Ionic interlayer film for safety glass and preparation method thereof

By combining EMMA-Zn with modified EVA, an ionic intermediate film for safety glass is prepared, and modified fillers are used to improve adhesion and ultraviolet resistance, which solves the problems of high SGP film price and poor UV protection effect in the prior art, and achieves the preparation of an intermediate film with low cost and excellent performance.

CN119242187BActive Publication Date: 2025-08-08SHENGDING HIGHTECH MATERIALS CO LTD
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Patent Information

Application Number
CN202411212123.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-30
Publication Date
2025-08-08
Estimated Expiration
2044-08-30

AI Technical Summary

Technical Problem

In the prior art, although the SGP intermediate film has excellent performance, it is high in price and is difficult to promote. The EVA intermediate film has poor UV protection and is prone to yellowing. It is necessary to develop an intermediate film for safety glass with low cost and good UV resistance.

Method used

The intermediate film is prepared by combining EMMA-Zn with modified EVA by grafting EVA with anti-ultraviolet derivatives and mixing it with modified filler. The modified filler is made of silica treated with a modification coupling agent to form a modified filler with a quaternary ammonium salt group, which improves adhesion and UV resistance.

Benefits of technology

It improves the ultraviolet resistance, mechanical properties and bonding properties of the intermediate film, enhances toughness and impact resistance, and meets the performance requirements of the ionic intermediate film.

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Abstract

The present invention discloses an ionic interlayer for safety glass and a preparation method thereof, belonging to the technical field of glass lamination. The interlayer of the present invention comprises the following components in parts by weight: 60-90 parts of EMMA-Zn, 10-40 parts of modified EVA, and 1-3 parts of a modified filler; the modified EVA is obtained by grafting an anti-UV derivative onto EVA, wherein the anti-UV derivative contains benzophenone groups and unsaturated double bonds; the modified filler is obtained by surface-modifying the filler using a modified coupling agent, wherein the modified coupling agent is obtained by reacting an anti-UV derivative with mercaptopropyltrimethoxysilane. The present invention obtains modified EVA by grafting the anti-UV derivative onto EVA, thereby improving the anti-UV performance and reducing the damage caused by ultraviolet rays to the material, thereby improving the mechanical and optical properties of the material. The anti-UV derivative contains benzophenone groups and unsaturated double bonds, and its molecular structure contains quaternary ammonium salt groups, which can undergo cross-linking when the interlayer is used, thereby improving its mechanical properties.
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Description

Technical Field

[0001] The present invention relates to the technical field of glass lamination, in particular to an ion-type interlayer for safety glass and a preparation method thereof. Background Art

[0002] Laminated glass is a type of safety glass that is currently widely used in the construction and automotive fields. Laminated glass has an interlayer in the middle. Commonly used interlayers include PVB (polyvinyl butyral), SGP (ethylene-methacrylic acid ionic copolymer), EVA (ethylene-vinyl acetate copolymer), TPU (polyurethane elastomer), etc. After undergoing a special high-temperature and high-pressure process, the glass and the interlayer are bonded together.

[0003] For example, patent publication number CN109796907A discloses an EVA interlayer for high-transmittance, aging-resistant laminated glass and its preparation method, while patent publication number CN108892906A discloses an infrared-blocking PVB interlayer and its preparation method. EVA interlayers offer good water resistance, fluidity, and toughness, but they offer poor UV protection and tend to darken and yellow after long-term exposure. However, due to their high cost-effectiveness, they are widely used in the consumer glass industry. PVB interlayers were originally developed for automotive glass and meet the performance requirements, but are sensitive to moisture, requiring the addition of various additives to compensate for these shortcomings. Furthermore, they require edge sealing for safety glass.

[0004] SGP interlayer has high tear strength. Even if the glass is broken, the SGP interlayer can still bond the glass to form a temporary structure after the damage, which greatly improves the safety of the glass. SGP interlayer also has good UV resistance and is not easy to yellow. Although SGP interlayer has excellent performance, its terminal price is high and it is difficult to promote in China. Therefore, it is necessary to develop a low-cost ion-type interlayer for safety glass. Summary of the Invention

[0005] In view of the above problems existing in the prior art, an object of the present invention is to provide an ionomeric interlayer for safety glass. Another object of the present invention is to provide a method for preparing the interlayer.

[0006] EMMA is a new copolymer with high rigidity, impact resistance, and excellent thermal stability. The presence of methyl methacrylate in the EMMA side chain enhances its adhesive properties, and the absence of tertiary hydrogen in the molecular chain gives it better UV resistance than EVA. Combining EVA and EMMA to create an interlayer film improves its UV resistance, imparting excellent toughness and impact resistance.

[0007] In order to solve the above problems, the technical solutions adopted by the present invention are as follows:

[0008] An ionomeric interlayer for safety glass comprises the following components in parts by weight: 60-90 parts of EMMA-Zn, 10-40 parts of modified EVA, and 1-3 parts of modified filler;

[0009] The modified EVA is obtained by grafting an anti-ultraviolet derivative onto EVA, wherein the anti-ultraviolet derivative contains a benzophenone group and an unsaturated double bond;

[0010] The modified filler is obtained by surface-modifying the filler using a modified coupling agent, and the modified coupling agent is obtained by reacting an anti-ultraviolet derivative with mercaptopropyltrimethoxysilane.

[0011] Furthermore, the mass ratio of the filler to the modified coupling agent is 1:1, and the filler is silicon dioxide.

[0012] A method for preparing an ion-type interlayer for safety glass comprises the following steps: mixing EMMA-Zn, modified EVA and modified filler, melting and extruding, casting into a film, cooling, pulling and shaping to form the interlayer.

[0013] Furthermore, the modified EVA is prepared by the following method:

[0014] The modified EVA is obtained by blending EVA and an anti-ultraviolet derivative, performing plate vulcanization, performing electron beam irradiation, and pelletizing.

[0015] Furthermore, the mass ratio of the EVA to the anti-ultraviolet derivative is 100:(0.5~2.0).

[0016] Furthermore, the process conditions of the electron beam irradiation are: in air atmosphere, the absorbed dose is 90-100 kGy, the dose rate is 4.0×10 5 ~4.4×10 5 kGy•h -1 .

[0017] Furthermore, the modified filler is prepared by the following method:

[0018] The filler and the modified coupling agent are mixed, ball-milled, cooled to room temperature, washed, centrifuged, dried and ground to obtain the modified filler.

[0019] Furthermore, the modified coupling agent is prepared by the following method:

[0020] Mix mercaptopropyltrimethoxysilane, anti-ultraviolet derivatives, and initiator, raise the temperature to 63-67° C., and react for 2.0-2.5 hours to obtain a modified coupling agent.

[0021] Furthermore, the mass ratio of the anti-ultraviolet derivative, mercaptopropyltrimethoxysilane, and the initiator is 10:(5.5-6.0):(0.04-0.12).

[0022] Furthermore, the anti-ultraviolet derivative is prepared by the following method:

[0023] 4-Bromomethylbenzophenone and dimethylaminoethyl methacrylate are mixed in a solvent, and reacted at 20-25° C. for 8-12 hours under nitrogen atmosphere to obtain an anti-ultraviolet derivative.

[0024] In the above technical solution, 4-bromomethylbenzophenone reacts with dimethylaminoethyl methacrylate to produce an anti-UV derivative containing quaternary ammonium groups and allyl groups. The modified EVA is obtained by grafting the anti-UV derivative onto the EVA. The formation of anti-UV derivative side chains on the EVA molecular chain increases the spacing between the EVA main chains, facilitates the movement of the modified EVA molecular chain, and improves the elongation at break of the resulting interlayer. The quaternary ammonium groups in the modified EVA form strong bonds with the surfaces of glass and inorganic fillers, thereby enhancing the adhesion of the resulting interlayer, improving the mechanical properties, and, to a certain extent, the optical properties.

[0025] In the above technical solution, the unsaturated double bonds of the UV-resistant derivative undergo a thermal click reaction with the mercapto groups in mercaptopropyltrimethoxysilane via the initiator AIBN, producing a siloxane containing UV-resistant groups and quaternary ammonium salt groups, referred to as a modified coupling agent. This agent is used to surface-modify the filler, increasing the number of UV-resistant groups within the interlayer system, organicizing the filler surface and imparting UV-absorbing properties. This agent, in synergistic with the UV-shielding capabilities of silica filler, further improves the UV resistance of the interlayer. It also helps improve the compatibility between the filler and the modified EVA, enabling the filler's full performance to be fully utilized within the interlayer. The quaternary ammonium salt groups on the surface of the modified filler form strong bonds to the glass surface, enhancing the adhesion of the resulting interlayer. The combination of the modified EVA and EMMA-Zn further enhances the toughness and impact resistance of the interlayer, bringing it up to the performance requirements of an ionic interlayer.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] (1) The present invention provides a method for preparing an ionic interlayer for safety glass. By grafting an anti-ultraviolet derivative onto EVA, a modified EVA is obtained, which improves the anti-ultraviolet performance, reduces the damage of ultraviolet rays to the interlayer, and helps improve its mechanical and optical properties. The anti-ultraviolet derivative contains benzophenone groups and unsaturated double bonds, and contains quaternary ammonium salt groups in its molecular structure. It can form strong bonds with inorganic fillers and glass surfaces, thereby improving the mechanical and adhesive properties of the prepared interlayer. The combination of modified EVA and EMMA-Zn further improves the toughness and impact resistance of the interlayer, so that it meets the performance requirements of an ionic interlayer.

[0028] (2) The method for preparing an ionic interlayer for safety glass of the present invention improves the adhesion of the interlayer to glass, improves the dispersion of silica in the interlayer, and enhances the compatibility of the interlayer with the glass, making the silica more evenly distributed in the material and forming a more stable composite material. The modified coupling agent is prepared from raw materials such as UV-resistant derivatives and can improve the compatibility of the filler while being compounded with the filler to enhance the UV resistance of the prepared interlayer. DETAILED DESCRIPTION

[0029] The present invention will be further described below with reference to specific embodiments.

[0030] In the following specific embodiments,

[0031] EMMA-Zn: Brand 9520, from Dow Chemical, USA;

[0032] EVA: CAS number: 24937-78-8, derived from MacLean reagent;

[0033] Silicon dioxide, CAS number: 14808-60-7, was obtained from Shandong Pingju Biotechnology Co., Ltd.

[0034] Dimethylaminoethyl methacrylate (CAS No. 2867-47-2), derived from MacLean's reagent;

[0035] 4-Bromomethylbenzophenone (CAS No. 32752-54-8), derived from MacLean's reagent;

[0036] UV absorber (CAS No.: 131-56-6) was obtained from Hubei Watson Chemical Technology Co., Ltd.

[0037] The rest are commercially available conventional chemicals.

[0038] The thickness of the intermediate film is 0.35mm~0.75mm.

[0039] The following specific implementation methods are laboratory tests and can be scaled up in equal proportions.

[0040] Example 1

[0041] A method for preparing an ion-type interlayer for safety glass comprises the following steps:

[0042] Step (1) Preparation of modified EVA:

[0043] 4-Bromomethylbenzophenone and dimethylaminoethyl methacrylate were mixed in acetone and reacted at 20°C for 10 hours under a nitrogen atmosphere. The white solid was filtered out, and the filtrate was evaporated to dryness. Another portion of the solid was washed with ether, and the two solids were combined and recrystallized with acetone to obtain an anti-UV derivative. The ratio of 4-bromomethylbenzophenone to acetone was 2.5 g / 100 mL; the molar ratio of 4-bromomethylbenzophenone to dimethylaminoethyl methacrylate was 1:1.

[0044] EVA and anti-ultraviolet derivatives were blended at 90°C for 10 min, flat-plate vulcanized at 110°C and 10 MPa, pressed into 1 mm sheets, hot-pressed for 2 min, preheated for 3 min before hot-pressing, and electron beam irradiated in air with an absorbed dose of 90 kGy and a dose rate of 4.4 × 105 kGy·h. -1 , pelletized to obtain modified EVA; the mass ratio of EVA and anti-ultraviolet derivative is 100:0.5.

[0045] Step (2) Preparation of modified filler:

[0046] Mercaptopropyltrimethoxysilane, an anti-ultraviolet derivative, and an initiator are mixed, heated to 63° C., and reacted for 2 hours to obtain a modified coupling agent; the mass ratio of the anti-ultraviolet derivative, mercaptopropyltrimethoxysilane, and the initiator is 10:5.5:0.04; and the initiator is azobisisobutyronitrile.

[0047] The silica and modified coupling agent were mixed and ball-milled at a ball-to-material mass ratio of 1:1, a ball mill speed of 400 r / min, and the forward and reverse rotations were performed for 2 hours each; the mixture was cooled to room temperature, washed, centrifuged at a centrifugal speed of 5000 r / min, and the centrifugal time was 5 minutes; the mixture was dried, and ground at a grinder speed of 200 r / min for 30 minutes to obtain a modified filler. The mass ratio of silica to the modified coupling agent was 1:1.

[0048] Step (3) Preparation of the intermediate film: EMMA-Zn, modified EVA and modified filler are mixed and conveyed to the barrel of the extruder through the equipment. The molten mixture in the extruder is cast into a film with a melting temperature of 70°C through the rotation of the screw, and then cooled, pulled and shaped to form an intermediate film with a thickness of 0.35 mm. The mass ratio of EMMA-Zn, modified EVA and modified filler is 90:10:1.

[0049] Example 2

[0050] A method for preparing an ion-type interlayer for safety glass comprises the following steps:

[0051] Step (1) Preparation of modified EVA:

[0052] 4-Bromomethylbenzophenone and dimethylaminoethyl methacrylate were mixed in acetone and reacted at 22°C for 10 hours under a nitrogen atmosphere. The white solid was filtered out, and the filtrate was evaporated to dryness. The remaining solid was washed with ether, and the two solids were combined and recrystallized with acetone to obtain an anti-UV derivative. The ratio of 4-bromomethylbenzophenone to acetone was 2.5 g / 100 mL; the molar ratio of 4-bromomethylbenzophenone to dimethylaminoethyl methacrylate was 1:1.3.

[0053] EVA and anti-ultraviolet derivatives were blended at 92°C for 13 minutes, flat-plate vulcanized at 112°C and 10 MPa, pressed into 1 mm sheets, hot-pressed for 2 minutes, preheated for 3 minutes before hot-pressing, and electron beam irradiated in air with an absorbed dose of 95 kGy and a dose rate of 4.6 × 105 kGy·h. -1 , pelletized to obtain modified EVA; the mass ratio of EVA and anti-ultraviolet derivative is 100:1.

[0054] Step (2) Preparation of modified filler:

[0055] Mercaptopropyltrimethoxysilane, an anti-ultraviolet derivative, and an initiator are mixed, heated to 65° C., and reacted for 2.3 hours to obtain a modified coupling agent; the mass ratio of the anti-ultraviolet derivative, mercaptopropyltrimethoxysilane, and the initiator is 10:5.7:0.08; and the initiator is azobisisobutyronitrile AIBN.

[0056] The silica and modified coupling agent were mixed and ball-milled at a ball-to-material mass ratio of 1:1, a ball mill speed of 450 r / min, and the forward and reverse rotations were performed for 2.3 h each; the mixture was cooled to room temperature, washed, centrifuged at a centrifugal speed of 5500 r / min, and the centrifugal time was 7 min, dried, and ground at a grinder speed of 250 r / min for 32 min to obtain a modified filler with a silica and modified coupling agent mass ratio of 1:1.

[0057] Step (3) is the same as step (3) in Example 1 to obtain an intermediate film. The mass ratio of EMMA-Zn, modified EVA, and modified filler is 75:25:2, and the thickness of the intermediate film is 0.55 mm.

[0058] Example 3

[0059] A method for preparing an ion-type interlayer for safety glass comprises the following steps:

[0060] Step (1) Preparation of modified EVA: 4-bromomethylbenzophenone and dimethylaminoethyl methacrylate were mixed in acetone and reacted at 25°C for 10 h under nitrogen atmosphere; a white solid was filtered out, and the other part of the solid obtained after evaporating the filtrate was washed with ether, and the solids obtained from the two times were combined and recrystallized with acetone to obtain an anti-ultraviolet derivative; the ratio of 4-bromomethylbenzophenone to acetone was 2.5 g / 100 mL; the molar ratio of 4-bromomethylbenzophenone to dimethylaminoethyl methacrylate was 1:1.5.

[0061] EVA and anti-UV derivatives were blended at 92°C for 15 min, flat-plate vulcanized at 115°C and 10 MPa, pressed into 1 mm sheets, hot-pressed for 2 min, preheated for 3 min before hot-pressing, and electron beam irradiated in air with an absorbed dose of 100 kGy and a dose rate of 4.8 × 105 kGy·h. -1 , pelletized to obtain modified EVA; the mass ratio of EVA and anti-ultraviolet derivative is 100:2.

[0062] Step (2) Preparation of modified filler:

[0063] Mercaptopropyltrimethoxysilane, an anti-ultraviolet derivative, and an initiator are mixed, heated to 67° C., and reacted for 2.5 hours to obtain a modified coupling agent; the mass ratio of the anti-ultraviolet derivative, mercaptopropyltrimethoxysilane, and the initiator is 10:6:0.12; and the initiator is azobisisobutyronitrile AIBN.

[0064] The silica and modified coupling agent were mixed and ball-milled at a ball-to-material mass ratio of 1:1, a ball mill speed of 500 r / min, and the forward and reverse rotations were performed for 2.5 h each; the mixture was cooled to room temperature, washed, centrifuged at a centrifugal speed of 6000 r / min, and the centrifugal time was 10 min, dried, and ground at a grinder speed of 300 r / min for 35 min to obtain a modified filler with a silica and modified coupling agent mass ratio of 1:1.

[0065] Step (3) is the same as step (3) in Example 1 to obtain an intermediate film; the mass ratio of EMMA-Zn, modified EVA, and modified filler is 60:40:3, and the thickness of the intermediate film is 0.75 mm.

[0066] Comparative Example 1

[0067] A method for preparing a glass interlayer film includes the following processes:

[0068] Step (1) Preparation of modified EVA:

[0069] EVA, 4-propyleneoxy-2-hydroxybenzophenone and dimethyldiallylammonium chloride were mixed at 90°C for 10 min, vulcanized at 110°C and 10 MPa, pressed into 1 mm sheets, and hot pressed for 2 min. Before hot pressing, the sheets were preheated for 3 min and irradiated with electron beams. The absorbed dose was 90 kGy and the dose rate was 4.4×105 kGy·h in air atmosphere. -1 , pelletizing to obtain modified EVA; the mass ratio of EVA, 4-propyleneoxy-2-hydroxybenzophenone, and dimethyldiallylammonium chloride is 100:0.3:0.2.

[0070] Step (2) Preparation of modified filler:

[0071] Silica and coupling agent (KH-570) were mixed and ball-milled at a ball-to-material mass ratio of 1:1, a ball mill speed of 400 r / min, and the forward and reverse rotations were performed for 2 hours each; cooled to room temperature, washed, centrifuged at a centrifugal speed of 5000 r / min, the centrifugal time was 5 minutes, dried, and ground at a grinder speed of 200 r / min for 30 minutes to obtain a modified filler with a silica:KH-570 mass ratio of 1:1.

[0072] Step (3) Preparation of the intermediate film: EMMA-Zn, modified EVA and modified filler are mixed and conveyed to the barrel of the extruder through the equipment. The molten mixture in the extruder is cast into a film with a melting temperature of 70°C through the rotation of the screw, and then cooled, pulled and shaped to form an intermediate film with a thickness of 0.35 mm. The mass ratio of EMMA-Zn, modified EVA and modified filler is 60:10:1.

[0073] Comparative Example 2

[0074] A method for preparing an interlayer film for glass, comprising the following steps:

[0075] Step (1) Preparation of modified EVA:

[0076] EVA and dimethyldiallylammonium chloride were blended at 90°C for 10 min, flat-plate vulcanized at 110°C and 10 MPa, pressed into 1 mm sheets, and hot-pressed for 2 min. Before hot-pressing, the sheets were preheated for 3 min and irradiated with electron beams. The absorbed dose was 90 kGy and the dose rate was 4.4×105 kGy·h in air atmosphere. -1 , pelletized to obtain modified EVA; the mass ratio of EVA and dimethyl diallyl ammonium chloride is 100:0.2.

[0077] Step (2) Preparation of modified filler:

[0078] Silica and coupling agent (KH-570) were mixed and ball-milled at a ball-to-material mass ratio of 1:1, a ball mill speed of 400 r / min, and the forward and reverse rotations were performed for 2 hours each; cooled to room temperature, washed, centrifuged at a centrifugal speed of 5000 r / min, the centrifugal time was 5 minutes, dried, and ground at a grinder speed of 200 r / min for 30 minutes to obtain a modified filler with a silica:KH-570 mass ratio of 1:1.

[0079] Step (3) Preparation of the intermediate film: EMMA-Zn, modified EVA, modified filler, and anti-ultraviolet absorber are mixed with a melting temperature of 70°C, and are transferred to the barrel of an extruder through an equipment. The molten mixture in the extruder is cast into a film by the rotation of the screw, and is cooled, pulled, and shaped to form an intermediate film. The thickness of the intermediate film is 0.35 mm. The mass ratio of EMMA-Zn, modified EVA, modified filler, and anti-ultraviolet absorber is 60:10:1:0.3.

[0080] Comparative Example 3

[0081] A method for preparing an interlayer film for glass, comprising the following steps:

[0082] Step (1) Preparation of modified filler:

[0083] Silica and coupling agent (KH-570) were mixed and ball-milled at a ball-to-material mass ratio of 1:1 at a ball mill speed of 400 r / min for 2 hours each in both forward and reverse directions; cooled to room temperature, washed, centrifuged at a centrifugal speed of 5000 r / min for 5 minutes, dried, and ground at a grinding speed of 200 r / min for 30 minutes to obtain a modified filler with a silica:KH-570 mass ratio of 1:1;

[0084] Step (2) Preparation of the intermediate film: EMMA-Zn, EVA, modified filler, and UV absorber are melt-mixed at a melting temperature of 70°C, and are transferred to the barrel of an extruder through an apparatus. The molten mixture in the extruder is cast into a film by the rotation of the screw, and is cooled, pulled, and shaped to form an intermediate film. The thickness of the intermediate film is 0.35 mm. The mass ratio of EMMA-Zn, EVA, modified filler, and UV absorber is 60:10:1:0.3.

[0085] Test experiment:

[0086] The interlayer films obtained in Examples 1 to 3 and Comparative Examples 1 to 3 were used to prepare samples, and their properties were tested and the test results were recorded.

[0087] Tensile performance test: GB / T 528 is used as the reference standard to test the tensile performance of the sample. The sample is dumbbell-shaped and the tensile rate is 100 mm / min.

[0088] Adhesion strength test: GB / T 2790 was used as the reference standard to test the adhesion strength between the sample and the glass. The interlayer sample was placed on the glass surface and laminated. The lamination process conditions were: lamination temperature of 145°C and lamination time of 10 minutes.

[0089] UV resistance test: The prepared interlayer was placed on a U-3010 spectrometer for UV spectrum detection, with a scanning wavelength range of 220-400nm and a scanning speed of 600nm•min -1 , with a step size of 1 nm. After UV irradiation for 144 h, the tensile properties of the samples were tested again.

[0090] The test results are as follows:

[0091]

[0092] According to the data in the above table, we can clearly draw the following conclusions:

[0093] The intermediate films obtained in Examples 1-3 were compared with those obtained in Comparative Examples 1-3. The test results show that:

[0094] Compared with Comparative Example 1, the intermediate films obtained in Examples 1-3 have better tensile strength, bonding strength and anti-ultraviolet tensile strength, which fully demonstrates that the setting of EMMA-Zn, modified EVA and modified filler in the present invention can effectively improve the tensile strength, bonding strength and anti-ultraviolet tensile strength of the intermediate films.

[0095] Compared to Example 1, Comparative Example 1 replaced the UV-resistant derivative with 4-propyleneoxy-2-hydroxybenzophenone and dimethyldiallylammonium chloride. During electron beam irradiation, 4-propyleneoxy-2-hydroxybenzophenone and dimethyldiallylammonium chloride were grafted onto EVA. The modified filler was made from KH-570-modified silica. The interlayer film obtained in Comparative Example 1 exhibited changes in the modified EVA side chains, resulting in decreased UV stability and a significant decrease in tensile strength and post-UV aging tensile strength.

[0096] Compared to Example 1, Comparative Example 2 replaced the UV-resistant derivative with dimethyldiallylammonium chloride, and the interlayer was a blend of modified EVA, modified filler, and UV absorber. The UV-resistant absorber did not form side chains on the EVA molecules. As shown in the table above, the interlayer obtained in Comparative Example 2 exhibited reduced tensile strength, adhesive strength, and tensile strength after UV aging.

[0097] Compared with Example 1, the intermediate film obtained in Comparative Example 3 is prepared by blending the intermediate film of EVA, modified filler and ultraviolet absorber. The intermediate film obtained in Comparative Example 3 has a significant decrease in tensile strength, adhesive strength and tensile strength data after ultraviolet aging. The reason is that the intermediate film obtained in Comparative Example 3 is a blend of EVA, modified filler and ultraviolet absorber, and the anti-ultraviolet absorber does not form a branched chain on the EVA molecule, nor does it form a quaternary ammonium salt group, which reduces the anti-ultraviolet stability of the modified EVA and weakens the bonding ability between the modified EVA and the glass and filler, which is reflected in the decrease in the tensile strength, adhesive strength and tensile strength after ultraviolet aging of the intermediate film. It can be seen that the preparation process of the intermediate film and the setting of the components used in this application can promote the comprehensive improvement of its mechanical properties, bonding properties and anti-ultraviolet properties.

[0098] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "include," "comprise," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or apparatus comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0099] Finally, it should be noted that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein with equivalents. Any modifications, equivalent replacements, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. An ionomeric interlayer for safety glass, characterized in that: The composition comprises the following components in parts by weight: 60-90 parts of EMMA-Zn, 10-40 parts of modified EVA, and 1-3 parts of modified filler; The modified EVA is obtained by grafting an anti-ultraviolet derivative onto EVA, wherein the anti-ultraviolet derivative contains a benzophenone group and an unsaturated double bond; The modified filler is obtained by surface-modifying the filler using a modified coupling agent, wherein the modified coupling agent is obtained by reacting an anti-ultraviolet derivative with mercaptopropyltrimethoxysilane; The anti-ultraviolet derivative is prepared by the following method: 4-Bromomethylbenzophenone and dimethylaminoethyl methacrylate are mixed in a solvent, and reacted at 20-25° C. for 8-12 hours under nitrogen atmosphere to obtain an anti-ultraviolet derivative.

2. The ionomeric interlayer for safety glass according to claim 1, characterized in that: The mass ratio of the filler to the modified coupling agent is 1:1, and the filler is silicon dioxide.

3. A method for preparing an ionomeric interlayer for safety glass according to any one of claims 1 or 2, characterized in that: The EMMA-Zn, modified EVA and modified filler are mixed, melt-extruded, cast into a film, cooled, pulled and shaped to form an intermediate film.

4. The method for preparing an ionic interlayer for safety glass according to claim 3, characterized in that: Described modified EVA is prepared by the following method: The modified EVA is obtained by blending EVA and an anti-ultraviolet derivative, performing plate vulcanization, performing electron beam irradiation, and pelletizing.

5. The method for preparing an ionomeric interlayer for safety glass according to claim 4, characterized in that: The mass ratio of the EVA to the anti-ultraviolet derivative is 100:(0.5-2.0).

6. The method for preparing an ionic interlayer for safety glass according to claim 4, characterized in that: The process conditions of the electron beam irradiation are: in air atmosphere, the absorbed dose is 90-100 kGy, the dose rate is 4.0×10 5 ~4.4×10 5 kGy•h -1 .

7. The method for preparing an ionomeric interlayer for safety glass according to claim 3, characterized in that: The modified filler is prepared by the following method: The filler and the modified coupling agent are mixed, ball-milled, cooled to room temperature, washed, centrifuged, dried and ground to obtain the modified filler.

8. The method for preparing an ionomeric interlayer for safety glass according to claim 7, characterized in that: The modified coupling agent is prepared by the following method: Mix mercaptopropyltrimethoxysilane, anti-ultraviolet derivatives, and initiator, raise the temperature to 63-67° C., and react for 2.0-2.5 hours to obtain a modified coupling agent.

9. The method for preparing an ionomeric interlayer for safety glass according to claim 8, characterized in that: The mass ratio of the anti-ultraviolet derivative, mercaptopropyltrimethoxysilane and the initiator is 10:(5.5-6.0):(0.04-0.12).

Citation Information

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  • Ionization modified ethylene-acrylic acid copolymer and preparation method thereof, and ionic polymer intermediate membrane and application thereof

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