Heat insulation glass and preparation method thereof
By using a composite insulation layer structure and modified aerogel, the problem of insufficient thermal insulation and mechanical properties of insulated glass is solved, achieving a combination of high-efficiency thermal insulation and high strength, thereby improving the overall performance and service life of the glass.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- FUNAN COUNTY YIYUN SANITARY FIXTURES CO LTD
- Filing Date
- 2026-01-26
- Publication Date
- 2026-04-28
AI Technical Summary
Existing insulated glass cannot achieve both excellent thermal insulation performance and mechanical properties. Furthermore, the brittleness and poor bonding of aerogel result in insufficient overall strength of the glass, affecting safety and service life.
The composite thermal insulation layer structure includes a core layer and a reinforcement layer. The core layer is composed of modified aerogel, PVB resin and functional particles, while the reinforcement layer is composed of PVB resin and glass fiber fabric. The toughness is improved by modifying the elastic polymer of the modified aerogel and plasma surface modification. Combined with a Low-E glass substrate and water-based polyurethane adhesive, a tightly bonded thermal insulation glass is formed.
It achieves a combination of ultra-low thermal conductivity and high mechanical strength, improving the heat insulation and impact resistance of glass, extending its service life, and meeting environmental protection requirements.
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Figure CN121928830A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of heat-insulating glass technology, specifically to a heat-insulating glass and its preparation method. Background Technology
[0002] With the rapid development of building energy conservation and green building, higher requirements have been placed on the thermal insulation performance of building envelopes. As an important component of building envelopes, the thermal insulation performance of glass directly affects the building's energy consumption and indoor thermal comfort.
[0003] Currently, the most common types of heat-insulating glass on the market include insulated glass, Low-E glass, vacuum glass, and laminated glass. Insulated glass mainly relies on an air gap for insulation, but its insulation effect is limited. Low-E glass reflects infrared rays through a low-emissivity film, but its insulation capacity is greatly affected by the film's performance and the environment. Vacuum glass offers good insulation, but it is expensive, has a complex manufacturing process, and poor impact resistance. While ordinary laminated glass provides some insulation and safety, it is difficult to balance excellent insulation performance with superior mechanical strength.
[0004] In existing technologies, some glass products also use aerogel as a thermal insulation material. Aerogel has extremely low thermal conductivity, but it is brittle, fragile, and has poor adhesion to the resin matrix, making it difficult to use directly in laminated glass. In addition, a single thermal insulation layer structure often results in insufficient overall strength of the glass, affecting its safety and service life.
[0005] Therefore, developing a type of heat-insulating glass that can achieve excellent thermal insulation performance, as well as good mechanical strength, weather resistance, and process feasibility has become an urgent technical problem to be solved in this field. Summary of the Invention
[0006] The present invention aims to solve the problem that existing heat-insulating glass is difficult to balance heat insulation performance and mechanical properties, so that both can achieve excellent results.
[0007] To address the aforementioned problems, this invention discloses a heat-insulating glass, comprising an inner glass substrate, a first adhesive layer, a composite heat-insulating layer, a second adhesive layer, and an outer glass substrate stacked sequentially; the composite heat-insulating layer comprises a core layer and reinforcing layers located on both sides of the core layer. The composite insulation layer comprises the following components by weight: The core layer comprises 50 parts of PVB resin, 30-50 parts of modified aerogel, 3-5 parts of silane coupling agent, 2-4 parts of carbon black, 5-8 parts of polyethylene glycol, 1-3 parts of nano ZnO, and 1-1.5 parts of crosslinking agent. The two reinforcing layers comprise 50 parts of PVB resin and 10-16 parts of glass fiber fabric; The modified aerogel is obtained by using silica aerogel as a matrix, followed by in-situ modification with an elastic polymer, loading with rutile TiO2 and hollow glass microspheres, and plasma surface modification.
[0008] The heat-insulating glass provided by this invention has, but is not limited to, the following beneficial effects compared to the prior art: The core layer of the heat-insulating glass of this invention uses PVB resin as the matrix and is compounded with a high proportion of modified aerogel as the core heat-insulating filler. It combines the radiation-enhancing effect of carbon black with the UV protection function of nano ZnO to achieve multi-functional integration of heat insulation, UV protection and radiative heat dissipation. The double-sided reinforcement layers are composited with PVB resin and glass fiber fabric to specifically solve the mechanical brittleness defect of aerogel, forming a complementary structure of core heat insulation and double-sided reinforcement, so that the glass has both ultra-low thermal conductivity and high mechanical strength.
[0009] The PVB resin distribution ratio between the core layer and the reinforcing layer ensures the heat insulation filler load of the core layer and achieves precise mechanical property enhancement through the glass fiber fabric of the reinforcing layer, avoiding excessive fiber from affecting light transmittance. The dosage range of silane coupling agent and crosslinking agent ensures the compatibility between the modified aerogel and the PVB matrix, while improving the structural stability of the composite heat insulation layer and preventing delamination and peeling after long-term use.
[0010] The modified aerogel, after in-situ modification with elastic polymers, loading with functional particles, and plasma surface modification, retains the ultra-low thermal conductivity of silica aerogel, while improving toughness through elastic polymer modification, enhancing solar reflectivity through rutile TiO2 and hollow glass microsphere loading, and improving dispersibility through plasma modification. This results in a significant improvement in the thermal insulation efficiency of the core layer compared to traditional single fillers, thereby enabling the thermal insulation and mechanical properties of the insulated glass to reach excellent levels.
[0011] Furthermore, the preparation method of the modified aerogel includes the following steps: (1) In-situ modification: Tetraethyl orthosilicate is mixed with polymethyl vinyl dimethoxysilane, an acid-base composite catalyst is added, and the mixture is reacted at 40-50℃ for 2-3 hours to obtain a wet gel; (2) Rutile TiO2 and hollow glass microspheres loading: Rutile TiO2 and hollow glass microspheres were mixed and ultrasonically dispersed for 30-40 min, added to wet gel and stirred evenly, and kept at 50℃ for 24 h to obtain aged wet gel. (3) Plasma surface modification: The aged wet gel was placed in a plasma treatment instrument, and vinyltrimethoxysilane vapor was introduced. It was treated at 100-120℃ and 0.1-0.3MPa for 30-60 min. After gradient drying, the modified aerogel was obtained. The mass ratio of tetraethyl orthosilicate, polymethylvinyl dimethoxysilane, rutile TiO2, hollow glass microspheres, and vinyltrimethoxysilane is 50:(10-15):(8-12):(5-8):(3-5).
[0012] Specifically, in-situ modification constructs an elastic framework within the aerogel through the copolymerization of polymethylvinyl dimethoxysilane and tetraethyl orthosilicate, thus solving the brittleness problem of pure silica aerogel; functional particle loading introduces high-reflectivity rutile TiO2 and low-thermal-conductivity hollow glass microspheres together to form a dual thermal insulation mechanism of reflection and barrier; plasma surface modification introduces hydrophilic groups through vinyltrimethoxysilane, solving the problem of aerogel aggregation in the PVB matrix, thereby achieving joint optimization of aerogel mechanics, thermal insulation, and dispersibility.
[0013] The precise mass ratio of tetraethyl orthosilicate, polymethylvinyl dimethoxysilane, rutile TiO2, hollow glass microspheres, and vinyltrimethoxysilane ensures that the elastic polymer modification does not damage the aerogel's pore structure, that the functional particle loading is sufficient without clogging the pores, and that the plasma modifier dosage is moderate and does not affect the aerogel's thermal insulation performance, thus stabilizing the thermal conductivity of the modified aerogel at 0.018-0.022 W / (m²). K), solar reflectivity ≥92%.
[0014] Furthermore, in step (1), the acid-base composite catalyst is a mixture of hydrochloric acid and ammonia water in a volume ratio of 1:2.
[0015] Specifically, hydrochloric acid is a strong acid that can rapidly promote the hydrolysis of tetraethyl orthosilicate to form uniform primary particles; ammonia is a weak base that can regulate the rate of polycondensation reaction, allowing the primary particles to aggregate in an orderly manner to form a loose and porous network structure; the 1:2 volume ratio of the two achieves efficient matching of hydrolysis and polycondensation, avoiding problems such as excessively small pore size caused by single acid catalysis and dense structure caused by single base catalysis, resulting in a wet gel with high porosity and uniform pore size distribution.
[0016] Moreover, the composite catalyst at this volume ratio will not react adversely with polymethylvinyldimethoxysilane, ensuring that the elastic polymer can be successfully polymerized in situ and embedded into the aerogel skeleton. This not only does not affect the thermal insulation performance of the aerogel, but also effectively improves its toughness, thereby enhancing the flexural strength of the modified aerogel. At the same time, hydrochloric acid and ammonia are common chemical raw materials that are readily available and used in small quantities. They can be removed by washing after the reaction, leaving no harmful residues, which meets environmental protection requirements and avoids the problems of high cost and pollution caused by using special catalysts.
[0017] Furthermore, in step (1), the amount of the acid-base composite catalyst added is 0.5-1% of the total mass of tetraethyl orthosilicate and polymethylvinyl dimethoxysilane.
[0018] Specifically, when the amount of acid-base composite catalyst added is less than 0.5%, the hydrolysis and condensation reaction rates will be too slow, the reaction will be incomplete, the wet gel structure will be loose, and the mechanical properties will be poor. When it is higher than 1%, the reaction rate will be too fast, which will lead to severe particle aggregation, destruction of the aerogel pore structure, and an increase in thermal conductivity. The dosage range of 0.5-1% can ensure that the reaction is completed within a reasonable time and form a uniform and stable aerogel network structure.
[0019] Meanwhile, this dosage will not cause catalyst residue in the aerogel, avoiding the reaction of residual catalyst with subsequent functional particles and plasma modifiers, ensuring that the various properties of the modified aerogel (thermal insulation, mechanical properties, and dispersibility) are not affected, and improving the performance stability of the core layer.
[0020] Furthermore, in step (3), the gradient drying method is as follows: first, dry at 60°C and normal pressure for 4 hours, and then dry at 120°C and 7.9MPa for 6-8 hours.
[0021] Specifically, pre-drying at 60℃ and normal pressure for 4 hours can slowly remove some of the solvent in the pores of the wet gel, reduce the amount of solvent residue during subsequent supercritical drying, and reduce the damage of capillary pressure to the aerogel skeleton; then drying at 120℃ and 7.9MPa for 6-8 hours can completely remove the remaining solvent, which can avoid structural shrinkage and cracking caused by normal pressure drying.
[0022] Furthermore, both the inner and outer glass substrates are Low-E glass.
[0023] Specifically, Low-E glass has high visible light transmittance and high infrared reflectance, reflecting infrared light from solar radiation (accounting for about 50% of solar energy) and reducing heat transfer. The composite insulation layer uses aerogel to block heat conduction and carbon black to increase infrared radiation emissivity, achieving triple insulation through reflection, blocking, and radiation. Moreover, the visible light transmittance of Low-E glass is ≥80%, which, in conjunction with the composite insulation layer, keeps the visible light transmittance of the finished insulated glass above 70%. Furthermore, the coating layer of Low-E glass has good weather resistance, which, in conjunction with the sealing structure of the composite insulation layer, reduces the impact of external environmental factors (such as ultraviolet rays and moisture) on the internal structure of the glass, extending the service life of the insulated glass.
[0024] Furthermore, both the first adhesive layer and the second adhesive layer are water-based polyurethane adhesives.
[0025] Specifically, waterborne polyurethane adhesives exhibit extremely strong adhesion to both Low-E glass substrates and composite insulation layers, ensuring a tight bond between the layers and preventing delamination or detachment during use. This enhances the overall mechanical properties and impact resistance of the glass. Furthermore, waterborne polyurethane adhesives use water as a solvent, emitting no volatile organic compounds (VOCs), thus meeting environmental standards and avoiding the environmental and health hazards associated with solvent-based adhesives. Additionally, after curing, they possess excellent flexibility, absorbing impact energy and further improving the glass's impact resistance.
[0026] The present invention also discloses a preparation method for preparing the heat-insulating glass as described above, comprising the following steps: Step 1: According to the weight ratio of the core layer, heat and melt the PVB resin, then add modified aerogel, silane coupling agent, carbon black, polyethylene glycol, nano ZnO, and crosslinking agent and disperse evenly to obtain the sandwich material; according to the weight ratio of the reinforcement layer, heat and melt the PVB resin, then add glass fiber fabric and disperse evenly to press into two reinforcement layers of the same size, then place the sandwich material between the two reinforcement layers, and hot press under ultraviolet light to obtain a composite heat insulation layer with a core layer sandwiched between the two reinforcement layers; Step 2: Wash and dry the inner and outer glass substrates. Step 3: Apply adhesive to the outer sides of the two reinforcing layers in the composite heat insulation layer, then attach the dried inner glass substrate and outer glass substrate respectively, and hot press to form a glass substrate; Step 4: Seal and encapsulate the edges of the glass substrate to obtain heat-insulating glass.
[0027] The method for preparing heat-insulating glass provided by this invention has, but is not limited to, the following beneficial effects compared to existing technologies: Step 1 focuses on the preparation of the composite insulation layer. Through the preparation of the core layer, the preparation of the reinforcement layer, hot pressing, and ultraviolet cross-linking, a tight bond between the core layer and the reinforcement layer is achieved. Ultraviolet cross-linking can promote the reaction of the cross-linking agent and improve the structural stability of the composite insulation layer. Steps 2-4 cover substrate pretreatment, assembly hot pressing, and edge sealing to ensure controllable product quality and avoid batch differences in industrial production. Through hot pressing under ultraviolet light irradiation, the PVB resin of the core layer and the reinforcement layer melts and cross-links to form an integrated structure, which solves the problem of loose interlayer bonding in traditional composite processes.
[0028] Meanwhile, the substrate is cleaned and dried to remove surface impurities and moisture, avoiding any impact on the bonding effect; the edge sealing prevents moisture intrusion and aerogel from absorbing moisture and failing, thus comprehensively improving the long-term stability of the product; each step is simple to operate and does not require special high-end equipment. Steps such as hot pressing and gluing can be automated and continuous, resulting in high production efficiency and product qualification rate, which can meet the needs of large-scale markets.
[0029] Furthermore, the hot pressing temperature is 150℃, the pressure is 0.3MPa, the time is 50-200s, and the ultraviolet light is 254nm and 300W.
[0030] Specifically, 150℃ is the optimal melting temperature for PVB resin, which allows PVB to melt completely, ensuring a tight bond with the modified aerogel and glass fiber fabric, while preventing the aerogel's pore structure from being damaged or the PVB from being degraded due to excessive temperature; a pressure of 0.3MPa ensures uniform density of the composite insulation layer, avoiding pores and defects, while also preventing the aerogel's porous structure from being crushed.
[0031] 254nm is the optimal absorption wavelength for the crosslinking agent (trimethylolpropane triacrylate). A power of 300W can quickly initiate the crosslinking reaction. The time range of 50-200s can be adapted to the reinforcing layer and core layer of different thicknesses (0.1-0.2mm), ensuring that the crosslinking reaction is sufficient and increasing the tensile strength of the composite insulation layer by more than 40%. Long-term use will not result in deformation or delamination.
[0032] Furthermore, the sealing and encapsulation method is as follows: a sealant with a thickness of 1-3 mm is applied to the edge of the glass substrate and cured at room temperature for 24 hours.
[0033] Specifically, a sealant thickness of 1-3mm can completely cover the edge gaps of the glass substrate, forming a continuous and dense sealing layer. This effectively blocks the intrusion of external moisture, dust, and other impurities, preventing the aerogel from absorbing moisture and causing pore structure damage, thus ensuring long-term stable thermal insulation performance. The sealant cures at room temperature for 24 hours, a gentle curing process that will not cause deformation of the glass substrate or failure of the bonding between layers due to high-temperature curing. The cured sealant has good flexibility and weather resistance, preventing the sealing layer from cracking. Attached Figure Description
[0034] The invention will now be further described with reference to the accompanying drawings.
[0035] Figure 1 This is a schematic diagram of the structure of the heat-insulating glass in Embodiment 1 of the present invention. Detailed Implementation
[0036] The specific embodiments of the present invention will be described in detail below, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments.
[0037] The terminology used in the embodiments of this application is for the purpose of describing particular implementations only and is not intended to be limiting of this application. The singular forms “a,” “the,” and “the” used in the implementations of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.
[0038] It should be understood that in the various embodiments of this application, the sequence number of each process does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the implementation regulations of this application.
[0039] The weights of the relevant components mentioned in the embodiments of this application can refer not only to the specific content of each component, but also to the proportional relationship between the weights of the components. Therefore, any scaling up or down of the content of the relevant components according to the embodiments of this application is within the scope disclosed in the embodiments of this application. Specifically, the mass described in the embodiments of this application can be a mass unit known in the chemical industry, such as μg, mg, g, or kg.
[0040] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.
[0041] Unless otherwise specified, all raw materials, reagents, instruments, and equipment used in this application can be purchased commercially or prepared using existing methods. For example, the types and sources of raw materials involved in the following preparation examples and embodiments are as follows: Tetraethyl orthosilicate: analytical grade, purity ≥99.0%, purchased from Sinopharm Chemical Reagent Co., Ltd.; Polymethylvinyldimethoxysilane: purity ≥98.0%, purchased from Shanghai Maclean Biochemical Technology Co., Ltd.; Acid-base compound: a mixture of hydrochloric acid (36% by mass) and ammonia (28% by mass) in a volume ratio of 1:2. Both hydrochloric acid and ammonia are analytical grade and were purchased from Sinopharm Chemical Reagent Co., Ltd. Rutile TiO2: Particle size 20-50nm, purity ≥99.5%, purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. Hollow glass microspheres: particle size 10-50μm, density 0.38g / cm³ 3 Purchased from Qinhuangdao Tongfa Glass Microbeads Co., Ltd. Vinyltrimethoxysilane: purity ≥98.0%, purchased from Nanjing Shuguang Chemical Group Co., Ltd.; PVB resin: Model PVB-1799, viscosity 25-30 mPa s, acetal degree 78-80%, purchased from Anhui Wanwei High-Tech Materials Co., Ltd.; Silane coupling agent KH-550: purity ≥97.0%, purchased from Hubei Xinlantian New Materials Co., Ltd.; Carbon black: particle size 10-20nm, purchased from Tianjin Dolphin Carbon Black Co., Ltd. PEG-400: Analytical grade, purchased from Sinopharm Chemical Reagent Co., Ltd.; Nano ZnO: Particle size 10-30nm, purity ≥99.0%, purchased from Zhejiang Fenghong New Material Co., Ltd. Trimethylolpropane triacrylate: purity ≥98.0%, purchased from Guangzhou Shuangjian Chemical Co., Ltd.; Fiberglass fabric: plain weave, 0.1mm thickness, 10μm fiber diameter, purchased from Changzhou Hongfa Fiberglass Products Co., Ltd. Waterborne polyurethane adhesive: solid content 35%, tensile shear strength ≥3MPa, purchased from Shanghai Sirda Chemical Co., Ltd. Silicone sealant: Shore A hardness 25-35, purchased from Guangzhou Baiyun Chemical Industry Co., Ltd. Inner glass substrate 100 and outer glass substrate 500: Low-E glass substrate, 5mm thick, visible light transmittance ≥85%, infrared reflectance ≥80%, purchased from CNS Glass Group Co., Ltd. Ordinary aerogels: particle size 10-50 μm, thermal conductivity 0.020 W / (m²). K), purchased from Hebei Baoying Environmental Protection Technology Co., Ltd.
[0042] Preparation Example 1
[0043] The modified aerogel was prepared by following these steps in sequence: (1) In-situ modification: 50g of tetraethyl orthosilicate and 12g of polymethyl vinyl dimethoxysilane were added to the reactor and mixed evenly. Then, 0.5g of acid-base composite catalyst was added and stirred evenly. The mixture was reacted at 45°C for 2.5h to obtain wet gel. (2) Rutile TiO2 and hollow glass microspheres loading: 10g rutile TiO2 and 6g hollow glass microspheres were added to an ultrasonic machine and ultrasonically dispersed at a rate of 4000r / min for 35min. Then, the mixture was added to the wet gel in the reactor and stirred evenly. The mixture was kept at 50℃ for 24h to obtain aged wet gel. (3) Plasma surface modification: The aged wet gel was placed in a plasma treatment instrument and 4g of vinyltrimethoxysilane vapor was introduced (by heating vinyltrimethoxysilane to 90℃ to vaporize it into vapor, and using nitrogen as a carrier gas to introduce it into the plasma treatment instrument). It was treated at 110℃ and 0.2MPa for 45min, and then transferred to a drying oven. It was first dried at 60℃ and atmospheric pressure for 4h, and then dried at 120℃ and 7.9MPa for 7h to obtain modified aerogel.
[0044] Preparation Example 2
[0045] The modified aerogel was prepared by following these steps in sequence: (1) In-situ modification: 50g of tetraethyl orthosilicate and 10g of polymethyl vinyl dimethoxysilane were added to the reactor and mixed evenly. Then, 0.5g of acid-base composite catalyst was added and stirred evenly. The mixture was reacted at 45°C for 2.5h to obtain wet gel. (2) Rutile TiO2 and hollow glass microspheres loading: 8g rutile TiO2 and 5g hollow glass microspheres were added to the ultrasonic machine and ultrasonically dispersed at a rate of 4000r / min for 35min. Then, they were added to the wet gel in the reactor and stirred evenly. The mixture was kept at 50℃ for 24h to obtain aged wet gel. (3) Plasma surface modification: The aged wet gel was placed in a plasma treatment instrument and 3g of vinyltrimethoxysilane vapor was introduced (by heating vinyltrimethoxysilane to 90℃ to vaporize it into vapor, and using nitrogen as a carrier gas to introduce it into the plasma treatment instrument). It was treated at 110℃ and 0.2MPa for 45min, and then transferred to a drying oven. It was first dried at 60℃ and atmospheric pressure for 4h, and then dried at 120℃ and 7.9MPa for 7h to obtain modified aerogel.
[0046] Preparation Example 3
[0047] The modified aerogel was prepared by following these steps in sequence: (1) In-situ modification: 50g of tetraethyl orthosilicate and 15g of polymethyl vinyl dimethoxysilane were added to the reactor and mixed evenly. Then, 0.5g of acid-base composite catalyst was added and stirred evenly. The mixture was reacted at 45°C for 2.5h to obtain wet gel. (2) Rutile TiO2 and hollow glass microspheres loading: 12g rutile TiO2 and 8g hollow glass microspheres were added to an ultrasonic machine and ultrasonically dispersed at a rate of 4000r / min for 35min. Then, the mixture was added to the wet gel in the reactor and stirred evenly. The mixture was kept at 50℃ for 24h to obtain aged wet gel. (3) Plasma surface modification: The aged wet gel was placed in a plasma treatment instrument and 5g of vinyltrimethoxysilane vapor was introduced (by heating vinyltrimethoxysilane to 90℃ to vaporize it into vapor, and using nitrogen as a carrier gas to introduce it into the plasma treatment instrument). It was treated at 110℃ and 0.2MPa for 45min, and then transferred to a drying oven. It was first dried at 60℃ and atmospheric pressure for 4h, and then dried at 120℃ and 7.9MPa for 7h to obtain modified aerogel.
[0048] Example 1
[0049] This embodiment discloses a heat-insulating glass, which is prepared by the following steps: Step 1: According to the weight ratio, in a reactor, 50 parts of PVB resin were heated and melted at 140°C, then 40 parts of the modified aerogel prepared in Preparation Example 1, 4 parts of silane coupling agent KH-550, 3 parts of carbon black, 6 parts of PEG-400, 2 parts of nano-ZnO, and 1.2 parts of trimethylolpropane triacrylate were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous to obtain a sandwich. In another reactor, 50 parts of PVB resin were heated and melted at 140°C, then 13 parts of glass fiber fabric were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous, and then pressed into two 20cm sections at 130°C and 0.3 MPa. 10cm A 0.18mm reinforcing layer 302 is formed, and then the clamping material is placed between the two reinforcing layers 302. The material is placed in a mold and irradiated with ultraviolet light with a wavelength of 254nm and a power of 300W. The material is then hot-pressed at 150℃ and 0.5MPa for 70s to obtain a composite heat insulation layer 300 with a core layer 301 sandwiched between the two reinforcing layers 302. At this time, the thickness of the core layer 301 is 0.38mm. Step 2: Wash and dry the inner glass substrate 100 and the outer glass substrate 500. Step 3: Apply a water-based polyurethane adhesive with a thickness of 0.08 mm to the outer side of the two reinforcing layers 302 in the composite heat insulation layer 300, then attach the dried inner glass substrate 100 and outer glass substrate 500 respectively, place them in a laminator, and hot press them at 140℃ and 0.4MPa for 30 minutes to form a glass substrate. Step 4: Apply a 2mm thick layer of silicone sealant to the edge of the glass substrate and cure at room temperature for 24 hours to obtain the desired result. Figure 1 The heat-insulating glass shown.
[0050] Example 2
[0051] This embodiment discloses a heat-insulating glass, which is prepared by the following steps: Step 1: According to the weight ratio, in a reactor, 50 parts of PVB resin were heated and melted at 140°C, then 30 parts of the modified aerogel prepared in Preparation Example 1, 3 parts of silane coupling agent KH-550, 2 parts of carbon black, 5 parts of PEG-400, 1 part of nano-ZnO, and 1 part of trimethylolpropane triacrylate were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous to obtain a sandwich. In another reactor, 50 parts of PVB resin were heated and melted at 140°C, then 5 parts of glass fiber fabric were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous, and then pressed into two 20cm sections at 130°C and 0.3 MPa. 10cm A 0.17mm reinforcing layer 302 is formed, and then the clamping material is placed between the two reinforcing layers 302. The material is placed in a mold and irradiated with ultraviolet light with a wavelength of 254nm and a power of 300W. The material is then hot-pressed at 150℃ and 0.5MPa for 70s to obtain a composite heat insulation layer 300 with a core layer 301 sandwiched between the two reinforcing layers 302. At this time, the thickness of the core layer 301 is 0.36mm. Step 2: Wash and dry the inner glass substrate 100 and the outer glass substrate 500. Step 3: Apply a water-based polyurethane adhesive with a thickness of 0.08 mm to the outer side of the two reinforcing layers 302 in the composite heat insulation layer 300, then attach the dried inner glass substrate 100 and outer glass substrate 500 respectively, place them in a laminator, and hot press them at 140℃ and 0.4MPa for 30 minutes to form a glass substrate. Step 4: Apply a 2mm thick layer of silicone sealant to the edge of the glass substrate and cure at room temperature for 24 hours to obtain heat-insulating glass.
[0052] Example 3
[0053] This embodiment discloses a heat-insulating glass, which is prepared by the following steps: Step 1: According to the weight ratio, in a reactor, 50 parts of PVB resin were heated and melted at 140°C, then 50 parts of the modified aerogel prepared in Preparation Example 1, 5 parts of silane coupling agent KH-550, 4 parts of carbon black, 8 parts of PEG-400, 3 parts of nano ZnO, and 1.5 parts of trimethylolpropane triacrylate were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous to obtain a sandwich. In another reactor, 50 parts of PVB resin were heated and melted at 140°C, then 13 parts of glass fiber fabric were added. The mixture was dispersed at 3500 rpm for 30 minutes until homogeneous, and then pressed into two 20cm sections at 130°C and 0.3 MPa. 10cm A 0.20mm reinforcing layer 302 is formed, and then the clamping material is placed between the two reinforcing layers 302. The material is placed in a mold and irradiated with ultraviolet light with a wavelength of 254nm and a power of 300W. The material is then hot-pressed at 150℃ and 0.5MPa for 70s to obtain a composite heat insulation layer 300 with a core layer 301 sandwiched between the two reinforcing layers 302. At this time, the thickness of the core layer 301 is 0.41mm. Step 2: Wash and dry the inner glass substrate 100 and the outer glass substrate 500. Step 3: Apply a water-based polyurethane adhesive with a thickness of 0.08 mm to the outer side of the two reinforcing layers 302 in the composite heat insulation layer 300, then attach the dried inner glass substrate 100 and outer glass substrate 500 respectively, place them in a laminator, and hot press them at 140℃ and 0.4MPa for 30 minutes to form a glass substrate. Step 4: Apply a 2mm thick layer of silicone sealant to the edge of the glass substrate and cure at room temperature for 24 hours to obtain heat-insulating glass.
[0054] Example 4
[0055] Compared with Example 1, the only difference is that the modified aerogel of Preparation Example 1 is replaced with the modified aerogel of Preparation Example 2, while the other steps and methods remain the same, and heat-insulating glass is finally obtained.
[0056] Example 5
[0057] Compared with Example 1, the only difference is that the modified aerogel of Preparation Example 1 is replaced with the modified aerogel of Preparation Example 3, while the other steps and methods remain the same, and heat-insulating glass is finally obtained.
[0058] Comparative Example 1
[0059] Compared with Example 1, the only difference is that the modified aerogel in Example 1 is omitted, while the other steps and methods remain the same, and heat-insulating glass is finally obtained.
[0060] Comparative Example 2
[0061] Compared with Example 1, the only difference is that the modified aerogel in Preparation Example 1 is replaced with commercially available ordinary aerogel, while the other steps and methods remain the same, and heat-insulating glass is finally obtained.
[0062] The performance of the heat-insulating glass in Examples 1-5 and Comparative Examples 1-2 was tested. The specific test items and methods are as follows: Thermal conductivity: Refer to GB / T 10294-2008; Visible light transmittance: Refer to GB / T 2680-2021; Bending strength: Refer to GB / T 9962-1999; Impact resistance (drop ball impact): Refer to GB / T 9962-2022.
[0063] The test results are listed in Table 1, as follows: Table 1
[0064] Analysis of the data in Table 1 shows that, compared with Comparative Examples 1-2, the thermal conductivity of the heat-insulating glass in Examples 1-5 is significantly lower, the visible light transmittance is not much different, and the bending strength and impact resistance are significantly better. This indicates that the heat-insulating glass of the present invention is superior in both heat insulation performance and mechanical properties.
[0065] The foregoing has described several embodiments of the present invention in detail, but these descriptions are merely preferred embodiments and should not be construed as limiting the scope of the invention. All equivalent variations and modifications made within the scope of the claims of this invention should still fall within the patent coverage of this invention.
Claims
1. A type of heat-insulating glass, characterized in that, It includes an inner glass substrate (100), a first adhesive layer (200), a composite heat insulation layer (300), a second adhesive layer (400), and an outer glass substrate (500) stacked in sequence; the composite heat insulation layer (300) includes a core layer (301) and reinforcing layers (302) located on both sides of the core layer. The composite insulation layer (300) comprises the following components by weight: The core layer (301) comprises 50 parts of PVB resin, 30-50 parts of modified aerogel, 3-5 parts of silane coupling agent, 2-4 parts of carbon black, 5-8 parts of polyethylene glycol, 1-3 parts of nano ZnO, and 1-1.5 parts of crosslinking agent. The two reinforcing layers (302) comprise 50 parts of PVB resin and 10-16 parts of glass fiber fabric; The modified aerogel is obtained by using silica aerogel as a matrix, followed by in-situ modification with an elastic polymer, loading with rutile TiO2 and hollow glass microspheres, and plasma surface modification.
2. The heat-insulating glass according to claim 1, characterized in that, The preparation method of the modified aerogel includes the following steps: (1) In-situ modification: Tetraethyl orthosilicate is mixed with polymethyl vinyl dimethoxysilane, an acid-base composite catalyst is added, and the mixture is reacted at 40-50℃ for 2-3 hours to obtain a wet gel; (2) Rutile TiO2 and hollow glass microspheres loading: Rutile TiO2 and hollow glass microspheres were mixed and ultrasonically dispersed for 30-40 min, added to wet gel and stirred evenly, and kept at 50℃ for 24 h to obtain aged wet gel. (3) Plasma surface modification: The aged wet gel was placed in a plasma treatment instrument, and vinyltrimethoxysilane vapor was introduced. It was treated at 100-120℃ and 0.1-0.3MPa for 30-60 min. After gradient drying, the modified aerogel was obtained. The mass ratio of tetraethyl orthosilicate, polymethylvinyl dimethoxysilane, rutile TiO2, hollow glass microspheres, and vinyltrimethoxysilane is 50:(10-15):(8-12):(5-8):(3-5).
3. The heat-insulating glass according to claim 2, characterized in that, In step (1), the acid-base composite catalyst is a mixture of hydrochloric acid and ammonia water in a volume ratio of 1:
2.
4. The heat-insulating glass according to claim 2, characterized in that, In step (1), the amount of the acid-base composite catalyst added is 0.5-1% of the total mass of tetraethyl orthosilicate and polymethylvinyl dimethoxysilane.
5. The heat-insulating glass according to claim 2, characterized in that, In step (3), the gradient drying method is as follows: first, dry at 60℃ and normal pressure for 4 hours, and then dry at 120℃ and 7.9MPa for 6-8 hours.
6. The heat-insulating glass according to claim 1, characterized in that, Both the inner glass substrate (100) and the outer glass substrate (500) are Low-E glass.
7. The heat-insulating glass according to claim 1, characterized in that, Both the first adhesive layer (200) and the second adhesive layer (400) are water-based polyurethane adhesives.
8. A preparation method for preparing the heat-insulating glass as described in any one of claims 1-7, characterized in that, Includes the following steps: Step 1: According to the weight ratio of the core layer (301), heat and melt the PVB resin, then add modified aerogel, silane coupling agent, carbon black, polyethylene glycol, nano ZnO, and crosslinking agent and disperse evenly to obtain the sandwich material; according to the weight ratio of the reinforcing layer (302), heat and melt the PVB resin, then add glass fiber fabric and disperse evenly to press into two reinforcing layers (302) of the same size, then place the sandwich material between the two reinforcing layers (302) and hot press it under ultraviolet light to obtain a composite heat insulation layer (300) with the core layer (301) sandwiched between the two reinforcing layers (302). Step 2: Wash and dry the inner glass substrate (100) and the outer glass substrate (500); Step 3: Apply adhesive to the outside of the two reinforcing layers (302) in the composite heat insulation layer (300), and then attach the dried inner glass substrate (100) and outer glass substrate (500) respectively. Hot press to form a glass substrate. Step 4: Seal and encapsulate the edges of the glass substrate to obtain heat-insulating glass.
9. The preparation method according to claim 8, characterized in that, In step 1, the hot pressing temperature is 150℃, the pressure is 0.3MPa, the time is 50-200s, and the ultraviolet light is 254nm and 300W.
10. The preparation method according to claim 8, characterized in that, In step 4, the sealing and encapsulation method is as follows: apply a sealant with a thickness of 1-3 mm to the edge of the glass substrate and cure it at room temperature for 24 hours.