Soundproofing interlayer and method for its production

Abstract

The present application relates to the technical field of interlayer film of laminated glass, and particularly relates to a sound insulation interlayer film and a preparation method thereof. The sound insulation interlayer film comprises a first surface layer, a sound insulation layer and a second surface layer which are stacked in sequence, one of the first surface layer and the sound insulation layer is provided with a first transition zone and / or one of the second surface layer and the sound insulation layer is provided with a second transition zone, the first transition zone is arranged at one side of the composite interface between the first surface layer and the sound insulation layer, the second transition zone is arranged at one side of the composite interface between the second surface layer and the sound insulation layer, and the first transition zone and the second transition zone are dispersed with micropowder particles, and the first surface layer, the sound insulation layer and the second surface layer all comprise a thermoplastic resin and a plasticizer. The sound insulation interlayer film has excellent sound insulation and weather resistance, the sound insulation performance does not attenuate under long-term conditions, and the plasticizer is not easy to migrate.

Description

Technical Field

[0001] This invention relates to the field of interlayer film technology in laminated glass, specifically to a sound-insulating interlayer film and its preparation method. Background Technology

[0002] With the increasing demands for sound insulation, noise reduction, and safety protection in the automotive and construction industries, sound-insulating interlayer films for laminated glass (especially those based on polyvinyl butyral (PVB)) have been widely used. These sound-insulating interlayer films typically employ a three-layer composite structure: a first surface layer, a sound-insulating layer, and a second surface layer, layered sequentially. The surface layer primarily serves to bond with the glass, provide mechanical support, and offer weather protection. The sound-insulating layer, designed with a high plasticizer content, exhibits high damping characteristics, effectively dissipating and blocking sound waves, making it the core carrier of sound insulation performance. However, existing PVB sound insulation interlayers face numerous problems during long-term use: plasticizer migration leads to a decline in sound insulation performance. To ensure sound insulation, a high proportion of plasticizer needs to be added to the sound insulation layer to lower the glass transition temperature (Tg) and improve viscoelastic damping. However, to ensure adhesion strength and structural stability with the glass, the surface layer has a significantly lower plasticizer content than the sound insulation layer, creating a clear plasticizer concentration gradient. Under temperature changes, long-term use, or external environmental influences, plasticizers in the sound insulation layer easily migrate and diffuse to the surface layer. This leads to plasticizer loss and decreased damping performance, resulting in a gradual decline in sound insulation over time. Furthermore, the surface layer becomes soft and sticky due to plasticizer accumulation, reducing the reliability of adhesion to the glass and even causing delamination and blistering, severely impacting the product's lifespan. Existing PVB sound insulation interlayer films have the technical defect of "plasticizer migration leading to a decrease in sound insulation performance". There is an urgent need to develop a sound insulation interlayer film structure and preparation method that can suppress the interlayer migration of plasticizers and take into account sound insulation performance, optical performance and long-term stability. Summary of the Invention

[0003] The first aspect of this invention provides a sound-insulating interlayer membrane, the primary objective of which is to solve the problem of plasticizer migration caused by the unevenness of plasticizers in the sound-insulating interlayer membrane. To achieve this technical objective, this invention provides the following technical solution.

[0004] A sound-insulating interlayer membrane, comprising a first surface layer, a sound-insulating layer, and a second surface layer stacked sequentially, wherein one of the first surface layer and the sound-insulating layer is provided with a first transition zone and / or one of the second surface layer and the sound-insulating layer is provided with a second transition zone, wherein the first transition zone is provided on one side of the composite interface between the first surface layer and the sound-insulating layer, and the second transition zone is provided on one side of the composite interface between the second surface layer and the sound-insulating layer, wherein micro-powder particles are dispersed in the first transition zone and the second transition zone, and wherein the first surface layer, the sound-insulating layer, and the second surface layer all comprise thermoplastic resin and plasticizer.

[0005] According to the above-described sound-insulating interlayer membrane, the sound-insulating interlayer membrane comprises a first surface layer, a sound-insulating layer, and a second surface layer stacked sequentially. The first surface layer, the sound-insulating layer, and the second surface layer all comprise polyvinyl acetal resin and a plasticizer. The peel strength between the first surface layer and the sound-insulating layer, or the peel strength between the second surface layer and the sound-insulating layer, is tested according to GB / T2791-1995 and is 20.0 N / cm-50.0 N / cm.

[0006] According to the sound-insulating interlayer membrane described above, the first surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer, and the second surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer. The content and / or type of plasticizer in the first surface layer may be the same as or different from the content and / or type of plasticizer in the second surface layer.

[0007] According to the above-described sound-insulating interlayer, the sound-insulating layer comprises 100 parts by weight of polyvinyl acetal resin and 60-120 parts by weight of plasticizer, wherein the plasticizer of the sound-insulating layer is the same as or different from the plasticizer of the first surface layer and / or the second surface layer.

[0008] According to the sound-insulating intermediate film described above, the type of polyvinyl acetal resin in the sound-insulating layer is the same as or different from the type of polyvinyl acetal resin in the first surface layer and / or the second surface layer.

[0009] According to the sound-insulating intermediate membrane described above, the thickness of the first transition zone and / or the second transition zone is 0.02-10 micrometers; the particle size of the micro powder particles is 10-500 nm, and the micro powder particles include heat-insulating particles and / or sound-insulating particles.

[0010] According to the sound-insulating interlayer membrane described above, the first surface layer, the sound-insulating layer, and the second surface layer all include 0.02-0.5 parts by weight of antioxidant.

[0011] According to the sound insulation interlayer film described above, the glass transition temperature of the first surface layer and / or the second surface layer is 5°C to 45°C, and the glass transition temperature of the sound insulation layer is -30°C to -10°C.

[0012] A second aspect of this invention provides a method for preparing a sound-insulating interlayer membrane, and the second objective is to solve the problem of preparing a sound-insulating interlayer membrane. To achieve this technical objective, the present invention adopts the following technical solution.

[0013] A method for preparing a sound-insulating interlayer membrane includes the preparation of a sound-insulating layer: the micro-powder particles are attached to the surface of the sound-insulating layer or / and the first surface layer and / or the second surface layer by means of micro-powder spraying, atomization spraying or coating.

[0014] According to the above-described method for preparing a sound-insulating interlayer membrane, the first surface layer and / or the second surface layer are laminated with the sound-insulating layer to form a sound-insulating interlayer membrane by means of lamination or roll forming.

[0015] Compared with the prior art, the present invention has the following technical effects: The sound-insulating interlayer film and its preparation method provided by this invention not only exhibit excellent sound insulation properties but also excellent weather resistance. Under long-term conditions, the plasticizer does not easily migrate, and the sound insulation performance does not degrade. Therefore, it can be used as a bonding film for glass in automobiles, buildings, etc., and exerts excellent performance.

[0016] Other features and advantages of the invention will become clear from the following detailed description of exemplary embodiments of the invention with reference to the accompanying drawings. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This diagram illustrates a sound-insulating intermediate membrane structure according to the present invention. Figure 2 This diagram shows another structural schematic of a sound-insulating interlayer membrane according to the present invention.

[0019] 1. First surface layer 1; 2. Sound insulation layer; 3. Second surface layer; 21. First transition zone; 22. Second transition zone. Detailed Implementation

[0020] 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. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0021] Techniques, methods, and equipment known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and equipment should be considered part of the specification.

[0022] In the description of this invention, it should be understood that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore should not be construed as limiting the scope of protection of this invention.

[0023] Furthermore, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other. The raw materials used in the present invention are all derived from commercially available products, such as polyvinyl butyral from Anhui Wanwei Company, etc.

[0024] A sound-insulating interlayer membrane includes a first surface layer 1, a sound-insulating layer 2, and a second surface layer 3 stacked sequentially. A first transition zone 21 is provided in one of the first surface layer 1 and the sound-insulating layer 2, and / or a second transition zone 22 is provided in one of the second surface layer 3 and the sound-insulating layer 2. The first transition zone 21 is located on one side of the composite interface between the first surface layer 1 and the sound-insulating layer 2, and the second transition zone 22 is located on one side of the composite interface between the second surface layer 3 and the sound-insulating layer 2. Microparticles are dispersed in the first transition zone 21 and the second transition zone 22. The first surface layer, the sound-insulating layer, and the second surface layer all comprise thermoplastic resin and a plasticizer.

[0025] Specifically, In one embodiment, the sound insulation interlayer membrane, as shown in the figure, includes a first surface layer, a sound insulation layer, and a second surface layer stacked sequentially. The first surface layer is provided with a first transition zone. As shown in the figure, the first transition zone is located on one side of the composite interface between the first surface layer and the sound insulation layer, that is, the first transition zone is close to the layer of the sound insulation layer. The second surface layer is provided with a second transition zone. The second transition zone is located on one side of the composite interface between the second surface layer and the sound insulation layer, that is, the second transition zone is close to the other layer of the sound insulation layer.

[0026] In another embodiment, such as Figure 1As shown, the sound insulation interlayer includes a first surface layer, a sound insulation layer, and a second surface layer stacked sequentially. A first transition zone and a second transition zone are respectively provided on two opposite surfaces of the sound insulation layer. The first transition zone is located on one side of the composite interface between the first surface layer and the sound insulation layer, and the second transition zone is located on one side of the composite interface between the second surface layer and the sound insulation layer.

[0027] Microparticles are dispersed in both the first and second transition zones. The microparticles are preferably inorganic microparticles, such as porous or mesoporous inorganic microparticles, for example, porous structures of nanomaterials such as SiO2, TiO2, and montmorillonite.

[0028] The sound-insulating interlayer membrane of this invention adopts a three-layer structure, possessing basic sound insulation performance. Simultaneously, it contains micro-particles at the composite interfaces of the first surface layer and the sound-insulating layer, and at the composite interfaces of the second surface layer and the sound-insulating layer. This enhances the sound insulation performance of the interlayer membrane and effectively solves the problem of plasticizer migration from the sound-insulating layer to the surface layer due to the presence of micro-particles. Preferably, the micro-particles are porous. Therefore, the sound-insulating interlayer membrane of this invention exhibits excellent sound insulation performance and weather resistance, effectively solving the problem of plasticizer migration.

[0029] In one specific embodiment, the sound-insulating interlayer comprises a first surface layer, a sound-insulating layer, and a second surface layer stacked sequentially. Each of the first surface layer, the sound-insulating layer, and the second surface layer comprises polyvinyl acetal resin and a plasticizer. The peel strength between the first surface layer and the sound-insulating layer, tested according to GB / T2791-1995, is 20.0 N / cm-50.0 N / cm, or the peel strength between the second surface layer and the sound-insulating layer is 20.0 N / cm-50.0 N / cm; preferably, the peel strength is 30.0 N / cm-50.0 N / cm.

[0030] Test method for peel strength of sound insulation interlayer: Cut 5 test specimens from the finished sound insulation interlayer. Specimen dimensions: length 200±5mm, width 25±0.5mm. Using a utility knife or craft blade, manually pre-peel along the interface between the first surface layer and the sound insulation layer of the specimen, controlling the pre-peel length to be 50±2mm. Clamp and fix the free end of the pre-peeled first surface layer to the clamp of a universal tensile testing machine, and clamp and fix the combined free end of the sound insulation layer and the second surface layer to the lower clamp of the tensile testing machine. All other test environment, loading rate, test procedure, and other conditions shall be performed in accordance with the provisions of GB / T 2791-1995 standard. Five specimens are tested in parallel for each group, and the arithmetic mean of the five test results is calculated as the final test value. If the relative error between the maximum and minimum values ​​of the five test data exceeds 15%, five more specimens need to be cut and the entire group test needs to be repeated. Use the same operating method and test conditions to complete the peel strength test between the second surface layer and the sound insulation layer.

[0031] The number of micro-particles per unit area in the first and second transition zones: The microstructure of the surface of the first or second transition zone of the PVB sound insulation film was observed using a scanning electron microscope. After ion sputtering with gold or carbon for conductive treatment, multiple microscopic images of different areas were randomly taken at 10,000 magnification. ImageJ software was used to complete the size calibration, image segmentation and particle counting, and the surface particle number density was calculated. The number of micro-particles within a 1 square millimeter area was finally counted through area conversion.

[0032] In one specific embodiment, the first surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer, and the second surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer. The content or type of plasticizer in the first surface layer may be the same as or different from the content or type of plasticizer in the second surface layer. For example, the first and second surface layers use the same brand of polyvinyl acetal resin and the same brand of plasticizer, and the content of polyvinyl acetal resin and plasticizer is the same, that is, the first and second surface layers are completely identical; the polyvinyl acetal resin in the first surface layer is polyvinyl butyral; the weight parts of the plasticizer are: 20, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50 parts by weight.

[0033] In one specific embodiment, the sound insulation layer comprises 100 parts by weight of polyvinyl acetal resin and 60-120 parts by weight of plasticizer, wherein the plasticizer of the sound insulation layer is the same as or different from the plasticizer of the first surface layer and / or the second surface layer.

[0034] To significantly improve the mid-frequency and low-frequency sound insulation performance of the interlayer, the sound insulation layer uses a much higher amount of plasticizer than conventional surface layers. The high plasticizer content can lower the glass transition temperature of polyvinyl acetal resin, so that the sound insulation layer is in a highly elastic damping state at room temperature, which greatly enhances the damping loss of sound wave vibration and weakens the transmission of sound energy. Meanwhile, the first and second surface layers use a low plasticizer ratio to ensure the overall mechanical strength, impact resistance, weather resistance and appearance smoothness of the interlayer, achieving a balance between structural strength and high sound insulation performance.

[0035] Preferably, the polyvinyl acetal resin is polyvinyl butyral resin (PVB resin). The plasticizer is selected from commonly used plasticizers of polyvinyl acetal resin, including esters of polyvalent aliphatic or aromatic acids, esters or ethers of polyvalent aliphatic or aromatic alcohols or oligoether diols having one or more unbranched or branched aliphatic or aromatic substituents.

[0036] Esters of polyvalent aliphatic or aromatic acids, such as dialkyl adipates like dihexyl adipate, dioctyl adipate, hexylcyclohexyl adipate, heptyl adipate and nonyl adipate mixtures, diisononyl adipate, heptylnonyl adipate and esters of adipate with alicyclic ester alcohols or ether-bonded ester alcohols, dialkyl sebacate like dibutyl sebacate and esters of sebacate with alicyclic ester alcohols or ether-bonded ester alcohols, esters of phthalic acid like butyl benzyl phthalate or bis-2-butoxyethyl phthalate, and esters of cyclohexanedicarboxylic acid like diisononyl 1,2-cyclohexanedicarboxylic acid.

[0037] Esters or ethers of polyvalent aliphatic or aromatic alcohols or oligoether diols having one or more unbranched or branched aliphatic or aromatic substituents, such as esters of di-, tri-, or tetra-diols with straight-chain or branched aliphatic or alicyclic carboxylic acids; diethylene glycol bis(2-ethylhexanoate), triethylene glycol bis(2-ethylhexanoate), triethylene glycol bis(2-ethylbutyrate), tetraethylene glycol bis(n-heptanoate), triethylene glycol bis(n-heptanoate), triethylene glycol bis(n-heptanoate), tetraethylene glycol dimethyl ether and / or dipropylene glycol benzoate, may be used as examples of the latter group of phosphate esters having aliphatic or aromatic ester alcohols, said phosphate esters being, for example, tri(2-ethylhexyl) phosphate (TOF) of citric acid, succinic acid and / or fumaric acid, triethyl phosphate, diphenyl-2-ethylhexyl phosphate and / or tricresyl phosphate.

[0038] Preferably, the plasticizer comprises one or more of the following: di(2-ethylhexyl) sebacate (DOS), di(2-ethylhexyl) adipate (DOA), dihexyl adipate (DHA), dibutyl sebacate (DBS), triethylene glycol di-n-heptanoate (3G7), tetraethylene glycol di-n-heptanoate, triethylene glycol bis(2-ethylhexanoate) (3GO), tetraethylene glycol bis(n-2-ethylhexanoate) (4GO or 4G8), di(2-butoxyethyl) adipate (DBEA), di(2-butoxyethoxyethyl) adipate (DBEEA), di(2-butoxyethyl) sebacate (DBES), di(2-ethylhexyl) phthalate (DOP), diisononyl phthalate (DINP), triethylene glycol bis(2-propylhexanoate), diisononyl 1,2-cyclohexanedicarboxylate (DINCH), and tri(2-ethylhexyl) phosphate. Ester (TOF) and dipropylene glycol benzoate.

[0039] As the plasticizer in the sound insulation layer is gradually improved, the molecular chain mobility of polyvinyl acetal resin is enhanced, the damping loss factor increases, and the sound insulation of the intermediate membrane is gradually improved. Moreover, regardless of whether the type of plasticizer is the same as or different from that of the surface layer, as long as the plasticizer in the sound insulation layer is controlled within the range of 60-120 parts by weight, a sound insulation effect superior to that of conventional ratios can be achieved. The difference in type only affects the interlayer compatibility and does not hinder the improvement of sound insulation performance.

[0040] In one specific embodiment, the type of polyvinyl acetal resin in the sound insulation layer may be the same as or different from the type of polyvinyl acetal resin in the first and / or second surface layers.

[0041] In this embodiment, a uniform resin base is preferred. The first surface layer, the second surface layer, and the middle sound insulation layer all use polyvinyl butyral resin as the main raw material, maintaining consistency in the resin type across all three layers. No difference is made between the resin types used in each layer; only the key structural parameters of the polyvinyl butyral resin are differentiated. The main difference lies in the hydroxyl content and acetalization degree of each layer. By controlling the differences in hydroxyl content and acetalization degree, the first and second surface layers possess excellent structural strength, weather resistance, and adhesion, while the sound insulation layer exhibits high damping characteristics, achieving excellent sound insulation and vibration reduction effects.

[0042] For example, the base resins of the first surface layer, the second surface layer, and the sound insulation layer are all polyvinyl butyral resins, and the resin types are exactly the same. The only difference between the layers is the hydroxyl content and acetal degree of the polyvinyl butyral resin: First surface layer: polyvinyl butyral resin with a hydroxyl content of 17% to 23% and an acetal degree of 70% to 80%; Second surface layer: the same formulation parameters as the first surface layer, using polyvinyl butyral resin with the same hydroxyl content and acetal degree; Sound insulation layer: still using polyvinyl butyral resin, with the resin type unchanged, but with a hydroxyl content of 10% to 14% and an acetal degree of 65% to 75%. By keeping the resin types of the three layers uniform and only differentiating the hydroxyl content and acetal degree of polyvinyl butyral, the surface layer can be given structural support, weather-resistant bonding properties, and the sound insulation layer can have exclusive properties such as damping sound absorption and shock absorption without changing the resin type. The overall structure has good compatibility, the molding process is simple, and the sound insulation and comprehensive mechanical properties are excellent.

[0043] In one specific embodiment, the thickness of the first transition region and / or the second transition region is 0.05-10 micrometers; the particle size of the microparticles is 10-500 nm, and the microparticles include heat-insulating particles and / or sound-insulating particles. Commonly used heat-insulating particles are selected from at least one of nano-antimony tin oxide (ATO), nano-indium tin oxide (ITO), aluminum-doped zinc oxide (AZO), cesium tungsten bronze, nano-silica, nano-titanium dioxide, and nano-zinc oxide; commonly used sound-insulating particles are selected from at least one of nano-montmorillonite, nano-calcium carbonate, nano-barium sulfate, silane-modified nano-montmorillonite, nano-kaolin, and nano-talc.

[0044] For example, such as Figure 1As shown, a sound-insulating interlayer membrane with both high-efficiency sound insulation and heat insulation functions has an overall structure consisting of a first surface layer, a sound-insulating layer, and a second surface layer stacked sequentially. A first transition zone (near the first surface layer) and a second transition zone (near the second surface layer) are formed on both sides of the sound-insulating layer, respectively. The thickness of the first transition zone is controlled at 0.5 μm, and the thickness of the second transition zone is also 0.5 μm, both falling within the optimized range of 0.02-10 μm. This ensures both the loading of microparticles and avoids stress concentration at the membrane interface. Embodiments 1, 2, and 3 of this invention, as well as Comparative Example 1, employ the following... Figure 1 The structure shown Another example, such as Figure 2 As shown, a sound-insulating interlayer membrane with both high-efficiency sound insulation and heat insulation functions has an overall structure consisting of a first surface layer, a sound-insulating layer, and a second surface layer stacked sequentially. A first transition zone is formed on one side of the first surface layer (the side closest to the sound-insulating layer), and a second transition zone is formed on one side of the second surface layer (the other side closest to the sound-insulating layer). The thickness of both the first and second transition zones is controlled at 0.5 μm, falling within the optimized range of 0.02-10 μm, ensuring both the loading of microparticles and avoiding stress concentration at the membrane interface. Embodiments 4, 5, and 6 of this invention, as well as Comparative Example 2, employ... Figure 2 The structure shown.

[0045] The micro-particles employ a composite system of "heat-insulating particles + sound-insulating particles." The heat-insulating particles are nano-antimony tin oxide (ATO, 15nm particle size) and nano-silica (SiO2, 10nm particle size). Their synergistic effect effectively blocks infrared heat, reducing the heat transfer coefficient of the laminated glass, while the ultra-small particle size avoids affecting the light transmittance of the film. The sound-insulating particles are nano-montmorillonite and nano-calcium carbonate (CaCO3, 135nm particle size). The plate-like structure of nano-montmorillonite enhances the sound wave damping effect, while nano-calcium carbonate weakens sound wave transmission by filling the resin gaps. The composite significantly improves the blocking efficiency for mid-to-low frequency noise. The nano-montmorillonite (MMT, purchased from Aladdin Reagent Network, montmorillonite K-10, with an average particle size of 376nm after grinding and dispersion) and nano-calcium carbonate used in this invention are also sourced from Aladdin Reagent Network.

[0046] All micro-particles are uniformly adhered to the surfaces of both sides of the sound insulation layer, the surface of the first surface layer, or the surface of the second surface layer through non-contact atomization spraying, micro-particle dispersion, or coating. Since the first surface layer, sound insulation layer, and second surface layer are subsequently rolled or laminated, the micro-particles are pressed into the surfaces of the sound insulation layer, the first surface layer, or the second surface layer, thus forming a first or second transition zone. The micro-particles are enriched only in the shallow surface and do not penetrate into the internal matrix of the sound insulation layer, ensuring the original flexibility and interlayer peel strength of the sound insulation layer. This embodiment comprehensively optimizes the transition zone structure, micro-particle type, and particle size parameters, enabling the sound insulation interlayer to possess excellent dual performance of heat insulation and sound insulation, making it suitable for various laminated glass applications such as automotive and architectural applications.

[0047] In one specific embodiment, the first surface layer, the sound insulation layer, and the second surface layer each include 0.02-0.5 parts by weight of antioxidant. Suitable antioxidants are commonly used in polyvinyl acetal interlayer films, including one or a combination of hindered phenolic antioxidants and phosphite-based auxiliary antioxidants. Specific options include: antioxidant 1010, antioxidant 1076, antioxidant 3114, antioxidant 168, and antioxidant 626. For example, 0.2 parts by weight of antioxidant are added to the first surface layer, the second surface layer, and the sound insulation layer, using a combination of antioxidant 1010 and antioxidant 168 (mass ratio 1:1). The antioxidant is uniformly dispersed in the resin matrix of each layer, effectively inhibiting resin thermo-oxidative aging, degradation, and yellowing during high-temperature processing and long-term use, maintaining stable mechanical properties and interlayer peel strength of each layer, without precipitation or migration, and without affecting the light transmittance, sound insulation performance, or interfacial composite strength of the interlayer film.

[0048] In other embodiments, the amount of antioxidant added can be arbitrarily selected within the range of 0.02 parts by weight, 0.1 parts by weight, 0.3 parts by weight, and 0.5 parts by weight. Each layer can use the same antioxidant, or different types of antioxidants can be used for different layers. All of these methods can improve the product's aging resistance and weather resistance without affecting the membrane structure and sound insulation effect.

[0049] In one specific embodiment, the glass transition temperature of the first surface layer and / or the second surface layer is 5°C to 45°C, and the glass transition temperature of the sound insulation layer is -30°C to -10°C.

[0050] In one specific embodiment, the sound-insulating interlayer is a three-layer composite structure consisting of a first surface layer, a sound-insulating layer, and a second surface layer. By matching the type of polyvinyl acetal resin and adjusting the amount of plasticizer added to each layer, the glass transition temperature of each layer is precisely controlled: the glass transition temperature of the surface layer is moderately high, so that the first and second surface layers have suitable hardness, mechanical strength, and interfacial adhesion performance at room temperature, ensuring the overall dimensional stability of the interlayer, scratch resistance, and resistance to delamination and warping after being laminated with glass; the glass transition temperature of the sound-insulating layer is much lower than room temperature, and it is in a high-damping viscoelastic state at room temperature, which can efficiently absorb and dissipate sound wave energy, greatly improving the sound insulation and vibration reduction effect of the interlayer.

[0051] In actual fabrication, the glass transition temperatures of the first and / or second surface layers can be set at approximately 5°C, 25°C, and 35°C, respectively, while the glass transition temperatures of the sound insulation layer can be set at approximately -30°C, -15°C, and -10°C. "Approximately" refers to an error of ±2°C.

[0052] It should be understood that the aforementioned 5℃, 25℃, 35℃, -30℃, -15℃, and -10℃ are only typical reference values ​​within the range, and do not require the glass transition temperature to be strictly limited to an exact integer value. Due to factors such as the distribution of resin polymerization degree, the accuracy of plasticizer ratio, and the mixing and film-forming process conditions, the actual glass transition temperature of the material may have reasonable small fluctuations and deviations. As long as the surface glass transition temperature falls within the overall range of 5℃~35℃ and the sound insulation layer glass transition temperature falls within the overall range of -30℃~-10℃, it falls within the protection scope of this technical solution.

[0053] Within this temperature range and within the allowable deviation range, the surface layer can maintain suitable hardness, dimensional stability, and adhesion strength to the glass; the sound insulation layer, within the corresponding low temperature range and under reasonable deviation, remains in a high-damping viscoelastic state at room temperature, which can effectively dissipate sound wave energy and ensure the stable sound insulation performance of the interlayer.

[0054] A method for preparing a sound-insulating interlayer includes the preparation of a sound-insulating layer: the nanoparticles are attached to the surface of the sound-insulating layer, a first surface layer, or a second surface layer by non-contact powder spraying, atomized spraying, or coating, forming a first transition zone and / or a second transition zone enriched with nanoparticles only on the surface of the sound-insulating layer, the first surface layer, or the second surface layer, and the powder particles do not penetrate into the matrix. The coating method employs conventional coating processes in the art; the powder spraying method involves spraying nanoparticles onto the surface to be attached at a set rate to achieve uniform adhesion, exemplarily, electrostatic spraying. This application uses a spraying method with a set rate of 50-200 m / s, preferably 60-100 m / s, and 70 m / s is used in this application.

[0055] In one specific embodiment, the first surface layer and / or the second surface layer are laminated with the sound insulation layer to form a sound insulation intermediate film by means of lamination or roll forming.

[0056]

[0057]

[0058] Test methods for the performance of sound-insulating interlayer membranes.

[0059] Preparation of laminated glass samples 1.1 Raw material preparation Glass sheet: Two pieces of automotive-grade float soda-lime glass, each with a thickness of 2.0mm or 2.5mm (2.0mm is used in this invention), a size of 300mm×400mm, and a clean surface, free of scratches and uneven stress. Intermediate membrane: Sound insulation intermediate membrane to be tested (Example / Comparative example); Auxiliary materials: dust-free paper, anhydrous ethanol, vacuum bags, high-temperature sealant.

[0060] 1.2 Piece Combination Operation Wipe the original glass slide with anhydrous ethanol and dry it with hot air until it is free of impurities and moisture. Place the sound-insulating interlayer horizontally between the two pieces of glass; Adjust the position of the membrane material to ensure that it is centered, without wrinkles, bubbles, or misalignment, and that its edges are aligned with the glass.

[0061] 1.3 Pre-compression degassing After lamination, the sheets are placed in a vacuum pre-compression device. Process parameters: Pre-compression temperature: 100℃±5°C Vacuum degree: -0.08MPa~-0.09MPa Pre-compression time: 23-27 minutes Objective: To completely eliminate air between the glass and the membrane material, and to achieve initial bonding and shaping.

[0062] 1.4 Autoclave curing Transfer to a high-pressure autoclave specifically designed for automotive laminated glass, and perform the standard curing process: Temperature increase: Increase to 140-145℃ at a rate of 5℃ / min; Pressurization: Synchronously increase the pressure to 1.4MPa~1.5MPa; Insulation and pressure maintenance: 140℃~145℃, 1.4MPa~1.5MPa for 35 minutes; Cooling and depressurization: Slowly reduce the pressure to room temperature or atmospheric pressure, then remove the sample; The final product is a laminated glass without bubbles or delamination.

[0063] Sound insulation performance was tested according to GMW14173 standard: the laboratory consisted of a reverberation chamber and an anechoic chamber, with the test sample installed between the two rooms. The test sample was the aforementioned laminated glass specimen, and the size of the laminated glass specimen needed to meet the test requirements; the sound transmission loss STL of the automotive glass was L. P -6-L I (dB) is the average sound pressure level measured in the sound-generating chamber minus the sound intensity level measured in the sound-receiving chamber minus 6dB, with a test frequency range of 1000Hz-4000Hz.

[0064] Plasticizer migration rate test under 80℃ heat aging for 500h: Five parallel samples of 100mm×100mm size were cut from the sound insulation interlayer. The surfaces were clean and undamaged. The mass m1 of the initial sound insulation layer plasticizer and the mass m2 of the initial sound insulation layer PVB resin, micro-particles, and antioxidants were calculated according to the formula. The five parallel samples were placed in a vacuum drying oven at 80℃ (vacuum degree -0.09MPa) for 500h. After cooling to room temperature, the sound insulation layer was peeled off from the interlayer using a paper cutter. The total weight m3 of the sound insulation layer was obtained by weighing. The plasticizer migration rate was calculated according to the following formula: Migration rate (%) = ((m1-(m3-m2) / m1))×100%; The arithmetic mean of the five parallel samples was taken as the final result and one decimal place was retained.

[0065] The haze was determined according to GB / T2410-2008 "Determination of transmittance and haze of transparent plastics": a 50mm×50mm sample was cut, and the surface was clean and free of scratches, bubbles, and wrinkles; the sample was conditioned at 23±2℃ and 50±10% relative humidity for ≥40h; the haze was measured using an integrating sphere haze meter, and the haze was expressed as a percentage of scattered light flux to total transmitted light flux; the arithmetic mean of 5 parallel samples was taken, and the result was retained to one decimal place.

[0066] The above description is merely an exemplary embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A sound-insulating interlayer membrane, characterized in that, The sound insulation interlayer includes a first surface layer (1), a sound insulation layer (2), and a second surface layer (3) stacked sequentially. One of the first surface layer (1) and the sound insulation layer (2) is provided with a first transition zone (21) and / or one of the second surface layer (3) and the sound insulation layer (2) is provided with a second transition zone (22). The first transition zone (21) is provided on one side of the composite interface between the first surface layer (1) and the sound insulation layer (2), and the second transition zone (22) is provided on one side of the composite interface between the second surface layer (3) and the sound insulation layer (2). Micro powder particles are dispersed in the first transition zone (21) and the second transition zone (22). The first surface layer (1), the sound insulation layer (2), and the second surface layer (3) all include thermoplastic resin and plasticizer.

2. The sound-insulating interlayer membrane according to claim 1, characterized in that, The sound insulation interlayer includes a first surface layer (1), a sound insulation layer (2), and a second surface layer (3) stacked sequentially. The first surface layer (1), the sound insulation layer (2), and the second surface layer (3) all include polyvinyl acetal resin and plasticizer. According to GB / T2791-1995, the peel strength between the first surface layer (1) and the sound insulation layer (2) is 20.0 N / cm-50.0 N / cm or the peel strength between the second surface layer (3) and the sound insulation layer (2) is 20.0 N / cm-50.0 N / cm.

3. The sound-insulating interlayer membrane according to claim 1, characterized in that, The first surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer, and the second surface layer comprises 100 parts by weight of polyvinyl acetal resin and 20-50 parts by weight of plasticizer. The content and / or type of plasticizer in the first surface layer may be the same as or different from the content and / or type of plasticizer in the second surface layer.

4. The sound-insulating interlayer membrane according to claim 3, characterized in that, The sound insulation layer comprises 100 parts by weight of polyvinyl acetal resin and 60-120 parts by weight of plasticizer, wherein the plasticizer of the sound insulation layer is the same as or different from the plasticizer of the first surface layer and / or the second surface layer.

5. The sound-insulating interlayer membrane according to claim 4, characterized in that, The type of polyvinyl acetal resin in the sound insulation layer may be the same as or different from the type of polyvinyl acetal resin in the first and / or second surface layers.

6. The sound-insulating interlayer membrane according to claim 1, characterized in that, The thickness of the first transition region and / or the second transition region is 0.02-10 micrometers; the particle size of the micro powder particles is 10-500 nm, and the micro powder particles include heat-insulating particles and / or sound-insulating particles.

7. The sound-insulating interlayer membrane according to claim 1, characterized in that, The first surface layer, the sound insulation layer, and the second surface layer each contain 0.02-0.5 parts by weight of antioxidant.

8. The sound-insulating interlayer membrane according to claim 1, characterized in that, The glass transition temperature of the first surface layer and / or the second surface layer is 5°C to 45°C, and the glass transition temperature of the sound insulation layer is -30°C to -10°C.

9. A method for preparing a sound-insulating interlayer membrane, characterized in that, The preparation of the sound insulation layer includes: the micro powder particles are attached to the surface of the sound insulation layer or / and the first surface layer or / and the second surface layer by means of micro powder spraying, atomization spraying or coating.

10. The method for preparing a sound-insulating interlayer membrane according to claim 9, characterized in that: The first surface layer and / or the second surface layer are laminated with the sound insulation layer to form a sound insulation intermediate film by means of lamination or roll forming.

Images