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

Abstract

The invention discloses 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, wherein the porous interlayer is obtained by gradually heating a mixed solution obtained by mixing a calcium gluconate solution and tetraethoxysilane according to a mass ratio of 1: (3-5) from room temperature to high temperature and curing; and the coating is obtained by curing slurry at 150-200 DEG C, wherein the slurry is obtained by mixing modified vermiculite containing organic cations and hexafluorosilicate according to the mass ratio of 1: (1-3). According to the invention, a mixed solution composed of calcium gluconate and tetraethoxysilane is gradually heated for toughening treatment to form a more compact silicon dioxide network structure, so that the binding force and high temperature resistance of a porous interlayer and common glass are improved; the hexafluorosilicate can form a compact protective film to delay the transfer of heat to the tempered glass, so that the tempered glass is effectively prevented from being broken due to overheating, and the explosion-proof performance is remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of glass manufacturing, and specifically to an explosion-proof and high-temperature resistant tempered glass and a preparation method thereof. Background Art

[0002] With the progress of technology, tempered glass has expanded from the early building field to high-end scenarios such as electronic products (such as mobile phone screens) and aerospace (cabin glass), and has become one of the indispensable materials in modern society. Through nanotechnology, coating processes, etc., tempered glass is extending towards multi-functional directions such as self-cleaning, heat insulation, and ultraviolet protection to meet the personalized needs of smart homes and green buildings. New products such as intelligent dimming glass and optoelectronic glass are also under research and development, leading the industry towards intelligence and integration.

[0003] However, the internal stress distribution of tempered glass is uneven, and after long-term use, stress release leads to cracking, and self-explosion may occur without direct external force; moreover, tempered glass will also crack due to excessive thermal stress. For example, local rapid cooling and heating may cause stress concentration and reduce the service life. Therefore, there is an urgent need to develop explosion-proof and high-temperature resistant tempered glass at present. Summary of the Invention

[0004] The purpose of the present invention is to provide an explosion-proof and high-temperature resistant tempered glass and a preparation method thereof to solve the problems existing in the prior art.

[0005] To solve the above 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 includes a porous interlayer and a coating, the porous interlayer is obtained by curing a mixed solution of calcium gluconate solution and tetraethyl orthosilicate in a mass ratio of 1:3 - 5 from room temperature to high temperature; the coating is obtained by curing a slurry obtained by mixing modified vermiculite containing organic cations and hexafluorosilicate in a mass ratio of 1:1 - 3 at 150 - 200 °C.

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

[0007] Further, the solvent is deionized water.

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

[0009] Further, the organic cation reagent is 1-butyl-3-methylimidazolium hexafluorophosphate.

[0010] Further, a preparation method of an explosion-proof and high-temperature resistant tempered glass includes the following preparation steps:

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

[0012] (2) Uniformly coat the mixed solution obtained in step (1) on the surface of clean ordinary glass, with the coating thickness controlled at 5 - 20 μm. Heat from room temperature to 180 - 220°C at a rate of 2 - 5°C per minute, keep warm for 30 - 60 minutes, then continue to heat to 220 - 600°C at a rate of 5 - 10°C per minute and keep warm for 1 - 2 hours; Place the ordinary glass in a toughening furnace, keep warm at 720 - 740°C for 10 - 20 minutes, and then quickly cool to room temperature to obtain toughened glass with a porous interlayer;

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

[0014] Further, the preparation method of the modified vermiculite in step (3) includes: Crush vermiculite to a particle size of 50 - 100 mesh, then dissolve it in water 5 - 10 times the mass of vermiculite, perform ultrasonic crushing at 60 - 100 kHz for 30 - 40 minutes, then filter, wash with deionized water, and dry at 60 - 80°C to obtain porous vermiculite particles with a pore size of 5 nm - 80 nm; Prepare an aqueous solution of an organic cation reagent with a concentration of 0.1 - 0.5 M, mix the porous vermiculite particles with the aqueous solution according to a solid-liquid ratio of 1:10 - 20, and stir at 60 - 80°C for 4 - 8 hours to insert the organic cation into the interlayer of the porous vermiculite particles through ion exchange. Then filter, wash until neutral, and vacuum dry at 60°C for 24 hours.

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

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

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

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

[0019] When preparing the explosion-proof and high-temperature resistant toughened glass of the present invention, a mixed solution composed of calcium gluconate and tetraethyl orthosilicate is first coated on the surface of the glass substrate, and then toughened treatment is carried out by gradually increasing the temperature to obtain toughened glass containing a porous interlayer; then a modified vermiculite containing organic cations and a hexafluorosilicate are mixed and coated on the surface of the toughened glass in a certain proportion to achieve the effect of high-temperature resistance and explosion-proof.

[0020] First, a mixed solution composed of calcium gluconate and tetraethyl orthosilicate is coated on ordinary glass. When the temperature is raised from room temperature to 180 - 220 °C, tetraethyl orthosilicate begins to hydrolyze to generate ethanol and silicon dioxide. After ethanol volatilizes, a porous silicon dioxide network structure is formed. At the same time, calcium gluconate decomposes into calcium carbonate and carbon dioxide gas. After the carbon dioxide gas and water vapor volatilize, calcium carbonate is evenly distributed in the silicon dioxide network structure. Subsequently, when the temperature is raised to 220 - 600 °C, tetraethyl orthosilicate further decomposes, and the organic components in the porous interlayer gradually volatilize, and the silicon dioxide skeleton solidifies to form a denser silicon dioxide network structure. Then physical toughening treatment is carried out at 720 - 740 °C. Calcium carbonate continues to decompose to produce carbon dioxide gas and calcium oxide. The porosity of the porous interlayer is increased by the escape of carbon dioxide gas. At the same time, calcium oxide reacts with silicon dioxide to generate calcium silicate, and calcium silicate can form chemical bonds with the silicon-oxygen bonds on the surface of ordinary glass, improving the bonding force and high-temperature resistance between the porous interlayer and ordinary glass.

[0021] Secondly, a modified vermiculite containing organic cations and a hexafluorosilicate are mixed in a certain proportion to obtain a slurry, which is coated on the surface of the toughened glass and then cured at high temperature. During this process, the modified vermiculite expands rapidly at high temperature to form a porous structure, which can block the diffusion of oxygen and heat, inhibit the spread of flames. At the same time, the hexafluorosilicate can form a dense protective film to delay the transfer of heat to the toughened glass, effectively preventing the toughened glass from overheating and cracking, and significantly improving the explosion-proof performance. In addition, the hexafluorosilicate has high hardness and wear resistance, and the layered structure of the modified vermiculite has a certain flexibility. The combined action of the two can avoid cracking caused by thermal expansion and contraction, and improve the stability of the toughened glass. Specific embodiments

[0022] Next, in combination with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts fall within the protection scope of the present invention.

[0023] Example 1

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

[0025] (2) Uniformly coat the mixed solution obtained in step (1) on the surface of a clean ordinary glass, with the coating thickness controlled at 7 μm. Heat from room temperature to 220°C at a rate of 5°C per minute, keep it warm for 50 minutes, and continue to heat to 600°C at a rate of 5°C per minute, and keep it warm for 2 hours; place the ordinary glass in a toughening furnace, keep it warm at 740°C for 20 minutes, and then quickly cool to room temperature at a speed of 200°C per second to obtain toughened glass containing a porous interlayer.

[0026] (3) Crush vermiculite to a particle size of 80 mesh, then dissolve it in water 8 times the mass of vermiculite, ultrasonically crush it at 80 kHz for 30 minutes, then filter, wash with deionized water, and dry at 60°C to obtain porous vermiculite particles with a pore size of 50 nm; prepare 1-butyl-3-methylimidazolium hexafluorophosphate into an aqueous solution of 0.3 M, mix the porous vermiculite particles with the aqueous solution according to a solid-liquid ratio of 1:20, stir at 80°C for 6 hours to insert organic cations into the interlayer of the porous vermiculite particles through ion exchange, then filter and wash until neutral, and vacuum dry at 60°C for 24 hours to obtain modified vermiculite.

[0027] (4) Mix potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite according to a mass ratio of 1:1 and stir at 800 rpm for 10 minutes, then add toluene 3 times the total mass of modified vermiculite and potassium hexafluorosilicate, while the stirring speed is 3000 rpm, and continuously stir for 30 minutes to form a uniform slurry; then use ultrasonic dispersion at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry; then coat the slurry on the surface of the toughened glass obtained in step (2), with the coating thickness controlled at 80 μm; cure at 200°C for 2 hours to obtain a coating.

[0028] Example 2

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

[0030] (2) Uniformly coat the mixed solution obtained in step (1) on the surface of clean ordinary glass, with the coating thickness controlled at 7 μm. Heat from room temperature to 220°C at a rate of 5°C per minute, keep it warm for 50 minutes, continue to heat to 600°C at a rate of 5°C per minute, and keep it warm for 2 hours; place the ordinary glass in a toughening furnace, keep it at 740°C for 20 minutes, and then quickly cool to room temperature at a speed of 200°C per second to obtain toughened glass with a porous interlayer;

[0031] (3) Crush vermiculite to a particle size of 80 mesh, then dissolve it in water 8 times the mass of vermiculite, ultrasonically crush it at 80 kHz for 30 minutes, then filter, wash with deionized water, and dry at 60°C to obtain porous vermiculite particles with a pore size of 50 nm; prepare 1-butyl-3-methylimidazolium hexafluorophosphate into a 0.3 M aqueous solution, mix the porous vermiculite particles with the aqueous solution according to a solid-liquid ratio of 1:20, stir 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 filter, wash until neutral, and vacuum dry at 60°C for 24 hours to obtain modified vermiculite;

[0032] (4) Mix potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite containing cations according to a mass ratio of 1:2 and stir at 800 rpm for 10 minutes. Then add toluene 3 times the total mass of the modified vermiculite and potassium hexafluorosilicate, while the stirring speed is 3000 rpm, and continuously stir for 30 minutes to form a uniform slurry; then use ultrasonic dispersion at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry; then coat the slurry on the surface of the toughened glass obtained in step (2), with the coating thickness controlled at 80 μm; cure at 200°C for 2 hours to obtain a coating.

[0033] Example 3

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

[0035] (2) The mixed solution obtained in step (1) is evenly coated on the surface of a clean ordinary glass, and the coating thickness is controlled at 7 μm. It is heated from room temperature to 220 °C at a rate of 5 °C per minute, held for 50 minutes, and then continuously heated to 600 °C at a rate of 5 °C per minute and held for 2 hours. The ordinary glass is placed in a toughening furnace, held at 740 °C for 20 minutes, and then rapidly cooled to room temperature at a speed of 200 °C per second to obtain toughened glass with a porous interlayer;

[0036] (3) Vermiculite is crushed to a particle size of 80 mesh, then dissolved in water eight times the mass of vermiculite, ultrasonically broken at 80 kHz for 30 minutes, then 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 is prepared into an aqueous solution of 0.3 M. The porous vermiculite particles and the aqueous solution are mixed at a solid-liquid ratio of 1:20 and stirred at 80 °C for 6 hours to insert organic cations into the interlayer of the porous vermiculite particles through ion exchange. Then it is filtered, washed to neutrality, 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 three times the total mass of the modified vermiculite and potassium hexafluorosilicate is added, and the stirring speed is 3000 rpm while continuously stirring for 30 minutes to form a uniform slurry. Subsequently, it is ultrasonically dispersed at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry. Then the slurry is coated on the surface of the toughened glass obtained in step (2), and the coating thickness is controlled at 80 μm. It is cured at 200 °C for 2 hours to obtain a coating.

[0038] Comparative Example 1

[0039] (1) Water is heated to boiling, and then calcium gluconate is added according to a mass ratio of water to calcium gluconate of 5:1. After stirring and dissolving, it is held at 60 °C, and tetraethyl orthosilicate is added. The stirring speed is 500 rpm, and it is stirred at 25 °C for 30 minutes until tetraethyl orthosilicate and the calcium gluconate solution are fully mixed to obtain a mixed solution. The mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3;

[0040] (2) The mixed solution obtained in step (1) is evenly coated on the surface of toughened glass, and the coating thickness is controlled at 7 μm. It is heated from room temperature to 220 °C at a rate of 5 °C per minute and held for 50 minutes to obtain pretreated toughened glass;

[0041] (3) Crush vermiculite to a particle size of 80 mesh, then dissolve it in water eight times the mass of the vermiculite. Ultrasonically break it at 80 kHz for 30 minutes, then filter, wash with deionized water, and dry at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm. Prepare an aqueous solution of 1-butyl-3-methylimidazolium hexafluorophosphate at 0.3 M. Mix the porous vermiculite particles with the aqueous solution at a solid-liquid ratio of 1:20, and stir at 80 °C for 6 hours to insert organic cations into the interlayer of the porous vermiculite particles through ion exchange. Then filter and wash until neutral, and vacuum dry at 60 °C for 24 hours to obtain modified vermiculite.

[0042] (4) Mix potassium hexafluorosilicate with a particle size of 5 μm and modified vermiculite in a mass ratio of 1:1 and stir at 800 rpm for 10 minutes. Then add toluene three times the total mass of the modified vermiculite and potassium hexafluorosilicate, and at the same time, the stirring speed is 3000 rpm, and continue to stir for 30 minutes to form a homogeneous slurry. Subsequently, ultrasonically disperse it at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry. Then coat the slurry on the surface of the tempered glass obtained in step (2), and control the coating thickness at 80 μm. Cure at 200 °C for 2 hours to obtain a coating.

[0043] Comparative Example 2

[0044] (1) Heat water to boiling, then add calcium gluconate according to a mass ratio of water to calcium gluconate of 5:1. After stirring and dissolving, keep it at 60 °C, add tetraethyl orthosilicate, and the stirring speed is 500 rpm. Stir at 25 °C for 30 minutes until tetraethyl orthosilicate is fully mixed with the calcium gluconate solution to obtain a mixed solution. The mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3.

[0045] (2) Uniformly coat the mixed solution obtained in step (1) on the surface of clean ordinary glass, and control the coating thickness at 7 μm. Heat from room temperature to 220 °C at a rate of 5 °C / minute, keep it warm for 50 minutes, and continue to heat to 600 °C at a rate of 5 °C / minute and keep it warm for 2 hours. Place the ordinary glass in a tempering furnace, keep it warm at 740 °C for 20 minutes, and then quickly cool to room temperature at a speed of 200 °C / second to obtain tempered glass.

[0046] Comparative Example 3

[0047] (1) Mix and tetraethyl orthosilicate in a mass ratio of 5:3, and the stirring speed is 500 rpm. Stir at 25 °C for 30 minutes to obtain a mixed solution.

[0048] (2) The mixed solution obtained in step (1) is evenly coated on the surface of a clean ordinary glass, and the coating thickness is controlled at 7 μm. It is heated from room temperature to 220 °C at a rate of 5 °C per minute, held for 50 minutes, and then continuously heated to 600 °C at a rate of 5 °C per minute and held for 2 hours. The ordinary glass is placed in a toughening furnace, held at 740 °C for 20 minutes, and then rapidly cooled to room temperature at a speed of 200 °C per second to obtain toughened glass with a porous interlayer;

[0049] (3) Vermiculite is crushed to a particle size of 80 mesh, then dissolved in water 8 times the mass of vermiculite, ultrasonically broken at 80 kHz for 30 minutes, then 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 is prepared into an aqueous solution of 0.3 M. The porous vermiculite particles are mixed with the aqueous solution at a solid-liquid ratio of 1:20, stirred at 80 °C for 6 hours, so that organic cations are inserted into the interlayer of the porous vermiculite particles through ion exchange, then filtered, washed to neutrality, 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 3 times the total mass of modified vermiculite and potassium hexafluorosilicate is added, and the stirring speed is 3000 rpm while continuously stirring for 30 minutes to form a uniform slurry. Subsequently, it is ultrasonically dispersed at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry. Then, the slurry is coated on the surface of the toughened glass obtained in step (2), and the coating thickness is controlled at 80 μm. It is cured at 200 °C for 2 hours to obtain a coating.

[0051] Comparative Example 4

[0052] (1) Heat water to boiling, then add calcium gluconate according to a mass ratio of water to calcium gluconate of 5:1, stir and dissolve to obtain a mixed solution;

[0053] (2) The mixed solution obtained in step (1) is evenly coated on the surface of a clean ordinary glass, and the coating thickness is controlled at 7 μm. It is heated from room temperature to 220 °C at a rate of 5 °C per minute, held for 50 minutes, and then continuously heated to 600 °C at a rate of 5 °C per minute and held for 2 hours. The ordinary glass is placed in a toughening furnace, held at 740 °C for 20 minutes, and then rapidly cooled to room temperature at a speed of 200 °C per second to obtain toughened glass with a porous interlayer;

[0054] (3) Vermiculite was crushed to a particle size of 80 mesh, then dissolved in water at 8 times the mass of vermiculite, ultrasonically broken at 80 kHz for 30 minutes, then 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 an aqueous solution of 0.3 M, and the porous vermiculite particles were mixed with the aqueous solution 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 filtered, washed to neutrality, and vacuum dried at 60 °C for 24 hours to obtain modified vermiculite;

[0055] (4) Potassium hexafluorosilicate with a particle size of 5 μm was mixed with modified vermiculite at a mass ratio of 1:1 and stirred at 800 rpm for 10 minutes, then toluene at 3 times the total mass of modified vermiculite and potassium hexafluorosilicate was added, and the stirring speed was 3000 rpm, and stirring was continued for 30 minutes to form a homogeneous slurry; subsequently, ultrasonic dispersion was carried out at 60 kHz and 400 W for 20 minutes to obtain a paste-like slurry; then the slurry was coated on the surface of the tempered glass obtained in step (2), and the coating thickness was controlled at 80 μm; it was cured at 200 °C for 2 hours to obtain a coating.

[0056] Comparative Example 5

[0057] (1) Water was heated to boiling, then calcium gluconate was added at a mass ratio of water to calcium gluconate of 5:1, stirred and dissolved, kept at 60 °C, tetraethyl orthosilicate was added, and the stirring speed was 500 rpm, and stirred at 25 °C for 30 minutes until tetraethyl orthosilicate was fully mixed with the calcium gluconate solution to obtain a mixed solution; the mass ratio of calcium gluconate to tetraethyl orthosilicate was 1:3;

[0058] (2) The mixed solution obtained in step (1) was evenly coated on the surface of clean ordinary glass, and the coating thickness was controlled at 7 μm, heated from room temperature to 220 °C at a rate of 5 °C / minute, kept warm for 50 minutes, and continued to be heated to 600 °C at a rate of 5 °C / minute, and kept warm for 2 hours; the ordinary glass was placed in a toughening furnace, kept warm at 740 °C for 20 minutes, and then rapidly cooled to room temperature at a speed of 200 °C / second to obtain tempered glass containing a porous interlayer;

[0059] (3) Potassium hexafluorosilicate with a particle size of 5 μm and toluene at 3 times the mass of potassium hexafluorosilicate were mixed, and the stirring speed was 3000 rpm, and stirring was continued for 30 minutes to form a homogeneous slurry; subsequently, ultrasonic dispersion was carried out at 60 kHz and 400 W for 20 minutes to obtain a slurry; then the slurry was coated on the surface of the tempered glass obtained in step (2), and the coating thickness was controlled at 80 μm; it was cured at 200 °C for 2 hours to obtain a coating.

[0060] Comparative Example 6

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

[0062] (2) Evenly coat the mixed solution obtained in step (1) on the surface of clean ordinary glass, with the coating thickness controlled at 7 μm. Heat from room temperature to 220°C at a rate of 5°C per minute, keep it warm for 50 minutes, then continue to heat to 600°C at a rate of 5°C per minute and keep it warm for 2 hours; Place the ordinary glass in a toughening furnace, keep it warm at 740°C for 20 minutes, and then quickly cool to room temperature at a speed of 200°C per second to obtain toughened glass with a porous interlayer;

[0063] (3) Crush vermiculite to a particle size of 80 mesh, then dissolve it in water 8 times the mass of vermiculite, ultrasonically crush it at 80 kHz for 30 minutes, then filter, wash with deionized water, and dry at 60°C to obtain porous vermiculite particles with a pore size of 50 nm; Prepare an aqueous solution of 1-butyl-3-methylimidazolium hexafluorophosphate with a concentration of 0.3 M, mix the porous vermiculite particles with the aqueous solution at a solid-liquid ratio of 1:20, and stir at 80°C for 6 hours to insert organic cations into the interlayer of the porous vermiculite particles through ion exchange, then filter, wash until neutral, and vacuum dry at 60°C for 24 hours to obtain modified vermiculite;

[0064] (4) Mix the modified vermiculite with toluene 3 times the mass of the modified vermiculite, with a stirring speed of 3000 rpm, and continuously stir for 30 minutes to form a uniform slurry; Then disperse it by ultrasonic wave at 60 kHz and 400 W for 20 minutes to obtain a slurry; Then coat the slurry on the surface of the toughened glass obtained in step (2), with the coating thickness controlled at 80 μm; Cure at 200°C for 2 hours to obtain a coating.

[0065] Comparative Example 7

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

[0067] (2) The mixture obtained in step (1) is evenly coated on the surface of a clean ordinary glass, and the coating thickness is controlled at 7 μm. It is heated from room temperature to 220 °C at a rate of 5 °C per minute, held for 50 minutes, and then continuously heated to 600 °C at a rate of 5 °C per minute and held for 2 hours. The ordinary glass is placed in a toughening furnace, held at 740 °C for 20 minutes, and then rapidly cooled to room temperature at a speed of 200 °C per second to obtain toughened glass with a porous interlayer;

[0068] (3) Vermiculite is crushed to a particle size of 80 mesh, then dissolved in water 8 times the mass of vermiculite, ultrasonically broken at 80 kHz for 30 minutes, then filtered, washed with deionized water, and dried at 60 °C to obtain porous vermiculite particles with a pore size of 50 nm;

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

[0070] Performance Test

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

[0072] The following Table 1 shows the results of the analysis of the high-temperature resistance and explosion-proof performance of Examples 1 to 3 and Comparative Examples 1 to 7 of the present invention.

[0073] Table 1

[0074]

[0075]

[0076] As can be seen from Table 1, in this application, a mixed solution composed of calcium gluconate and tetraethyl orthosilicate is coated on ordinary glass to form a dense silica network structure. Calcium carbonate decomposes to produce calcium oxide, and 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 ordinary glass and the high-temperature resistance performance. A slurry is obtained by mixing modified vermiculite containing organic cations and hexafluorosilicate in a certain proportion, and the slurry is coated on the surface of tempered glass and then cured at high temperature. During this process, the modified vermiculite expands rapidly at high temperature to form a porous structure, which can block the diffusion of oxygen and heat, inhibit the spread of flames. At the same time, hexafluorosilicate can form a dense protective film to delay the transfer of heat to the tempered glass, effectively preventing the tempered glass from overheating and breaking, and significantly improving the explosion-proof performance.

[0077] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above-described exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be construed as limiting the claims involved.

Claims

1. An explosion-proof and high-temperature resistant toughened glass, comprising a toughened glass, a porous interlayer, and a coating, characterized in that, The porous interlayer is obtained by curing a mixed solution prepared by mixing a calcium gluconate solution and tetraethyl orthosilicate in a mass ratio of 1:3 to 5 by gradually heating from room temperature to a high temperature; the coating is obtained by curing a slurry prepared by mixing modified vermiculite and hexafluorosilicate in a mass ratio of 1:1 to 3 at 150 to 200 °C.

2. An explosion-proof and high-temperature resistant toughened glass according to claim 1, characterized in that, The calcium gluconate solution is obtained by mixing calcium gluconate and a solvent in a mass ratio of 1:5 to 10.

3. An explosion-proof and high-temperature resistant toughened glass according to claim 2, characterized in that, The solvent is deionized water.

4. An explosion-proof and high-temperature resistant toughened glass according to claim 1, characterized in that, The modified vermiculite is obtained by mixing porous vermiculite particles and an organic cation solution at a solid-liquid ratio of 1:10 to 20.

5. An explosion-proof and high-temperature resistant toughened glass according to claim 4, characterized in that, The organic cation reagent is 1-butyl-3-methylimidazolium hexafluorophosphate.

6. A preparation method of explosion-proof and high-temperature resistant toughened glass, characterized in that, It includes the following preparation steps: (1) Heat water to boiling, then add calcium gluconate according to a mass ratio of water to calcium gluconate of 5 to 10:1, stir to dissolve, keep warm at 60 °C, add tetraethyl orthosilicate, stir at a speed of 500 to 800 rpm, and stir at 25 to 35 °C for 20 to 30 minutes until tetraethyl orthosilicate and the calcium gluconate solution are fully mixed to obtain a mixed solution; the mass ratio of calcium gluconate to tetraethyl orthosilicate is 1:3 to 5; (2) Uniformly coat the mixed solution obtained in step (1) on the surface of a clean ordinary glass, control the coating thickness to 5 to 20 μm, heat from room temperature to 180 to 220 °C at a rate of 2 to 5 °C per minute, keep warm for 30 to 60 minutes, and continue to heat to 500 to 600 °C at a rate of 5 to 10 °C per minute, keep warm for 1 to 2 hours; place the ordinary glass in a toughening furnace, keep warm at 720 to 740 °C for 10 to 20 minutes, and then quickly cool to room temperature to obtain tempered glass containing a porous interlayer; (3) Mix hexafluorosilicate and modified vermiculite containing cations in a mass ratio of 1:1 to 3 and stir at 500 to 800 rpm for 10 - 20 minutes, then add an organic solvent 1 to 3 times the total mass of the modified vermiculite and hexafluorosilicate, and at the same time increase the stirring speed to 3000 to 5000 rpm, continuously stir 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 - 40 minutes to obtain a paste-like slurry; coat the slurry on the surface of the tempered glass obtained in step (2), and control the coating thickness to 50 to 150 μm; Cure at 150 to 200 °C for 1 to 2 hours to obtain the coating.

7. The preparation method of an explosion-proof and high-temperature resistant toughened glass according to claim 6, wherein, The preparation method of the modified vermiculite in step (3) includes: crushing vermiculite to a particle size of 50 to 100 mesh, then dissolving it in water 5 to 10 times the mass of vermiculite, performing ultrasonic crushing at 60 - 100 kHz for 30 to 40 minutes, then filtering, washing with deionized water, and drying at 60 to 80 °C to obtain porous vermiculite particles with a pore size of 5 nm to 80 nm; prepare an aqueous solution of the organic cation reagent with a concentration of 0.1 to 0.5 M, mix the porous vermiculite particles and the aqueous solution at a solid-liquid ratio of 1:10 to 20, stir at 60 to 80 °C for 4 to 8 hours to allow the organic cation to insert into the interlayer of the porous vermiculite particles through ion exchange, then filter, wash until neutral, and vacuum dry at 60 °C for 24 hours.

8. The preparation method of an explosion-proof and high-temperature resistant toughened glass according to claim 6, characterized in that, In step (1), the mass ratio of calcium gluconate to tetraethyl orthosilicate is preferably 1:

4.

9. The preparation method of an explosion-proof and high-temperature resistant toughened glass according to claim 6, characterized in that, In the said step (3), the mass ratio of hexafluorosilicate to modified vermiculite is preferably 1:

2.

10. The preparation method of an explosion-proof and high-temperature resistant toughened glass according to claim 6, characterized in that, In the said step (3), the hexafluorosilicate is potassium hexafluorosilicate or sodium hexafluorosilicate; the particle size of the hexafluorosilicate is ≤5 μm.

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