Aerogel composite fireproof and thermal insulation glass and a preparation method thereof

Abstract

This invention belongs to the field of energy-saving glass manufacturing technology, and provides an aerogel composite fireproof and heat-insulating glass and its manufacturing method. The fireproof glass comprises multiple tempered glass panes, a spacer frame, and multiple isolated sealed cavities forming a composite structure. The cavity near the interior side is filled with composite silica aerogel particles, while the cavity on the fire-facing side is filled with a fire-resistant medium containing phytic acid, boric acid, and xylitol aluminum complex oligomers. A heat-shielding precursor layer formed by polyvinyl alcohol, borate, guanidine phosphate, and gallic acid is introduced onto the surface of the aerogel particles. This composite structure can form a multi-level heat-insulating barrier under fire conditions, slowing heat transfer to the un-fired side and delaying the temperature rise of the un-fired surface. It also helps maintain the overall stability of the glass component, making it suitable for fireproof windows, fireproof partitions, and skylights.

Description

Technical Field

[0001] This invention belongs to the field of energy-saving glass preparation technology, and relates to an aerogel composite fireproof and heat-insulating glass and its preparation method. Background Technology

[0002] Fire-resistant glass, as an important component in building fire-resistant partition and energy-saving systems, is widely used in fire-resistant windows, fire-resistant partitions, lighting components, and other applications requiring both light transmission and fire resistance. Existing fire-resistant glass typically employs a laminated or hollow structure formed by multiple panes of glass with an intermediate fire-resistant medium. When exposed to fire, the fire-resistant medium absorbs heat, expands, carbonizes, or forms a heat-insulating layer to prevent the transmission of flames and high temperatures to the unexposed side.

[0003] Existing composite fire-resistant glass still has certain shortcomings in practical use. On the one hand, existing solutions mostly rely on a single fire-resistant medium to bear the main heat-insulating function. As the fire continues to develop and the exposure time increases, the ability to control the temperature rise on the unexposed side is prone to decline. Especially under sustained high temperatures, the single-layer heat-insulating mechanism is difficult to balance the initial fire resistance integrity and the later heat insulation stability. On the other hand, some fire-resistant medium systems are prone to water loss, delamination, aging, changes in fluidity, or insufficient compatibility with glass and partition structures after long-term use, which in turn affects the service stability of the fire-resistant glass and its heat-insulating effect under fire.

[0004] Furthermore, while the application of aerogel materials in fire-resistant glass offers new insights into fire-resistant insulation, existing technologies generally suffer from insufficient synergy between materials and structure. For example, the uniformity, density, electrostatic distribution, particle flowability, and compatibility with other fire-resistant media in the aerogel particles within the cavity all significantly impact the final heat-insulating effect. If aerogel is simply introduced as a common filler, it is often difficult to form multi-level heat-insulating pathways under fire conditions, and it is also difficult to simultaneously address the issues of delayed temperature rise on the unexposed side, maintenance of structural integrity, and long-term stability of the component. Therefore, it remains necessary to provide an aerogel composite fire-resistant glass with a more rationally designed structure and material system, along with its preparation method, to improve its heat insulation performance and overall reliability under fire conditions. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide an aerogel composite fireproof and heat-insulating glass and its preparation method. By constructing a fireproof medium cavity and an aerogel particle cavity in a composite cavity formed by multiple glass sheets, and introducing a heat-shielding precursor layer on the surface of the aerogel particles, a synergistic heat-insulating structure is formed when exposed to fire, which slows down the transfer of heat to the unexposed side and delays the temperature rise of the unexposed surface. At the same time, it improves the overall stability and reliability of the component, thereby meeting the needs of actual production.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides an aerogel composite fireproof and heat-insulating glass, comprising at least three tempered glass panels arranged in parallel from the fire-facing side to the indoor side, wherein adjacent tempered glass panels are separated by a fireproof partition frame and enclosed to form at least two independent sealed cavities.

[0008] Among them, the sealed cavity located on the indoor side and directly adjacent to the indoor tempered glass panel is an aerogel particle cavity, which is filled with composite silica aerogel particles.

[0009] At least one sealed cavity located on the fire-facing side of the aerogel particle cavity is a fire-resistant medium cavity, and the fire-resistant medium cavity is filled with fire-resistant medium A, wherein the fire-resistant medium A uses phytic acid-boric acid-xylitol aluminum complex oligomer as a layering precursor.

[0010] The composite silica aerogel particles are composed of silica aerogel particles and a rear heat shielding precursor layer loaded on their surface. The rear heat shielding precursor layer contains polyvinyl alcohol, borate, guanidine phosphate, gallic acid and glycerol.

[0011] The fireproof partition frame is provided with an edge sealing structure around its perimeter;

[0012] The aerogel particle cavity is under negative pressure and sealed after being filled with particles.

[0013] Preferably, the aerogel composite fireproof and heat-insulating glass has a triple-glazed two-cavity, quadruple-glazed three-cavity, or pentaglazed four-cavity structure.

[0014] Preferably, the tempered glass sheet is ultra-clear tempered glass or float tempered glass, with a single sheet thickness of 3-12mm. The thickness of each tempered glass sheet in the same aerogel composite fireproof and heat-insulating glass may be the same or different.

[0015] Preferably, the width of the fireproof partition frame is 4-16mm;

[0016] The fireproof partition frame is provided with 1-3 filling ports, and the diameter of the filling ports is 2-10mm;

[0017] The fireproof partition frame is reserved with one air extraction hole, the diameter of which is 1-6mm.

[0018] Preferably, the edge sealing structure includes a filling port seal, an air extraction port seal, and a second layer of sealant;

[0019] The filling port seal is a flexible barrier strip made of silicone, and the second sealant is silicone sealant.

[0020] Preferably, the fire-retardant medium A, in addition to the phytic acid-boric acid-xylitol aluminum complex oligomer, also contains deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone.

[0021] Preferably, in the fire-retardant medium A, the mass ratio of phytic acid aqueous solution, boric acid, xylitol, aluminum nitrate nonahydrate, deionized water, glycerol, ethylene glycol, polyvinyl alcohol and polyvinylpyrrolidone is (18-22):(4-6):(6-8):(3-5):(83-107):(8-12):(4-8):(2-4):(1-3); wherein the mass fraction of the phytic acid aqueous solution is 50 wt.%.

[0022] Preferably, the silica aerogel particles have a porosity of 85%-98.9% and a thermal conductivity ≤0.02W / (m·K).

[0023] Preferably, the rear heat shielding precursor layer comprises polyvinyl alcohol, borax, guanidine phosphate, gallic acid and glycerol in a mass ratio of (8-12):(0.3-0.8):(0.5-1.5):(0.03-0.12):(1-3).

[0024] Preferably, the rear thermal shielding precursor layer is distributed on the surface of the silica aerogel particles and the contact points between the particles in a loading manner, and its total loading amount is 0.4-3.5 wt.% of the mass of the silica aerogel particles.

[0025] Preferably, the filling density of the composite silica aerogel particles in the aerogel particle cavity is above 95%.

[0026] Preferably, the aerogel particle cavity is subjected to a vacuum treatment to form a negative pressure before sealing, and the absolute pressure after vacuuming is 5-20 kPa.

[0027] Secondly, the present invention provides a method for preparing the aforementioned aerogel composite fireproof and heat-insulating glass, the method comprising:

[0028] S1, Preparation of silica aerogel particles;

[0029] S2, preparing fire-retardant medium A with phytic acid-boric acid-xylitol aluminum complex oligomer as a layering precursor;

[0030] S3, prepare a downstream heat shielding precursor solution containing polyvinyl alcohol, borate, guanidine phosphate, gallic acid and glycerol;

[0031] S4, the rear heat shielding precursor liquid is loaded onto the surface of silica aerogel particles to obtain composite silica aerogel particles.

[0032] S5 involves cleaning, destaticating, and drying the tempered glass sheet before assembling it with a fireproof partition frame to form a triple-glazed, quadruple-glazed, or quintuple-glazed insulated glass cavity.

[0033] S6, fill the composite silica aerogel particles into the aerogel particle cavity near the indoor side, and perform vibration or impact, static electricity removal and vacuum negative pressure treatment during the filling process;

[0034] S7. Fire-resistant medium A is filled into one or more fire-resistant medium cavities on the fire-facing side of the aerogel particle cavity to complete the sealing, curing and double sealing, and obtain aerogel composite fire-resistant and heat-insulating glass.

[0035] The preparation method specifically includes:

[0036] S1. Mix silicon source, ethanol, and deionized water, and stir at 25-40℃ for 5-10 min. Add glacial acetic acid to adjust the pH to 2-4, and continue stirring for 1-3 h. Then add 25 wt.% ammonia water to adjust the pH to 8-10, stir for 3-10 min, pour into a mold, and let stand at 25-60℃ for 1-6 h to form a wet gel. Place the wet gel and mold in a constant temperature water bath at 30-70℃, and add 1.0-1.5 times the volume of the wet gel in an aging solution for aging. After aging for 5 h, remove the wet gel and cut it into particles with a diameter of 1-20 mm. Then, aging them at the same temperature... The particles were aged for another 24 hours. The aged wet gel particles were placed in an autoclave filled with ethanol, pre-charged with nitrogen to 3 MPa and repeatedly purged and purged 2-4 times. The temperature was then increased to 250-270℃ at a rate of 5-10℃ / min and maintained at 8-14 MPa for 3-6 hours. After that, the pressure was released at a rate of 0.10-0.22 MPa / min. When the pressure dropped to 2-3 MPa, nitrogen was introduced to flush for 10-20 minutes. The temperature was then reduced to room temperature at a rate of 15-30℃ / min. The particles were then sieved and classified through 8, 10, 12, 14, and 16 mesh sieves to collect silica aerogel particles in the target particle size range.

[0037] S2, a 50 wt.% aqueous solution of phytic acid, boric acid, xylitol, and first deionized water are mixed and stirred at 45-55℃ for 20-30 min to obtain a mixed solution. Then, aluminum nitrate nonahydrate is dissolved in deionized water to prepare an aluminum salt solution, and the aluminum salt solution is added dropwise to the mixed solution at 50-60℃. After the addition is completed, the mixture is kept warm and stirred for 1.0-2.0 h to obtain a fire-retardant precursor liquid. The fire-retardant precursor liquid is degassed for 10-20 min at 45-55℃ and an absolute pressure of 0.07-0.09 MPa. After cooling to room temperature, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone are added. The mixture is stirred at 55-65℃ for 40-60 min, and then filtered through a 100-200 mesh filter and degassed to obtain fire-retardant medium A.

[0038] S3, mix polyvinyl alcohol with deionized water, heat and stir at 90-95℃ for 1.0-1.5h and cool to 45-55℃, then add guanidine phosphate, gallic acid, glycerol and Tween-20, and disperse at 40-50℃ by high-speed shearing and / or ultrasonication for 30-60min to obtain dispersion B1, then dissolve borax in deionized water to obtain borate crosslinking solution B2;

[0039] S4. Place the silica aerogel particles in a drum mixer, spray the dispersion liquid B1 while turning it over, continue turning it over for 5-15 minutes, then spray the borate crosslinking liquid B2 in a misting manner, continue turning it over for 5-15 minutes, and dry it at 35-45℃ for 30-60 minutes to obtain composite silica aerogel particles.

[0040] S5, the ultra-clear tempered glass and / or float tempered glass are pre-treated in sequence. The pre-treatment includes: washing with deionized water at 40-60℃ for 5-10 minutes, then removing static electricity with ion air for 1-3 minutes, and then drying at 80-120℃ for 30-60 minutes. Fireproof spacer strips and / or silicone are selected according to the glass size to splice the fireproof spacer frame. The fireproof spacer frame is set on the edge of the lower cover glass and the upper cover glass is covered on it. Filling ports and air extraction holes are reserved at the top and bottom of the fireproof spacer frame to obtain the hollow glass cavity.

[0041] S6. Fill the cavity near the indoor side with composite silica aerogel particles. During the filling process, continuously vibrate and / or impact for 10-15 seconds each time. Continue filling and repeat the vibration and / or impact operation 5-8 times until the particle filling density reaches more than 95%. During the filling process, the composite silica aerogel particles and the hollow glass cavity are simultaneously subjected to ion wind static elimination treatment. After the particle filling is completed, temporarily seal the filling port and evacuate the cavity near the indoor side through the air extraction port to form a negative pressure state with an absolute pressure of 5-20 kPa. Then seal the air extraction port to obtain a particle aerogel glass accessory with an indoor side aerogel particle insulation and cooling layer.

[0042] S7. The aerogel glass component is assembled with the remaining hollow glass cavities to obtain a composite glass structure of three-pane two-cavity, four-pane three-cavity, or five-pane four-cavity glass. Then, fire-retardant medium A is filled into one or more cavities on the non-indoor side through the filling port of the non-indoor side cavity, and the filling volume is controlled to be more than 95% of the corresponding cavity volume. During the filling process, air bubbles are removed by adjusting the angle of the flipping table. After filling, a flexible silicone barrier strip is embedded and the filling port is sealed with silicone sealant. Then, the glass assembly is cured at 60-100℃ for 6-12 hours. After curing, a second sealant is applied and the glass is left to stand at room temperature for 24 hours to obtain aerogel composite fireproof and heat-insulating glass.

[0043] Preferably, in S1, the silicon source is tetraethyl orthosilicate and / or methyl orthosilicate.

[0044] Preferably, the molar ratio of the silicon source, ethanol and deionized water is 1:(6-10):(2-4).

[0045] Preferably, in the ethanol / silicon source mixed aging solution, the volume ratio of ethanol to silicon source is 1:1.

[0046] Preferably, in S2, the mass ratio of aluminum nitrate nonahydrate to deionized water in the aluminum salt solution is (3-5):(8-12).

[0047] Preferably, in S3, the mass ratio of borax to deionized water in the borate crosslinking solution B2 is (0.3-0.8):(10-15).

[0048] Preferably, in S4, the mass ratio of the silica aerogel particles, dispersion B1 and borate crosslinking liquid B2 is 100:(5-20):(2-10).

[0049] Preferably, in S5, the ion wind static elimination specifically involves: a static elimination voltage of 5-15kV and a distance of 10-20cm between the glass surface and the ion wind outlet.

[0050] Under acidic conditions, the silicon source first undergoes alkoxy hydrolysis to generate silanol intermediates. Upon transitioning to alkaline conditions, the condensation between silanols and between silanols and residual alkoxy groups accelerates, forming a three-dimensional network dominated by silicon-oxygen-silicon bonds. During aging, insufficiently condensed silanols continue to polymerize, and weak connections are strengthened through dissolution-redeposition and structural rearrangement, resulting in a decrease in local stress. Phosphate groups in phytic acid dissociate in water and coordinate with aluminum ions at multiple sites, forming aluminum-phytic acid coordination nodes. Boric acid forms a borate ester and borate salt equilibrium with the ortho-hydroxyl groups of xylitol, transforming the boron center from tricoordinate to tetracoordinate. Aluminum ions can simultaneously undergo coordination exchange with oxygen-containing sites around xylitol and borate esters, transforming the system from a simple hydrogen bond and borate ester equilibrium network into a network containing metal coordination bonds, borate ester bonds, and hydrogen bonds. Polyphosphonic acid sites in phytic acid form oligomeric coordination aggregates with aluminum centers. After the addition of polyvinyl alcohol and polyvinylpyrrolidone, the hydroxyl groups of polyvinyl alcohol form hydrogen bonds with phytic acid, borate esters and the residual hydroxyl groups of xylitol, and form chain segment entanglements with the hydrophilic regions around the coordination nodes; the carbonyl groups of polyvinylpyrrolidone form dipole-hydrogen bonds with phosphate groups, hydroxyl groups and coordination water, which inhibits the delamination of coordination aggregates.

[0051] After polyvinyl alcohol (PVA) forms a continuous phase in water, guanidine phosphate is dispersed in the system as ion pairs and binds to PVA segments through hydrogen bonding and ion-dipole interactions. The carboxyl and phenolic hydroxyl groups in gallic acid form multi-point hydrogen bonds with PVA and associate with the phosphate groups in guanidine phosphate. Upon the addition of borax, the borate groups form reversible borate ester crosslinking sites with the hydroxyl groups on the PVA chain and compete for coordination with the phenolic hydroxyl groups of gallic acid.

[0052] After the heat-shielding precursor solution is loaded onto silica aerogel particles, polyvinyl alcohol (PVA), gallic acid (GLA), and guanidine phosphate preferentially enter the open pores and rough depressions on the particle surface. Residual silanol on the silica surface forms hydrogen bonds with the hydroxyl groups of PVA and the phenolic hydroxyl groups of GLA. Rolling and atomized spraying enrich the precursor solution in the protrusions, pore edges, and narrow gaps between particle contacts on the particle surface. Subsequent addition of borax induces cross-linking of the borate esters involving PVA and GLA, transforming the flowable dispersion into a loaded layer adhering to the surface and contact areas. During drying, moisture evaporation causes PVA segments to converge, increasing the hydrogen bond density, shifting the borate ester equilibrium towards the bound state, and fixing guanidine phosphate and GLA from the dispersed state into the loaded layer. Because the loading mainly occurs on the particle surface and in the stacked contact areas, the bulk pore structure of the particles is preserved, and continuous gas-phase channels remain between particles.

[0053] Under flame heating conditions, free water and coordinated water in the fire-resistant medium migrate and vaporize first, and the heat is absorbed by the phase change. The phosphate groups in phytic acid continue to dehydrate and condense, forming a polyphosphoric acid structure; the hydroxyl groups of xylitol, glycerol, and ethylene glycol dehydrate in the phosphorus-rich environment, generating carbon-containing intermediates that undergo esterification and condensation with the polyphosphoric acid structure to form a phosphorus-containing carbon skeleton. Boric acid and its esters simultaneously dehydrate, forming a boron-oxygen network that intercalates with the phosphorus-oxygen network. The aluminum center transforms from a coordinated sol state to an inorganic node containing aluminum-oxygen bridges, and the phytic acid-aluminum coordination structure shrinks into a continuous phase rich in aluminum, phosphorus, boron, and oxygen. Polyvinyl alcohol and polyvinylpyrrolidone dehydrate and crack in this environment, and their residual carbon skeletons are incorporated into the aforementioned network, resulting in the formation of a continuous heat-insulating layer in the fire-resistant medium cavity on the fire-facing side.

[0054] Upon heating, the thermally shielded precursor layer within the particle cavity undergoes several transformations. Polyvinyl alcohol (PVA) first dehydrates and transforms into an unsaturated structure, while gallic acid undergoes oxidative dehydrogenation and condensation, forming a carbonized precursor phase rich in aromatic structures. Guanidine phosphate decomposes, releasing phosphoric acid-containing species and nitrogen-containing intermediates. These acidic species catalyze further dehydration and carbonization of PVA and gallic acid, with the nitrogen-containing intermediates entering the carbon layer to form a nitrogen-carbon structure. Borax transforms into a boron-oxygen structure, entering the space between the carbon layer and the surface silica-oxygen layer, forming a boron-carbon-oxygen phase and a boron-silicon-oxygen interface. Silanol on the silica surface continues to condense, and the hydrogen bonds between the supported layer and the silica surface transform into a more stable interfacial connection. Because the precursor layer is initially enriched on the particle surface and in the particle contact region, bridging phases are preferentially generated at particle connection sites after pyrolysis, transforming the particle bed from purely mechanically packed to a framework with chemical bridging. The fireproof medium layer on the fire-facing side restricts heat flow, the gas phase channels in the particle accumulation layer on the unfired side restrict heat conduction, and the phosphorus-, nitrogen-, boron-, and carbon layer and silicon-oxygen interface phase formed by the pyrolysis of the particle surface load layer inhibit radiative coupling and contact heat transfer between particles, thereby delaying the temperature rise on the unfired side.

[0055] Compared with the prior art, the beneficial effects of the present invention are as follows: The present invention constructs mutually isolated fire-resistant medium cavities and aerogel particle cavities between multiple glass panes. The complex oligomer system in the fire-resistant medium cavity on the fire-facing side can form a continuous heat-insulating phase after being heated, weakening the direct transfer of high temperature to the unfired side. The aerogel particle cavity near the indoor side utilizes the synergistic effect of the porous channels formed by particle accumulation and the heat-shielding precursor layer on the particle surface to continue to inhibit heat penetration and delay the temperature rise on the unfired side. This structure enables the component to have both fire resistance integrity and fire insulation capability under fire conditions. The heat-shielding precursor layer is loaded on the particle surface and the contact area between particles, which helps to improve the stability of the particle layer under heating conditions and weaken particle displacement, collapse and local thermal bridge formation. The fire-resistant medium and particle loading system used can be matched with the multi-cavity glass structure, which is convenient for filling, sealing and assembly. The component has good overall integrity and is suitable for occasions such as fireproof windows, fireproof partitions and lighting components that need to simultaneously take into account the requirements of light transmission, fire resistance and fire insulation. Attached Figure Description

[0056] Figure 1 This is a schematic diagram of the cross-sectional structure of the aerogel composite fireproof and heat-insulating glass provided by the present invention.

[0057] In the diagram: 1. Tempered glass panel on the fire-facing side; 2. Fire-resistant medium cavity; 3. Middle tempered glass panel; 4. Aerogel particle cavity; 5. Tempered glass panel on the indoor side; 6. Fire-resistant partition frame; 7. Second layer of adhesive. Detailed Implementation

[0058] The technical solutions of the present invention will be described in detail below with reference to specific embodiments and accompanying drawings. The embodiments described herein are specific implementations of the present invention, used to illustrate the concept of the present invention; these descriptions are explanatory and exemplary, and should not be construed as limiting the implementation methods or the scope of protection of the present invention. In addition to the embodiments described herein, those skilled in the art can employ other obvious technical solutions based on the content disclosed in the claims and specification of this application. These technical solutions include those that make any obvious substitutions and modifications to the embodiments described herein.

[0059] The chemical reagents used in the embodiments and comparative examples of this invention are all commercially available products and have not undergone any further purification treatment.

[0060] Figure 1 This is a cross-sectional structural diagram of aerogel composite fireproof glass, where: 1. Tempered glass panel on the fire-facing side; 2. Fireproof medium cavity; 3. Middle tempered glass panel; 4. Aerogel particle cavity; 5. Tempered glass panel on the indoor side; 6. Fireproof partition frame; 7. Secondary adhesive.

[0061] Example 1

[0062] This embodiment provides an aerogel composite fireproof and heat-insulating glass and its preparation method, specifically including:

[0063] S1. Tetraethyl orthosilicate, ethanol, and deionized water are mixed in a molar ratio of 1:6:4 and stirred at 25°C for 10 min. Glacial acetic acid is added to adjust the pH to 2, and stirring continues for 3 h. Then, 25 wt.% ammonia is added to adjust the pH to 8, and the mixture is stirred for 10 min. The mixture is then poured into a mold and allowed to stand at 60°C for 1 h to form a wet gel. The wet gel, along with the mold, is placed in a 70°C constant temperature water bath. An ethanol / tetraethyl orthosilicate mixed aging solution with a volume of 1.0 times the volume of the wet gel is added for aging. The volume ratio of ethanol to tetraethyl orthosilicate in the ethanol / tetraethyl orthosilicate mixed aging solution is 1:1. After aging for 5 h, the wet gel is removed. The gel was cut into particles with a diameter of 1 mm and aged for another 24 h at the same temperature. The aged wet gel particles were placed in an autoclave filled with ethanol, pre-charged with nitrogen to 3 MPa and repeatedly purged and purged twice. The temperature was then increased to 250 °C at a rate of 10 °C / min and maintained at 14 MPa for 3 h. The pressure was then released at a rate of 0.22 MPa / min. When the pressure dropped to 2 MPa, nitrogen was introduced to flush for 20 min. The temperature was then reduced to room temperature at a rate of 15 °C / min. The particles were then sieved and graded through 8, 10, 12, 14 and 16 mesh sieves to collect silica aerogel particles in the target particle size range.

[0064] S2, a 50 wt.% aqueous solution of phytic acid, boric acid, xylitol, and first deionized water are mixed and stirred at 45°C for 30 min to obtain a mixed solution. Then, aluminum nitrate nonahydrate is dissolved in deionized water to prepare an aluminum salt solution, wherein the mass ratio of aluminum nitrate nonahydrate to deionized water in the aluminum salt solution is 3:12. The aluminum salt solution is added dropwise to the mixed solution at 50°C, and after the addition is complete, the mixture is kept at this temperature and stirred for 2.0 h to obtain a fire-retardant precursor liquid. The fire-retardant precursor liquid is then stirred at 45°C... Degassing was performed for 10 minutes under reduced pressure conditions of ℃ and 0.09 MPa. After cooling to room temperature, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone were added. The mass ratio of the phytic acid aqueous solution, boric acid, xylitol, first deionized water, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone was 18:6:6:30:55:12:4:4:1. The mixture was stirred at 55℃ for 60 minutes, then filtered through a 100-mesh sieve and degassed to obtain fire-retardant medium A2.

[0065] S3, polyvinyl alcohol and deionized water are mixed, heated and stirred at 90°C for 1.5 h and cooled to 45°C, then guanidine phosphate, gallic acid, glycerol and Tween-20 are added. The mass ratio of polyvinyl alcohol, deionized water, guanidine phosphate, gallic acid, glycerol and Tween-20 is 8:100:0.5:0.12:1:0.3. The mixture is then subjected to high-speed shearing at 40°C for 30 min to obtain dispersion B1. Borax is then dissolved in deionized water to obtain borate crosslinking solution B2. The mass ratio of borax to deionized water in borate crosslinking solution B2 is 0.3:15.

[0066] S4, place the silica aerogel particles in a drum mixer, spray the dispersion liquid B1 while turning it over, continue turning it over for 15 minutes, then spray the borate crosslinking liquid B2 in an atomized manner. The mass ratio of the silica aerogel particles, dispersion liquid B1 and borate crosslinking liquid B2 is 100:5:10. Continue turning it over for 5 minutes, and dry it at 35°C for 60 minutes to obtain composite silica aerogel particles.

[0067] S5, pre-treat a single piece of ultra-clear tempered glass with a thickness of 3mm in sequence. The pre-treatment includes: cleaning with 40℃ deionized water for 10 minutes, then removing static electricity with ion wind for 1 minute. The static electricity removal with ion wind is specifically: the static electricity removal voltage is 15kV, the distance between the glass surface and the ion wind outlet is 10cm, and then drying at 80℃ for 60 minutes. Select fireproof partition frame 6 according to the glass size and splice it. Assemble the fire-facing tempered glass panel 1, the middle tempered glass panel 3 and the indoor tempered glass panel 5 in sequence, and set the fireproof partition frame 6 at the edge of the lower cover glass. The width of the fireproof partition frame 6 is 4mm, and the upper cover glass is covered on it. Reserve a filling port with a diameter of 3mm and an air extraction hole with a diameter of 2mm in the fireproof partition frame 6 to obtain the hollow glass cavity.

[0068] S6. Composite silica aerogel particles are filled into the aerogel particle cavity 4 near the indoor tempered glass panel 5. During the filling process, vibration is continuously performed for 10 seconds each time. The filling is repeated 8 times until the particle filling density reaches more than 95%. During the filling process, the composite silica aerogel particles and the hollow glass cavity are simultaneously subjected to ion wind static elimination treatment. After the particle filling is completed, the filling port is temporarily sealed, and the cavity near the indoor tempered glass panel 5 is evacuated through the air extraction port to form a negative pressure state with an absolute pressure of 5 kPa. The air extraction port is then sealed to obtain a particle aerogel glass accessory with an indoor aerogel particle insulation and cooling layer.

[0069] S7, the aerogel glass component is assembled with the remaining hollow glass cavities to obtain a three-pane, two-cavity composite glass structure. The cavity on the side of the tempered glass panel 1 closest to the fire-facing side is the fire-resistant medium cavity. Fire-resistant medium A2 is then injected into one of the non-indoor cavities through the filling port of the non-indoor cavity, controlling the filling volume to be more than 95% of the corresponding cavity volume. During the filling process, air bubbles are removed by adjusting the angle of the flipping table. After filling, a flexible silicone barrier strip is embedded and the filling port is sealed with silicone sealant. Then, the glass assembly is cured at 60°C for 12 hours. After curing, a second layer of sealant 7 is applied and the glass is left to stand at room temperature for 24 hours to obtain aerogel composite fireproof and heat-insulating glass.

[0070] Example 2

[0071] This embodiment provides an aerogel composite fireproof and heat-insulating glass and its preparation method, specifically including:

[0072] S1. Methyl orthosilicate, ethanol, and deionized water are mixed in a molar ratio of 1:10:2 and stirred at 40°C for 5 minutes. Glacial acetic acid is added to adjust the pH to 4, and stirring continues for 1 hour. Then, 25 wt.% ammonia is added to adjust the pH to 10, and the mixture is stirred for 3 minutes. The mixture is then poured into a mold and allowed to stand at 25°C for 6 hours to form a wet gel. The wet gel, along with the mold, is placed in a 30°C constant temperature water bath. An ethanol / methyl orthosilicate mixed aging solution with a volume 1.5 times that of the wet gel is added for aging. The volume ratio of ethanol to methyl orthosilicate in the ethanol / methyl orthosilicate mixed aging solution is 1:1. After aging for 5 hours, the wet gel is removed. The gel was cut into particles with a diameter of 20 mm and aged for another 24 h at the same temperature. The aged wet gel particles were placed in an autoclave filled with ethanol, pre-charged with nitrogen to 3 MPa and repeatedly purged and purged 4 times. The temperature was then increased to 270 °C at a rate of 5 °C / min and maintained at 8 MPa for 6 h. After that, the pressure was released at a rate of 0.10 MPa / min. When the pressure dropped to 3 MPa, nitrogen was introduced to flush for 10 min. The temperature was then reduced to room temperature at a rate of 30 °C / min. The particles were then sieved and classified through 8, 10, 12, 14 and 16 mesh sieves to collect silica aerogel particles in the target particle size range.

[0073] S2, a 50 wt.% aqueous solution of phytic acid, boric acid, xylitol, and deionized water are mixed and stirred at 55°C for 20 min to obtain a mixed solution. Then, aluminum nitrate nonahydrate is dissolved in deionized water to prepare an aluminum salt solution, wherein the mass ratio of aluminum nitrate nonahydrate to deionized water in the aluminum salt solution is 5:8. The aluminum salt solution is then added dropwise to the mixed solution at 60°C. After the addition is complete, the mixture is stirred and kept at this temperature for 1.0 h to obtain a fire-retardant precursor solution. The fire-retardant precursor solution is then stirred at 55°C... Degassing was performed for 20 minutes under reduced pressure conditions of ℃ and 0.07 MPa. After cooling to room temperature, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone were added. The mass ratio of the phytic acid aqueous solution, boric acid, xylitol, first deionized water, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone was 22:4:8:20:65:8:8:2:3. The mixture was stirred at 65℃ for 40 minutes, then filtered through a 200-mesh sieve and degassed to obtain fire-retardant medium A2.

[0074] S3, polyvinyl alcohol and deionized water are mixed, heated and stirred at 95°C for 1.0 h and cooled to 55°C, then guanidine phosphate, gallic acid, glycerol and Tween-20 are added. The mass ratio of polyvinyl alcohol, deionized water, guanidine phosphate, gallic acid, glycerol and Tween-20 is 12:88:1.5:0.03:3:0.1. The mixture is ultrasonically dispersed at 50°C for 60 min to obtain dispersion B1. Borax is then dissolved in deionized water to obtain borate crosslinking solution B2. The mass ratio of borax to deionized water in borate crosslinking solution B2 is 0.8:10.

[0075] S4, place the silica aerogel particles in a drum mixer, spray the dispersion liquid B1 while turning it over, continue turning it over for 5 minutes, then spray the borate crosslinking liquid B2 in an atomized manner. The mass ratio of the silica aerogel particles, dispersion liquid B1 and borate crosslinking liquid B2 is 100:20:2. Continue turning it over for 15 minutes, and dry it at 45°C for 30 minutes to obtain composite silica aerogel particles.

[0076] S5, pre-treat a single piece of 12mm thick float tempered glass sequentially. The pre-treatment includes: washing with 60℃ deionized water for 5 minutes, then removing static electricity with ion air for 3 minutes. Specifically, the static electricity removal voltage is 5kV, and the distance between the glass surface and the ion air outlet is 20cm. Then, dry at 120℃ for 30 minutes. Select a silicone fireproof partition frame 6 according to the glass size and splice it. Assemble the fire-facing tempered glass panel 1, the middle tempered glass panel 3, and the indoor tempered glass panel 5 sequentially. Set the fireproof partition frame 6 at the edge of the lower cover glass. The width of the fireproof partition frame 6 is 16mm. Cover it with the upper cover glass. Reserve 3 filling ports with a diameter of 8mm and 1 air extraction hole with a diameter of 8mm in the fireproof partition frame 6 to obtain the hollow glass cavity.

[0077] S6. Composite silica aerogel particles are filled into the aerogel particle cavity 4 near the indoor tempered glass panel 5. During the filling process, impact is continuously performed for 15 seconds each time. The filling is then repeated 5 times until the particle filling density reaches more than 95%. During the filling process, the composite silica aerogel particles and the hollow glass cavity are simultaneously subjected to ion wind static elimination treatment. After the particle filling is completed, the filling port is temporarily sealed, and the cavity near the indoor tempered glass panel 5 is evacuated through the air extraction port to form a negative pressure state with an absolute pressure of 20 kPa. The air extraction port is then sealed to obtain a particle aerogel glass accessory with an indoor aerogel particle insulation and cooling layer.

[0078] S7, the aerogel glass component is assembled with the remaining hollow glass cavities to obtain a four-pane, three-cavity composite glass structure. The two cavities on the side of the tempered glass panel 1 closest to the fire-facing side are fire-resistant medium cavities. Fire-resistant medium A2 is then injected into the two cavities on the non-indoor side through the filling port of the non-indoor side cavity, controlling the filling volume to be more than 95% of the corresponding cavity volume. During the filling process, air bubbles are removed by adjusting the angle of the flipping table. After filling, a flexible silicone barrier strip is embedded and the filling port is sealed with silicone sealant. Then, the glass assembly is cured at 100°C for 6 hours. After curing, a second layer of sealant 7 is applied and the glass is left to stand at room temperature for 24 hours to obtain aerogel composite fireproof and heat-insulating glass.

[0079] Example 3

[0080] This embodiment provides an aerogel composite fireproof and heat-insulating glass and its preparation method, specifically including:

[0081] S1, Tetraethyl orthosilicate, ethanol, and deionized water are mixed in a molar ratio of 1:8:3 and stirred at 32°C for 8 minutes. Glacial acetic acid is added to adjust the pH to 3, and stirring continues for 2 hours. Then, 25 wt.% ammonia is added to adjust the pH to 9, and stirring is continued for 6 minutes. The mixture is then poured into a mold and allowed to stand at 40°C for 3 hours to form a wet gel. The wet gel, along with the mold, is placed in a 50°C constant temperature water bath. An ethanol / tetraethyl orthosilicate mixed aging solution with a volume 1.2 times that of the wet gel is added for aging. The volume ratio of ethanol to tetraethyl orthosilicate in the ethanol / tetraethyl orthosilicate mixed aging solution is 1:1. After aging for 5 hours, the wet gel is removed and... Cut into particles with a diameter of 3 mm, and continue aging at the same temperature for 24 h. Place the aged wet gel particles in an autoclave filled with ethanol, pre-charge with nitrogen to 3 MPa and repeatedly vent and recharge 3 times, then heat to 255 °C at a heating rate of 8 °C / min and maintain at 11 MPa for 4.5 h. Then depressurize at a rate of 0.16 MPa / min. When the pressure drops to 2.5 MPa, purge with nitrogen for 15 min, then cool to room temperature at a rate of 22 °C / min. Then classify and collect silica aerogel particles in the target particle size range by sieving through 8, 10, 12, 14 and 16 mesh screens.

[0082] S2, a 50 wt.% aqueous solution of phytic acid, boric acid, xylitol, and first deionized water are mixed and stirred at 50°C for 25 min to obtain a mixed solution. Then, aluminum nitrate nonahydrate is dissolved in deionized water to prepare an aluminum salt solution, wherein the mass ratio of aluminum nitrate nonahydrate to deionized water in the aluminum salt solution is 4:10. The aluminum salt solution is then added dropwise to the mixed solution at 55°C. After the addition is complete, the mixture is kept at this temperature and stirred for 1.5 h to obtain a fire-retardant precursor liquid. The fire-retardant precursor liquid is then stirred at 50°C... Degassing was performed for 15 minutes under reduced pressure conditions of ℃ and 0.08 MPa. After cooling to room temperature, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone were added. The mass ratio of the phytic acid aqueous solution, boric acid, xylitol, first deionized water, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone was 20:5:7:25:60:10:6:3:2. The mixture was stirred at 60℃ for 50 minutes, then filtered through a 150-mesh sieve and degassed to obtain fire-retardant medium A2.

[0083] S3, polyvinyl alcohol and deionized water are mixed, heated and stirred at 92°C for 1.2 h and cooled to 50°C, then guanidine phosphate, gallic acid, glycerol and Tween-20 are added. The mass ratio of polyvinyl alcohol, deionized water, guanidine phosphate, gallic acid, glycerol and Tween-20 is 10:94:1.0:0.08:2:0.2. The mixture is then dispersed by high-speed shearing and ultrasonication at 45°C for 45 min to obtain dispersion B1. Borax is then dissolved in deionized water to obtain borate crosslinking solution B2. The mass ratio of borax to deionized water in borate crosslinking solution B2 is 0.5:12.

[0084] S4, place the silica aerogel particles in a drum mixer, spray the dispersion liquid B1 while turning it over, continue turning it over for 10 minutes, then spray the borate crosslinking liquid B2 in an atomized manner. The mass ratio of the silica aerogel particles, dispersion liquid B1 and borate crosslinking liquid B2 is 100:12:6. Continue turning it over for 10 minutes, and dry it at 40°C for 45 minutes to obtain composite silica aerogel particles.

[0085] S5, pre-treat a single piece of ultra-clear tempered glass with a thickness of 5mm in sequence. The pre-treatment includes: cleaning with 50℃ deionized water for 8 minutes, then removing static electricity with ion wind for 2 minutes. The static electricity removal with ion wind is specifically: the static electricity removal voltage is 10kV, the distance between the glass surface and the ion wind outlet is 15cm, and then drying at 100℃ for 45 minutes. Select fireproof partition frame 6 according to the glass size and splice it. Assemble the fire-facing tempered glass panel 1, the middle tempered glass panel 3 and the indoor tempered glass panel 5 in sequence. Set the fireproof partition frame 6 at the edge of the lower cover glass. The width of the fireproof partition frame 6 is 8mm. Cover it with the upper cover glass. Reserve two filling ports with a diameter of 5mm and one air extraction hole with a diameter of 4mm in the fireproof partition frame 6 to obtain the hollow glass cavity.

[0086] S6. Composite silica aerogel particles are filled into the aerogel particle cavity 4 near the indoor tempered glass panel 5. During the filling process, vibration and impact are continuously performed for 12 seconds each time. Filling is continued, and the vibration and impact operation is repeated 6 times until the particle filling density reaches more than 95%. During the filling process, the composite silica aerogel particles and the hollow glass cavity are simultaneously subjected to ion wind static elimination treatment. After the particle filling is completed, the filling port is temporarily sealed, and the cavity near the indoor tempered glass panel 5 is evacuated through the air extraction port to form a negative pressure state with an absolute pressure of 12 kPa. Then the air extraction port is sealed to obtain a particle aerogel glass accessory with an indoor aerogel particle insulation and cooling layer.

[0087] S7, the aerogel glass component is assembled with the remaining hollow glass cavities to obtain a five-pane, four-cavity composite glass structure. The three cavities on the side of the tempered glass panel 1 closest to the fire-facing side are fire-resistant medium cavities. Fire-resistant medium A2 is then injected into the three cavities on the non-indoor side through the filling port of the non-indoor side cavity, controlling the filling volume to be more than 95% of the corresponding cavity volume. During the filling process, air bubbles are removed by adjusting the angle of the flipping table. After filling, a flexible silicone barrier strip is embedded and the filling port is sealed with silicone sealant. Then, the glass assembly is placed at 80°C for 9 hours to cure. After curing, a second layer of sealant 7 is applied and the glass is left to stand at room temperature for 24 hours to obtain aerogel composite fireproof and heat-insulating glass.

[0088] Example 4

[0089] This embodiment provides an aerogel composite fireproof and heat-insulating glass and its preparation method, specifically including:

[0090] S1. Tetraethyl orthosilicate, ethanol, and deionized water are mixed in a molar ratio of 1:9:3.5 and stirred at 35°C for 6 minutes. Glacial acetic acid is added to adjust the pH to 3.5, and stirring continues for 2.5 hours. Then, 25 wt.% ammonia is added to adjust the pH to 9.5, and the mixture is stirred for 8 minutes. The mixture is then poured into a mold and allowed to stand at 30°C for 4 hours to form a wet gel. The wet gel, along with the mold, is placed in a 60°C constant temperature water bath. An ethanol / tetraethyl orthosilicate mixed aging solution with a volume 1.3 times that of the wet gel is added for aging. The volume ratio of ethanol to tetraethyl orthosilicate in the ethanol / tetraethyl orthosilicate mixed aging solution is 1:1. After aging for 5 hours, the mixture is taken... The wet gel was extracted and cut into particles with a diameter of 4 mm. It was then aged for another 24 h at the same temperature. The aged wet gel particles were placed in an autoclave filled with ethanol, pre-charged with nitrogen to 3 MPa and repeatedly purged and purged 3 times. The temperature was then increased to 265 °C at a rate of 9 °C / min and maintained at 12 MPa for 5 h. After that, the pressure was released at a rate of 0.18 MPa / min. When the pressure dropped to 2.2 MPa, nitrogen was introduced for flushing for 18 min. The temperature was then reduced to room temperature at a rate of 20 °C / min. The particles were then sieved and classified through 8, 10, 12, 14 and 16 mesh sieves to collect silica aerogel particles in the target particle size range.

[0091] S2, a 50 wt.% aqueous solution of phytic acid, boric acid, xylitol, and deionized water are mixed and stirred at 52°C for 28 min to obtain a mixed solution. Then, aluminum nitrate nonahydrate is dissolved in deionized water to prepare an aluminum salt solution, wherein the mass ratio of aluminum nitrate nonahydrate to deionized water in the aluminum salt solution is 4.5:11. The aluminum salt solution is then added dropwise to the mixed solution at 58°C. After the addition is complete, the mixture is stirred and kept at this temperature for 1.8 h to obtain a fire-retardant precursor liquid. The fire-retardant precursor liquid is then subjected to a process of heating at 52°C and... Degassing was performed under reduced pressure of 0.085 MPa for 18 min. After cooling to room temperature, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone were added. The mass ratio of the phytic acid aqueous solution, boric acid, xylitol, first deionized water, second deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone was 21:5:7.5:28:62:11:7:3.5:2.5. The mixture was stirred at 62°C for 55 min, then filtered through a 180-mesh sieve and degassed to obtain fire-retardant medium A2.

[0092] S3, polyvinyl alcohol and deionized water are mixed, heated and stirred at 93°C for 1.3 h and cooled to 52°C, then guanidine phosphate, gallic acid, glycerol and Tween-20 are added. The mass ratio of polyvinyl alcohol, deionized water, guanidine phosphate, gallic acid, glycerol and Tween-20 is 11:90:1.2:0.10:2.5:0.25. The mixture is then subjected to high-speed shearing at 48°C for 50 min to obtain dispersion B1. Borax is then dissolved in deionized water to obtain borate crosslinking solution B2. The mass ratio of borax to deionized water in borate crosslinking solution B2 is 0.6:13.

[0093] S4, place the silica aerogel particles in a drum mixer, spray the dispersion liquid B1 while turning it over, continue turning it over for 12 minutes, then spray the borate crosslinking liquid B2 in an atomized manner. The mass ratio of the silica aerogel particles, dispersion liquid B1 and borate crosslinking liquid B2 is 100:15:8. Continue turning it over for 12 minutes, and dry it at 42℃ for 50 minutes to obtain composite silica aerogel particles.

[0094] S5, pre-treat a single piece of 7mm thick float tempered glass sequentially. The pre-treatment includes: cleaning with 55℃ deionized water for 6 minutes, followed by ion wind static removal for 2.5 minutes. Specifically, the static removal voltage is 12kV, and the distance between the glass surface and the ion wind outlet is 18cm. Then, dry at 110℃ for 50 minutes. Select silicone according to the glass size to splice the fireproof partition frame 6. Assemble the fire-facing tempered glass panel 1, the middle tempered glass panel 3, and the indoor tempered glass panel 5 sequentially. Set the fireproof partition frame 6 at the edge of the lower cover glass. The width of the fireproof partition frame 6 is 10mm. Cover it with the upper cover glass. Reserve two 7mm diameter filling ports and one 5mm diameter air extraction hole in the fireproof partition frame 6 to obtain the hollow glass cavity.

[0095] S6. Composite silica aerogel particles are filled into the aerogel particle cavity 4 near the indoor tempered glass panel 5. During the filling process, vibration is continuously performed for 13 seconds each time. The filling is repeated 6 times until the particle filling density reaches more than 95%. During the filling process, the composite silica aerogel particles and the hollow glass cavity are simultaneously subjected to ion wind static elimination treatment. After the particle filling is completed, the filling port is temporarily sealed, and the cavity near the indoor tempered glass panel 5 is evacuated through the air extraction port to form a negative pressure state with an absolute pressure of 15 kPa. The air extraction port is then sealed to obtain a particle aerogel glass accessory with an indoor aerogel particle insulation and cooling layer.

[0096] S7, the aerogel glass component is assembled with the remaining hollow glass cavities to obtain a three-pane, two-cavity composite glass structure. The cavity on the side of the tempered glass panel 1 closest to the fire-facing side is the fire-resistant medium cavity. Fire-resistant medium A2 is then filled into one of the non-indoor cavities through the filling port of the non-indoor cavity, controlling the filling volume to be more than 95% of the corresponding cavity volume. During the filling process, air bubbles are removed by adjusting the angle of the flipping table. After filling, a flexible silicone barrier strip is embedded and the filling port is sealed with silicone sealant. Then, the glass assembly is cured at 90°C for 8 hours. After curing, a second layer of sealant 7 is applied and the glass is left to stand at room temperature for 24 hours to obtain aerogel composite fireproof and heat-insulating glass.

[0097] Comparative Example 1

[0098] This comparative example provides an aerogel composite fireproof and heat-insulating glass and its preparation method. The difference between this example and Example 1 is that the fireproof medium A2 containing phytic acid-boric acid-xylitol aluminum complex oligomer is not used in the non-indoor side fireproof medium cavity. Instead, a conventional inorganic fireproof liquid is used. The conventional inorganic fireproof liquid is mainly prepared from ammonium dihydrogen phosphate, boric acid and aluminum hydroxide. Other process parameters and operating conditions are exactly the same as in Example 1.

[0099] Comparative Example 2

[0100] This comparative example provides an aerogel composite fireproof and heat-insulating glass and its preparation method. The difference between this example and Example 1 is that the cavity near the interior is filled with silica aerogel particles that have not been treated with heat shielding precursor liquid, and the dispersion liquid B1 and borate crosslinking liquid B2 are not sprayed and dried. Other process parameters and operating conditions are exactly the same as in Example 1.

[0101] Comparative Example 3

[0102] This comparative example provides an aerogel composite fireproof and heat-insulating glass and its preparation method. The difference between this example and Example 1 is that the aerogel particle cavity 4 near the indoor tempered glass plate 5 is still filled with the composite silica aerogel particles obtained in Example 1. However, during the filling process, repeated vibration is not performed, and ion wind static electricity removal treatment is not performed. After filling, air is not pumped to form a negative pressure state. The cavity is only sealed under normal pressure. Other process parameters and operating conditions are exactly the same as in Example 1.

[0103] Performance testing:

[0104] The test method for heat transfer coefficient refers to GB / T 5990-2021;

[0105] Fire resistance integrity shall conform to GB / T 15763.2-2005, and the standard test shall be ≥120 min.

[0106] The test results are shown in Table 1.

[0107] Table 1. Test results of aerogel composite fireproof and heat-insulating glass in Examples 1-4 and Comparative Examples 1-3

[0108]

[0109] As shown in Table 1, compared with Example 1, the heat transfer coefficient of Comparative Example 1 increased, the fire resistance time decreased, and the average temperature of the unexposed surface increased; the heat transfer coefficient of Comparative Example 2 increased, the fire resistance time decreased, and the average temperature of the unexposed surface increased; and the heat transfer coefficient of Comparative Example 3 increased, the fire resistance time decreased, and the average temperature of the unexposed surface increased.

[0110] This is because the conventional inorganic fire retardant liquid in Comparative Example 1 lacks a phytic acid-boronic acid-xylitol-aluminum complex oligomer system. After being exposed to fire, it relies solely on water evaporation and simple dehydration to absorb heat, and cannot form a continuous and dense phosphorus-, boron-, and aluminum-containing multi-element heat-insulating layer. The high-temperature heat flow quickly penetrates the fire retardant medium cavity, shortening the fire resistance time and significantly increasing the temperature of the unexposed surface.

[0111] In Comparative Example 2, the aerogel particles were not subjected to heat shielding precursor liquid loading treatment. After being exposed to fire, the particle surface could not form phosphorus-, nitrogen-, and boron-containing carbonized bridging phases. The radiative coupling and contact heat transfer between particles were not effectively suppressed. At high temperatures, the stability of the stacked layer decreased and local thermal bridges were easily generated. Therefore, the refractory time decreased and the temperature of the unexposed surface increased.

[0112] In Comparative Example 3, without vibration densification, ion wind static elimination, and negative pressure treatment, it is difficult to establish a stable contact structure between particles, which leads to an increase in the heat transfer coefficient, an accelerated temperature rise on the unexposed side, and a shortened refractory time.

[0113] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. Aerogel composite fireproof thermal insulation glass, characterized by, It includes at least three parallel tempered glass panels arranged sequentially from the fire-facing side to the indoor side. Adjacent tempered glass panels are separated by a fireproof partition frame (6) and enclosed to form at least two independent sealed cavities. The fireproof partition frame (6) has an edge sealing structure around its perimeter. Among them, the sealed cavity located on the indoor side and directly adjacent to the indoor tempered glass plate (5) is the aerogel particle cavity (4), which is filled with composite silica aerogel particles. At least one sealed cavity located on the fire-facing side of the aerogel particle cavity (4) is a fire-resistant medium cavity (2), and the fire-resistant medium cavity (2) is filled with fire-resistant medium A, wherein the fire-resistant medium A uses phytic acid-boric acid-xylitol aluminum complex oligomer as a layering precursor. The composite silica aerogel particles are composed of silica aerogel particles and a rear heat shielding precursor layer loaded on their surface. The rear heat shielding precursor layer contains polyvinyl alcohol, borate, guanidine phosphate, gallic acid and glycerol.

2. Aerogel composite fireproof and thermal insulation glass according to claim 1, characterized in that, The aerogel composite fireproof and heat-insulating glass has a triple-glazed two-cavity, quadruple-glazed three-cavity, or pentaglazed four-cavity structure.

3. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The tempered glass sheet is ultra-clear tempered glass or float tempered glass, with a single sheet thickness of 3-12mm. The thickness of each tempered glass sheet in the same aerogel composite fireproof and heat-insulating glass may be the same or different.

4. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The width of the fireproof partition frame (6) is 4-16mm; The fireproof partition frame (6) is provided with 1-3 filling ports, the diameter of which is 2-10mm; The fireproof partition frame (6) has a reserved air extraction hole with a diameter of 1-6mm.

5. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The edge sealing structure includes a filling port seal, an air extraction port seal, and two layers of sealant. The filling port seal is a flexible barrier strip made of silicone, and the second sealant is silicone sealant.

6. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The fireproof partition frame (6) is filled with 3A molecular sieve or 4A molecular sieve, and the filling amount is 60%-85% of the internal volume of the fireproof partition frame (6).

7. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, In addition to the phytic acid-boric acid-xylitol aluminum complex oligomer, the fire-retardant medium A also contains deionized water, glycerol, ethylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone.

8. The aerogel composite fireproof and heat-insulating glass according to claim 7, characterized in that, In the fire-retardant medium A, the mass ratio of phytic acid aqueous solution, boric acid, xylitol, aluminum nitrate nonahydrate, deionized water, glycerol, ethylene glycol, polyvinyl alcohol and polyvinylpyrrolidone is (18-22):(4-6):(6-8):(3-5):(83-107):(8-12):(4-8):(2-4):(1-3).

9. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The silica aerogel particles have a porosity of 85%-98.9% and a thermal conductivity of ≤0.02W / (m·K).

10. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The mass ratio of polyvinyl alcohol, borax, guanidine phosphate, gallic acid and glycerol is (8-12):(0.3-0.8):(0.5-1.5):(0.03-0.12):(1-3).

11. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The rear thermal shielding precursor layer is distributed on the surface of the silica aerogel particles and the contact points between the particles in a loading manner, and its total loading amount is 0.4-3.5 wt.% of the mass of the silica aerogel particles.

12. The aerogel composite fireproof and heat-insulating glass according to claim 1, characterized in that, The filling density of the composite silica aerogel particles in the aerogel particle cavity (4) is above 95%. The aerogel particle cavity (4) is subjected to air extraction to form a negative pressure before being sealed, and the absolute pressure after air extraction is 5-20 kPa.

13. A method for preparing aerogel composite fireproof and heat-insulating glass according to any one of claims 1-12, characterized in that, Includes the following steps: S1, Preparation of silica aerogel particles; S2, preparing fire-retardant medium A with phytic acid-boric acid-xylitol aluminum complex oligomer as a layering precursor; S3, prepare a downstream heat shielding precursor solution containing polyvinyl alcohol, borate, guanidine phosphate, gallic acid and glycerol; S4, the rear heat shielding precursor liquid is loaded onto the surface of silica aerogel particles to obtain composite silica aerogel particles. S5, the tempered glass plate is pretreated by cleaning, static electricity removal and drying, and assembled into a three-pane two-cavity, four-pane three-cavity or five-pane four-cavity hollow glass cavity by fireproof partition frame (6); S6, fill the composite silica aerogel particles into the aerogel particle cavity (4) near the indoor side, and perform vibration or impact, static electricity removal and vacuum negative pressure treatment during the filling process; S7, fireproof medium A is filled into one or more fireproof medium cavities (2) on the fire-facing side of the aerogel particle cavity (4) to complete the sealing, curing and double sealing, and obtain aerogel composite fireproof and heat-insulating glass.

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