Thermal and acoustic insulation pvc interlayer and method for its production
By mixing modified nanocellulose and additives and processing them, the heat insulation and aging resistance problems of PVB interlayer were solved, and the multi-functional performance of high-strength architectural glass was improved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-16
- Publication Date
- 2026-04-14
AI Technical Summary
Existing PVB interlayer films have insufficient thermal insulation performance and poor aging resistance in the field of high-strength architectural glass. They cannot meet the stringent thermal insulation requirements and are prone to aging in complex environments, affecting the optical performance and structural stability of the glass.
By mixing PVB resin with additives such as modified nanocellulose, modified lanthanum hexaboride, composite light stabilizer and modified cerium oxide, and combining it with casting molding and hot pressing, a multi-layer functional structure is formed, which enhances the heat insulation, sound insulation and aging resistance properties.
It significantly improves the thermal insulation and aging resistance of PVB interlayer, ensuring that its performance does not degrade during long-term use, and enhances the sound insulation and structural stability of architectural glass.
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Figure CN120399292B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of composite material technology, specifically to a heat-insulating and sound-insulating PVB interlayer and its preparation method. Background Technology
[0002] PVB interlayer, as a key non-metallic additive material, plays a vital role in the construction industry, especially in the application of high-strength architectural glass. Its main component, polyvinyl butyral resin, exhibits numerous superior properties due to its unique chemical structure, such as excellent adhesion to glass, high transparency, and outstanding toughness and weather resistance. Since its introduction, PVB interlayer has continuously evolved. As the construction industry's requirements for glass safety, energy efficiency, and sound insulation have gradually increased, its application scope has continued to expand, making it one of the core materials for ensuring the quality and performance of architectural glass. From initially primarily meeting basic safety needs to now accommodating multiple functional requirements in complex building environments, the importance of PVB interlayer in the architectural glass market is becoming increasingly prominent.
[0003] Currently, the insufficient thermal insulation and aging resistance of PVB interlayers have become bottlenecks restricting their further development in the field of high-strength architectural glass. Regarding thermal insulation, with the continuous upgrading of global building energy efficiency standards, existing PVB interlayers, relying solely on their material properties, are insufficient to meet stringent insulation requirements. Their limited ability to block heat transfer leads to buildings consuming more energy for cooling in summer. As for aging resistance, PVB interlayers are exposed to complex environments such as ultraviolet radiation and alternating high and low temperatures for extended periods. Their antioxidant systems are unable to resist environmental erosion, causing the interlayer to yellow and become brittle, affecting not only the optical properties of the glass but also its structural stability and shortening its service life. Breakthroughs in performance through material innovation and process optimization are urgently needed.
[0004] Therefore, a heat-insulating and sound-insulating PVB interlayer film and its preparation method are proposed. Summary of the Invention
[0005] The purpose of this invention is to design a heat-insulating and sound-insulating PVB interlayer and its preparation method. This invention involves pre-plasticizing PVB resin and shear-mixing it with silane coupling agent-modified reinforced nanocellulose, then sequentially adding plasticizers, molybdenum trioxide-loaded lanthanum hexaboride, composite light stabilizers, modified cerium oxide, and other additives. The resulting PVB interlayer is prepared through casting and hot-pressing. Specifically, modified lanthanum hexaboride enhances infrared shielding, and the composite light stabilizer and modified cerium oxide synergistically improve aging resistance. Through material synergy and process coordination, the PVB interlayer achieves a comprehensive improvement in heat insulation, sound insulation, and aging resistance, making it suitable for high-strength architectural glass applications.
[0006] To achieve the above objectives, the present invention provides the following technical solution:
[0007] This invention provides a method for preparing a heat-insulating and sound-insulating PVB interlayer film, the method comprising the following steps:
[0008] PVB resin was pre-plasticized and then shear-mixed with reinforced nanocellulose to obtain a preliminary mixture; the reinforced nanocellulose was obtained by modifying nanocellulose with a silane coupling agent.
[0009] Plasticizer, modified lanthanum hexaboride, composite light stabilizer, modified cerium oxide, composite nanofiller, and composite antioxidant were added sequentially to the initial mixture, and the mixture was stirred to obtain a final mixture. Modified lanthanum hexaboride was obtained by loading lanthanum hexaboride with molybdenum trioxide. Modified cerium oxide was obtained by grafting cerium oxide with an ultraviolet absorber.
[0010] The mixture is cooled after being cast and hot-pressed to obtain a PVB interlayer film.
[0011] Preferably, the preparation method of reinforced nanocellulose by weight is as follows: 90-100 parts of nanocellulose are slowly added to 600 parts of anhydrous ethanol, and a suspension is obtained after stirring for 45 min; under continuous stirring, 1-5 parts of silane coupling agent KH550 are slowly added dropwise to the suspension at a dropping rate of 1 mL / min, and then stirring is continued for 15 min to obtain a mixed solution; the mixed solution is transferred to a three-necked flask, and the temperature is raised to 70℃ under a nitrogen protective atmosphere, and the reaction is continuously stirred at this temperature for 2-4 h. After the reaction is completed, the nanocellulose is centrifuged, washed, and vacuum dried to obtain reinforced nanocellulose; the average diameter of the nanocellulose is 10-50 nm and the length is 0.5-5 μm.
[0012] Preferably, the preparation method of the initial mixture by weight is as follows: 95-105 parts of PVB resin are put into a twin-screw extruder, the temperature is set to 100℃, the screw speed is 180 rpm, and the preplasticization time is 12 min to obtain preplasticized PVB; 5-10 parts of reinforcing nanocellulose are added to the preplasticized PVB, the speed is increased to 350 rpm, the temperature is 120℃-140℃, and the mixing time is 18 min to obtain the initial mixture.
[0013] Preferably, the modified lanthanum hexaboride is prepared by the following method by weight: 45-55 parts of lanthanum hexaboride are added to 100 parts of anhydrous ethanol and stirred until a suspension is formed; 3 parts of polyvinylpyrrolidone are added to the suspension and stirred for 30 min to obtain a homogeneous solution; 5-10 parts of molybdenum trioxide are slowly added to the homogeneous solution and stirred for 1.5 h to obtain a mixed solution; the mixed solution is transferred to a reaction vessel, the pressure is controlled at 0.5-1.0 MPa, and the temperature is raised to 180℃ for 3-5 h; after the reaction is completed, the mixture is cooled to room temperature, filtered, washed, and vacuum dried to obtain modified lanthanum hexaboride.
[0014] Preferably, the modified cerium oxide is prepared by means of the following method: 5-15 parts of cerium oxide are placed in a high-temperature furnace and calcined at 450°C for 2.5 h. After cooling, pretreated cerium oxide is obtained. The pretreated cerium oxide is added to 30 parts of toluene and ultrasonically dispersed for 45 min to obtain a dispersion. 1-2 parts of ultraviolet absorber UV-326 are added to 10 parts of toluene, stirred and heated to 55°C to obtain an ultraviolet absorber solution. 0.2 parts of KH550 are added to the ultraviolet absorber solution and stirred for 30 min to obtain a mixture. The dispersion is slowly added to the mixture, and the mixture is reacted at 80°C-100°C for 7 h under stirring conditions. After the reaction is completed, the mixture is filtered, washed, and vacuum dried to obtain modified cerium oxide.
[0015] Preferably, the mixture is prepared by the following method by weight: 25 parts of plasticizer diisobutyl phthalate, 3-8 parts of modified lanthanum hexaboride, 2-5 parts of composite light stabilizer, 2-4 parts of modified cerium oxide, 5-10 parts of composite nanofiller and 1.5 parts of composite antioxidant are added to the initial mixture in sequence, and the mixture is stirred and mixed in a high-speed mixer at a stirring speed of 1000 rpm, a mixing temperature of 90℃ and a mixing time of 25 min to obtain the mixture.
[0016] Preferably, the casting and hot pressing process is as follows: the mixture is conveyed to the casting equipment, the mold temperature is set to 150°C, and casting is performed through the periodic shrinkage-expansion channel in the mold (shrinkage ratio 1:3). The casting speed is controlled at 0.5m / min-1.0m / min to obtain a film blank with a thickness of 0.3mm-0.8mm. The film blank is transferred to a hot press for hot pressing treatment, the hot pressing temperature is set to 120°C-140°C, the pressure is 3MPa-5MPa, the hot pressing time is 10min-15min, and it is allowed to cool naturally to obtain a PVB intermediate film.
[0017] Preferably, the composite light stabilizer is composed of boron nitride quantum dots and light stabilizer HALS-770, with a weight ratio of boron nitride quantum dots to light stabilizer HALS-770 of 1:1-3; the composite antioxidant includes antioxidant 1010 and antioxidant 168, with a weight ratio of antioxidant 1010 to antioxidant 168 of 1-3:1.
[0018] Preferably, the composite nanofiller includes nano-montmorillonite and carbon black, with a weight ratio of nano-montmorillonite to carbon black of 3-5:1.
[0019] Another aspect of the present invention provides a heat-insulating and sound-insulating PVB interlayer film, which includes PVB resin, reinforced nanocellulose, plasticizer, modified lanthanum hexaboride, composite light stabilizer, modified cerium oxide, composite nanofiller and composite antioxidant.
[0020] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0021] 1. The pre-plasticizing process gives PVB resin suitable fluidity, which facilitates thorough mixing with reinforcing nanocellulose. The silane coupling agent forms chemical bonds at the interface between the two, enhancing compatibility. It significantly improves the structural density of the PVB interlayer, forming a "maze structure" for sound wave propagation. Through multiple reflections and scattering, sound energy is consumed, greatly improving sound insulation performance. On the other hand, the dense structure effectively hinders heat conduction. Combined with the low thermal conductivity of nanocellulose itself, it reduces the thermal conductivity of the membrane, synergistically enhancing the heat insulation effect.
[0022] 2. Modified lanthanum hexaboride utilizes its unique electronic structure to shield infrared radiation, while the composite nanofiller forms a multi-level structure to regulate the direction of heat conduction. The two complement each other in terms of thermal insulation. Modified lanthanum hexaboride enhances the infrared shielding rate, reducing heat radiation transmission; the composite nanofiller, by forming a thermally anisotropic structure, inhibits heat transfer along the thickness direction, thereby increasing the reflectivity of sunlight across the entire wavelength range and significantly enhancing thermal insulation performance. Simultaneously, the dense structure formed by the composite nanofiller also contributes to improved sound insulation performance.
[0023] 3. Modified cerium oxide, through grafted UV-326, efficiently absorbs ultraviolet light, converting light energy into other forms of energy and reducing the damage of ultraviolet rays to the PVB interlayer. The boron nitride quantum dots in the composite light stabilizer utilize their high specific surface area to uniformly disperse and continuously release the light stabilizer, capturing free radicals generated by light exposure and preventing chain degradation reactions initiated by free radicals. The composite antioxidant targets oxidation reactions, capturing oxidative free radicals and peroxides generated at different stages, interrupting the oxidative aging pathway. The three work synergistically to block the aging process of the PVB interlayer, ensuring that its thermal insulation and sound insulation properties do not degrade during long-term use.
[0024] 4. The shear force generated by the periodic shrinkage-expansion flow channels in the casting mold promotes the gradient distribution of additives in the PVB resin, constructing a multi-layered functional structure and laying the foundation for improved performance of the PVB interlayer. The surface layer's carbon black enrichment enhances electromagnetic shielding, the core layer's nano-montmorillonite orientation improves mechanical strength, and the dense structure enhances sound insulation performance. Hot pressing works closely with other processes in this process. On one hand, by applying temperature and pressure, it strengthens the interfacial bonding between the PVB resin and additives, ensuring a firm bond between the functional layers, preventing delamination, and guaranteeing structural stability. On the other hand, hot pressing removes internal air bubbles, further densifying the material structure, reducing sound transmission channels, and enhancing sound insulation. Attached Figure Description
[0025] Figure 1 The diagram shows the thermal insulation performance of Example 6 and Comparative Examples 4-8 in this invention. Detailed Implementation
[0026] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0027] For details, please refer to [link / reference]. Figure 1 This invention provides a heat-insulating and sound-insulating PVB interlayer film and its preparation method, the technical solution of which is as follows:
[0028] Example 1
[0029] 95 parts of nanocellulose were slowly added to 600 parts of anhydrous ethanol and stirred for 45 min to obtain a suspension. Under continuous stirring, 3 parts of silane coupling agent KH550 were slowly added dropwise to the suspension at a rate of 1 mL / min. The mixture was then stirred for 15 min to obtain a mixed solution. The mixed solution was transferred to a three-necked flask and heated to 70 °C under a nitrogen atmosphere. The mixture was stirred and reacted at this temperature for 3 h. After the reaction was completed, the mixture was centrifuged, washed, and vacuum dried to obtain reinforced nanocellulose.
[0030] 50 parts of lanthanum hexaboride were added to 100 parts of anhydrous ethanol and stirred until a suspension was formed. 3 parts of polyvinylpyrrolidone were added to the suspension and stirred for another 30 minutes to obtain a homogeneous solution. 8 parts of molybdenum trioxide were slowly added to the homogeneous solution and stirred for 1.5 hours to obtain a mixed solution. The mixed solution was transferred to a reaction vessel, and the pressure was controlled within the range of 0.5-1.0 MPa. The temperature was raised to 180℃ and the reaction was carried out for 4 hours. After the reaction was completed, the mixture was cooled to room temperature, filtered, washed, and vacuum dried to obtain modified lanthanum hexaboride.
[0031] Ten parts of cerium oxide were placed in a high-temperature furnace and calcined at 450°C for 2.5 h. After cooling, pretreated cerium oxide was obtained. The pretreated cerium oxide was added to 30 parts of toluene and ultrasonically dispersed for 45 min to obtain a dispersion. 1.5 parts of UV absorber UV-326 were added to 10 parts of toluene, stirred, and heated to 55°C to obtain a UV absorber solution. 0.2 parts of KH550 were added to the UV absorber solution and stirred for 30 min to obtain a mixture. The dispersion was slowly added to the mixture, and the mixture was reacted at 90°C for 7 h under stirring. After the reaction was completed, the mixture was filtered, washed, and vacuum dried to obtain modified cerium oxide.
[0032] The composite light stabilizer consists of boron nitride quantum dots and light stabilizer HALS-770, with a weight ratio of 1:2. The composite antioxidant includes antioxidant 1010 and antioxidant 168, with a weight ratio of 2:1. The composite nanofiller includes nano-montmorillonite and carbon black, with a weight ratio of 4:1.
[0033] 100 parts of PVB resin were fed into a twin-screw extruder, the temperature was set to 100℃, the screw speed was set to 180 rpm, and the preplasticization time was set to 12 min to obtain preplasticized PVB; 8 parts of reinforcing nanocellulose were added to the preplasticized PVB, the speed was increased to 350 rpm, the temperature was set to 130℃, and the mixing time was set to 18 min to obtain the initial mixture.
[0034] 25 parts of plasticizer diisobutyl phthalate, 5 parts of modified lanthanum hexaboride, 4 parts of composite light stabilizer, 3 parts of modified cerium oxide, 8 parts of composite nanofiller and 1.5 parts of composite antioxidant were added to the initial mixture in sequence and stirred in a high-speed mixer at a stirring speed of 1000 rpm, a mixing temperature of 90℃ and a mixing time of 25 min to obtain the mixture.
[0035] The mixture is fed to a casting molding equipment, the mold temperature is set to 150℃, the casting speed is controlled to 0.8m / min, and a film preform with a thickness of 0.5mm is obtained. The film preform is then transferred to a hot press for hot pressing treatment, the hot pressing temperature is set to 130℃, the pressure is 4MPa, the hot pressing time is 12min, and it is allowed to cool naturally to obtain a PVB intermediate film.
[0036] Examples 2-5 refer to the parameter conditions in Example 1, with specific differences shown in Table 1.
[0037] Table 1 Parameters and Conditions for Examples 1-5
[0038]
[0039] Comparative Example 1 follows the same parameters and conditions as in Example 1, except that the nanocellulose is not modified with a silane coupling agent.
[0040] Comparative Example 2 follows the same parameters and conditions as in Example 1, except that no reinforcing nanocellulose is added.
[0041] Comparative Example 3 follows the same parameters and conditions as in Example 1, except that the PVB resin is not pre-plasticized.
[0042] Experiment Example 1: Sound Insulation and Thermal Stability Performance Test
[0043] The sound insulation performance of Examples 1-5 and Comparative Examples 1-3 was tested according to GB / T 8485-2008 standard. The glass structure was 2mm glass + PVB interlayer + 2mm glass. Square specimens of 100mm × 100mm were cut from Examples 1-5 and Comparative Examples 1-3. The specimens were placed in a 60℃ oven for 15 minutes, removed, cooled, and the side length was measured. The calculation formula was: heat shrinkage rate (%) = (100mm - side length after testing) / 100mm × 100%. The results are shown in Table 2.
[0044] Table 2 Sound insulation and thermal stability performance of Examples 1-5 and Comparative Examples 1-3
[0045]
[0046]
[0047] Table 2 shows that the examples exhibit good sound insulation and heat insulation performance. In Comparative Example 1, the nanocellulose was not modified with a silane coupling agent, resulting in insufficient bonding between the nanocellulose and PVB resin. This leads to an imperfect internal structure, making it difficult to effectively dissipate sound energy through the interaction between the nanocellulose and resin interfaces during sound propagation, thus reducing sound insulation. Furthermore, when heated, the nanocellulose cannot effectively restrict the movement of PVB resin molecular chains, making them more prone to thermal motion and shrinkage, resulting in a relatively high thermal shrinkage rate. In Comparative Example 2, no reinforcing nanocellulose was added, and the material lost the skeletal support of nanocellulose, resulting in a looser internal structure. This reduces the obstacles encountered by sound during propagation, allowing it to easily penetrate the material and significantly reducing sound insulation. In Comparative Example 3, the lack of pre-plasticization of PVB resin makes it difficult for PVB resin to be evenly dispersed when mixed with other additives. This leads to uneven distribution of components within the material, forming localized weak areas, affecting the uniform propagation of sound and energy dissipation within the material, resulting in unstable and reduced sound insulation performance. When heated, the unplasticized PVB resin molecular chains, due to their initially disordered state, are more prone to irregular thermal motion and shrinkage, leading to increased thermal shrinkage and reduced thermal stability of the material.
[0048] In summary, the modification of nanocellulose, the addition of reinforcing nanocellulose, and the preplasticization of PVB resin work synergistically throughout the process. The modification and reinforcement of nanocellulose together optimize the internal structure of the material, improving its density and stability, thus enhancing sound insulation performance and reducing thermal shrinkage. The preplasticization of PVB resin ensures that nanocellulose and other additives are evenly distributed within the resin, fully utilizing their functions to further improve sound insulation performance and reduce thermal shrinkage, ultimately achieving excellent sound insulation and thermal stability performance in the PVB interlayer.
[0049] Example 6 uses the same parameters as Example 1.
[0050] Examples 7-8 refer to the parameter conditions in Example 6, with specific differences shown in Table 3.
[0051] Table 3 Parameters and Conditions for Examples 6-8
[0052]
[0053] Comparative Example 4 follows the same parameters and conditions as in Example 6, except that lanthanum hexaboride is not loaded with molybdenum trioxide.
[0054] Comparative Example 5 follows the same parameters and conditions as in Example 6, except that modified lanthanum hexaboride is not added.
[0055] Comparative Example 6 follows the same parameters and conditions as in Example 6, except that only nano-montmorillonite is added as a nanofiller.
[0056] Comparative Example 7 follows the same parameters and conditions as in Example 6, except that only carbon black is added as a nanofiller.
[0057] Comparative Example 8 follows the same parameters and conditions as in Example 6, except that no composite nanofiller is added.
[0058] Experiment Example 2: Thermal Insulation Performance Test
[0059] The thermal insulation performance of Examples 6-8 and Comparative Examples 4-8 was tested according to GB / T 2680-2021, and the results are shown in Table 4. The thermal insulation performance of Examples 6 and Comparative Examples 4-8 is as follows: Figure 1 As shown.
[0060] Table 4 Thermal insulation performance of Examples 6-8 and Comparative Examples 4-8
[0061] Example Infrared blocking rate / % UV blocking rate / % Example 6 98.5 99.1 Example 7 98.3 99.0 Example 8 98.2 98.8 Comparative Example 4 93.1 94.8 Comparative Example 5 85.7 90.5 Comparative Example 6 91.6 94.6 Comparative Example 7 91.2 94.3 Comparative Example 8 88.6 90.1
[0062] From Table 4 and Figure 1It can be observed that the thermal insulation performance of the embodiments is better. Comparative Example 4, by not loading lanthanum hexaboride with molybdenum trioxide, affects its crystal structure and surface properties, preventing it from fully utilizing its absorption and scattering capabilities for infrared and ultraviolet light. The modification process alters the band structure of lanthanum hexaboride, making it more conducive to absorbing light of specific wavelengths. Without modification, this optimization cannot be achieved, leading to a decrease in infrared and ultraviolet blocking efficiency. Comparative Example 5, by not adding modified lanthanum hexaboride, lacks the strong absorption capabilities of lanthanum hexaboride in the infrared and ultraviolet regions. Lanthanum hexaboride possesses a unique electronic structure and optical properties, providing excellent blocking effects for infrared and ultraviolet light; its absence significantly reduces the overall thermal insulation performance of the material. While the nano-montmorillonite in Comparative Example 6 possesses a certain layered structure and blocking properties, its absorption and scattering mechanisms for infrared and ultraviolet light differ from those of modified lanthanum hexaboride. Using nano-montmorillonite alone cannot achieve efficient blocking across multiple wavelength ranges like composite nanofillers; its interlayer structure has limited light blocking effect, especially in the infrared region. The carbon black in Comparative Example 7 primarily exhibits strong absorption of visible light, while its absorption capacity in the infrared and ultraviolet bands is relatively weak. The particle size and surface properties of carbon black determine its light absorption characteristics. In terms of heat insulation, it cannot effectively block infrared and ultraviolet light like modified lanthanum hexaboride, resulting in low infrared and ultraviolet blocking rates. Comparative Example 8, without the addition of composite nanofillers, shows poor blocking effects for infrared and ultraviolet light, failing to meet the requirements for high-efficiency heat insulation.
[0063] In summary, modified lanthanum hexaboride and composite nanofillers exhibit synergistic effects. After modification with molybdenum trioxide, modified lanthanum hexaboride possesses strong absorption and scattering capabilities in the infrared and ultraviolet bands, making it the primary heat-insulating component. The layered structure of nano-montmorillonite further hinders light propagation, increasing light scattering and reflection within the material. Synergistically, it enhances the blocking effect against infrared and ultraviolet light in conjunction with modified lanthanum hexaboride. While carbon black has relatively weaker blocking capabilities against infrared and ultraviolet light, it can absorb some visible light and a small amount of infrared light. Combined with the other two fillers, it achieves more comprehensive blocking across the entire light spectrum.
[0064] Example 9 uses the same parameters and conditions as Example 1.
[0065] Examples 10-11 refer to the parameter conditions in Example 9, with specific differences shown in Table 5.
[0066] Table 5 Parameters and Conditions for Examples 9-11
[0067]
[0068] Comparative Example 9 follows the same parameters and conditions as in Example 9, except that cerium oxide is not modified.
[0069] Comparative Example 10 follows the same parameters and conditions as in Example 9, except that modified cerium oxide is not added.
[0070] Comparative Example 11 follows the same parameters and conditions as in Example 9, except that only boron nitride quantum dots are added as a light stabilizer.
[0071] Comparative Example 12 follows the same parameters and conditions as in Example 9, except that only HALS-770 is added as a light stabilizer.
[0072] Comparative Example 13 follows the same parameters and conditions as in Example 9, except that no composite light stabilizer is added.
[0073] Comparative Example 14 follows the same parameters and conditions as in Example 9, except that only antioxidant 1010 is added as an antioxidant.
[0074] Comparative Example 15 follows the same parameters and conditions as in Example 9, except that only antioxidant 168 is added as an antioxidant.
[0075] Comparative Example 16 follows the same parameters and conditions as in Example 9, except that no composite antioxidant is added.
[0076] Experiment Example 3: Thermal Insulation and Aging Resistance Test
[0077] The UV blocking rates of Examples 9-11 and Comparative Examples 9-16 were tested using the test method of Experimental Example 2; and the conventional heat resistance and radiation resistance tests were performed on Examples 9-11 and Comparative Examples 9-16. The results are shown in Table 6.
[0078] Table 6 Thermal insulation and aging resistance of Examples 9-11 and Comparative Examples 9-16
[0079]
[0080]
[0081] Table 6 shows that the examples exhibit better heat insulation and aging resistance. Comparative Example 9, without cerium oxide modification, suffers from reduced compatibility with the PVB interlayer system and compromised photostability, leading to a decrease in UV blocking efficiency. Regarding heat resistance and radiation resistance, the modified cerium oxide provides better protection against external factors damaging the PVB interlayer, while the unmodified version is more susceptible to performance changes under heat and radiation. Comparative Example 10, without modified cerium oxide, lacks its role in UV absorption and photostability, resulting in a significant decrease in UV blocking efficiency. Furthermore, without the synergistic effect of cerium oxide, the PVB interlayer lacks effective protection during heat and radiation resistance, leading to more pronounced performance changes. Comparative Examples 11-12, which only added boron nitride quantum dots or HALS-770 as photostability stabilizers, while possessing some photostability, do not achieve the same synergistic effect as composite photostability stabilizers. Therefore, their UV blocking, heat resistance, and radiation resistance are slightly inferior to the examples. Comparative Example 13, without the addition of a composite light stabilizer, has an incomplete light stabilization system, failing to effectively inhibit various light-induced degradation reactions. This results in a decrease in UV blocking rate, significantly worse heat resistance and radiation resistance, and the interlayer is more susceptible to damage from light and heat. Comparative Examples 14-15 use only single antioxidants. While antioxidants 1010 and 168 can capture free radicals and provide some antioxidant protection, composite antioxidants are typically a combination of multiple antioxidants that exert their antioxidant effects at different stages and through different mechanisms. Using them alone cannot comprehensively and effectively improve heat resistance and radiation resistance like a composite antioxidant. Comparative Example 16, without the addition of a composite antioxidant, shows that the PVB interlayer is prone to oxidation during heating and irradiation, leading to performance degradation, affected UV blocking rate, and significantly worse heat resistance and radiation resistance. Without the protection of antioxidants, the molecular structure of the interlayer is more easily damaged.
[0082] In summary, there is a synergistic effect among modified cerium oxide, the composite light stabilizer, and the composite antioxidant. Modified cerium oxide effectively absorbs ultraviolet light, improving the ultraviolet blocking rate, while also providing physical shielding and stabilization in terms of heat resistance and radiation resistance. Different components in the composite light stabilizer, such as boron nitride quantum dots and HALS-770, work synergistically with modified cerium oxide to leverage their respective advantages in light stabilization, inhibiting photodegradation reactions from different angles and improving the photoaging resistance of the PVB interlayer. The composite antioxidants, specifically antioxidants 1010 and 168, inhibit oxidation reactions at different stages and through different mechanisms. Synergistically with the light stabilizer and modified cerium oxide, they jointly improve the stability of the PVB interlayer during heat and radiation resistance processes, reducing performance changes. This results in the PVB interlayer exhibiting superior overall performance in terms of ultraviolet blocking, heat resistance, and radiation resistance.
[0083] Example 12 has the same parameters and conditions as Example 1.
[0084] Examples 13-14 refer to the parameter conditions in Example 12, with specific differences shown in Table 7.
[0085] Table 7 Parameters and Conditions for Examples 12-14
[0086]
[0087] Comparative Example 2 follows the same parameters and conditions as in Example 1, except that no reinforcing nanocellulose is added.
[0088] Comparative Example 6 follows the same parameters and conditions as in Example 6, except that only nano-montmorillonite is added as a nanofiller.
[0089] Comparative Example 7 follows the same parameters and conditions as in Example 6, except that only carbon black is added as a nanofiller.
[0090] Comparative Example 8 follows the same parameters and conditions as in Example 6, except that no composite nanofiller is added.
[0091] Comparative Example 17 uses the same parameters and conditions as in Example 12, except that the shrinkage ratio in the casting process is 1:1.
[0092] Comparative Example 18 follows the same parameters and conditions as in Example 12, except that hot pressing is not performed.
[0093] Experiment Example 4: Mechanical Properties and Sound Insulation Performance Tests
[0094] The mechanical properties of Examples 12-14, Comparative Examples 2, Comparative Examples 6-8, and Comparative Examples 17-18 were tested according to GB / T 1040.3-2006 standard; the sound insulation properties of Examples 12-14, Comparative Examples 2, Comparative Examples 6-8, and Comparative Examples 17-18 were tested according to the test method of Experimental Example 1. The results are shown in Table 8.
[0095] Table 8 Mechanical and sound insulation properties of Examples 12-14, Comparative Examples 2, Comparative Examples 6-8 and Comparative Examples 17-18
[0096] Example Tensile strength / MPa Elongation at break / % Sound insulation / dB Example 12 45 344 43 Example 13 42 341 41 Example 14 44 340 41 Comparative Example 2 32 254 34 Comparative Example 6 38 308 37 Comparative Example 7 35 285 36 Comparative Example 8 30 257 33 Comparative Example 17 36 311 38 Comparative Example 18 32 278 35
[0097] Table 8 shows that the mechanical and sound insulation properties of the examples are relatively good. In Comparative Example 2, no reinforcing nanocellulose was added. Since reinforcing nanocellulose has high strength and modulus, it plays a reinforcing role in the PVB interlayer. Without reinforcing nanocellulose, the overall mechanical strength of the material decreases, weakening its resistance to damage from external environmental factors. In practical applications, it may be more prone to breakage and deformation. Furthermore, sound waves can more easily penetrate the material, leading to poorer sound insulation. In Comparative Examples 6-7, only a single nanofiller was added, which has a certain effect on enhancing mechanical properties and sound insulation, but its effect is singular and not as good as composite nanofillers. In Comparative Example 8, no composite nanofiller was added. Without the reinforcing effect of nanofillers, the PVB interlayer lacks the mechanical and sound insulation properties, which will significantly decrease. The properties of the PVB resin itself are insufficient to achieve high levels of mechanical and sound insulation performance. In Comparative Example 17, the shrinkage ratio in the casting process is 1:1, which will cause changes in the structure and density of the film during the molding process, making the internal structure of the film less compact and affecting its mechanical and sound insulation properties. In Comparative Example 18, without hot pressing, the film's density and intermolecular bonding are insufficient, affecting its mechanical and sound insulation properties. Hot pressing helps enhance the bonding between PVB resin and other components, improving the overall performance of the film.
[0098] In summary, reinforced nanocellulose, with its high specific strength and modulus, forms the reinforcing framework of the material. The composite nanofiller components each play a unique role in reinforcement and sound insulation. Together, they intertwine to form a dense network structure, uniformly dispersing stress and hindering sound wave propagation. Casting promotes uniform distribution of the components and the formation of an oriented structure, reducing sound wave transmission channels. Hot pressing strengthens interfacial bonding, eliminates internal defects, and increases density. These four processes work synergistically: reinforced nanocellulose and composite nanofiller lay the foundation for performance; cast molding optimizes the distribution structure; and hot pressing consolidates the molding effect. From microstructure to macroscopic performance, these processes provide a comprehensive and synergistic improvement, resulting in a significant enhancement of the material's mechanical and sound insulation properties.
[0099] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a heat-insulating and sound-insulating PVB interlayer, characterized in that: The preparation method, by weight, includes the following steps: 95-105 parts of PVB resin were fed into a twin-screw extruder, the temperature was set to 100℃, the screw speed was set to 180 rpm, and the pre-plasticization time was set to 12 min to obtain pre-plasticized PVB; the pre-plasticized PVB and reinforced nanocellulose were sheared and mixed to obtain a preliminary mixture; the reinforced nanocellulose was obtained by modifying nanocellulose with a silane coupling agent. A plasticizer, modified lanthanum hexaboride, a composite light stabilizer, modified cerium oxide, a composite nanofiller, and a composite antioxidant are added sequentially to the initial mixture, and the mixture is stirred to obtain a final mixture; the modified lanthanum hexaboride is obtained by loading lanthanum hexaboride with molybdenum trioxide; the modified cerium oxide is obtained by grafting cerium oxide with an ultraviolet absorber; The mixture is subjected to casting and hot pressing, followed by cooling to obtain the PVB interlayer film.
2. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The method for preparing the enhanced nanocellulose is as follows: 90-100 parts of the nanocellulose are slowly added to 600 parts of anhydrous ethanol, and the mixture is stirred for 45 minutes to obtain a suspension. Under continuous stirring, 1-5 parts of silane coupling agent KH550 were slowly added dropwise to the suspension at a rate of 1 mL / min. The mixture was then stirred for 15 min to obtain a mixed solution. The mixed solution was transferred to a three-necked flask and heated to 70°C under a nitrogen atmosphere. The mixture was stirred continuously at this temperature for 2-4 h. After the reaction was completed, the mixture was centrifuged, washed, and vacuum dried to obtain the reinforced nanocellulose.
3. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The initial mixture is prepared by adding 5-10 parts of the enhanced nanocellulose to the preplasticized PVB, increasing the rotation speed to 350 rpm, the temperature to 120℃-140℃, and the mixing time to 18 min to obtain the initial mixture.
4. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The modified lanthanum hexaboride is prepared as follows: 45-55 parts of the lanthanum hexaboride are added to 100 parts of anhydrous ethanol and stirred until a suspension is formed; 3 parts of polyvinylpyrrolidone are added to the suspension and stirred for 30 min to obtain a homogeneous solution; 5-10 parts of molybdenum trioxide are slowly added to the homogeneous solution and stirred for 1.5 h to obtain a mixed solution; the mixed solution is transferred to a reaction vessel and heated to 180℃ for 3-5 h; after the reaction is completed, the mixture is cooled to room temperature, filtered, washed, and vacuum dried to obtain the modified lanthanum hexaboride.
5. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The modified cerium oxide is prepared as follows: 5-15 parts of the cerium oxide are placed in a high-temperature furnace and calcined at 450°C for 2.5 hours. After cooling, pretreated cerium oxide is obtained. The pretreated cerium oxide is added to 30 parts of toluene and ultrasonically dispersed for 45 minutes to obtain a dispersion. 1-2 parts of ultraviolet absorber UV-326 are added to 10 parts of the toluene, stirred, and heated to 55°C to obtain an ultraviolet absorber solution. 0.2 parts of KH550 are added to the ultraviolet absorber solution and stirred for 30 minutes to obtain a mixture. The dispersion is slowly added to the mixture, and the mixture is reacted at 80°C-100°C for 7 hours under stirring conditions. After the reaction is completed, the mixture is filtered, washed, and vacuum dried to obtain the modified cerium oxide.
6. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The mixture is prepared by adding 25 parts of the plasticizer diisobutyl phthalate, 3-8 parts of the modified lanthanum hexaboride, 2-5 parts of the composite light stabilizer, 2-4 parts of the modified cerium oxide, 5-10 parts of the composite nanofiller, and 1.5 parts of the composite antioxidant to the initial mixture in sequence, and stirring and mixing in a high-speed mixer at a stirring speed of 1000 rpm, a mixing temperature of 90℃, and a mixing time of 25 min to obtain the mixture.
7. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The casting and hot pressing process is as follows: the mixture is conveyed to the casting equipment, the mold temperature is set to 150℃, the casting speed is controlled to be 0.5m / min-1.0m / min, and a film blank with a thickness of 0.3mm-0.8mm is obtained; the film blank is transferred to a hot press for hot pressing treatment, the hot pressing temperature is set to 120℃-140℃, the pressure is 3MPa-5MPa, the hot pressing time is 10min-15min, and it is naturally cooled to obtain the PVB intermediate film.
8. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The composite light stabilizer is composed of boron nitride quantum dots and light stabilizer HALS-770, with the weight ratio of boron nitride quantum dots to light stabilizer HALS-770 being 1:1-3; the composite antioxidant includes antioxidant 1010 and antioxidant 168, with the weight ratio of antioxidant 1010 to antioxidant 168 being 1-3:
1.
9. The method for preparing a heat-insulating and sound-insulating PVB interlayer according to claim 1, characterized in that: The composite nanofiller includes nano-montmorillonite and carbon black, and the weight ratio of nano-montmorillonite to carbon black is 3-5:
1.
10. A heat-insulating and sound-insulating PVB interlayer, characterized in that: The PVB interlayer is prepared by the preparation method according to any one of claims 1-9; the PVB interlayer comprises PVB resin, reinforced nanocellulose, plasticizer, modified lanthanum hexaboride, composite light stabilizer, modified cerium oxide, composite nanofiller and composite antioxidant.
Citation Information
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