Reaction compatibilized wide temperature range sound insulation resin film and preparation method and application thereof

Abstract

The present application relates to the technical field of high polymer functional materials and interlayer film of laminated glass, and particularly relates to a reaction compatibilized wide-temperature-range sound insulation resin film and a preparation method and application thereof. The present application is based on a blending system of polyvinyl butyral and thermoplastic polyurethane elastomer, and solves the compatibility problem of polyvinyl butyral and thermoplastic polyurethane elastomer through in-situ ring-opening esterification bridging reaction compatibilization, while significantly improving the low-temperature damping performance and tear resistance of the film material and inhibiting the migration of plasticizer. The preparation method provided by the present application realizes one-step in-situ compatibilization and film formation, and is suitable for existing industrial production lines. Overall, the reaction compatibilized wide-temperature-range sound insulation resin film provided by the present application has good compatibility of components, and has excellent wide-temperature-range sound insulation performance, high mechanical strength and stable optical performance, and has a wide application prospect in the fields of automobiles, buildings, rail transit or packaging glass.

Description

Technical Field

[0001] This invention relates to the field of polymer functional materials and interlayer glass technology, and particularly to a reaction-compressed wide-temperature-range sound-insulating resin film, its preparation method, and its application. Background Technology

[0002] Laminated glass, as a type of safety glass, is widely used in the automotive, construction, and rail transportation industries, with common applications including car windshields, building curtain walls, and rail transit windows. Polyvinyl butyral (PVB) is the core substrate of the interlayer in laminated glass. Based on the sound insulation requirements of these industries, engineers have modified its sound insulation properties. Existing sound insulation technologies mostly achieve sound insulation at room temperature by controlling the vinyl acetate (VAc) content in different layers of the PVB film, but significant technical shortcomings remain. For example, the damping temperature range is narrow; the damping value is less than 8% in low-temperature environments below -10℃, failing to meet the low-temperature sound insulation requirements of vehicles and outdoor buildings in cold regions. The soft sound-insulating core layer has poor tear resistance and puncture resistance, making it prone to film breakage and interlayer separation during processing and use. Under long-term use at high temperatures, plasticizers tend to migrate to the surface, leading to a decrease in sound insulation performance and delamination from the glass.

[0003] To improve the low-temperature damping and mechanical properties of PVB films, the industry has attempted to modify them by blending PVB with thermoplastic polyurethane elastomer (TPU). However, PVB is a strongly polar polymer, while TPU is a weakly polar polymer. Direct blending of the two presents a core problem: poor compatibility. This easily leads to macroscopic phase separation, resulting in increased haze, a sharp drop in light transmittance, and poor interlayer bonding in the PVB film. Consequently, it fails to meet the optical and functional requirements of laminated glass, hindering industrial applications. Researchers have attempted to improve compatibility by pre-synthesizing graft compatibilizers, but the compatibilization effect is limited, and the process is lengthy and costly, making it incompatible with existing PVB film production lines. Some grafting modification methods also suffer from numerous side reactions, resin yellowing and degradation, and poor processing stability.

[0004] Therefore, developing a PVB film that combines excellent wide-temperature-range sound insulation performance, high mechanical strength, and stable optical performance, and whose preparation process is simple and suitable for industrial production, has become an urgent technical problem to be solved in this field. Summary of the Invention

[0005] In view of this, the present invention provides a reaction compatibilized wide-temperature-range sound-insulating resin film, its preparation method and application. The reaction compatibilized wide-temperature-range sound-insulating resin film provided by the present invention has good compatibility of its components and combines excellent wide-temperature-range sound insulation performance, high mechanical strength and stable optical properties.

[0006] This invention provides a reaction-compressed wide-temperature-range sound-insulating resin film, comprising a sound-insulating core layer and an adhesive surface layer covering the sound-insulating core layer; the sound-insulating core layer has one or more layers; the adhesive surface layer has one or more layers; the sound-insulating core layer comprises the following components in parts by weight: 60-80 parts PVB, 5-30 parts TPU, 20-40 parts plasticizer, 0.1-2 parts maleic anhydride (MAH), and 0.01-2 parts additives; the maleic anhydride forms a PVB-MAH-TPU covalently bridged structure with the hydroxyl groups on the molecular chain of PVB and the terminal hydroxyl groups on the molecular chain of TPU; the adhesive surface layer comprises the following components in parts by weight: 70-85 parts PVB, 15-30 parts plasticizer, and 0.1-2 parts additives.

[0007] Preferably, the content of vinyl acetate units (based on polyvinyl acetate) of PVB in the sound insulation core layer is 5-8 mol%, and the hydroxyl content (based on polyvinyl alcohol) is 10-14 wt%.

[0008] Preferably, the TPU in the sound insulation core layer has a Shore hardness of A70~A90, a weight-average molecular weight of 50,000~120,000, a terminal hydroxyl value of 20~80 mgKOH / g, and a functionality of 2; the TPU is a terminal hydroxyl polyester TPU.

[0009] Preferably, the additives in the sound insulation core layer include one or more of the following: ultraviolet absorbers, antioxidants, adhesion modifiers, and esterification reaction catalysts.

[0010] Preferably, the vinyl acetate unit content (based on polyvinyl acetate) of PVB in the adhesive surface layer is 0.1~11 mol%, and the hydroxyl content (based on polyvinyl alcohol) is 17~22 wt%.

[0011] Preferably, the reaction-compressed wide-temperature-range sound-insulating resin film comprises a first adhesive surface layer, a sound-insulating core layer, and a second adhesive surface layer (ABA structure) stacked sequentially; the first adhesive surface layer and the second adhesive surface layer are identical.

[0012] The present invention also provides a method for preparing the reaction-compressed wide-temperature-range sound-insulating resin film described above, comprising the following steps: (1) PVB, TPU, plasticizer, maleic anhydride and additives are mixed and melted to carry out in-situ ring-opening esterification bridging reaction to obtain sound insulation core layer melt; (2) Mix PVB, plasticizer and additives, melt them to obtain a bonding surface melt; (3) The sound insulation core melt and the adhesive surface melt are co-extruded and then cast to obtain the reaction compatibilized wide temperature range sound insulation resin film; There is no requirement for the time order of steps (1) and (2).

[0013] Preferably, in step (1), the temperature of the molten screw is 150~210℃ and the screw speed is 200~400rpm.

[0014] Preferably, in step (2), the temperature of the molten screw is 140~200℃ and the screw speed is 200~400rpm.

[0015] The present invention also provides the application of the reaction-compressed wide-temperature-range sound-insulating resin film described above in the automotive, construction, rail transportation, or encapsulation glass fields.

[0016] Compared with the prior art, the present invention has achieved the following beneficial effects: This invention, based on a PVB and TPU blend system, solves the compatibility problem between PVB and TPU through in-situ ring-opening esterification bridging reaction, while significantly improving the low-temperature damping performance and tear resistance of the film material and inhibiting plasticizer migration. The preparation method provided by this invention achieves one-step in-situ compatibility enhancement and film formation, adaptable to existing industrial production lines. Overall, the reaction-compressed wide-temperature-range sound-insulating resin film provided by this invention exhibits good compatibility among its components and combines excellent wide-temperature-range sound insulation performance, high mechanical strength, and stable optical properties. Specifically: 1) One-step in-situ capacity enhancement with excellent compatibility between PVB and TPU: This invention incorporates maleic anhydride during the premixing stage, simultaneously completing the directional esterification reaction and film formation during melt extrusion. This eliminates the need for separate synthesis of graft compatibilizers, resulting in a shorter process flow and controllable costs. The in-situ generated bridging structure achieves molecular-level compatibility between PVB and TPU, suppressing macroscopic phase separation and ensuring high light transmittance and low haze of the film material. This solves the problems of poor optical performance and easy delamination in existing PVB and TPU blend systems.

[0017] 2) Significantly widens the damping temperature range, greatly improving low-temperature sound insulation performance: TPU has a lower glass transition temperature than PVB. After forming a bicontinuous phase structure with PVB, the damping peaks of the two are superimposed, effectively widening the damping temperature range. Compared with the pure PVB sound insulation system, the reaction-enhanced wide-temperature-range sound insulation resin film provided by this invention improves the damping value by more than 100% at -10℃, while maintaining a damping of more than 23% at room temperature, achieving excellent sound insulation performance across the entire temperature range of -10 to 40℃, and adapting to the usage requirements of all climate scenarios.

[0018] 3) Significantly improves mechanical properties and long-term stability: The addition of TPU significantly improves the tear resistance and puncture resistance of the sound insulation core layer, exceeding that of pure PVB core layer by more than 30%, solving the problem of easy breakage during processing of soft sound insulation films. At the same time, the molecular bridges and interface bonds formed by the in-situ ring-opening esterification bridging reaction can effectively lock the plasticizer, inhibit plasticizer migration, and greatly improve the long-term performance stability of the film material, avoiding the degradation of sound insulation performance and glass delamination.

[0019] 4) The reaction is highly controllable, has good processing adaptability, and is easy to promote industrially: The directional esterification reaction used in this invention has no side reactions, stable melt flow, wide processing window, and good batch consistency. The preparation method is fully compatible with existing multilayer co-extrusion production lines for PVB films, requiring no large-scale equipment modification. The reaction compatibilization and film formation are completed in one step, resulting in high production efficiency and easy large-scale industrial production. Detailed Implementation

[0020] This invention provides a reaction-compressed wide-temperature-range sound-insulating resin film, comprising a sound-insulating core layer and an adhesive surface layer covering the sound-insulating core layer; the sound-insulating core layer has one or more layers; the adhesive surface layer has one or more layers; the sound-insulating core layer comprises the following components in parts by weight: 60-80 parts PVB, 5-30 parts TPU, 20-40 parts plasticizer, 0.1-2 parts maleic anhydride (MAH), and 0.01-2 parts additives; the maleic anhydride forms a PVB-MAH-TPU covalently bridged structure with the hydroxyl groups on the molecular chain of PVB and the terminal hydroxyl groups on the molecular chain of TPU; the adhesive surface layer comprises the following components in parts by weight: 70-85 parts PVB, 15-30 parts plasticizer, and 0.1-2 parts additives.

[0021] The sound insulation core layer comprises 60 to 80 parts of PVB, preferably 65 to 75 parts, and more preferably 70 parts, by weight.

[0022] In this invention, the vinyl acetate unit content (based on polyvinyl acetate) of PVB in the sound insulation core layer is preferably 5-8 mol%, more preferably 6-7 mol%, and the hydroxyl content (based on polyvinyl alcohol) is preferably 10-14 wt%, more preferably 11-12 wt%. The use of PVB with the above specifications in this invention better meets the basic requirements of sound insulation.

[0023] Based on PVB in the sound insulation core layer, the sound insulation core layer includes 5 to 30 parts of TPU, preferably 10 to 25 parts, and more preferably 15 to 20 parts.

[0024] In this invention, the Shore hardness of the TPU is preferably A70~A90, the weight-average molecular weight is preferably 50,000~120,000, more preferably 70,000~100,000, the terminal hydroxyl value is preferably 20~80 mgKOH / g, more preferably 40~60 mgKOH / g, and the functionality is preferably 2.

[0025] In this invention, the TPU is preferably a hydroxyl-terminated polyester TPU; the hydroxyl-terminated polyester TPU preferably includes one or more of adipic acid-based polyester TPU, polycaprolactone-based polyester TPU, and polycarbonate-based TPU.

[0026] The present invention uses the above-mentioned TPU, whose soft segment structure can provide excellent low-temperature damping performance, the terminal hydroxyl groups provide active sites for reaction compatibilization, and the polyester groups form hydrogen bonds with the hydroxyl groups of PVB, which ensures basic compatibility.

[0027] Based on PVB in the sound insulation core layer, the sound insulation core layer includes 20 to 40 parts of plasticizer, preferably 25 to 35 parts, and more preferably 30 parts.

[0028] In this invention, the plasticizer preferably includes one or more of the following: triethylene glycol diisooctanoate (3GO), triethylene glycol di-n-heptanoate (3G7), diisooctyl adipate (DOA), diisooctyl sebacate (DOS), and diisononyl 1,2-cyclohexanedicarboxylate (DINCH).

[0029] Based on the PVB in the sound insulation core layer, the sound insulation core layer includes 0.1 to 2 parts of maleic anhydride, preferably 0.3 to 1.6 parts, more preferably 0.6 to 1.2 parts, and even more preferably 0.8 parts.

[0030] Based on the PVB in the sound insulation core layer, the sound insulation core layer includes 0.01 to 2 parts of additives, preferably 0.05 to 1.5 parts, more preferably 0.1 to 1 part, and even more preferably 0.5 parts.

[0031] In this invention, the additives preferably include one or more of the following: a UV absorber, an antioxidant, an adhesion modifier, and an esterification catalyst; the UV absorber is preferably 2-(2'-hydroxy-3',5'-di-tert-butylphenyl)-5-chlorobenzotriazole; the antioxidant is preferably pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]; the adhesion modifier is preferably acetate; the acetate preferably includes one or more of magnesium acetate and potassium acetate; the esterification catalyst preferably includes one or more of dibutyltin dilaurate and triethylamine; based on the PVB in the sound insulation core layer, the amount of the esterification catalyst added is preferably 0.01~0.1 parts. The adhesion modifier in this invention can simultaneously provide Lewis acid catalysis for the in-situ ring-opening esterification bridging reaction.

[0032] The adhesive surface layer comprises 70 to 85 parts of PVB, preferably 75 to 80 parts, by weight.

[0033] In this invention, the vinyl acetate unit content (based on polyvinyl acetate) of PVB in the adhesive surface layer is preferably 0.1-11 mol%, more preferably 0.1-4 mol%, and even more preferably 1-4 mol%, and the hydroxyl content (based on polyvinyl alcohol) is preferably 17-22 wt%, more preferably 18-21 wt%, and even more preferably 20 wt%. The use of PVB of the above specifications in this invention ensures excellent adhesion performance and mechanical stability with glass.

[0034] Based on the PVB in the adhesive surface layer, the adhesive surface layer includes 15 to 30 parts of plasticizer, preferably 18 to 27 parts, and more preferably 21 to 23 parts.

[0035] In this invention, the plasticizer preferably includes one or more of the following: triethylene glycol diisooctanoate (3GO), triethylene glycol di-n-heptanoate (3G7), diisooctyl adipate (DOA), diisooctyl sebacate (DOS), and diisononyl 1,2-cyclohexanedicarboxylate (DINCH).

[0036] Based on the PVB in the adhesive surface layer, the adhesive surface layer includes 0.1 to 2 parts of additives, preferably 0.4 to 1.6 parts, more preferably 0.7 to 1.2 parts, and even more preferably 1 part.

[0037] In this invention, the additives preferably include one or more of the following: ultraviolet absorber, antioxidant, adhesion modifier, and esterification reaction catalyst; the ultraviolet absorber is preferably 2-(2'-hydroxy-3',5'-di-tert-butylphenyl)-5-chlorobenzotriazole; the antioxidant is preferably pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]; the adhesion modifier is preferably acetate; the acetate preferably includes one or more of magnesium acetate and potassium acetate; the esterification reaction catalyst preferably includes one or more of dibutyltin dilaurate and triethylamine; based on the PVB in the sound insulation core layer, the amount of the esterification reaction catalyst added is preferably 0.01~0.1 parts.

[0038] In this invention, the thickness of the reaction-compressed wide-temperature-range sound-insulating resin film is preferably 0.38~1.14mm, more preferably 0.55~0.9mm, and even more preferably 0.76mm; the number of layers of the sound-insulating core layer is preferably 1~2 layers; the thickness of a single layer of the sound-insulating core layer is preferably 0.05~0.3mm, more preferably 0.1~0.2mm; the number of layers of the adhesive surface layer is preferably 1~5 layers; and the thickness of a single layer of the adhesive surface layer is preferably 0.2~0.4mm, more preferably 0.3mm.

[0039] In this invention, the reaction-compressed wide-temperature-range sound-insulating resin film preferably comprises a first adhesive surface layer, a sound-insulating core layer, and a second adhesive surface layer (ABA structure) stacked sequentially; the first adhesive surface layer and the second adhesive surface layer are preferably identical. The ABA structure ensures consistent adhesion between the reaction-compressed wide-temperature-range sound-insulating resin film and the glass on both sides, avoiding uneven interlayer stress.

[0040] The reaction-compensated wide-temperature-range sound-insulating resin film provided by this invention exhibits the following performance characteristics after lamination of glass (2mm thick) / intermediate film (the reaction-compensated wide-temperature-range sound-insulating resin film of this invention, 0.76mm thick) / glass (2mm thick): In terms of optical performance, visible light transmittance ≥75%, haze ≤1.0%; in terms of damping performance, damping value at room temperature (20℃) ≥23%, at low temperature (-10℃) ≥16%, and at high temperature (40℃) ≥15%; in terms of mechanical performance, tear strength ≥120kN / m, interlayer peel strength ≥50N / 25mm; and in terms of migration resistance, after 1000h of heat aging at 85℃, plasticizer migration ≤1.5wt%, and damping performance retention ≥90%.

[0041] The present invention also provides a method for preparing the reaction-compressed wide-temperature-range sound-insulating resin film described above, comprising the following steps: (1) PVB, TPU, plasticizer, maleic anhydride and additives are mixed and melted to carry out in-situ ring-opening esterification bridging reaction to obtain sound insulation core layer melt; (2) Mix PVB, plasticizer and additives, melt them to obtain a bonding surface melt; (3) The sound insulation core melt and the adhesive surface melt are co-extruded and then cast to obtain the reaction compatibilized wide temperature range sound insulation resin film; There is no requirement for the time order of steps (1) and (2).

[0042] This invention involves mixing PVB, TPU, plasticizer, maleic anhydride, and additives (referred to as the first mixture), melting them (referred to as the first melt), and then performing an in-situ ring-opening esterification bridging reaction to obtain a sound-insulating core layer melt. In this invention, the first mixture is preferably stirred, with a stirring speed preferably of 1000-2000 rpm, more preferably 1500 rpm; the temperature of the first mixture is preferably 70-90℃, more preferably 80℃; and the mixing time is preferably 10-20 min, more preferably 15 min.

[0043] In this invention, the screw temperature of the first melting is preferably 150~210℃, more preferably 160℃, 180℃, 195℃, 200℃, 195℃ and 190℃ respectively, and the screw speed is preferably 200~400rpm, more preferably 300rpm.

[0044] This invention involves mixing PVB, plasticizer, and additives (referred to as the second mixture), melting them (referred to as the second melt), and obtaining a bonding surface melt. In this invention, the second mixture is preferably stirred, with a stirring speed preferably of 1000-1500 rpm, more preferably 1200 rpm; the temperature of the second mixture is preferably 70-90℃, more preferably 80℃; and the mixing time is preferably 5-15 min, more preferably 10 min.

[0045] In this invention, the screw temperature of the second melting is preferably 140~200℃, more preferably 150℃, 180℃, 190℃ and 185℃ respectively, and the screw speed is preferably 200~400rpm, more preferably 300rpm.

[0046] After obtaining the sound-insulating core melt and the adhesive surface melt, the present invention co-extrudes and casts the sound-insulating core melt and the adhesive surface melt to obtain the reaction-compressed wide-temperature-range sound-insulating resin film. In the present invention, the co-extrusion die preferably includes a multi-layer co-extrusion die; the temperature of the die is preferably 185~195℃, more preferably 190℃.

[0047] In this invention, the casting apparatus includes a first cooling roller and a second cooling roller; the temperature of the first cooling roller is preferably 28~32°C, more preferably 30°C; the temperature of the second cooling roller is preferably 22~28°C, more preferably 25°C.

[0048] In this invention, the process of casting preferably includes cooling the resulting product; the cooling is preferably natural cooling to room temperature. After cooling, the product is measured for thickness, rolled up, and stored.

[0049] The core compatibilization mechanism utilized in the preparation method provided by this invention is as follows: Maleic anhydride is uniformly dispersed in the sound insulation core layer mixture. During the melt extrusion process of a twin-screw extruder, the five-membered ring anhydride group of maleic anhydride is activated by heat and undergoes a directional nucleophilic in-situ ring-opening esterification bridging reaction with the secondary hydroxyl groups on the PVB molecular chain and the terminal hydroxyl groups on the TPU molecular chain, forming a PVB-MAH-TPU covalent bridging structure in situ. This bridging structure, as an in-situ compatibilizer, can significantly reduce the interfacial tension between the PVB and TPU phases. At the same time, the carboxyl groups generated by ring opening can form high-density intermolecular hydrogen bonds with the hydroxyl groups of PVB and the urethane bonds of TPU, further strengthening the interfacial bonding force between the two phases, achieving stable compatibility between PVB and TPU, inhibiting macroscopic phase separation, and simultaneously completing the in-situ ring-opening esterification bridging reaction and film formation.

[0050] The present invention also provides the application of the reaction-compressed wide-temperature-range sound-insulating resin film described above in the automotive, construction, rail transportation, or encapsulation glass fields.

[0051] The reaction compatibilized wide-temperature-range sound-insulating resin film provided by this invention has good compatibility among its components and combines excellent wide-temperature-range sound insulation performance, high mechanical strength and stable optical properties. It is suitable for the automotive, construction, rail transportation or encapsulation glass fields, such as applications in automotive laminated glass, architectural safety glass, rail transportation portholes and photovoltaic encapsulation glass.

[0052] To further illustrate the present invention, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments thereof.

[0053] In the specific embodiments and comparative examples of the present invention, the specifications of the raw materials used are as follows: The PVB in the sound insulation core layer contains 6.5 mol% vinyl acetate units and 12.8 wt% hydroxyl groups; it is of industrial grade. PVB in the adhesive surface layer: vinyl acetate unit content 1.0 mol%, hydroxyl content 20.2 wt%, industrial grade; TPU: 1) Adipic acid-based TPU: Wanhua Chemical WHT-1185, terminal hydroxyl value 45mgKOH / g, Shore A85, weight average molecular weight 80,000, industrial grade; 2) Polycaprolactone-type TPU: BASF Elastollan C85A, hydroxyl terminal value 38mgKOH / g, Shore A85, weight average molecular weight 75,000, industrial grade; 3) Polycarbonate TPU: Covestro Desmopan 785, hydroxyl terminal value 42mgKOH / g, Shore A85, weight average molecular weight 82,000, industrial grade; Plasticizer: 3GO, industrial grade; MAH: Analytical grade; Additives: UV-327 ultraviolet absorber, antioxidant 1010 and magnesium acetate, all of which are industrial grade.

[0054] Examples 1-8: Examples 1-5 were the basic formulation control group, with the core variables being the amount of TPU and MAH added. Examples 6-8 were the TPU type control group, using adipic acid-based TPU, polycaprolactone-based TPU, or polycarbonate-based TPU, respectively, to verify the performance differences of TPUs with different structures. Examples 1-8 all used an ABA three-layer symmetrical structure with a total thickness of 0.76 mm, a 0.3 mm thickness for each of the two adhesive surface layers, and a 0.16 mm thickness for the sound-insulating core layer. The formulations of the sound-insulating core layer in Examples 1-8 are shown in Table 1. Table 1. Formulations of the sound insulation core layer in Examples 1-8 (unit: parts by mass):

[0055] The formulations (parts by weight) of the adhesive surface layer in Examples 1 to 8 are as follows: 78 parts PVB, 21.5 parts 3GO, 0.3 parts UV-327, 0.2 parts antioxidant 1010, and 0.1 parts magnesium acetate.

[0056] The preparation method of the reaction-compressed wide-temperature-range sound-insulating resin film in Examples 1-8 is as follows: 1) Premixing: Add all the raw materials of the sound insulation core layer to a high-speed mixer according to the ratio, and mix for 15 minutes at 80℃ and 1500 rpm to obtain a uniform sound insulation core layer mixture; add all the raw materials of the bonding surface layer to a high-speed mixer according to the ratio, and mix for 10 minutes at 80℃ and 1200 rpm to obtain the bonding surface layer mixture. 2) Compatibilization through melt extrusion and in-situ ring-opening esterification bridging reaction: The sound insulation core layer mixture is fed into a twin-screw extruder with screw temperatures set at 160℃, 180℃, 195℃, 200℃, 195℃, and 190℃, and screw speed at 300 rpm. During extrusion, the in-situ ring-opening esterification bridging reaction of maleic anhydride is completed. The bonding surface layer mixture is fed into two twin-screw extruders with screw temperatures set at 150℃, 180℃, 190℃, and 185℃, and screw speed at 300 rpm. 3) Co-extrusion film formation: The melt from the twin-screw extruder and two twin-screw extruders is fed into the ABA three-layer co-extrusion die. The die temperature is 190℃. After the melt is extruded through the co-extrusion die, it is cast (the temperature of the first cooling roller is 30℃ and the temperature of the second cooling roller is 25℃), cooled, the thickness is measured, and it is wound up to obtain a reaction-compressed wide-temperature-range sound-insulating resin film.

[0057] Comparative Examples 1-3: Comparative Example 1 used a pure PVB sound insulation core layer (without TPU or MAH), Comparative Example 2 was a direct blend of PVB and TPU (without MAH), and Comparative Example 3 was a pre-synthesized MAH-modified PVB re-blended system. The formulations of the sound insulation core layers in Comparative Examples 1-3 are shown in Table 2. The bonding surface layer, overall structure, overall thickness, thickness of each layer, and overall preparation method are all consistent with Examples 1-8.

[0058] Table 2. Formulations of sound insulation core layers in Comparative Examples 1-3 (unit: parts by mass):

[0059] Test Example 1: The performance of the reaction-compressed wide-temperature-range sound-insulating resin films of Examples 1-8 and Comparative Examples 1-3 was tested, and the test standards used for the tests are as follows: 1) Damping performance: Tested according to ISO / PAS 16940 standard, with test temperatures of -10℃, -20℃, 20℃, and 40℃ respectively; 2) Optical performance: Visible light transmittance and haze were tested according to GB / T 2410-2008; 3) Tear resistance: Tested according to GB / T 529-2008; 4) Plasticizer migration: After heat aging at 85℃ for 1000 hours, the migration was tested by Soxhlet extraction. 5) Interlayer peel strength: Tested according to GB / T 2790-1995. The test results are shown in Table 3.

[0060] Table 3 Performance test results of Examples 1-8 and Comparative Examples 1-3:

[0061] As shown in Table 3, Examples 1 to 8 all achieved excellent wide-temperature-range damping performance. The damping value at -10℃ was more than 100% higher than that of the pure PVB system in Comparative Example 1, while the damping at room temperature remained excellent, verifying the significant improvement effect of TPU on low-temperature damping. With the increase of TPU addition, the low-temperature damping and tear strength increased simultaneously. The increase of MAH addition can further strengthen the interfacial bonding force and reduce the amount of plasticizer migration.

[0062] Comparative Example 2, without MAH compatibilizer, exhibited severe phase separation with a haze as high as 3.9%, and its damping and mechanical properties decreased significantly, verifying the necessity of the in-situ compatibilizer system of this invention. Comparative Example 3, using a pre-modified compatibilizer, performed far worse than the one-step in-situ compatibilizer system of this invention, verifying the compatibilizer advantage of the in-situ ring-opening esterification bridging reaction of this invention.

[0063] Different TPUs produce reaction-compressed wide-temperature-range sound-insulating resin films with varying performance characteristics. Example 6 (polycaprolactone-based TPU): achieves a damping value of 15.8% at -20℃, a 55% improvement over adipic acid-based TPUs, effectively expanding the sound insulation temperature range to -20℃, making it suitable for automotive and architectural glass applications in cold regions like Northeast and Northwest China. Example 8 (polycarbonate-based TPU): after 3000 hours of xenon lamp aging, its yellowing index is only 1.2, with a damping performance retention rate of 95%, demonstrating significantly better weather resistance than other TPUs, making it suitable for long-term outdoor applications such as building-integrated photovoltaics (BIPV) and high-speed rail windows. Example 1 (adipic acid-based TPU): exhibits the best overall performance and the lowest raw material cost, making it suitable for large-scale production applications such as automotive side windows and ordinary architectural glass.

[0064] The tear strength of Examples 1-8 is more than 30% higher than that of the pure PVB system, and the amount of plasticizer migration is significantly reduced, which verifies the effect of the present invention on improving mechanical properties and long-term use stability.

[0065] The embodiments of the present invention have been described above; however, these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. All other embodiments obtained by those skilled in the art based on the above embodiments of the present invention without inventive effort are within the protection scope of the present invention.

Claims

1. A reaction-compressed wide-temperature-range sound-insulating resin film, characterized in that, It includes a sound-insulating core layer and an adhesive surface layer covering the sound-insulating core layer; The sound insulation core layer has one or more layers; The adhesive surface layer has one or more layers; The sound insulation core layer comprises the following components in parts by weight: 60-80 parts of polyvinyl butyral, 5-30 parts of thermoplastic polyurethane elastomer, 20-40 parts of plasticizer, 0.1-2 parts of maleic anhydride, and 0.01-2 parts of additives. The maleic anhydride forms a PVB-MAH-TPU covalently bridged structure with the hydroxyl groups on the molecular chain of polyvinyl butyral and the hydroxyl groups at the top of the molecular chain of thermoplastic polyurethane elastomer. The adhesive surface layer comprises the following components in parts by weight: 70-85 parts of polyvinyl butyral, 15-30 parts of plasticizer, and 0.1-2 parts of additives.

2. The reaction-compressed wide-temperature-range sound-insulating resin membrane according to claim 1, characterized in that, The sound insulation core layer contains 5-8 mol of vinyl acetate units of polyvinyl butyral and 10-14 wt% of hydroxyl groups.

3. The reaction-compressed wide-temperature-range sound-insulating resin membrane according to claim 1, characterized in that, The thermoplastic polyurethane elastomer in the sound insulation core layer has a Shore hardness of A70~A90, a weight-average molecular weight of 50,000~120,000, a terminal hydroxyl value of 20~80 mgKOH / g, and a functionality of 2; the thermoplastic polyurethane elastomer is a hydroxyl-terminated polyester thermoplastic polyurethane elastomer.

4. The reaction-compressed wide-temperature-range sound-insulating resin membrane according to claim 1, characterized in that, The additives in the sound insulation core layer include one or more of the following: ultraviolet absorbers, antioxidants, adhesion modifiers, and esterification reaction catalysts.

5. The reaction-compressed wide-temperature-range sound-insulating resin membrane according to claim 1, characterized in that, The adhesive surface layer contains 0.1-11 mol of vinyl acetate units of polyvinyl butyral and 17-22 wt% of hydroxyl groups.

6. The reaction-compressed wide-temperature-range sound-insulating resin membrane according to claim 1, characterized in that, The reaction-compressed wide-temperature-range sound-insulating resin film comprises a first adhesive surface layer, a sound-insulating core layer, and a second adhesive surface layer stacked sequentially; the first adhesive surface layer and the second adhesive surface layer are identical.

7. A method for preparing a reaction-compressed wide-temperature-range sound-insulating resin film, characterized in that, The reaction-compressed wide-temperature-range sound-insulating resin film is the reaction-compressed wide-temperature-range sound-insulating resin film according to any one of claims 1 to 6, comprising the following steps: (1) Mix polyvinyl butyral, thermoplastic polyurethane elastomer, plasticizer, maleic anhydride and additives, melt and carry out in-situ ring-opening esterification bridging reaction to obtain sound insulation core melt; (2) Mix polyvinyl butyral, plasticizer and additives, melt them to obtain a bonding surface melt; (3) The sound insulation core melt and the adhesive surface melt are co-extruded and then cast to obtain the reaction compatibilized wide temperature range sound insulation resin film; There is no requirement for the time order of steps (1) and (2).

8. The preparation method according to claim 7, characterized in that, In step (1), the temperature of the molten screw is 150~210℃ and the screw speed is 200~400rpm.

9. The preparation method according to claim 7, characterized in that, In step (2), the temperature of the molten screw is 140~200℃ and the screw speed is 200~400rpm.

10. The application of a reaction-compressed wide-temperature-range sound-insulating resin film in the automotive, construction, rail transportation, or encapsulation glass fields, characterized in that, The reaction-compressed wide-temperature-range sound-insulating resin membrane is the reaction-compressed wide-temperature-range sound-insulating resin membrane according to any one of claims 1 to 6.

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