CN117866559A - Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof - Google Patents
Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof Download PDFInfo
- Publication number
- CN117866559A CN117866559A CN202311624318.2A CN202311624318A CN117866559A CN 117866559 A CN117866559 A CN 117866559A CN 202311624318 A CN202311624318 A CN 202311624318A CN 117866559 A CN117866559 A CN 117866559A
- Authority
- CN
- China
- Prior art keywords
- oca
- parts
- adhesive
- utg
- folded
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
本发明公开了一种对UTG材料具有高粘特性的折叠OCA胶黏剂、胶膜及其制备方法,该胶黏剂包括按重量份计的以下原料组分:OCA胶水80~90份、热固化剂0.02~0.04份、第一溶剂10~20份;OCA胶水的原料组分包括:丙烯酸异辛酯15~20份、丙烯酸丁酯9~12份、丙烯酸4‑羟丁酯2.5~3.5份、甲基丙烯酸甲酯3‰份、丙烯酸异十八烷基酯3‰份、引发剂0.6‰~0.8‰份、第二溶剂65~75份。本发明提供的OCA胶黏剂通过添加与体系相容性较好的单体ISTA,调节丙烯酸共聚物的玻璃化转变温度,以此获得了高粘性OCA,制得的OCA对UTG材料具有极高的粘性,同时改善了胶粘剂的蠕变回复及应力松弛性。The present invention discloses a folding OCA adhesive, an adhesive film and a preparation method thereof having high viscosity to UTG materials, wherein the adhesive comprises the following raw material components by weight: 80-90 parts of OCA glue, 0.02-0.04 parts of a thermosetting agent, and 10-20 parts of a first solvent; the raw material components of the OCA glue include: 15-20 parts of isooctyl acrylate, 9-12 parts of butyl acrylate, 2.5-3.5 parts of 4-hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 3‰ parts of isooctadecyl acrylate, 0.6‰-0.8‰ parts of an initiator, and 65-75 parts of a second solvent. The OCA adhesive provided by the present invention is obtained by adding a monomer ISTA having good compatibility with the system and adjusting the glass transition temperature of an acrylic copolymer, thereby obtaining a high-viscosity OCA, and the obtained OCA has extremely high viscosity to the UTG material, while improving the creep recovery and stress relaxation of the adhesive.
Description
技术领域Technical Field
本发明涉及胶黏材料领域,特别涉及一种对UTG材料具有高粘特性的折叠OCA胶黏剂、胶膜及其制备方法。The present invention relates to the field of adhesive materials, and in particular to a folded OCA adhesive having high adhesive properties for UTG materials, an adhesive film and a preparation method thereof.
背景技术Background technique
近年来,可折叠设备由于其优异的便携性,越来越受到人们的青睐,也越来越广泛的应用于折叠手机、智能穿戴、车载、电子设备等领域。超薄玻璃(Ultra-Thin Glass,UTG)是指厚度在0.1mm以下的玻璃。由于其超薄特性,具有优异的可弯折性和高硬度的耐刮擦性,成为继CPI薄膜材料之后,在可折叠柔性盖板领域具有重要地位的材料。可折叠OCA(Optically Clear Adhesive)将UTG与可折叠保护膜进行贴合,一般情况下,可折叠设备使用的OCA胶粘剂需要具备对环境变化的使用耐久性的同时,还应当具备较强的粘接性能,优异的高低温模量稳定性以及较好的蠕变回复性,从而减少不可逆的形变,避免内聚破坏失效的产生,这样才能够提高可折叠设备的使用寿命。In recent years, foldable devices have become increasingly popular due to their excellent portability, and are increasingly widely used in the fields of foldable mobile phones, smart wearables, vehicles, electronic equipment, etc. Ultra-thin glass (UTG) refers to glass with a thickness of less than 0.1mm. Due to its ultra-thin characteristics, it has excellent bendability and high hardness scratch resistance, making it an important material in the field of foldable flexible cover panels after CPI film materials. Foldable OCA (Optically Clear Adhesive) bonds UTG to a foldable protective film. Generally, the OCA adhesive used in foldable devices needs to have durability against environmental changes, as well as strong bonding properties, excellent high and low temperature modulus stability, and good creep recovery, so as to reduce irreversible deformation and avoid cohesive failure, thereby increasing the service life of foldable devices.
在某些情况下,可弯折设备会随着温度变低而出现胶粘剂层变硬的现象,比如在低温环境下对可弯折设备进行折叠时,很容易出在折叠层处发生白化或者断裂的情况。另外,如果所使用的OCA胶粘剂不能够在特定的环境下保持较好的粘性,也会造成胶膜与UTG之间出现气泡甚至脱落的风险。更重要的一点是,如果在较低或者较高的温度下使用可折叠设备时,对OCA胶必须要求有较好的蠕变回复性,对于这一点,CN108753185A开发了一种TP用OCA光学胶带以及其制备方法,以重量份计包括50-70份丙烯酸酯聚合物、20-50份丙烯酸酯类单体、0.05-0.5份交联剂、0.5-0.8份光引发剂以及0.2-0.4份助剂。该OCA光学胶蠕变回复、应力松弛不佳,导致其在折叠次数增多后会出现折痕的现象。In some cases, the adhesive layer of the bendable device will become hard as the temperature decreases. For example, when the bendable device is folded in a low temperature environment, it is easy to whiten or break at the folding layer. In addition, if the OCA adhesive used cannot maintain good viscosity under a specific environment, it will also cause the risk of bubbles or even falling off between the film and the UTG. More importantly, if the foldable device is used at a lower or higher temperature, the OCA adhesive must have good creep recovery. For this, CN108753185A has developed an OCA optical tape for TP and a preparation method thereof, which includes 50-70 parts of acrylate polymer, 20-50 parts of acrylate monomer, 0.05-0.5 parts of cross-linking agent, 0.5-0.8 parts of photoinitiator and 0.2-0.4 parts of auxiliary agent by weight. The OCA optical adhesive has poor creep recovery and stress relaxation, resulting in creases after the number of folds increases.
目前为止,市场上用于UTG的OCA胶粘剂产品,在不同温度下的高蠕变回复性低,粘性较低,在弯折过程中OCA胶材与UTG剥离,综合性能远不能满足消费者的需求,因此,开发一种与UTG材料具有良好的粘结性,同时具有良好的蠕变回复及应力松弛性的OCA胶粘剂是本领域目前研究的重点。So far, the OCA adhesive products used for UTG on the market have low creep recovery at different temperatures and low viscosity. During the bending process, the OCA adhesive material peels off from the UTG, and the comprehensive performance is far from meeting the needs of consumers. Therefore, developing an OCA adhesive that has good adhesion to UTG materials and good creep recovery and stress relaxation properties is the current research focus in this field.
发明内容Summary of the invention
本发明所要解决的技术问题在于针对上述现有技术中的不足,提供一种对UTG材料具有高粘特性的折叠OCA胶黏剂、胶膜及其制备方法。The technical problem to be solved by the present invention is to provide a folded OCA adhesive, an adhesive film and a preparation method thereof having high adhesion properties to UTG materials in view of the deficiencies in the above-mentioned prior art.
为解决上述技术问题,本发明采用的技术方案是:本发明的第一方面,提供一种对UTG材料具有高粘特性的折叠OCA胶黏剂,包括按重量份计的以下原料组分:OCA胶水80~90份、热固化剂0.02~0.04份、第一溶剂10~20份;In order to solve the above technical problems, the technical solution adopted by the present invention is: in the first aspect of the present invention, a folding OCA adhesive having high adhesive properties for UTG materials is provided, comprising the following raw material components by weight: 80-90 parts of OCA glue, 0.02-0.04 parts of thermal curing agent, and 10-20 parts of a first solvent;
其中,所述OCA胶水是由按重量份计的以下的原料组分经聚合反应制备得到:丙烯酸异辛酯(2-EHA)15~20份、丙烯酸丁酯(BA)9~12份、丙烯酸4-羟丁酯(4-HBA)2.5~3.5份、甲基丙烯酸甲酯(MMA)3‰份、丙烯酸异十八烷基酯(ISTA)3‰份、引发剂(AIBN)0.6‰~0.8‰份、第二溶剂65~75份。Among them, the OCA glue is prepared by polymerization reaction of the following raw material components in parts by weight: 15-20 parts of isooctyl acrylate (2-EHA), 9-12 parts of butyl acrylate (BA), 2.5-3.5 parts of 4-hydroxybutyl acrylate (4-HBA), 3‰ parts of methyl methacrylate (MMA), 3‰ parts of isostearyl acrylate (ISTA), 0.6‰-0.8‰ parts of initiator (AIBN), and 65-75 parts of the second solvent.
优选的是,所述OCA胶水通过以下方法制备得到:Preferably, the OCA glue is prepared by the following method:
按照重量份配比,将丙烯酸异辛酯、丙烯酸丁酯、丙烯酸4-羟丁酯、甲基丙烯酸甲酯、丙烯酸异十八烷基酯(ISTA)与部分第二溶剂混合,通入氮气,加热下搅拌,然后加入部分引发剂,加热搅拌反应;随后升温反应;加入剩余部分引发剂,继续升温度反应;反应结束后冷却,加入剩余部分第二溶剂稀释,得到OCA胶水。According to the weight ratio, isooctyl acrylate, butyl acrylate, 4-hydroxybutyl acrylate, methyl methacrylate, isostearyl acrylate (ISTA) and part of the second solvent are mixed, nitrogen is introduced, and the mixture is heated and stirred. Then, part of the initiator is added, and the mixture is heated and stirred for reaction; the temperature is then increased to react; the remaining part of the initiator is added, and the temperature is continued to be increased for reaction; after the reaction is completed, the mixture is cooled, and the remaining part of the second solvent is added for dilution to obtain OCA glue.
优选的是,所述OCA胶水通过以下方法制备得到:Preferably, the OCA glue is prepared by the following method:
按照重量份配比,将丙烯酸异辛酯、丙烯酸丁酯、丙烯酸4-羟丁酯、甲基丙烯酸甲酯、丙烯酸异十八烷基酯(ISTA)与部分第二溶剂混合,通入氮气,60~62℃下搅拌至少30分钟后加入部分引发剂,保持温度,搅拌反应1-4小时;随后升温至63-68℃反应3~4h;加入剩余部分引发剂,升高温度至70~72℃继续反应3-6小时;冷却至室温后加入剩余部分第二溶剂稀释,得到OCA胶水。According to the weight ratio, isooctyl acrylate, butyl acrylate, 4-hydroxybutyl acrylate, methyl methacrylate, isooctadecyl acrylate (ISTA) and part of the second solvent are mixed, nitrogen is introduced, and part of the initiator is added after stirring at 60-62° C. for at least 30 minutes, the temperature is maintained, and the reaction is stirred for 1-4 hours; then the temperature is raised to 63-68° C. for reaction for 3-4 hours; the remaining part of the initiator is added, the temperature is raised to 70-72° C. for continuous reaction for 3-6 hours; after cooling to room temperature, the remaining part of the second solvent is added for dilution to obtain OCA glue.
优选的是,所述OCA胶水通过以下方法制备得到:Preferably, the OCA glue is prepared by the following method:
按照重量份配比,将丙烯酸异辛酯、丙烯酸丁酯、丙烯酸4-羟丁酯、甲基丙烯酸甲酯、丙烯酸异十八烷基酯(ISTA)与部分第二溶剂混合,通入氮气,60~62℃下搅拌至少30分钟后加入部分引发剂,保持温度,搅拌反应2小时;随后升温至65℃反应3h;加入剩余部分引发剂,升高温度至70~72℃继续反应5小时;冷却至室温后加入剩余部分第二溶剂稀释,得到固含量为25~30%的OCA胶水。According to the weight ratio, isooctyl acrylate, butyl acrylate, 4-hydroxybutyl acrylate, methyl methacrylate, isostearyl acrylate (ISTA) and part of the second solvent are mixed, nitrogen is introduced, and part of the initiator is added after stirring at 60-62° C. for at least 30 minutes, and the temperature is maintained and stirred for 2 hours; then the temperature is raised to 65° C. and reacted for 3 hours; the remaining part of the initiator is added, the temperature is raised to 70-72° C. and the reaction is continued for 5 hours; after cooling to room temperature, the remaining part of the second solvent is added for dilution to obtain OCA glue with a solid content of 25-30%.
优选的是,所述第一溶剂和第二溶剂均为乙酸乙酯。Preferably, the first solvent and the second solvent are both ethyl acetate.
优选的是,所述引发剂为AIBN。Preferably, the initiator is AIBN.
优选的是,所述热固化剂为六亚甲基二异氰酸酯。Preferably, the thermal curing agent is hexamethylene diisocyanate.
本发明的第二方面,提供一种对UTG材料具有高粘特性的折叠OCA胶膜,其采用如上所述的OCA胶黏剂制备得到。A second aspect of the present invention provides a folded OCA adhesive film having high adhesion to UTG materials, which is prepared using the OCA adhesive as described above.
本发明的第三方面,提供一种如上所述的对UTG材料具有高粘特性的折叠OCA胶膜的制备方法,包括以下步骤:A third aspect of the present invention provides a method for preparing a folded OCA adhesive film having high adhesion to UTG material as described above, comprising the following steps:
S1、将OCA胶水、热固化剂以及第一溶剂混合,搅拌均匀,得到对UTG材料具有高粘特性的折叠OCA胶黏剂;S1, mixing OCA glue, a thermal curing agent and a first solvent, and stirring evenly to obtain a folding OCA adhesive having high adhesion to UTG material;
S2、将该折叠OCA胶黏剂涂布在第一离型膜上,控制干胶厚度为30-80μm,放入烘箱,在110-130℃下烘干1-4min,在形成的干胶层的胶面贴合第二离型膜,50-70℃下熟化24-48h,得到所述的对UTG材料具有高粘特性的折叠OCA胶膜。S2. Apply the folded OCA adhesive on the first release film, control the dry adhesive thickness to 30-80 μm, put it into an oven, dry it at 110-130° C. for 1-4 min, adhere the second release film to the adhesive surface of the formed dry adhesive layer, and ripen it at 50-70° C. for 24-48 h to obtain the folded OCA adhesive film with high adhesion to the UTG material.
优选的是,所述的对UTG材料具有高粘特性的折叠OCA胶膜的制备方法包括以下步骤:Preferably, the method for preparing the folded OCA adhesive film having high adhesion to the UTG material comprises the following steps:
S1、在23~25℃,湿度50±3%的条件下,将OCA胶水、热固化剂以及第一溶剂混合,搅拌均匀,得到对UTG材料具有高粘特性的折叠OCA胶黏剂;S1. Under the conditions of 23-25° C. and 50±3% humidity, mix the OCA glue, the thermal curing agent and the first solvent, and stir evenly to obtain a folding OCA adhesive having high adhesion to the UTG material;
S2、将该折叠OCA胶黏剂涂布在第一离型膜上,控制干胶厚度为50μm,放入烘箱,由25℃升到120℃,然后在120℃下烘干2min,在形成的干胶层的胶面贴合第二离型膜,60℃下熟化36h,得到所述的对UTG材料具有高粘特性的折叠OCA胶膜。S2. Apply the folded OCA adhesive on the first release film, control the dry adhesive thickness to 50 μm, put it into an oven, raise the temperature from 25°C to 120°C, and then dry it at 120°C for 2 minutes, adhere the second release film to the adhesive surface of the formed dry adhesive layer, and ripen it at 60°C for 36 hours to obtain the folded OCA adhesive film with high adhesion to the UTG material.
本发明的有益效果是:The beneficial effects of the present invention are:
本发明提供了一种对UTG材料具有高粘特性的折叠OCA胶黏剂、胶膜及其制备方法,本发明提供的OCA胶黏剂中通过添加与体系相容性较好的单体ISTA,调节丙烯酸共聚物的玻璃化转变温度,以此获得了高粘性OCA,制得的OCA对UTG材料具有极高的粘性,同时改善了胶粘剂的蠕变回复及应力松弛性,能够避免通过提高反应的交联度来实现上述效果时带来的可能会造成胶水的内聚较差、体系均匀性较差的缺陷;The present invention provides a folded OCA adhesive and an adhesive film having high viscosity to UTG materials and a preparation method thereof. The OCA adhesive provided by the present invention is obtained by adding a monomer ISTA having good compatibility with the system and adjusting the glass transition temperature of an acrylic copolymer, and the obtained OCA has extremely high viscosity to the UTG material, and at the same time improves the creep recovery and stress relaxation of the adhesive, and can avoid the defects of poor cohesion of the glue and poor uniformity of the system caused by achieving the above effect by increasing the crosslinking degree of the reaction;
本发明中添加的ISTA单体与丙烯酸酯反应的共聚物有较强的粘接能力,且其反应活性较高,能快速发生聚合反应,且能够提供较好的粘性,对后期成膜后的低模量起着关键作用;ISTA有很好的润湿性能,这种长链单体自身的物理缠结也可提高内聚强度,同时4-HBA内聚强度高,ISTA与4-HBA搭配可以极大提高胶膜的内聚强度,增强胶膜与UTG的粘结性能。The copolymer of the ISTA monomer added in the present invention and the acrylate reaction has strong bonding ability, and its reaction activity is high, and it can quickly undergo polymerization reaction and provide good viscosity, which plays a key role in the low modulus after the later film formation; ISTA has good wetting properties, and the physical entanglement of this long-chain monomer itself can also improve the cohesive strength. At the same time, 4-HBA has high cohesive strength. The combination of ISTA and 4-HBA can greatly improve the cohesive strength of the film and enhance the bonding performance between the film and UTG.
具体实施方式Detailed ways
下面结合实施例对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.
应当理解,本文所使用的诸如“具有”、“包含”以及“包括”术语并不排除一个或多个其它元件或其组合的存在或添加。It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.
下列实施例中所使用的试验方法如无特殊说明,均为常规方法。下列实施例中所用的材料试剂等,如无特殊说明,均可从商业途径得到。下列实施例中未注明具体条件者,按照常规条件或者制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。The test methods used in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the following examples are all commercially available unless otherwise specified. In the following examples, if no specific conditions are specified, the experiments were carried out under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.
本发明提供一种对UTG材料具有高粘特性的折叠OCA胶黏剂,包括按重量份计的以下原料组分:OCA胶水80~90份、热固化剂0.02~0.04份、第一溶剂10~20份;The present invention provides a folding OCA adhesive having high adhesive properties for UTG materials, comprising the following raw material components by weight: 80 to 90 parts of OCA glue, 0.02 to 0.04 parts of a thermal curing agent, and 10 to 20 parts of a first solvent;
其中,OCA胶水是由按重量份计的以下的原料组分经聚合反应制备得到:丙烯酸异辛酯(2-EHA)15~20份、丙烯酸丁酯(BA)9~12份、丙烯酸4-羟丁酯(4-HBA)2.5~3.5份、甲基丙烯酸甲酯(MMA)3‰份(千分之3份,即0.003份,其余类似)、丙烯酸异十八烷基酯(ISTA)3‰份、引发剂(AIBN)0.6‰~0.8‰份、第二溶剂65~75份。Among them, OCA glue is prepared by polymerization reaction of the following raw material components in parts by weight: 15-20 parts of isooctyl acrylate (2-EHA), 9-12 parts of butyl acrylate (BA), 2.5-3.5 parts of 4-hydroxybutyl acrylate (4-HBA), 3‰ parts of methyl methacrylate (MMA) (3 thousandths, i.e. 0.003 parts, and the rest are similar), 3‰ parts of isostearyl acrylate (ISTA), 0.6‰-0.8‰ parts of initiator (AIBN), and 65-75 parts of the second solvent.
在优选的实施例中,OCA胶水通过以下方法制备得到:In a preferred embodiment, OCA glue is prepared by the following method:
按照重量份配比,将丙烯酸异辛酯、丙烯酸丁酯、丙烯酸4-羟丁酯、甲基丙烯酸甲酯、丙烯酸异十八烷基酯(ISTA)与部分第二溶剂混合,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,60~62℃下搅拌至少30分钟后加入部分引发剂,保持温度,搅拌反应2小时;随后升温至65℃反应3h;加入剩余部分引发剂,升高温度至70~72℃继续反应5小时;冷却至室温后加入剩余部分第二溶剂稀释,得到固含量为25~30%的OCA胶水。According to the weight ratio, isooctyl acrylate, butyl acrylate, 4-hydroxybutyl acrylate, methyl methacrylate, isostearyl acrylate (ISTA) and part of the second solvent are mixed, placed in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, nitrogen is introduced, and part of the initiator is added after stirring at 60-62° C. for at least 30 minutes, the temperature is maintained, and the reaction is stirred for 2 hours; then the temperature is raised to 65° C. for 3 hours; the remaining part of the initiator is added, the temperature is raised to 70-72° C. and the reaction is continued for 5 hours; after cooling to room temperature, the remaining part of the second solvent is added for dilution to obtain OCA glue with a solid content of 25-30%.
本发明制备的OCA胶水中,加入丙烯酸异十八烷基酯(ISTA),不仅满足了胶水低温低模量的特性,而且提升了胶水的粘性。ISTA与丙烯酸酯反应的共聚物有较强的粘接能力。UTG表面光滑,平整度高,这就需要胶膜对UTG材料有极高的粘结性;ISTA有很好的润湿性能,这种长链单体自身的物理缠结也可提高内聚强度,同时4-HBA内聚强度高,ISTA与4-HBA搭配可以极大提高胶膜的内聚强度,增强胶膜与UTG的粘结性能。In the OCA glue prepared by the present invention, isooctadecyl acrylate (ISTA) is added, which not only meets the low-temperature and low-modulus characteristics of the glue, but also improves the viscosity of the glue. The copolymer of ISTA and acrylate has a strong bonding ability. UTG has a smooth surface and high flatness, which requires the film to have extremely high adhesion to the UTG material; ISTA has good wetting properties, and the physical entanglement of this long-chain monomer itself can also improve the cohesive strength. At the same time, 4-HBA has high cohesive strength. The combination of ISTA and 4-HBA can greatly improve the cohesive strength of the film and enhance the bonding performance between the film and UTG.
在优选的实施例中,第一溶剂和第二溶剂均为乙酸乙酯。In a preferred embodiment, the first solvent and the second solvent are both ethyl acetate.
在优选的实施例中,引发剂为AIBN(偶氮二异丁腈)。In a preferred embodiment, the initiator is AIBN (azobisisobutyronitrile).
在优选的实施例中,热固化剂为六亚甲基二异氰酸酯,其能够与OCA胶水进行快速的交联固化反应,提高其交联度并增强内聚力。In a preferred embodiment, the thermal curing agent is hexamethylene diisocyanate, which can undergo a rapid cross-linking and curing reaction with the OCA glue, thereby increasing its cross-linking degree and enhancing its cohesive force.
在优选的实施例中,本发明的胶粘剂交联固化成膜后,Tg值在-30~-45℃之间。且-20℃的储能模量为0.1~0.2MPa之间。In a preferred embodiment, after the adhesive of the present invention is cross-linked and cured to form a film, the Tg value is between -30 and -45°C, and the storage modulus at -20°C is between 0.1 and 0.2 MPa.
在优选的实施例中,本发明的胶粘剂具有较好的蠕变性能,施加20KPa的条件下,20KPa应力条件下-20℃下的蠕变回复率超过90%,最大应变大于100%。In a preferred embodiment, the adhesive of the present invention has good creep performance. Under the condition of applying 20 KPa, the creep recovery rate at -20°C under the stress condition of 20 KPa exceeds 90%, and the maximum strain is greater than 100%.
在优选的实施例中,本发明的胶粘剂交联固化成膜后,常温下24h对UTG材料的剥离力测试结果不低于20N/25mm,85℃下对UTG的剥离力测试结果不低于800N/25mm。In a preferred embodiment, after the adhesive of the present invention is cross-linked and cured to form a film, the peel strength test result of the UTG material at room temperature for 24 hours is not less than 20N/25mm, and the peel strength test result of the UTG at 85°C is not less than 800N/25mm.
在优选的实施例中,本发明的胶粘剂交联固化成膜后,凝胶分率在70%以上。In a preferred embodiment, after the adhesive of the present invention is cross-linked and cured to form a film, the gel fraction is above 70%.
本发明还提供一种对UTG材料具有高粘特性的折叠OCA胶膜,其采用如上的OCA胶黏剂制备得到,具体步骤包括:The present invention also provides a folded OCA adhesive film having high adhesion to UTG material, which is prepared by using the above OCA adhesive, and the specific steps include:
S1、在23~25℃,湿度50±3%的条件下,将OCA胶水、热固化剂以及第一溶剂混合,搅拌均匀,得到对UTG材料具有高粘特性的折叠OCA胶黏剂;S1. Under the conditions of 23-25° C. and 50±3% humidity, mix the OCA glue, the thermal curing agent and the first solvent, and stir evenly to obtain a folding OCA adhesive having high adhesion to the UTG material;
S2、将该折叠OCA胶黏剂涂布在第一离型膜上,控制干胶厚度为50μm,放入烘箱,由25℃升到120℃,然后在120℃下烘干2min,在形成的干胶层的胶面贴合第二离型膜,60℃下熟化36h,得到的对UTG材料具有高粘特性的折叠OCA胶膜。S2. Apply the folded OCA adhesive on the first release film, control the dry adhesive thickness to 50 μm, put it into an oven, raise the temperature from 25°C to 120°C, and then dry it at 120°C for 2 minutes, adhere the second release film to the adhesive surface of the formed dry adhesive layer, and ripen it at 60°C for 36 hours to obtain a folded OCA adhesive film with high adhesion to UTG material.
以上为本发明的总体构思,以下在其基础上提供详细的实施例和对比例,以对本发明做进一步说明。The above is the overall concept of the present invention, and detailed embodiments and comparative examples are provided below on the basis of the overall concept of the present invention to further illustrate the present invention.
实施例1Example 1
一种对UTG材料具有高粘特性的折叠OCA胶膜,其通过以下方法制备得到:A folded OCA adhesive film having high adhesive properties to UTG material is prepared by the following method:
S1、制备OCA胶水:S1. Preparation of OCA glue:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯3‰份、ISTA(丙烯酸异十八烷基酯)3‰份、乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。According to weight, 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 3‰ parts of ISTA (isostearyl acrylate), and 48 parts of ethyl acetate were accurately weighed, placed in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, nitrogen was introduced, and 0.25‰ parts of AIBN were added after stirring at 62°C for 45 minutes, and the temperature was maintained and stirred for 2 hours; then the temperature was raised to 65°C for reaction for 3 hours; 0.6‰ parts of AIBN were added, the temperature was raised to 72°C and the reaction was continued for 5 hours; after cooling, 22 parts of ethyl acetate were added for dilution to obtain OCA glue with a solid content of 30%.
S2、制备OCA胶膜:S2. Preparation of OCA film:
在23~25℃,湿度50±3%的条件下,将OCA胶水、占OCA胶水质量分数0.03%的异氰酸酯固化剂以及占OCA胶水质量分数%的乙酸乙酯混合,搅拌均匀,得到合适的涂布粘度的对UTG材料具有高粘特性的折叠OCA胶黏剂;Under the conditions of 23-25°C and humidity of 50±3%, OCA glue, 0.03% isocyanate curing agent accounting for the mass fraction of OCA glue, and ethyl acetate accounting for the mass fraction of OCA glue are mixed and stirred evenly to obtain a folding OCA adhesive with a suitable coating viscosity and high adhesion to UTG materials;
S2、将该折叠OCA胶黏剂涂布在第一离型膜(PET离型膜)上,控制干胶厚度为50μm,放入烘箱,由25℃升到120℃,然后在120℃下烘干2min,在形成的干胶层的胶面贴合第二离型膜(PET离型膜),60℃下熟化36h,得到的对UTG材料具有高粘特性的折叠OCA胶膜。S2. Apply the folded OCA adhesive on the first release film (PET release film), control the dry adhesive thickness to 50 μm, put it into an oven, raise the temperature from 25°C to 120°C, and then dry it at 120°C for 2 minutes, adhere the second release film (PET release film) to the adhesive surface of the formed dry adhesive layer, and ripen it at 60°C for 36 hours to obtain a folded OCA adhesive film with high adhesion to UTG material.
实施例2Example 2
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯15份、甲基丙烯酸甲酯3‰份、ISTA(丙烯酸异十八烷基酯)3‰份、乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。Accurately weigh 15 parts of isooctyl acrylate, 15 parts of butyl acrylate, 3‰ parts of methyl methacrylate, 3‰ parts of ISTA (isostearyl acrylate), and 48 parts of ethyl acetate by weight, place them in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, introduce nitrogen, stir at 62°C for 45 minutes, then add 0.25‰ parts of AIBN, maintain the temperature and stir to react for 2 hours; then raise the temperature to 65°C and react for 3 hours; add 0.6‰ parts of AIBN, raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 22 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
实施例3Example 3
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯4‰份、ISTA(丙烯酸异十八烷基酯)2‰份、乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.4‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。According to weight, 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, 4‰ parts of methyl methacrylate, 2‰ parts of ISTA (isostearyl acrylate), and 48 parts of ethyl acetate were accurately weighed, placed in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, nitrogen was introduced, and 0.4‰ parts of AIBN were added after stirring at 62°C for 45 minutes, and the temperature was maintained and stirred for 2 hours; then the temperature was raised to 65°C for reaction for 3 hours; 0.6‰ parts of AIBN were added, the temperature was raised to 72°C and the reaction was continued for 5 hours; after cooling, 22 parts of ethyl acetate was added for dilution to obtain OCA glue with a solid content of 30%.
实施例4Example 4
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯27份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯3‰份、ISTA(丙烯酸异十八烷基酯)3‰份、乙酸乙酯50份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入20份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。According to weight, accurately weigh 27 parts of isooctyl acrylate, 3 parts of hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 3‰ parts of ISTA (isostearyl acrylate), and 50 parts of ethyl acetate, place them in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, pass nitrogen, stir at 62°C for 45 minutes, then add 0.25‰ parts of AIBN, maintain the temperature and stir to react for 2 hours; then raise the temperature to 65°C and react for 3h; add 0.6‰ parts of AIBN, raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 20 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
实施例5Example 5
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯3‰份、ISTA(丙烯酸异十八烷基酯)2‰份、LA(丙烯酸十二烷基酯)1‰份、乙酸乙酯43份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入27份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。According to weight, 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 2‰ parts of ISTA (isooctadecyl acrylate), 1‰ part of LA (dodecyl acrylate), and 43 parts of ethyl acetate were accurately weighed, placed in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, nitrogen was introduced, and 0.25‰ parts of AIBN were added after stirring at 62°C for 45 minutes, and the temperature was maintained and stirred for 2 hours; then the temperature was raised to 65°C for reaction for 3 hours; 0.6‰ parts of AIBN were added, the temperature was raised to 72°C and the reaction was continued for 5 hours; after cooling, 27 parts of ethyl acetate was added for dilution to obtain OCA glue with a solid content of 30%.
实施例6Example 6
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯3‰份、ISTA(丙烯酸异十八烷基酯)2‰份、LMA(甲基丙烯酸月桂酯)1‰份,乙酸乙酯56份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.5‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.7‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入14份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。According to weight, accurately weigh 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 2‰ parts of ISTA (isostearyl acrylate), 1‰ part of LMA (lauryl methacrylate), and 56 parts of ethyl acetate, put them in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, pass nitrogen, stir at 62°C for 45 minutes, then add 0.5‰ parts of AIBN, maintain the temperature and stir to react for 2 hours; then raise the temperature to 65°C and react for 3h; add 0.7‰ parts of AIBN, raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 14 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
对比例1Comparative Example 1
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。Accurately weigh 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, and 48 parts of ethyl acetate by weight, place in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, introduce nitrogen, stir at 62°C for 45 minutes, then add 0.25‰ parts of AIBN, maintain the temperature and stir to react for 2 hours; then raise the temperature to 65°C to react for 3 hours; raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 22 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
对比例2Comparative Example 2
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。Accurately weigh 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, and 48 parts of ethyl acetate by weight, place them in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, introduce nitrogen, stir at 62°C for 45 minutes, then add 0.25‰ parts of AIBN, maintain the temperature and stir for 2 hours; then raise the temperature to 65°C and react for 3 hours; add 0.6‰ parts of AIBN, raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 22 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
对比例3Comparative Example 3
本例与实施例1的不同之处仅在于OCA胶水的制备方法,本例中,OCA胶水具体通过以下方法制备得到:The difference between this example and Example 1 is only the preparation method of OCA glue. In this example, OCA glue is prepared by the following method:
按重量份计,准确称取丙烯酸异辛酯15份、丙烯酸丁酯12份、丙烯酸羟丁酯3份,甲基丙烯酸甲酯3‰份、C-17A(丙烯酸十七烷基酯)3‰份、乙酸乙酯48份,置于装有搅拌器、冷凝器和氮气管的四口烧瓶中,通入氮气,62℃搅拌45分钟后加入0.25‰份的AIBN,保持温度搅拌反应2小时;随后升温至65℃反应3h;补加0.6‰份的AIBN,升高温度至72℃继续反应5小时;经冷却后加入22份的乙酸乙酯稀释,得到固含量为30%的OCA胶水。Accurately weigh 15 parts of isooctyl acrylate, 12 parts of butyl acrylate, 3 parts of hydroxybutyl acrylate, 3‰ parts of methyl methacrylate, 3‰ parts of C-17A (heptadecadecyl acrylate), and 48 parts of ethyl acetate by weight, place them in a four-necked flask equipped with a stirrer, a condenser and a nitrogen tube, introduce nitrogen, stir at 62°C for 45 minutes, then add 0.25‰ parts of AIBN, maintain the temperature and stir to react for 2 hours; then raise the temperature to 65°C and react for 3 hours; add 0.6‰ parts of AIBN, raise the temperature to 72°C and continue to react for 5 hours; after cooling, add 22 parts of ethyl acetate to dilute to obtain OCA glue with a solid content of 30%.
实施例1-6和对比例1-3的OCA胶水的配方具体如下表1所示:The formula of the OCA glue of Examples 1-6 and Comparative Examples 1-3 is specifically shown in Table 1 below:
表1Table 1
将实施例1-6和对比例1-3制备的胶膜产品进行如下性能测试:The film products prepared in Examples 1-6 and Comparative Examples 1-3 were subjected to the following performance tests:
(1)剥离力测试:剥离力是按照压敏胶粘带180°剥离强度试验方法,参照GB/T2792—1998实施进行。(1) Peel strength test: The peel strength test is carried out according to the 180° peel strength test method for pressure-sensitive adhesive tapes and in accordance with GB/T2792-1998.
(2)凝胶率测试:将1克重的胶膜放置于镍网中浸泡于甲苯和乙酸乙酯(1:1)的混合溶剂中,静置72h后将样品取出,150℃干燥2h后称重,胶膜的残留重量与原重量之比即为凝胶率。(2) Gel fraction test: A 1 gram film was placed on a nickel mesh and immersed in a mixed solvent of toluene and ethyl acetate (1:1). After standing for 72 hours, the sample was taken out and dried at 150°C for 2 hours and then weighed. The ratio of the residual weight of the film to the original weight was the gel fraction.
(3)内聚力测试:将样品制成制样25mm*150mm大小(双面胶背面需贴25umPET作为背衬),测试板SUS304镜面板,贴合后,2kg压辊,来回滚压3次,20min后挂重1kg,常温/24h后位移量≤1.0mm、70℃/24h后位移量≤2.0mm即为合格(PASS)。(3) Cohesion test: The sample is made into a 25mm*150mm size (the back of the double-sided tape needs to be pasted with 25um PET as the backing), and the test board is SUS304 mirror plate. After lamination, a 2kg roller is used to roll back and forth 3 times. After 20 minutes, a 1kg weight is hung. The displacement after room temperature/24h is ≤1.0mm, and the displacement after 70℃/24h is ≤2.0mm, which is qualified (PASS).
(4)蠕变回复测试:TA流变仪施加20kpa的剪切应力,回复时间600s,常温蠕变回复率超过90%,最大应变超过300%,-20℃蠕变回复率超过85%,最大应变超过90%,即为合格(PASS)。(4) Creep recovery test: The TA rheometer applies a shear stress of 20 kPa, with a recovery time of 600 s. The creep recovery rate at room temperature exceeds 90%, and the maximum strain exceeds 300%. The creep recovery rate at -20 °C exceeds 85%, and the maximum strain exceeds 90%, which is considered qualified (PASS).
(5)静态弯折测试:将50μm厚的胶膜两面贴合50μm的PET,然后裁成160mm长*40mm宽的样条,然后将样品尾部通过高温绝缘胶纸固定1N重砝码(100g),悬挂于半径R=1.5mm的治具上,投入65℃/95%RH存储实验箱中24h,待冷却后取出测量尾部折痕宽度,根据行业现状,测量宽度达到35mm即具备较好的耐弯折性能,即为合格(PASS)。(5) Static bending test: a 50 μm thick film is laminated with 50 μm PET on both sides, and then cut into 160 mm long * 40 mm wide strips. A 1N weight (100 g) is fixed to the tail of the sample through high-temperature insulating tape and hung on a fixture with a radius of R = 1.5 mm. The sample is placed in a 65°C/95% RH storage test box for 24 hours. After cooling, the sample is taken out and the width of the crease at the tail is measured. According to the current industry situation, a measured width of 35 mm indicates good bending resistance and is considered qualified (PASS).
测试结果如下表2所示:The test results are shown in Table 2 below:
表2Table 2
从实验数据可以看出,实施例1-6制备的胶膜产品的各项测试性能均比较优异。It can be seen from the experimental data that the film products prepared in Examples 1-6 have excellent performance in various tests.
对比例1未在高温段进行滴加引发剂,无法满足低模量与高粘性能,蠕变性能测试不达标;Comparative Example 1 did not add the initiator in the high temperature section, could not meet the low modulus and high viscosity performance, and the creep performance test did not meet the standard;
对比例2缺少长碳链单体ISTA,也无法同时满足低模量与高粘性,蠕变性能测试也不达标;Comparative Example 2 lacks the long carbon chain monomer ISTA, and cannot simultaneously meet the requirements of low modulus and high viscosity, and the creep performance test also fails to meet the standards;
对比例3添加长链单体C-17A代替ISTA,效果不佳,粘性差。Comparative Example 3 adds long-chain monomer C-17A instead of ISTA, but the effect is not good and the viscosity is poor.
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311624318.2A CN117866559A (en) | 2023-11-30 | 2023-11-30 | Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311624318.2A CN117866559A (en) | 2023-11-30 | 2023-11-30 | Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117866559A true CN117866559A (en) | 2024-04-12 |
Family
ID=90580150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311624318.2A Pending CN117866559A (en) | 2023-11-30 | 2023-11-30 | Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117866559A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120156162A (en) * | 2025-05-16 | 2025-06-17 | 太仓展新胶粘材料股份有限公司 | Composite glass protective sticker for flexible folding screen and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180340098A1 (en) * | 2015-11-25 | 2018-11-29 | Toyo Ink Sc Holdings Co., Ltd. | Adhesive and adhesive tape |
| JP2020083996A (en) * | 2018-11-21 | 2020-06-04 | 日東電工株式会社 | Adhesive sheet, manufacturing method thereof, and manufacturing method of image display device |
| WO2022210638A1 (en) * | 2021-04-02 | 2022-10-06 | 積水化学工業株式会社 | Pressure-sensitive adhesive tape |
| JP2023053776A (en) * | 2021-10-01 | 2023-04-13 | アイカ工業株式会社 | adhesive composition |
-
2023
- 2023-11-30 CN CN202311624318.2A patent/CN117866559A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180340098A1 (en) * | 2015-11-25 | 2018-11-29 | Toyo Ink Sc Holdings Co., Ltd. | Adhesive and adhesive tape |
| JP2020083996A (en) * | 2018-11-21 | 2020-06-04 | 日東電工株式会社 | Adhesive sheet, manufacturing method thereof, and manufacturing method of image display device |
| WO2022210638A1 (en) * | 2021-04-02 | 2022-10-06 | 積水化学工業株式会社 | Pressure-sensitive adhesive tape |
| JP2023053776A (en) * | 2021-10-01 | 2023-04-13 | アイカ工業株式会社 | adhesive composition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN120156162A (en) * | 2025-05-16 | 2025-06-17 | 太仓展新胶粘材料股份有限公司 | Composite glass protective sticker for flexible folding screen and preparation method thereof |
| CN120156162B (en) * | 2025-05-16 | 2025-08-08 | 太仓展新胶粘材料股份有限公司 | Composite glass protective paste for flexible folding screen and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI741191B (en) | Adhesive sheet | |
| CN116478643B (en) | Bending-resistant low-modulus OCA glue for folding screens and preparation method thereof, and OCA adhesive | |
| TW200923041A (en) | Indium-tin-oxide compatible optically clear adhesive | |
| CN117866559A (en) | Folding OCA adhesive and film with high adhesive properties for UTG materials and preparation method thereof | |
| CN117701196A (en) | Low-modulus acrylic ester adhesive film and preparation method and application thereof | |
| CN116218423B (en) | UV tackifying adhesive and preparation method thereof | |
| EP4431579A1 (en) | Adhesive film and preparation method therefor, composite component, and electronic device | |
| CN113773770B (en) | Double-curing pressure-sensitive adhesive and preparation method of support film protective adhesive tape thereof | |
| CN116042107A (en) | Acrylic foam adhesive tape resistant to high-temperature and high-humidity environment and preparation method thereof | |
| CN105745293A (en) | Double-sided adhesive sheet and method for producing double-sided adhesive sheet | |
| WO2025087200A1 (en) | Oled display module device | |
| CN115340834B (en) | Explosion-proof membrane and preparation method thereof | |
| CN118853031A (en) | Acrylic pressure-sensitive adhesive for flexible OLED support film, support film and preparation method thereof | |
| TWI714932B (en) | Adhesive for flexible optical film | |
| CN115991967B (en) | Glue forming composition, glue and flexible display device | |
| CN116285865A (en) | Organic silicon pressure-sensitive adhesive, preparation method thereof and pressure-sensitive adhesive tape | |
| CN105745296A (en) | Adhesive composition and method for producing adhesive sheet | |
| CN116640525A (en) | Flexible display screen PI support film and preparation method thereof | |
| CN116376463A (en) | A kind of preparation method of composite silica gel OCA film for touch screen | |
| CN118389101A (en) | Dual-curable high-viscosity folding OCA adhesive, adhesive film and preparation method | |
| CN119709060B (en) | OCA optical cement with strong creep property, low storage modulus and self-repairing function and preparation method thereof | |
| CN117701195A (en) | High-adhesion bending-resistant OCA glue and adhesive, and preparation methods and applications thereof | |
| CN119161820A (en) | Bending resistant optical adhesive sheet | |
| CN119193030A (en) | Optical adhesive sheet for protective film | |
| CN119736044A (en) | OCA glue, OCA adhesive, adhesive film and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |