Ionic intermediate membrane and preparation method thereof
By using a three-layer ionic interlayer design and additive formulation, the problems of insufficient boiling water solubility and insufficient impact resistance of ionic interlayers in existing technologies have been solved, enabling the application of laminated glass with high safety and optical performance.
Patent Information
- Application Number
- CN202511138827.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-14
- Publication Date
- 2025-11-21
AI Technical Summary
Existing ionic interlayer films are easily dissolved in boiling tests and have insufficient impact values, making it difficult to meet the high safety requirements of laminated glass standards, and there is a risk of cross-linking during processing.
An ionic intermediate membrane with a three-layer structure is used. The intermediate layer is composed of Sarin resin A and B, and the surface layer uses Kuraray Plus edge material. Silane coupling agent, antioxidant, UV cut-off agent and plasticizer are added. It is prepared by co-extrusion through a composite mold. The material ratio and additive dosage are optimized to improve boiling water solubility and impact value.
It achieves excellent resistance to boiling water hydrolysis of ionomer interlayer, meets the impact value standard for laminated glass, and meets the requirements for visible light transmittance and haze, thus improving the safety of the processing.
Smart Images

Figure CN120986019A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of ionic intermediate membrane technology, specifically relating to an ionic intermediate membrane and its preparation method. Background Technology
[0002] Laminated glass is typically a composite glass product made by bonding one or more layers of polymer interlayer between two or more panes of glass. This bonding process involves high-temperature pre-pressing (or vacuuming) and high-temperature, high-pressure lamination, permanently bonding the glass and interlayer together. The main purpose of using a polymer interlayer is to prevent the laminated glass from breaking after severe vibration or impact, or to prevent large-scale glass detachment if it does break.
[0003] Currently, the commonly used interlayer films for laminated glass are EVA, PVB, and ionomer interlayer films. Among them, EVA and PVB are far inferior to ionomer interlayer films in terms of load-bearing strength and tear strength. Therefore, ionomer interlayer films are generally used in laminated glass applications with higher safety requirements.
[0004] Enterprises generally use the standards GB 15763.3-2009 Safety Glass for Building Part 3: Laminated Glass, JCT 2763-2023 Ionic Interlayer for Laminated Glass, and TZBH 014-2021 Ionic Interlayer Film as benchmarks to define the requirements for laminated glass made with ionic interlayer film. In addition to the characteristics of the interlayer film itself, laminated glass manufacturers pay attention to the boiling test, impact test, radiation resistance test, moisture resistance test, baking test, falling ball impact test, and shot bag impact test of laminated glass products.
[0005] The main material used in ionic interlayer membranes is saline resin, which is produced by copolymerizing ethylene and methacrylic acid and then neutralizing with sodium or zinc. For ionic interlayer membranes, some saline resins, such as common saline resins AE4500 and PC2200, are soluble in boiling water, leading to insufficient adhesive around the edges of the sample after boiling tests, which can easily result in failure. Furthermore, the methacrylic acid content of commercially available saline resins is relatively low, resulting in a low tapping value during use. Therefore, ionic interlayer membranes sometimes have a silane-based adhesion promoter coated on the glass before lamination to improve the tapping value.
[0006] Chinese patent CN 114196330 A discloses an ionomer-type interlayer for laminated glass and its preparation method. It uses Surlyn PC2000, Surlyn AE4500, Surlyn 8940, and Surlyn 8920 resins, with the addition of silane, organic peroxides, plasticizers, heat stabilizers, and other additives, followed by extrusion of the film. Performance testing showed that only the 40% Surlyn AE4500+60% Surlyn 8940, 50% Surlyn AE4500+50% Surlyn 8940, and 100% Surlyn 9150 solutions met the knocking value requirements of JCT 2763-2023 Ionic Interlayers for Laminated Glass. However, the 100% Surlyn 9150 solution did not meet the haze requirements for laminated glass. Furthermore, a boiling test was not performed. In the formulations of AE4500 + 60% Surlyn 8940 and 50% Surlyn AE4500 + 50% Surlyn 8940, the film contains a relatively high amount of AE4500. During the boiling test, significant glue deficiency occurs, resulting in the boiling test failing to meet the requirements of glass processing companies. Furthermore, in this patent, if organic peroxides are used as additives, the decomposition temperature of organic peroxides is 70-100℃, while the melting point of saline resin is generally above 80℃, and the processing temperature is generally above 120℃. Therefore, there is a risk of cross-linking of saline resin during extrusion, requiring extremely high processing standards.
[0007] Chinese Patent CN 110615934 A discloses a method for modifying ionic intermediate membrane raw materials, comprising the following steps: (1) stirring a sarin substrate with a certain proportion of KH550 and ECH additives; (2) adding an anti-ultraviolet additive and an antioxidant additive to the mixture in step (1) and stirring at high speed; (3) adding the mixture in step (2) to a granulator and granulating and modifying it at 170°C. The principle is to graft KH550 and ECH onto the sarin resin to form a hydrophobic layer, thereby blocking the dissolution of the resin by boiling water, thus increasing the probability of the ionic intermediate membrane passing the boiling test. At the same time, the granulation and grafting of KH550 onto the sarin resin restricts the free movement of KH550, reducing the probability of cross-linking of the sarin resin and the appearance of extruded particle crystal points caused by the reaction of the sarin resin with a large amount of KH550. However, ECH has certain toxicity and potential carcinogenic risks, which limits its use. In addition, in this patent, the ratio of Sarin resin to KH550 is 10:1. Even if the risk of crosslinking is reduced by granulation and grafting, the processing and storage requirements for the grafted material are extremely high. Summary of the Invention
[0008] To solve the above-mentioned technical problems, the present invention provides an ionic interlayer and its preparation method. The ionic interlayer has excellent resistance to boiling water hydrolysis, and its knock value meets the requirements of the knock value specified in JCT 2763-2023 Ionic Interlayer for Laminated Glass. Moreover, its visible light transmittance and haze meet the requirements of laminated glass.
[0009] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0010] An ionic intermediate membrane, the ionic intermediate membrane being composed of an intermediate layer and a surface layer;
[0011] The intermediate layer comprises the following raw materials by weight percentage: 20-50% Saryn resin A and 50-80% Saryn resin B; wherein Saryn resin A is any one or more of Surlyn AE4500, Surlyn PC2000, Surlyn PC2200, and Surlyn AE4800; and wherein Saryn resin B is any one or more of Surlyn 8940, Surlyn 8920, Surlyn 8150, and Surlyn 9150.
[0012] The surface layer comprises the following raw materials by weight percentage: 20%–90% intermediate layer raw materials, Kuraray. Plus, scrap material accounts for 10% to 80%.
[0013] Furthermore, the thickness of the intermediate layer is 50% to 90% of the thickness of the ionic intermediate film. (Kuraray) Plus edge material is generally the edge material left over from the lamination and cutting process in laminated glass factories. It has poor cleanliness. If the surface layer thickness is too large, it will lead to a poor appearance of the ionomer interlayer. However, if the surface layer thickness is too small, the inner layer material will cross-contaminate in some places due to fluctuations in the processing equipment. Therefore, it is necessary to control the thickness of the interlayer to 50% to 90% of the thickness of the ionomer interlayer. While ensuring that the inner layer material does not cross-contaminate, the surface layer thickness should be reduced as much as possible.
[0014] The raw materials for both the intermediate and surface layers also include silane coupling agents, antioxidants, UV cut-off agents, and plasticizers.
[0015] In the intermediate layer, the mass of the silane coupling agent, antioxidant, UV cut-off agent, and plasticizer are 0.5%-1.5%, 0.1%-0.6%, 0.1%-0.5%, and 0.5%-2% of the sum of the masses of Sarin resin A and Sarin resin B, respectively.
[0016] In the surface layer, the mass percentages of silane coupling agent, antioxidant, UV cut-off agent, and plasticizer are 0.1%-1%, 0.1%-0.6%, 0.1%-0.5%, and 0.5%-2% of the sum of the masses of Sarin resin A and Sarin resin B, respectively.
[0017] The silane coupling agent is any one or more of γ-methacryloxypropyltrimethoxysilane, vinyltris(2-methoxyethoxy)silane, vinyltrimethylsilane, γ-(2,3-epoxypropoxy)propyltrimethoxysilane, and 3-aminopropyltriethoxysilane.
[0018] The antioxidant is any one or more of the following: pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 4-[(4,6-dioctylthio-1,3,5-triazin-2-yl)amino]-2,6-di-tert-butylphenol, propoxyglycerol triacrylate, octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, tris(2,4-di-tert-butylphenyl) phosphite, tri-tert-butyl-p-hydroxyphenylpropane, poly(4-hydroxy-2,2,6,6-tetramethyl-1-piperidine ethanol) ester, and bis-2,2,6,6-tetramethylpiperidinol sebacate.
[0019] The UV cutoff agent is any one or more of [2-hydroxy-4-(octoxy)phenyl]phenyl ketone, 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-(2-hydroxy-3,5-bis(a,a-dimethylbenzyl)phenyl)benzotriazole, and 2-(2H-benzotriazol-2-yl)-4-(1,1,3,3-tetramethylbutyl)phenol.
[0020] The plasticizer is any one or more of triethylene glycol diisooctyl ester, oleic acid, 3-octenic acid, diisononyl phthalate, and dioctyl sebacate.
[0021] The present invention also provides a method for preparing the ionic intermediate film, the method comprising the following steps: mixing the surface layer and intermediate layer raw materials evenly, extruding them by melt co-extrusion through a composite mold, casting them into a film, and then cooling, trimming, and winding them to obtain the finished product.
[0022] The ionic intermediate membrane provided by this invention has a three-layer structure. The intermediate layer is made by compounding particles, combining sarin resin A, which is easily soluble in boiling water, with sarin resin B, which is insoluble in boiling water. The ratio is adjusted to meet the optical performance requirements while minimizing the amount of sarin resin A, which is easily soluble in boiling water, thereby improving the boiling water solubility of the intermediate layer. In addition, a small amount of silane coupling agent can be added to further improve the hydrolysis resistance of the compounded particles by reacting silane with sarin resin. Antioxidants, UV cut-off agents, plasticizers and other additives can also be added to improve the plasticity and antioxidant properties of the ionic intermediate membrane.
[0023] The surface layer combines the intermediate layer raw materials with Kuraray. Plus edge material compounding, supplementing the ionomer interlayer and glass impact resistance, and improving the surface hydrolysis resistance, imported Kuraray. The high methacrylic acid content in the Plus edge material can improve the knock value of the ionic intermediate film. In addition, a small amount of silane coupling agent can be added to further improve the hydrolysis resistance of the surface layer by reacting silane with sarin resin. Antioxidants, UV cut-off agents, plasticizers and other additives can also be added to improve the plasticity and antioxidant properties of the ionic intermediate film.
[0024] The method for preparing the ionic intermediate membrane provided by the present invention is simple. The ionic intermediate membrane with a surface-intermediate-surface structure can be obtained by co-extrusion through a composite mold.
[0025] The present invention also provides a laminated glass, wherein the laminated glass uses the ionized interlayer film described in the present invention, and the impact value, visible light transmittance and haze of the laminated glass all meet the requirements for use of laminated glass.
[0026] Compared with the prior art, the present invention has the following beneficial effects:
[0027] The preparation method of the ionic interlayer provided by the present invention is simple. The ionic interlayer has excellent resistance to boiling water hydrolysis, and the knock value meets the requirements of the knock value specified in "JCT 2763-2023 Ionic Interlayer for Laminated Glass". The visible light transmittance and haze meet the requirements of laminated glass. Attached Figure Description
[0028] Figure 1 This is a schematic diagram of the structure of the ionic intermediate membrane in this invention, where 1 is the intermediate layer and 2 is the surface layer. Detailed Implementation
[0029] The present invention will now be described in detail with reference to the embodiments.
[0030] Example 1
[0031] An ionic intermediate membrane, consisting of an intermediate layer and a surface layer;
[0032] The main ingredients and their weight percentages in the intermediate layer are: 20% Surlyn AE4500, 60% Surlyn 8940, and 20% Surlyn 8920. Vinyltrimethylsilane, 3-aminopropyltriethoxysilane, antioxidants, UV cut-off agents, and plasticizers are added as additives, with addition amounts of 0.6%, 0.3%, 0.2%, 0.1%, and 1.2% of the above main ingredients by weight, respectively.
[0033] The main ingredients and their weight percentage in the surface layer are: 50% intermediate layer ingredients, 50% Kuraray.
[0034] Plus edge material, wherein the middle layer material is composed of the following raw materials by weight percentage: 20% Surlyn AE4500, 60% Surlyn 8940, and 20% Surlyn 8920; the surface layer material also contains 3-aminopropyltriethoxysilane, antioxidant, UV cut-off agent, and plasticizer as additives, and their addition amounts are 0.2%, 0.2%, 0.1%, and 1.2% of the above main materials by weight, respectively.
[0035] In this embodiment, the antioxidant, UV cut-off agent, and plasticizer are pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], [2-hydroxy-4-(octoxy)phenyl]phenyl ketone, and triethylene glycol diisooctanoate, respectively.
[0036] The thickness of the intermediate layer is 60% of the thickness of the ionic intermediate film.
[0037] The method for preparing the ionic intermediate membrane includes the following steps:
[0038] (1) Ingredients: Mix the main ingredients and additives in the middle layer and the surface layer according to the formula; control the mixing temperature at 50-70℃ and the mixing speed at 5-20 rpm.
[0039] (2) Melt co-extrusion: The intermediate layer material and the surface layer material are fed into the extruder for melt extrusion, and then enter the composite mold to form a film. After cooling, trimming and winding, the finished product is obtained. The conditions for melt co-extrusion are: the temperature of the extruder feed port section is set at 70-100℃, the temperature of other areas of the screw is set at 130-220℃, and the temperature of the composite mold is set at 150-200℃.
[0040] Example 2
[0041] An ionic intermediate membrane, consisting of an intermediate layer and a surface layer;
[0042] The main ingredients and their weight percentages in the intermediate layer are: 20% Surlyn AE4500, 60% Surlyn 8940, and 20% Surlyn 8920. Vinyltrimethylsilane, 3-aminopropyltriethoxysilane, antioxidants, UV cut-off agents, and plasticizers are added as additives, with addition amounts of 0.6%, 0.3%, 0.2%, 0.1%, and 1.2% of the above main ingredients by weight, respectively.
[0043] The main ingredients and their weight percentages in the surface layer are: 30% intermediate layer ingredients, 70% Kuraray.
[0044] Plus edge material, wherein the middle layer material is composed of the following raw materials by weight percentage: 20% Surlyn AE4500, 60% Surlyn 8940, and 20% Surlyn 8920; the surface layer material also contains 3-aminopropyltriethoxysilane, antioxidant, UV cut-off agent, and plasticizer as additives, and their addition amounts are 0.2%, 0.2%, 0.1%, and 1.2% of the above main materials by weight, respectively.
[0045] In this embodiment, the antioxidant, UV cut-off agent, and plasticizer are propoxylated glycerol triacrylate, 2,4-dihydroxybenzophenone, and 3-octenic acid, respectively.
[0046] The thickness of the intermediate layer is 60% of the thickness of the ionic intermediate film.
[0047] The method for preparing the ionic intermediate membrane includes the following steps:
[0048] (1) Ingredients: Mix the main ingredients and additives in the middle layer and the surface layer according to the formula; control the mixing temperature at 50-70℃ and the mixing speed at 5-20 rpm.
[0049] (2) Melt co-extrusion: The intermediate layer material and the surface layer material are fed into the extruder for melt extrusion, and then enter the composite mold to form a film. After cooling, trimming and winding, the finished product is obtained. The conditions for melt co-extrusion are: the temperature of the extruder feed port section is set at 70-100℃, the temperature of other areas of the screw is set at 130-220℃, and the temperature of the composite mold is set at 150-200℃.
[0050] Example 3
[0051] An ionic intermediate membrane, consisting of an intermediate layer and a surface layer;
[0052] The main ingredients and their weight percentages in the intermediate layer are: 30% Surlyn PC2000, 60% Surlyn 8940, and 10% Surlyn 8920. Vinyltrimethylsilane, 3-aminopropyltriethoxysilane, antioxidants, UV cut-off agents, and plasticizers are added as additives, with addition amounts of 0.6%, 0.3%, 0.2%, 0.1%, and 1.2% of the above main ingredients by weight, respectively.
[0053] The main ingredients and their weight percentage in the surface layer are: 60% intermediate layer ingredients, 40% Kuraray.
[0054] Plus edge material, wherein the middle layer material is composed of the following raw materials by weight percentage: 30% Surlyn PC2000, 60% Surlyn 8940, 10% Surlyn 8920; the surface layer material also contains 3-aminopropyltriethoxysilane, antioxidant, UV cut-off agent and plasticizer as additives, and their addition amounts are 0.2%, 0.2%, 0.1% and 1.2% of the above main materials by weight, respectively.
[0055] In this embodiment, the antioxidant, UV cut-off agent, and plasticizer are tris(2,4-di-tert-butylphenyl) phosphite, 2-hydroxy-4-methoxybenzophenone, and dioctyl sebate, respectively.
[0056] The thickness of the intermediate layer is 50% of the thickness of the ionic intermediate film.
[0057] The method for preparing the ionic intermediate membrane includes the following steps:
[0058] (1) Ingredients: Mix the main ingredients and additives in the middle layer and the surface layer according to the formula; control the mixing temperature at 50-70℃ and the mixing speed at 5-20 rpm.
[0059] (2) Melt co-extrusion: The intermediate layer material and the surface layer material are fed into the extruder for melt extrusion, and then enter the composite mold to form a film. After cooling, trimming and winding, the finished product is obtained. The conditions for melt co-extrusion are: the temperature of the extruder feed port section is set at 70-100℃, the temperature of other areas of the screw is set at 130-220℃, and the temperature of the composite mold is set at 150-200℃.
[0060] Comparative Example 1
[0061] The rest is the same as in Example 1, except that the main ingredients and their weight percentages in the surface layer are: 95% intermediate layer raw materials, 5% Kuraray. Plus edge material.
[0062] Comparative Example 2
[0063] An ionic intermediate membrane, consisting of an intermediate layer and a surface layer;
[0064] The main ingredients and their weight percentages in the intermediate layer are: 60% Surlyn AE4500, 20% Surlyn 8940, and 20% Surlyn 8920. Vinyltrimethylsilane, 3-aminopropyltriethoxysilane, antioxidants, UV cut-off agents, and plasticizers are added as additives, with addition amounts of 0.6%, 0.3%, 0.2%, 0.1%, and 1.2% of the above main ingredients by weight, respectively.
[0065] The main ingredients and their weight percentage in the surface layer are: 50% intermediate layer ingredients, 50% Kuraray.
[0066] Plus edge material, wherein the middle layer material is composed of the following raw materials by weight percentage: 60% Surlyn AE4500, 20% Surlyn 8940, 20% Surlyn 8920; the surface layer material also contains 3-aminopropyltriethoxysilane, antioxidant, UV cut-off agent and plasticizer as additives, and their addition amounts are 0.2%, 0.2%, 0.1% and 1.2% of the above main materials by weight, respectively.
[0067] In this embodiment, the antioxidant, UV cut-off agent, and plasticizer are tris(2,4-di-tert-butylphenyl) phosphite, 2-hydroxy-4-methoxybenzophenone, and dioctyl sebate, respectively.
[0068] The thickness of the intermediate layer is 50% of the thickness of the ionic intermediate film.
[0069] The method for preparing the ionic intermediate membrane includes the following steps:
[0070] (1) Ingredients: Mix the main ingredients and additives in the middle layer and the surface layer according to the formula; control the mixing temperature at 50-70℃ and the mixing speed at 5-20 rpm.
[0071] (2) Melt co-extrusion: The intermediate layer material and the surface layer material are fed into the extruder for melt extrusion, and then enter the composite mold to form a film. After cooling, trimming and winding, the finished product is obtained. The conditions for melt co-extrusion are: the temperature of the extruder feed port section is set at 70-100℃, the temperature of other areas of the screw is set at 130-220℃, and the temperature of the composite mold is set at 150-200℃.
[0072] Test case
[0073] The ionic interlayer films in the above embodiments and comparative examples were tested for impact value, boiling test, visible light transmittance, haze, tensile fracture stress, tensile fracture strain, and tear strength. The test methods are as follows:
[0074] Impact value: Refer to standard JCT 2763-2023 Ionic interlayer for laminated glass. Three sets of tests are performed on each sample. A 300mm*300mm sample is placed between two 5mm thick 300mm*300mm untempered float glass sheets. The tin side of the glass is bonded to the film. Before lamination, the glass is cleaned with deionized water and dried. Lamination is performed according to the glass factory's SGP roll pressing + autoclave process or vacuum + autoclave process. Roll pressing process: first stage temperature 120±10℃, second stage temperature 135±10℃, third stage temperature 145±10℃, fourth stage temperature 130±10℃, fifth stage temperature 120±15℃; the first roll pressing height is the total glass thickness minus 1-2mm, the second roll pressing height is the total glass thickness minus 2-4mm; the roll pressing speed is 0.5m-0.9m / min; the glass surface temperature is controlled at 60-80℃ when exiting the roll press. The vacuuming process uses vacuum bags to wrap the samples, achieving a vacuum level of -0.1 MPa. The autoclave lamination process is as follows: First stage: 40±10 min, temperature 70±10℃, pressure: 0 MPa; Second stage: 20±10 min, temperature 110±10℃, pressure: 0 MPa; Third stage: 20±10 min, temperature 130±10℃, pressure: 0 MPa; Fourth stage: 120±10 min, temperature 130±10℃, pressure: 0 MPa; Fifth stage: 20±10 min, temperature 138±10℃, pressure: 0 MPa. The pressure was 1.2±0.5 MPa at 10℃; the sixth stage lasted 110±10 min at 138±10℃, with a pressure of 1.2±0.5 MPa; the seventh stage lasted 25±10 min at 65±10℃, with a pressure of 1.2±0.5 MPa; the eighth stage lasted 60±10 min at 45±10℃, with a pressure of 1.2±0.5 MPa; after the eighth stage, the pressure was manually maintained and the temperature was lowered for 80 min before the pressure was manually released from the autoclave. After the sample was prepared, it was placed at 20±5℃ and 40%-80% humidity for at least 2 hours. The tapping was also carried out under this environment. The sample was placed in the tapping box, and the glass was tapped horizontally from the bottom with a hammer. The force of each tap should be uniform, and the force should be enough to break the glass. Each subsequent tap should cover about half of the area hit by the previous tap, until the sample was broken within 150 mm of its length. After proper tapping, the intermediate layer remains intact, and all original glass surfaces are destroyed. There should be no visible original glass surfaces. If some glass surfaces are not destroyed, gently tap them repeatedly with a hammer, changing the tapping direction to the length direction, until all original glass surfaces are broken. Gently shake off the glass fragments from the intermediate layer surface, and then compare them with a standard sample or calculate the tapping value by counting the exposed area.
[0075] Boiling Test: Prepare samples according to the method in the impact value test. Refer to the standard "JCT 2763-2023 Ionic Interlayer for Laminated Glass", and test 3 sets for each sample. Vertically and completely immerse the sample in 100°C water in a boiling test chamber for 2 hours (to avoid thermal stress causing cracks in the sample, the sample can be preheated in warm water). After the heat preservation is completed, remove the sample from the boiling water and cool it to below 30°C. Under good natural or diffused light background conditions, observe the sample at a distance of 600mm. No missing adhesive is allowed on the edge of the sample, and no bubbles, delamination, turbidity, or discoloration should appear in the part exceeding 15mm from the edge.
[0076] Visible light transmittance: Prepare the sample according to the method in the impact value test. Place the sample on a haze meter and read the visible light transmittance.
[0077] Haze: Prepare the sample according to the method in the tapping value test. Place the sample on a haze meter and read the haze.
[0078] Tensile breaking stress: Referring to the standard "JCT 2763-2023 Ionic interlayer for laminated glass", five Type 5 specimens conforming to GB / T-1040.3-2006 were cut from the interlayer film. The length direction of the specimens was the extrusion longitudinal direction. The thickness of the dumbbell part in the middle was measured at three points using a 0.001 mm micrometer and the average value was taken. The specimens were placed at 23±2℃ and 20%-60% humidity for at least 3 hours and tested under this environment. The test was carried out according to GB / T-1040.1. The test speed was (50±10) mm / min. The average value of the five samples was taken.
[0079] Tensile fracture strain: Referring to the standard "JCT 2763-2023 Ionic interlayer for laminated glass", five Type 5 specimens conforming to GB / T-1040.3-2006 were cut from the interlayer film. The length direction of the specimens was the extrusion longitudinal direction. The thickness of the dumbbell part in the middle was measured at three points using a 0.001 mm micrometer and the average value was taken. The specimens were placed at 23±2℃ and 20%-60% humidity for at least 3 hours and tested under this environment. The test was carried out according to GB / T-1040.1. The test speed was (50±10) mm / min. The average value of the five samples was taken.
[0080] Tear strength: Referencing the standard "JCT 2763-2023 Ionic interlayer for laminated glass", cut five uncut right-angled specimens conforming to GB / T-529-2008 from the interlayer film. The length direction of the specimens should be the extrusion longitudinal direction. Use a 0.001mm micrometer to measure the thickness of the torn area at three points and take the median value. Place the specimens at 23±2℃ and 20%-60% humidity for at least 3 hours and test them under this environment. The test should be carried out according to GB / T-529-2008, with a test speed of (500±50)mm / min. Take the average value of the five samples tested.
[0081] The test results are shown in Table 1.
[0082] Table 1
[0083]
[0084]
[0085] As can be seen from Table 1, the ionic interlayer provided by the present invention has excellent resistance to boiling water hydrolysis, the impact value meets the requirements of the impact value specified in JCT 2763-2023 Ionic Interlayer for Laminated Glass, and the visible light transmittance and haze meet the requirements of laminated glass.
[0086] In Comparative Example 1, the Kuraray SentryGlas used in the ionic intermediate membrane surface layer... The less material used in the Plus process results in a poorer impact value, and the visible light transmittance and haze cannot meet the requirements for laminated glass.
[0087] In Comparative Example 2, the high proportion of sarin resin, which is not resistant to boiling water, used in the intermediate and surface layers resulted in poor boiling water resistance of the ionic intermediate membrane.
[0088] The above detailed description of an ionic intermediate membrane and its preparation method with reference to the embodiments is illustrative rather than limiting. Several embodiments can be listed according to the defined scope. Therefore, changes and modifications without departing from the overall concept of the present invention should be within the protection scope of the present invention.
Claims
1. An ionic intermediate membrane, characterized in that, The ionic intermediate membrane consists of an intermediate layer and a surface layer; The intermediate layer comprises the following raw materials by weight percentage: 20-50% Saryn resin A and 50-80% Saryn resin B; wherein Saryn resin A is any one or more of Surlyn AE4500, Surlyn PC2000, Surlyn PC2200, and Surlyn AE4800; and wherein Saryn resin B is any one or more of Surlyn 8940, Surlyn 8920, Surlyn 8150, and Surlyn 9150. The surface layer comprises the following raw materials by weight percentage: 20%–90% intermediate layer raw materials, Kuraray. Plus, scrap material accounts for 10% to 80%.
2. The ionic intermediate membrane according to claim 1, characterized in that, The thickness of the intermediate layer is 50% to 90% of the thickness of the ionic intermediate film.
3. The ionic intermediate membrane according to claim 1, characterized in that, The raw materials for both the intermediate and surface layers also include silane coupling agents, antioxidants, UV cut-off agents, and plasticizers.
4. The ionic intermediate membrane according to claim 3, characterized in that, In the intermediate layer, the mass of the silane coupling agent, antioxidant, UV cut-off agent, and plasticizer are 0.5%-1.5%, 0.1%-0.6%, 0.1%-0.5%, and 0.5%-2% of the sum of the masses of Sarin resin A and Sarin resin B, respectively.
5. The ionic intermediate membrane according to claim 5, characterized in that, In the surface layer, the mass percentages of silane coupling agent, antioxidant, UV cut-off agent, and plasticizer are 0.1%-1%, 0.1%-0.6%, 0.1%-0.5%, and 0.5%-2% of the sum of the masses of Sarin resin A and Sarin resin B, respectively.
6. The ionic intermediate membrane according to any one of claims 3-5, characterized in that, The silane coupling agent is any one or more of γ-methacryloxypropyltrimethoxysilane, vinyltris(2-methoxyethoxy)silane, vinyltrimethylsilane, γ-(2,3-epoxypropoxy)propyltrimethoxysilane, and 3-aminopropyltriethoxysilane.
7. The ionic intermediate membrane according to any one of claims 3-6, characterized in that, The antioxidant is any one or more of the following: pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 4-[(4,6-dioctylthio-1,3,5-triazin-2-yl)amino]-2,6-di-tert-butylphenol, propoxyglycerol triacrylate, octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, tris(2,4-di-tert-butylphenyl) phosphite, tri-tert-butyl-p-hydroxyphenylpropane, poly(4-hydroxy-2,2,6,6-tetramethyl-1-piperidine ethanol) ester, and bis-2,2,6,6-tetramethylpiperidinol sebacate.
8. The ionic intermediate membrane according to any one of claims 3-6, characterized in that, The UV cutoff agent is any one or more of [2-hydroxy-4-(octoxy)phenyl]phenyl ketone, 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-(2-hydroxy-3,5-bis(a,a-dimethylbenzyl)phenyl)benzotriazole, and 2-(2H-benzotriazol-2-yl)-4-(1,1,3,3-tetramethylbutyl)phenol; the plasticizer is any one or more of triethylene glycol diisooctanoate, oleic acid, 3-octenic acid, diisononyl phthalate, and dioctyl sebate.
9. The method for preparing the ionic intermediate membrane according to any one of claims 1-8, characterized in that, The preparation method includes the following steps: mixing the surface layer and intermediate layer raw materials evenly, extruding them through a composite mold by melt co-extrusion, casting them into a film, and then cooling, trimming, and winding them to obtain the finished product.
10. A laminated glass, characterized in that, The laminated glass uses the ionic interlayer as described in any one of claims 1-8.
Citation Information
Patent Citations
Method for modifying ionic middle film raw material
CN110615934A
Ionomer type laminated glass intermediate film and preparation method thereof
CN114196330A