Self-explosion-proof tempered glass and preparation method thereof

Abstract

The invention relates to the technical field of tempered glass, in particular to self-explosion-proof tempered glass and a preparation method thereof.A modified PVB film is arranged between two pieces of tempered glass, and the safety of the glass is improved by adding the modified PVB film. When the glass is subjected to external violent impact, the modified PVB film can be tightly bonded with glass fragments, so that the fragments are prevented from flying, the safety of personnel is protected, and the possibility of spontaneous explosion of the toughened glass can be effectively reduced. The silicon dioxide-silicon nitride fiber compound added in the glass has high strength, silicon nitride fibers and silicon dioxide are compounded together, and lysozyme is used for modification, so that the dispersity of the silicon dioxide-silicon nitride fiber compound is improved, the agglomeration phenomenon of the compound is improved, and the glass has good heat resistance and heat resistance. Therefore, the mechanical property of the glass is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of tempered glass, in particular to self-explosion-proof tempered glass and a preparation method thereof. Background Art

[0002] In modern architecture and the automotive industry, tempered glass is widely used for its exceptional strength and safety. By heating above its softening point and rapidly cooling it, tempered glass develops an internal stress distribution, resulting in high strength and impact resistance under external forces. However, tempered glass also presents some practical challenges, the most notable of which is spontaneous explosion.

[0003] Self-explosion refers to the sudden rupture of tempered glass without any external impact. The quality of the raw materials and the manufacturing process of tempered glass also affect the overall performance of the glass. The presence of impurities in the raw materials or lax manufacturing process control can increase the risk of self-explosion.

[0004] In order to solve the above problems and improve the mechanical properties of tempered glass, the present invention provides an anti-self-explosion tempered glass and a preparation method thereof. Summary of the Invention

[0005] The object of the present invention is to provide an anti-self-explosion tempered glass and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0006] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0007] A method for preparing self-explosion-proof tempered glass comprises the following steps:

[0008] Step 1: Take lysozyme and phosphate buffer, mix and stir for 10-15 minutes, add silica-silicon nitride fiber composite, ultrasonically disperse for 20-30 minutes, shake at 30-35°C for 3-4 hours, centrifuge, collect precipitate, and dry at 60-65°C for 22-24 hours to obtain modified silica-silicon nitride fiber composite;

[0009] Step 2: Grind limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate for 20-30 minutes, add sodium oxide, bismuth oxide, lithium oxide, modified silica-silicon nitride fiber composite, copper sulfate pentahydrate, sodium hydroxide, potassium permanganate, and polyethylene glycol ester, and melt at 1500-1550° C. to obtain glass liquid, pour the glass liquid into a liquid pool containing molten liquid tin, shape it, cool it to 520-560° C., and cool it to obtain a glass substrate;

[0010] Step 3: Take the glass substrate, cut, clean, and dry it, then send it into a tempering furnace for heating at 700-800°C, and then cool, clean, and dry it to obtain a tempered glass substrate;

[0011] Step 4: Take the tempered glass substrate, place the modified PVB film between two pieces of tempered glass substrates, and press them to obtain anti-self-explosion tempered glass.

[0012] More optimally, the glass substrate comprises the following components, by weight: 12-17 parts of limestone, 40-50 parts of silica, 4-6 parts of borax, 6-7 parts of calcium carbonate, 5-9 parts of bauxite, 10-14 parts of calcium silicate, 4-5 parts of sodium oxide, 4-5 parts of lithium oxide, 5-7 parts of bismuth oxide, 10-12 parts of modified silica-silicon nitride fiber composite, 4-8 parts of copper sulfate, 4-7 parts of sodium hydroxide, 8-12 parts of potassium permanganate, and 1-2 parts of polyethylene glycol ester.

[0013] More optimally, the preparation method of the silica-silicon nitride fiber composite includes the following steps: taking silicon nitride fiber, deionized water, and ethanol, ultrasonically dispersing, adding hexadecyltrimethylammonium bromide, stirring for 20-30 minutes, adding ammonia water, stirring for 15-20 minutes, and then adding tetraethyl orthosilicate solution, stirring for 10-12 hours, centrifuging, washing, and drying to obtain a silica-silicon nitride fiber composite.

[0014] More optimally, the preparation method of the modified PVB film is: take mercaptopropyl triethoxysilane, anhydrous ethanol and deionized water, mix and stir for 30-40 minutes, add PVB film, soak for 3-5 minutes, and then dry and cure at 100-105°C for 2-3 minutes to obtain the modified PVB film.

[0015] More optimally, the preparation method of the PVB film is: take amino polyvinyl alcohol, hydrochloric acid, and butyraldehyde, stir for 30-40 minutes, add plasticizer dioctyl phthalate, stir for 5-10 minutes, and press to obtain the PVB film.

[0016] More optimally, the preparation method of the amino polyvinyl alcohol is as follows: polyvinyl alcohol and dimethyl sulfoxide are stirred at 55-60°C for 20-30 minutes, triethylamine and succinic anhydride are added, and the reaction is carried out for 2-3 hours. 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide are added, and the reaction is carried out at 25-30°C for 35-40 minutes. The amino-terminated hyperbranched polymer is added dropwise, and the mixture is stirred for 22-24 hours to obtain the amino polyvinyl alcohol.

[0017] More optimally, the preparation method of the amino-terminated hyperbranched polymer is as follows: diethylenetriamine is cooled to 1-2°C, methyl acrylate and methanol are added dropwise under nitrogen protection, and then the mixture is reacted at 25-30°C for 3-4 hours, and the temperature is further raised to 145-150°C and the reaction is carried out under reduced pressure for 4-5 hours to obtain the amino-terminated hyperbranched polymer.

[0018] More optimally, the thickness of the modified PVB film is 0.38-0.4 mm.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] (1) The present invention prepares a tempered glass and places a modified PVB film between two pieces of tempered glass. The addition of the modified PVB film improves the safety of the glass. When the glass is subjected to a severe external impact, the modified PVB film can tightly adhere to the glass fragments, thereby preventing the fragments from flying, protecting personnel safety, and effectively reducing the possibility of the tempered glass exploding.

[0021] (2) The silica-silicon nitride fiber composite added to the glass of the present invention has high strength. Silicon nitride fiber is compounded with silica and modified with lysozyme, thereby improving the dispersibility of the silica-silicon nitride fiber composite and improving the agglomeration of the composite, thereby improving the mechanical properties of the glass.

[0022] (3) The present invention grafts mercaptopropyl triethoxysilane onto the surface of the PVB film. At this time, the surface of the modified PVB film is grafted with thiol, and the modified silica-silicon nitride fiber composite contains lysozyme, which can be adsorbed with the thiol group, thereby improving the adhesion between the tempered glass and the PVB film and reducing the possibility of the tempered glass exploding on its own.

[0023] The invention uses an amino-terminated hyperbranched polymer to prepare an amino polyvinyl alcohol. The amino polyvinyl alcohol can react with silanol groups in glass to enhance the adhesion between the tempered glass and the PVB film, further reducing the self-explosion rate of the tempered glass. DETAILED DESCRIPTION

[0024] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0025] The sources and types of all raw materials involved in the present invention are not particularly limited, and exemplary examples include:

[0026] Silicon nitride fiber: diameter: 100-200 nm, length: 10-15 μm; polyvinyl alcohol: model: S30196, can be purchased from Shanghai Yuanye Biotechnology Co., Ltd.; silicon dioxide: particle size: 30-50 nm.

[0027] Example 1: A method for preparing self-explosion-proof tempered glass, comprising the following steps:

[0028] Step 1: Preparation of silica-silicon nitride fiber composite:

[0029] Take 1g of silicon nitride fiber, 10mL of deionized water, and 90mL of 95% ethanol, ultrasonically disperse them, add 0.2g of hexadecyltrimethylammonium bromide, stir for 25min, add 1mL of 28% ammonia water, stir for 17min, then add 1mL of tetraethyl orthosilicate solution, stir for 11h, centrifuge, wash, and dry to obtain a silica-silicon nitride fiber composite;

[0030] Step 2: Preparation of modified silica-silicon nitride fiber composite:

[0031] 1.5 g of lysozyme and 300 mL of phosphate buffer with a pH of 7 were mixed and stirred for 10 min, 8 g of silica-silicon nitride fiber composite was added, ultrasonically dispersed for 25 min, and constantly shaken at 32°C for 3.5 h. The mixture was centrifuged, the precipitate was collected, and dried at 62°C for 23 h to obtain a modified silica-silicon nitride fiber composite.

[0032] Step 3: Preparation of amination polyvinyl alcohol:

[0033] Take 60 mL of diethylenetriamine and cool it to 1.5°C. Under nitrogen protection, add 47 mL of methyl acrylate and 100 mL of methanol dropwise. Then react at 27°C for 3.5 hours. Then continue to heat to 147°C and react under reduced pressure for 4.5 hours to obtain an amino-terminated hyperbranched polymer.

[0034] Take 6 g of polyvinyl alcohol and 100 mL of dimethyl sulfoxide, stir at 58 ° C for 25 minutes, add 0.2 mL of triethylamine and 0.65 g of succinic anhydride, react for 2.5 hours, add 1.2 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.62 g of N-hydroxysuccinimide, react at 28 ° C for 37 minutes, add 26 mL of amino-terminated hyperbranched polymer dropwise, and stir for 23 hours to prepare amino-polyvinyl alcohol;

[0035] Step 4: Preparation of tempered glass substrate:

[0036] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 25 minutes, and sodium oxide, lithium oxide, bismuth oxide, a modified silica-silicon nitride fiber composite, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1520°C to obtain a glass liquid, which was then poured into a liquid pool for shaping, cooled to 540°C, and cooled to obtain a glass substrate.

[0037] The liquid in the liquid pool is molten liquid tin;

[0038] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 750°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0039] Step 5: Preparation of modified PVB film:

[0040] Take 25g of amino polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 35min, add 11g of plasticizer dioctyl phthalate, stir for 7min, and press to obtain a PVB film;

[0041] 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol, and 210 mL of deionized water were mixed and stirred for 35 minutes, added to the PVB film, immersed for 34 minutes, and then dried and cured at 102°C for 2.5 minutes to obtain a modified PVB film;

[0042] The thickness of the modified PVB film is 0.4 mm;

[0043] Step 6: Preparation of anti-self-explosion tempered glass:

[0044] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 32MPa to obtain anti-self-explosion tempered glass;

[0045] The glass substrate includes the following components, by weight: 15 parts of limestone, 45 parts of silicon dioxide, 5 parts of borax, 6.5 parts of calcium carbonate, 7 parts of bauxite, 12 parts of calcium silicate, 4.5 parts of sodium oxide, 4.5 parts of lithium oxide, 6 parts of bismuth oxide, 11 parts of modified silicon dioxide-silicon nitride fiber composite, 6 parts of copper sulfate, 6 parts of sodium hydroxide, 10 parts of potassium permanganate, and 1.5 parts of polyethylene glycol ester.

[0046] Example 2: A method for preparing self-explosion-proof tempered glass, comprising the following steps:

[0047] Step 1: Preparation of silica-silicon nitride fiber composite:

[0048] Take 1g of silicon nitride fiber, 10mL of deionized water, and 90mL of 95% ethanol, ultrasonically disperse them, add 0.2g of hexadecyltrimethylammonium bromide, stir for 20min, add 1mL of 28% ammonia water, stir for 15min, then add 1mL of tetraethyl orthosilicate solution, stir for 10h, centrifuge, wash, and dry to obtain a silica-silicon nitride fiber composite;

[0049] Step 2: Preparation of modified silica-silicon nitride fiber composite:

[0050] 1.5 g of lysozyme and 300 mL of phosphate buffer with a pH of 7 were mixed and stirred for 10 min, 8 g of silica-silicon nitride fiber composite was added, ultrasonically dispersed for 20 min, constant temperature oscillation was performed at 30°C for 3 h, centrifuged, and the precipitate was collected and dried at 60°C for 22 h to obtain a modified silica-silicon nitride fiber composite.

[0051] Step 3: Preparation of amination polyvinyl alcohol:

[0052] Take 60 mL of diethylenetriamine and cool it to 1°C. Add 47 mL of methyl acrylate and 100 mL of methanol dropwise under nitrogen protection. Then react at 25°C for 3 hours. Then continue to heat to 145°C and react under reduced pressure for 4 hours to obtain an amino-terminated hyperbranched polymer.

[0053] Take 6 g of polyvinyl alcohol and 100 mL of dimethyl sulfoxide, stir at 55°C for 20 min, add 0.2 mL of triethylamine and 0.65 g of succinic anhydride, react for 2 h, add 1.2 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.62 g of N-hydroxysuccinimide, react at 25°C for 35 min, add 26 mL of amino-terminated hyperbranched polymer dropwise, and stir for 22 h to obtain amino-polyvinyl alcohol;

[0054] Step 4: Preparation of tempered glass substrate:

[0055] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 20 minutes, and sodium oxide, lithium oxide, bismuth oxide, a modified silica-silicon nitride fiber composite, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1500°C to obtain a glass liquid, which was then poured into a liquid pool for shaping, cooled to 520°C, and cooled to obtain a glass substrate.

[0056] The liquid in the liquid pool is molten liquid tin;

[0057] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 700°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0058] Step 5: Preparation of modified PVB film:

[0059] Take 25g of amino polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 30min, add 11g of plasticizer dioctyl phthalate, stir for 5min, and press to obtain a PVB film;

[0060] Take 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol and 210 mL of deionized water, mix and stir for 30 minutes, add PVB film, soak for 3 minutes, and then dry and cure at 100°C for 2 minutes to obtain a modified PVB film;

[0061] The thickness of the modified PVB film is 0.4 mm;

[0062] Step 6: Preparation of anti-self-explosion tempered glass:

[0063] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 30MPa to obtain anti-self-explosion tempered glass;

[0064] The glass substrate includes the following components, by weight: 12 parts of limestone, 40 parts of silicon dioxide, 4 parts of borax, 6 parts of calcium carbonate, 5 parts of bauxite, 10 parts of calcium silicate, 4 parts of sodium oxide, 4 parts of lithium oxide, 5 parts of bismuth oxide, 10 parts of modified silicon dioxide-silicon nitride fiber composite, 4 parts of copper sulfate, 4 parts of sodium hydroxide, 8 parts of potassium permanganate, and 1 part of polyethylene glycol ester.

[0065] Example 3: A method for preparing self-explosion-proof tempered glass, comprising the following steps:

[0066] Step 1: Preparation of silica-silicon nitride fiber composite:

[0067] Take 1g of silicon nitride fiber, 10mL of deionized water, and 90mL of 95% ethanol, ultrasonically disperse them, add 0.2g of hexadecyltrimethylammonium bromide, stir for 30min, add 1mL of 28% ammonia water, stir for 20min, then add 1mL of tetraethyl orthosilicate solution, stir for 12h, centrifuge, wash, and dry to obtain a silica-silicon nitride fiber composite;

[0068] Step 2: Preparation of modified silica-silicon nitride fiber composite:

[0069] 1.5 g of lysozyme and 300 mL of phosphate buffer with a pH of 7 were mixed and stirred for 10 min, 8 g of silica-silicon nitride fiber composite was added, ultrasonic dispersion was performed for 30 min, constant temperature oscillation was performed at 35°C for 4 h, centrifugation was performed, the precipitate was collected, and dried at 65°C for 24 h to obtain a modified silica-silicon nitride fiber composite;

[0070] Step 3: Preparation of amination polyvinyl alcohol:

[0071] Take 60 mL of diethylenetriamine and cool it to 2°C. Add 47 mL of methyl acrylate and 100 mL of methanol dropwise under nitrogen protection. Then react at 30°C for 4 hours. Then continue to heat to 150°C and react under reduced pressure for 5 hours to obtain an amino-terminated hyperbranched polymer.

[0072] Take 6 g of polyvinyl alcohol and 100 mL of dimethyl sulfoxide, stir at 60°C for 30 min, add 0.2 mL of triethylamine and 0.65 g of succinic anhydride, react for 3 h, add 1.2 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.62 g of N-hydroxysuccinimide, react at 30°C for 40 min, add 26 mL of amino-terminated hyperbranched polymer dropwise, and stir for 24 h to prepare amino-polyvinyl alcohol;

[0073] Step 4: Preparation of tempered glass substrate:

[0074] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 30 minutes, and sodium oxide, lithium oxide, bismuth oxide, a modified silica-silicon nitride fiber composite, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1550°C to obtain a glass liquid, which was then poured into a liquid pool for shaping, cooled to 560°C, and cooled to obtain a glass substrate.

[0075] The liquid in the liquid pool is molten liquid tin;

[0076] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 800°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0077] Step 5: Preparation of modified PVB film:

[0078] Take 25g of amino polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 40min, add 11g of plasticizer dioctyl phthalate, stir for 10min, and press to obtain a PVB film;

[0079] 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol, and 210 mL of deionized water were mixed and stirred for 40 minutes, added to the PVB film, immersed for 5 minutes, and then dried and cured at 105°C for 3 minutes to obtain a modified PVB film;

[0080] The thickness of the modified PVB film is 0.4 mm;

[0081] Step 6: Preparation of anti-self-explosion tempered glass:

[0082] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 35MPa to obtain anti-self-explosion tempered glass;

[0083] The glass substrate includes the following components, by weight: 17 parts of limestone, 50 parts of silicon dioxide, 6 parts of borax, 7 parts of calcium carbonate, 9 parts of bauxite, 14 parts of calcium silicate, 5 parts of sodium oxide, 5 parts of lithium oxide, 7 parts of bismuth oxide, 12 parts of modified silicon dioxide-silicon nitride fiber composite, 8 parts of copper sulfate, 7 parts of sodium hydroxide, 12 parts of potassium permanganate, and 2 parts of polyethylene glycol ester.

[0084] Comparative Example 1: No lysozyme modification was added, and the rest was the same as Example 1:

[0085] Step 1: Preparation of silica-silicon nitride fiber composite:

[0086] Take 1g of silicon nitride fiber, 10mL of deionized water, and 90mL of 95% ethanol, ultrasonically disperse them, add 0.2g of hexadecyltrimethylammonium bromide, stir for 25min, add 1mL of 28% ammonia water, stir for 17min, then add 1mL of tetraethyl orthosilicate solution, stir for 11h, centrifuge, wash, and dry to obtain a silica-silicon nitride fiber composite;

[0087] Step 2: Preparation of amination polyvinyl alcohol:

[0088] Take 60 mL of diethylenetriamine and cool it to 1.5°C. Under nitrogen protection, add 47 mL of methyl acrylate and 100 mL of methanol dropwise. Then react at 27°C for 3.5 hours. Then continue to heat to 147°C and react under reduced pressure for 4.5 hours to obtain an amino-terminated hyperbranched polymer.

[0089] Take 6 g of polyvinyl alcohol and 100 mL of dimethyl sulfoxide, stir at 58 ° C for 25 minutes, add 0.2 mL of triethylamine and 0.65 g of succinic anhydride, react for 2.5 hours, add 1.2 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.62 g of N-hydroxysuccinimide, react at 28 ° C for 37 minutes, add 26 mL of amino-terminated hyperbranched polymer dropwise, and stir for 23 hours to prepare amino-polyvinyl alcohol;

[0090] Step 3: Preparation of tempered glass substrate:

[0091] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 25 minutes, and sodium oxide, lithium oxide, bismuth oxide, silica-silicon nitride fiber composite, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1520°C to obtain glass liquid, which was then poured into a liquid pool for shaping, cooled to 540°C, and cooled to obtain a glass substrate.

[0092] The liquid in the liquid pool is molten liquid tin;

[0093] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 750°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0094] Step 4: Preparation of modified PVB film:

[0095] Take 25g of amino polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 35min, add 11g of plasticizer dioctyl phthalate, stir for 7min, and press to obtain a PVB film;

[0096] 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol, and 210 mL of deionized water were mixed and stirred for 35 minutes, added to the PVB film, immersed for 34 minutes, and then dried and cured at 102°C for 2.5 minutes to obtain a modified PVB film;

[0097] The thickness of the modified PVB film is 0.4 mm;

[0098] Step 5: Preparation of anti-self-explosion tempered glass:

[0099] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 32MPa to obtain anti-self-explosion tempered glass;

[0100] The glass substrate includes the following components, by weight: 15 parts of limestone, 45 parts of silicon dioxide, 5 parts of borax, 6.5 parts of calcium carbonate, 7 parts of bauxite, 12 parts of calcium silicate, 4.5 parts of sodium oxide, 4.5 parts of lithium oxide, 6 parts of bismuth oxide, 11 parts of silicon dioxide-silicon nitride fiber composite, 6 parts of copper sulfate, 6 parts of sodium hydroxide, 10 parts of potassium permanganate, and 1.5 parts of polyethylene glycol ester.

[0101] Comparative Example 2: The silicon nitride fiber and silicon dioxide are not compounded together, and the rest is the same as in Example 1:

[0102] Step 1: Preparation of modified silicon nitride fiber:

[0103] 1.5 g of lysozyme and 300 mL of phosphate buffer with a pH of 7 were mixed and stirred for 10 min, 8 g of silicon nitride fiber was added, ultrasonic dispersion was performed for 25 min, constant temperature oscillation was performed at 32°C for 3.5 h, centrifugation was performed, the precipitate was collected, and dried at 62°C for 23 h to obtain modified silicon nitride fiber;

[0104] Step 2: Preparation of amination polyvinyl alcohol:

[0105] Take 60 mL of diethylenetriamine and cool it to 1.5°C. Under nitrogen protection, add 47 mL of methyl acrylate and 100 mL of methanol dropwise. Then react at 27°C for 3.5 hours. Then continue to heat to 147°C and react under reduced pressure for 4.5 hours to obtain an amino-terminated hyperbranched polymer.

[0106] Take 6 g of polyvinyl alcohol and 100 mL of dimethyl sulfoxide, stir at 58 ° C for 25 minutes, add 0.2 mL of triethylamine and 0.65 g of succinic anhydride, react for 2.5 hours, add 1.2 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.62 g of N-hydroxysuccinimide, react at 28 ° C for 37 minutes, add 26 mL of amino-terminated hyperbranched polymer dropwise, and stir for 23 hours to prepare amino-polyvinyl alcohol;

[0107] Step 3: Preparation of tempered glass substrate:

[0108] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 25 minutes, and sodium oxide, lithium oxide, bismuth oxide, modified silicon nitride fiber, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1520°C to obtain a glass liquid, which was then poured into a liquid pool for shaping, cooled to 540°C, and cooled to obtain a glass substrate.

[0109] The liquid in the liquid pool is molten liquid tin;

[0110] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 750°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0111] Step 4: Preparation of modified PVB film:

[0112] Take 25g of amino polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 35min, add 11g of plasticizer dioctyl phthalate, stir for 7min, and press to obtain a PVB film;

[0113] 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol, and 210 mL of deionized water were mixed and stirred for 35 minutes, added to the PVB film, immersed for 34 minutes, and then dried and cured at 102°C for 2.5 minutes to obtain a modified PVB film;

[0114] The thickness of the modified PVB film is 0.4 mm;

[0115] Step 5: Preparation of anti-self-explosion tempered glass:

[0116] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 32MPa to obtain anti-self-explosion tempered glass;

[0117] The glass substrate includes the following components, by weight: 15 parts of limestone, 45 parts of silicon dioxide, 5 parts of borax, 6.5 parts of calcium carbonate, 7 parts of bauxite, 12 parts of calcium silicate, 4.5 parts of sodium oxide, 4.5 parts of lithium oxide, 6 parts of bismuth oxide, 11 parts of modified silicon nitride fiber, 6 parts of copper sulfate, 6 parts of sodium hydroxide, 10 parts of potassium permanganate, and 1.5 parts of polyethylene glycol ester.

[0118] Comparative Example 3: Polyvinyl alcohol was used instead of amino polyvinyl alcohol, and the rest was the same as in Example 1:

[0119] Step 1: Preparation of silica-silicon nitride fiber composite:

[0120] Take 1g of silicon nitride fiber, 10mL of deionized water, and 90mL of 95% ethanol, ultrasonically disperse them, add 0.2g of hexadecyltrimethylammonium bromide, stir for 25min, add 1mL of 28% ammonia water, stir for 17min, then add 1mL of tetraethyl orthosilicate solution, stir for 11h, centrifuge, wash, and dry to obtain a silica-silicon nitride fiber composite;

[0121] Step 2: Preparation of modified silica-silicon nitride fiber composite:

[0122] 1.5 g of lysozyme and 300 mL of phosphate buffer with a pH of 7 were mixed and stirred for 10 min, 8 g of silica-silicon nitride fiber composite was added, ultrasonically dispersed for 25 min, and constantly shaken at 32°C for 3.5 h. The mixture was centrifuged, the precipitate was collected, and dried at 62°C for 23 h to obtain a modified silica-silicon nitride fiber composite.

[0123] Step 3: Preparation of tempered glass substrate:

[0124] Limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate were ground for 25 minutes, and sodium oxide, lithium oxide, bismuth oxide, a modified silica-silicon nitride fiber composite, polyethylene glycol ester, copper sulfate pentahydrate, potassium permanganate, and sodium hydroxide were added and melted at 1520°C to obtain a glass liquid, which was then poured into a liquid pool for shaping, cooled to 540°C, and cooled to obtain a glass substrate.

[0125] The liquid in the liquid pool is molten liquid tin;

[0126] The glass substrate is cut, cleaned, and dried, and then placed in a tempering furnace for heating at 750°C, followed by cooling, cleaning, and drying to obtain a tempered glass substrate;

[0127] Step 4: Preparation of modified PVB film:

[0128] Take 25g of polyvinyl alcohol, 22g of hydrochloric acid, and 43g of butyraldehyde, stir for 35min, add 11g of plasticizer dioctyl phthalate, stir for 7min, and press to obtain a PVB film;

[0129] 2 g of mercaptopropyl triethoxysilane, 90 mL of anhydrous ethanol, and 210 mL of deionized water were mixed and stirred for 35 minutes, added to the PVB film, immersed for 34 minutes, and then dried and cured at 102°C for 2.5 minutes to obtain a modified PVB film;

[0130] The thickness of the modified PVB film is 0.4 mm;

[0131] Step 5: Preparation of anti-self-explosion tempered glass:

[0132] Take a tempered glass substrate, place the modified PVB film between two tempered glass substrates, and press at 32MPa to obtain anti-self-explosion tempered glass;

[0133] The glass substrate includes the following components, by weight: 15 parts of limestone, 45 parts of silicon dioxide, 5 parts of borax, 6.5 parts of calcium carbonate, 7 parts of bauxite, 12 parts of calcium silicate, 4.5 parts of sodium oxide, 4.5 parts of lithium oxide, 6 parts of bismuth oxide, 11 parts of modified silicon dioxide-silicon nitride fiber composite, 6 parts of copper sulfate, 6 parts of sodium hydroxide, 10 parts of potassium permanganate, and 1.5 parts of polyethylene glycol ester.

[0134] experiment:

[0135] The performance test of the self-explosion-proof tempered glass prepared in Examples 1-3 and Comparative Examples 1-3 was carried out with reference to GB 15763.2-2005, and the obtained data are shown below:

[0136]

[0137] Conclusion: Comparing the data in the table shows that in Comparative Example 1, where no lysozyme modification was added, the dispersibility of the silica-silicon nitride fiber composite was poor, the mechanical properties of the glass decreased, the adhesion between the tempered glass and the PVB film deteriorated, and the spontaneous explosion rate of the tempered glass increased. In Comparative Example 2, where the silicon nitride fiber and silica were not combined, the dispersibility of the silicon nitride fiber composite decreased, and the mechanical properties of the glass decreased. In Comparative Example 3, where polyvinyl alcohol was used instead of amino-polyvinyl alcohol, the adhesion between the tempered glass and the PVB film was poor, and the spontaneous explosion rate of the tempered glass increased.

[0138] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing self-explosion-proof tempered glass, characterized in that: The following steps are involved: Step 1: Take lysozyme and phosphate buffer, mix and stir for 10-15 minutes, add silica-silicon nitride fiber composite, ultrasonically disperse for 20-30 minutes, shake at 30-35°C for 3-4 hours, centrifuge, collect precipitate, and dry at 60-65°C for 22-24 hours to obtain modified silica-silicon nitride fiber composite; Step 2: Grind limestone, borax, silica, calcium carbonate, bauxite, and calcium silicate for 20-30 minutes, add sodium oxide, bismuth oxide, lithium oxide, modified silica-silicon nitride fiber composite, copper sulfate pentahydrate, sodium hydroxide, potassium permanganate, and polyethylene glycol ester, and melt at 1500-1550° C. to obtain glass liquid, pour the glass liquid into a liquid pool containing molten liquid tin, shape it, cool it to 520-560° C., and cool it to obtain a glass substrate; Step 3: Take the glass substrate, cut, clean, and dry it, then send it into a tempering furnace for heating at 700-800°C, and then cool, clean, and dry it to obtain a tempered glass substrate; Step 4: Take the tempered glass substrate, place the modified PVB film between two pieces of tempered glass substrates, and press them to obtain anti-self-explosion tempered glass.

2. The method for preparing a self-explosion-proof tempered glass according to claim 1, wherein: The glass substrate includes the following components, by weight: 12-17 parts of limestone, 40-50 parts of silicon dioxide, 4-6 parts of borax, 6-7 parts of calcium carbonate, 5-9 parts of bauxite, 10-14 parts of calcium silicate, 4-5 parts of sodium oxide, 4-5 parts of lithium oxide, 5-7 parts of bismuth oxide, 10-12 parts of modified silicon dioxide-silicon nitride fiber composite, 4-8 parts of copper sulfate, 4-7 parts of sodium hydroxide, 8-12 parts of potassium permanganate, and 1-2 parts of polyethylene glycol ester.

3. The method for preparing a self-explosion-proof tempered glass according to claim 1, wherein: The preparation method of the silica-silicon nitride fiber composite comprises the following steps: taking silicon nitride fiber, deionized water, and ethanol, ultrasonically dispersing, adding hexadecyltrimethylammonium bromide, stirring for 20-30 minutes, adding ammonia water, stirring for 15-20 minutes, then adding tetraethyl orthosilicate solution, stirring for 10-12 hours, centrifuging, washing, and drying to obtain the silica-silicon nitride fiber composite.

4. The method for preparing self-explosion-proof tempered glass according to claim 1, wherein: The preparation method of the modified PVB film is as follows: mercaptopropyl triethoxysilane, anhydrous ethanol and deionized water are mixed and stirred for 30-40 minutes, a PVB film is added, the film is immersed for 3-5 minutes, and then dried and cured at 100-105° C. for 2-3 minutes to obtain the modified PVB film.

5. The method for preparing self-explosion-proof tempered glass according to claim 4, characterized in that: The preparation method of the PVB film is as follows: taking amino polyvinyl alcohol, hydrochloric acid and butyraldehyde, stirring for 30-40 minutes, adding plasticizer dioctyl phthalate, stirring for 5-10 minutes, and rolling to obtain the PVB film.

6. The method for preparing self-explosion-proof tempered glass according to claim 4, characterized in that: The preparation method of the amino polyvinyl alcohol comprises the following steps: taking polyvinyl alcohol and dimethyl sulfoxide, stirring at 55-60° C. for 20-30 minutes, adding triethylamine and succinic anhydride, reacting for 2-3 hours, adding 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, reacting at 25-30° C. for 35-40 minutes, adding amino-terminated hyperbranched polymer dropwise, and stirring for 22-24 hours to obtain the amino polyvinyl alcohol.

7. The method for preparing self-explosion-proof tempered glass according to claim 6, characterized in that: The preparation method of the amino-terminated hyperbranched polymer comprises the following steps: cooling diethylenetriamine to 1-2° C., dropwise adding methyl acrylate and methanol under nitrogen protection, reacting at 25-30° C. for 3-4 hours, and then heating to 145-150° C. and reacting under reduced pressure for 4-5 hours to obtain the amino-terminated hyperbranched polymer.

8. The method for preparing self-explosion-proof tempered glass according to claim 1, wherein: The thickness of the modified PVB film is 0.38-0.4 mm.

9. Anti-self-explosion tempered glass prepared according to the method for preparing anti-self-explosion tempered glass according to any one of claims 1 to 8.

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