a mixture of calcium gluconate solution and tetraethyl orthosilicate at a mass ratio of 1:3 to 5 and curing it from room temperature to a high temperature; the coating is obtained by curing a slurry of modified vermiculite containing organic cations and hexafluorosilicate at a mass ratio of 1:1 to 3 at 150 to 200°C.

[0006] Furthermore, the calcium gluconate solution is obtained by mixing calcium gluconate and a solvent in a mass ratio of 1:5 to 10.

[0007] Furthermore, the solvent is deionized water.

[0008] Furthermore, the modified vermiculite is obtained by mixing porous vermiculite particles with an organic cation solution at a solid-liquid ratio of 1:10 to 20.

[0009] Furthermore, the organic cationic reagent is 1-butyl-3-methylimidazolium hexafluorophosphate.

[0010] Furthermore, a method for preparing explosion-proof and high-temperature resistant tempered glass includes the following preparation steps:

[0011] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5-10:1. Stir to dissolve, keep warm at 60°C, add tetraethyl orthosilicate, and stir at 500-800 rpm for 20-30 minutes at 25-35°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3-5.

[0012] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface. The coating thickness is controlled at 5-20 μm. The temperature is increased from room temperature to 180-220°C at a rate of 2-5°C / min and held for 30-60 minutes. The temperature is then increased to 220-600°C at a rate of 5-10°C / min and held for 1-2 hours. The ordinary glass is placed in a tempering furnace and held at 720-740°C for 10-20 minutes. Then it is rapidly cooled to room temperature to obtain tempered glass with a porous interlayer.

[0013] (3) Mix hexafluorosilicate and modified vermiculite containing cations at a mass ratio of 1:1 to 3 and stir at 500 to 800 rpm for 10 to 20 minutes. Then add organic solvent at a mass ratio of 1 to 3 times that of the total mass of modified vermiculite and hexafluorosilicate, and increase the stirring speed to 3000 to 5000 rpm. Continue stirring for 20 to 30 minutes to form a uniform slurry. Then use ultrasonic dispersion at 40 to 60 kHz and 200 to 400 W for 20 to 40 minutes to obtain a paste-like slurry. Coat the slurry onto the tempered glass surface obtained in step (2) with a coating thickness controlled at 50 to 150 μm. Cure at 150 to 200 °C for 1 to 2 hours to obtain a coating.

[0014] Furthermore, the preparation method of modified vermiculite in step (3) includes: pulverizing vermiculite to a particle size of 50-100 mesh, dissolving it in water at 5-10 times the mass of vermiculite, ultrasonically crushing it at 60-100 kHz for 30-40 minutes, then filtering, washing with deionized water, and drying at 60-80℃ to obtain porous vermiculite particles with a pore size of 5nm-80nm; preparing an organic cation reagent into a 0.1-0.5M aqueous solution, mixing the porous vermiculite particles and the aqueous solution at a solid-liquid ratio of 1:10-20, stirring at 60-80℃ for 4-8 hours to allow the organic cations to insert into the interlayer of the porous vermiculite particles through ion exchange, then filtering, washing until neutral, and vacuum drying at 60℃ for 24 hours.

[0015] Furthermore, in step (1), the mass ratio of calcium gluconate to tetraethyl orthosilicate is preferably 1:4.

[0016] Furthermore, in step (3), the preferred mass ratio of hexafluorosilicate to modified vermiculite is 1:2.

[0017] Furthermore, in step (3), the hexafluorosilicate is potassium hexafluorosilicate or sodium hexafluorosilicate; the particle size of the hexafluorosilicate is ≤5μm.

[0018] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0019] In preparing explosion-proof and high-temperature resistant tempered glass, the present invention first coats a mixture of calcium gluconate and tetraethyl orthosilicate onto the surface of a glass substrate, and then tempers it by gradually increasing the temperature to obtain tempered glass with a porous interlayer; then, a mixture of modified vermiculite containing organic cations and hexafluorosilicate is coated onto the surface of the tempered glass in a certain proportion to achieve the effect of high-temperature resistance and explosion protection.

[0020] First, a mixture of calcium gluconate and tetraethyl orthosilicate is coated onto ordinary glass. As the temperature rises from room temperature to 180-220°C, tetraethyl orthosilicate begins to hydrolyze, producing ethanol and silica. After the ethanol evaporates, a porous silica network structure is formed. Simultaneously, calcium gluconate decomposes into calcium carbonate and carbon dioxide gas. After the carbon dioxide gas and water vapor evaporate, calcium carbonate is uniformly distributed within the silica network structure. Subsequently, when the temperature is raised to 220-600°C, tetraethyl orthosilicate further decomposes, the organic components in the porous interlayer gradually evaporate, and the silica framework solidifies, forming a denser silica network structure. Then, a physical tempering treatment is performed at 720-740°C. Calcium carbonate continues to decompose, producing carbon dioxide gas and calcium oxide. The escape of carbon dioxide gas increases the porosity of the porous interlayer, while calcium oxide reacts with silica to form calcium silicate. Calcium silicate can form chemical bonds with the silicon-oxygen bonds on the surface of ordinary glass, improving the bonding strength between the porous interlayer and the ordinary glass, as well as its high-temperature resistance.

[0021] Secondly, a slurry is prepared by mixing modified vermiculite containing organic cations and hexafluorosilicate in a certain proportion, which is then coated onto the surface of tempered glass and cured at high temperature. During this process, the modified vermiculite rapidly expands at high temperature, forming a porous structure that can block the diffusion of oxygen and heat, inhibiting the spread of flames. At the same time, hexafluorosilicate forms a dense protective film, delaying the transfer of heat to the tempered glass and effectively preventing the tempered glass from overheating and cracking, significantly improving its explosion-proof performance. In addition, hexafluorosilicate has high hardness and wear resistance, while the layered structure of modified vermiculite has a certain degree of flexibility. The combined effect of these two factors can prevent cracking caused by thermal expansion and contraction, improving the stability of the tempered glass. Detailed Implementation

[0022] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] Example 1

[0024] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0025] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0026] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0027] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite are mixed at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times that of modified vermiculite and potassium hexafluorosilicate is added and stirred at 3000 rpm for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion at 60 kHz and 400 W is used for 20 minutes to obtain a paste-like slurry. The slurry is then coated on the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0028] Example 2

[0029] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 7:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:4.

[0030] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0031] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0032] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite containing cations are mixed at a mass ratio of 1:2 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass of 3 times the total mass of modified vermiculite and potassium hexafluorosilicate is added and stirred at 3000 rpm for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion at 60 kHz and 400 W is used for 20 minutes to obtain a paste-like slurry. Then, the slurry is coated on the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0033] Example 3

[0034] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 9:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:5.

[0035] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0036] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0037] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite containing cations are mixed at a mass ratio of 1:3 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times that of the total mass of modified vermiculite and potassium hexafluorosilicate is added, and the stirring speed is 3000 rpm. Stirring is continued for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion is performed at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry. The slurry is then coated on the tempered glass surface obtained in step (2), and the coating thickness is controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0038] Comparative Example 1

[0039] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0040] (2) The mixture obtained in step (1) is uniformly coated on the surface of tempered glass. The coating thickness is controlled at 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and kept at the temperature for 50 minutes to obtain pretreated tempered glass.

[0041] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0042] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite are mixed at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times that of modified vermiculite and potassium hexafluorosilicate is added and stirred at 3000 rpm for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion at 60 kHz and 400 W is used for 20 minutes to obtain a paste-like slurry. The slurry is then coated on the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0043] Comparative Example 2

[0044] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0045] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface. The coating thickness is controlled at 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass.

[0046] Comparative Example 3

[0047] (1) Mix tetraethyl orthosilicate at a mass ratio of 5:3, stir at 500 rpm for 30 minutes at 25°C to obtain a mixture;

[0048] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0049] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0050] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite are mixed at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times that of modified vermiculite and potassium hexafluorosilicate is added and stirred at 3000 rpm for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion at 60 kHz and 400 W is used for 20 minutes to obtain a paste-like slurry. The slurry is then coated on the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0051] Comparative Example 4

[0052] (1) Heat the water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate), stir to dissolve, and obtain a mixture.

[0053] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0054] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0055] (4) Potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite are mixed at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times that of modified vermiculite and potassium hexafluorosilicate is added and stirred at 3000 rpm for 30 minutes to form a uniform slurry. Then, ultrasonic dispersion at 60 kHz and 400 W is used for 20 minutes to obtain a paste-like slurry. The slurry is then coated on the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0056] Comparative Example 5

[0057] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0058] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0059] (3) Mix potassium hexafluorosilicate with a particle size of 5 μm and toluene with a mass of 3 times that of potassium hexafluorosilicate. Stir at 3000 rpm for 30 minutes to form a uniform slurry. Then, use ultrasonic dispersion at 60 kHz and 400 W for 20 minutes to obtain the slurry. Then, coat the slurry onto the tempered glass surface obtained in step (2) with a coating thickness controlled at 80 μm. Cur at 200℃ for 2 hours to obtain the coating.

[0060] Comparative Example 6

[0061] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0062] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0063] (3) The vermiculite was crushed to a particle size of 80 mesh, then dissolved in water with a mass of 8 times that of the vermiculite, and ultrasonically crushed at 80 kHz for 30 minutes. Then it was filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. 1-Butyl-3-methylimidazolium hexafluorophosphate was prepared into a 0.3 M aqueous solution. The porous vermiculite particles and the aqueous solution were mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to allow organic cations to be inserted into the interlayer of the porous vermiculite particles through ion exchange. Then it was filtered, washed until neutral, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite.

[0064] (4) Mix modified vermiculite and toluene at 3 times the mass of modified vermiculite, and stir at 3000 rpm for 30 minutes to form a uniform slurry; then use 60 kHz, 400 W ultrasonic dispersion for 20 minutes to obtain the slurry; then coat the slurry onto the tempered glass surface obtained in step (2), and control the coating thickness to 80 μm; cure at 200℃ for 2 hours to obtain the coating.

[0065] Comparative Example 7

[0066] (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5:1 (water to calcium gluconate). After stirring to dissolve, keep the temperature at 60°C, add tetraethyl orthosilicate, and stir at 500 rpm for 30 minutes at 25°C until the tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0067] (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface with a coating thickness of 7 μm. The temperature is increased from room temperature to 220°C at a rate of 5°C / min and held for 50 minutes. The temperature is then increased to 600°C at a rate of 5°C / min and held for 2 hours. The ordinary glass is placed in a tempering furnace and held at 740°C for 20 minutes. Then it is rapidly cooled to room temperature at a rate of 200°C / second to obtain tempered glass with a porous interlayer.

[0068] (3) Crush the vermiculite to a particle size of 80 mesh, then dissolve it in water with a mass of 8 times that of the vermiculite, ultrasonically crush it at 80 kHz for 30 minutes, then filter it, wash it with deionized water, and dry it at 60 ℃ to obtain porous vermiculite particles with a pore size of 50 nm.

[0069] (4) Potassium hexafluorosilicate with a particle size of 5 μm is mixed with porous vermiculite particles at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes. Then, toluene with a mass ratio of 3 times the total mass of porous vermiculite particles and potassium hexafluorosilicate is added, and the stirring speed is 3000 rpm. The mixture is stirred continuously for 30 minutes to form a uniform slurry. Then, the slurry is ultrasonically dispersed at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry. The slurry is then coated onto the tempered glass surface obtained in step (2), and the coating thickness is controlled at 80 μm. The coating is cured at 200℃ for 2 hours to obtain a coating.

[0070] Performance testing

[0071] The rigid glass obtained in each embodiment and the comparative material were made with the same size, shape and thickness, and the softening point was tested according to the standard method of GB / T28195-2011. The results are shown in Table 1.

[0072] Table 1 below shows the performance analysis results of high temperature resistance and explosion protection of the embodiments 1 to 3 and comparative examples 1 to 7 of the present invention.

[0073] Table 1

[0074]

[0075]

[0076] As shown in Table 1, this application utilizes a mixture of calcium gluconate and tetraethyl orthosilicate, coated onto ordinary glass to form a dense silica network structure. Calcium carbonate decomposes to produce calcium oxide, which reacts with silica to form calcium silicate. Calcium silicate can form chemical bonds with the silicon-oxygen bonds on the surface of ordinary glass, improving the bonding strength and high-temperature resistance of the porous interlayer with ordinary glass. A slurry is prepared by mixing modified vermiculite containing organic cations and hexafluorosilicate in a certain proportion, coated onto the surface of tempered glass, and then cured at high temperature. During this process, the modified vermiculite rapidly expands at high temperature, forming a porous structure that blocks oxygen and heat diffusion, inhibiting flame spread. Simultaneously, hexafluorosilicate forms a dense protective film, delaying heat transfer to the tempered glass, effectively preventing overheating and cracking, and significantly improving explosion-proof performance.

[0077] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A method for preparing explosion-proof and high-temperature resistant tempered glass, characterized in that, The preparation steps include the following: (1) Heat water to boiling, then add calcium gluconate at a mass ratio of 5~10:

1. Stir to dissolve, keep warm at 60℃, add tetraethyl orthosilicate, stir at 500~800 rpm, stir at 25~35℃ for 20~30 minutes until tetraethyl orthosilicate and calcium gluconate solution are fully mixed to obtain a mixture; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3~5. (2) The mixture obtained in step (1) is uniformly coated on a clean ordinary glass surface. The coating thickness is controlled at 5~20μm. The temperature is increased from room temperature to 180~220℃ at a rate of 2~5℃ / min and held for 30~60 minutes. The temperature is then increased to 500~600℃ at a rate of 5~10℃ / min and held for 1~2 hours. The ordinary glass is placed in a tempering furnace and held at 720~740℃ for 10~20 minutes. Then it is rapidly cooled to room temperature to obtain tempered glass with porous interlayer. (3) Mix hexafluorosilicate and modified vermiculite containing cations at a mass ratio of 1:1~3 and stir at 500~800 rpm for 10-20 minutes. Then add organic solvent at a mass ratio of 1~3 times that of the total mass of modified vermiculite and hexafluorosilicate, and increase the stirring speed to 3000~5000 rpm and continue stirring for 20~30 minutes to form a uniform slurry. Then use ultrasonic dispersion at 40~60 kHz and 200~400 W for 20-40 minutes to obtain a paste-like slurry. Coat the slurry onto the tempered glass surface obtained in step (2) with a coating thickness controlled at 50~150 μm. The coating is obtained by curing at 150~200℃ for 1~2 hours. The preparation method of modified vermiculite in step (3) includes: crushing vermiculite to a particle size of 50-100 mesh, dissolving it in water at 5-10 times the mass of vermiculite, ultrasonically crushing it at 60-100 kHz for 30-40 minutes, then filtering, washing with deionized water, and drying at 60-80℃ to obtain porous vermiculite particles with a pore size of 5nm-80nm; preparing an organic cation reagent into a 0.1-0.5 M aqueous solution, mixing the porous vermiculite particles and the aqueous solution at a solid-liquid ratio of 1:10-20, stirring at 60-80℃ for 4-8 hours to allow the organic cations to insert into the interlayer of the porous vermiculite particles through ion exchange, then filtering, washing until neutral, and vacuum drying at 60℃ for 24 hours.

2. The method for preparing explosion-proof and high-temperature resistant tempered glass according to claim 1, characterized in that, In step (1), the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:

4.

3. The method for preparing explosion-proof and high-temperature resistant tempered glass according to claim 1, characterized in that, In step (3), the mass ratio of hexafluorosilicate to modified vermiculite is 1:

2.

4. The method for preparing explosion-proof and high-temperature resistant tempered glass according to claim 1, characterized in that, In step (3), the hexafluorosilicate is potassium hexafluorosilicate or sodium hexafluorosilicate; the particle size of the hexafluorosilicate is ≤5 μm.

Citation Information

Patent Citations

  • Toughened glass thermal insulation coating and preparation method thereof

    CN112408763A