WO2024103441A1 - Ultra-low-viscosity sprayable ocr glue for full-lamination module, and preparation method therefor - Google Patents

Ultra-low-viscosity sprayable ocr glue for full-lamination module, and preparation method therefor Download PDF

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Publication number
WO2024103441A1
WO2024103441A1 PCT/CN2022/134939 CN2022134939W WO2024103441A1 WO 2024103441 A1 WO2024103441 A1 WO 2024103441A1 CN 2022134939 W CN2022134939 W CN 2022134939W WO 2024103441 A1 WO2024103441 A1 WO 2024103441A1
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Prior art keywords
acrylate
weight
parts
ultra
sprayable
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PCT/CN2022/134939
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French (fr)
Chinese (zh)
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金闯
梁哲会
冉光富
齐杰
丁豪杰
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太仓斯迪克新材料科技有限公司
江苏斯迪克新材料科技股份有限公司
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Publication of WO2024103441A1 publication Critical patent/WO2024103441A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
    • B65B33/00—Packaging articles by applying removable, e.g. strippable, coatings
    • B65B33/04—Packaging large articles, e.g. complete machines, aircraft
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • 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
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the invention relates to the field of OCR glue, and in particular to an ultra-low-viscosity, sprayable OCR glue for a full film lamination set and a preparation method thereof.
  • Capacitive touch screens are made by coating a transparent thin-film conductive layer on a glass screen, and then adding a protective glass outside the conductive layer.
  • the double-glass design can completely protect the conductive layer and the sensor.
  • capacitive touch screens are mainly bonded using optical-grade pressure-sensitive adhesive tape (OCA).
  • the touch display integrated module is divided into three layers: display screen, touch screen and protective glass.
  • the three-layer integrated structure is formed by laminating. It can be laminated by full lamination or frame lamination.
  • the frame lamination mainly uses double-sided adhesive film to fix the four sides together, and there will be an air layer between the layers.
  • the full lamination technology uses OCA film or OCR glue to glue the screens together seamlessly, eliminating the air gap between the screens, greatly reducing the reflection of light, reducing the loss of transmitted light, and thus improving the brightness and enhancing the display effect.
  • the thickness of the fully laminated screen is reduced by more than 100 microns compared to the ordinary lamination method, making the body thinner and lighter.
  • the close combination of the touch screen and the display panel can not only improve the strength, but also effectively reduce the impact of noise on the touch screen, and improve the smoothness of the touch operation. It also helps with the narrow frame design, making the frame narrower.
  • OCA Optically clear pressure-sensitive adhesive tape
  • OCA Optically clear pressure-sensitive adhesive tape
  • It has the advantages of optical transparency, high transmittance, good bonding strength, no special requirements for the substrate of the bonding product, uniform thickness, high production efficiency, no glue overflow problem, controllable bonding area, no corrosion problem, etc. It is particularly suitable for bonding small-sized products; however, there are problems such as difficulty in rework, need to be cut according to the shape and size of the substrate, easy to cause the adhesive material to fall off, insufficient contact between the adhesive layer and the bonding surface, or easy mixing of bubbles or dents on the bonding surface.
  • Liquid optically clear adhesive is colorless and transparent, has high transmittance, good bonding strength, and can be cured under light or heat conditions. It can be used for laminating flat, curved and uneven surfaces, especially for large-size lamination; it has special advantages over OCA film in terms of regular shapes, sizes, gaps and comprehensive costs of laminating surfaces, and can solve the limitations of OCA film.
  • patent CN 102426494 A introduces block olefins into acrylic resin to greatly improve the adhesion of OCR glue, but the disadvantage is also obvious.
  • the viscosity of the product is too high to be sprayed;
  • patent CN 114316895 A uses a silicone system to prepare OCR glue, which greatly improves the optical properties and chemical resistance, but the high viscosity is still a major defect that makes it impossible to spray.
  • Patent CN 113831848 A uses an acrylic system and has a low viscosity that can be sprayed, but there is only a description of tg ⁇ 0°C without a specific numerical value.
  • the relatively high glass transition temperature is obviously not conducive to peel strength.
  • the patented product does not describe or reflect the peel strength.
  • the first object of the present invention is to provide an ultra-low viscosity, sprayable OCR glue for a fully laminated module, which is composed of the following raw materials in weight ratio:
  • the auxiliary agent is a defoamer, a wetting and dispersing agent, an adhesion promoter or a silane coupling agent;
  • the acrylic resin is at least one of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate.
  • the photoinitiator is at least one of 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, benzoin dimethyl ether, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, and 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester.
  • the photoinitiator is a combination of 1-hydroxycyclohexyl phenyl ketone (184) and photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO).
  • TPO 2,4,6-trimethylbenzoyl-diphenylphosphine oxide
  • the acrylic monomer is at least one of isobornyl acrylate, tetrahydrofuran acrylate, silane acrylate, lauric acid acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, butyl acrylate, 4-(1-oxo-2-propenyl)morpholine, stearic acid acrylate, isooctyl acrylate, and isodecyl acrylate.
  • the acrylic monomer is isodecyl acrylate or a mixture comprising isodecyl acrylate.
  • the antioxidant is a hindered phenol antioxidant.
  • the present invention also relates to a method for preparing the ultra-low viscosity, sprayable OCR glue for a full lamination set as described above, comprising the following steps:
  • step S1 mixing is performed under the conditions of being protected from light and having a humidity of less than 50%.
  • step S1 acrylic resin, acrylic monomer, photoinitiator, antioxidant and auxiliary agent are weighed in parts by weight and mixed, and stirred at a speed of 500 RPM for 30 minutes using a high-speed disperser to obtain a uniform mixed solution.
  • the beneficial effect of the present invention is that the present invention provides an ultra-low viscosity, sprayable OCR glue for full lamination modules, which is composed of the following raw materials in weight ratio: 15-25 parts of acrylic resin; 65-80 parts of acrylic monomer; 0.5-4 parts of photoinitiator; 0.1-0.5 parts of antioxidant; 0.1-0.5 parts of auxiliary agent; wherein the auxiliary agent is a defoamer, a wetting dispersant, an adhesion promoter or a silane coupling agent; the acrylic resin is one or more of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate.
  • the present invention also relates to a preparation method of the OCR glue, and the OCR glue prepared thereby has high bonding strength, high elongation, good optical properties, stable modulus under heavy and high temperature, low tg, and is suitable for Inkjet spraying viscosity.
  • the present invention relates to an ultra-low-viscosity, sprayable OCR glue for a fully-fitted module, which is composed of the following raw materials in the following weight ratio:
  • the additive is a defoamer, a wetting and dispersing agent, an adhesion promoter or a silane coupling agent; specifically, the additive can be BYK-088, BYK A530, BYK DISPER 163, BYK 3550, BYK 4500, BYK 4510, A187, A1120, A174, etc.;
  • Acrylic resin is a mixture of one or more of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate; the molecules of acrylic resin contain a variety of characteristic functional groups, so that the cured OCR glue has excellent wear resistance, adhesion, flexibility, peel strength, low temperature resistance, optical properties and weather resistance.
  • the acrylic resin can be CN9004, CN152, CN153, CN2273, CN9023, CN9021, CN9018, etc.
  • the present invention fully cooperates with each other, takes the advantages and makes up for the shortcomings, and the OCR glue obtained has excellent properties; and in the process of touch screen production, it can be sprayed and fully bonded efficiently, and there will be no air residue between the screens, fast curing speed, high production efficiency, extremely low viscosity, high peel strength, good light transmittance, low haze, stable medium and high temperature modulus, good yellowing resistance, and has excellent usability and curing performance.
  • OCR glue can be prepared using silicone system theory to a certain extent, but excessive viscosity is always a problem that needs to be solved for efficient spraying.
  • Acrylic resin 15-25 parts The acrylic resin content within this weight range plays a very important role in peel strength. Too low will cause a sharp drop in peel strength, and too high will cause an increase in viscosity.
  • the photoinitiator is one or a mixture of 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexylphenyl ketone, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, benzoin dimethyl ether, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester.
  • the photoinitiator is a combination of 1-hydroxycyclohexylphenyl ketone (184) and photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO).
  • the acrylic monomer is one or a mixture of one or more of isobornyl acrylate, tetrahydrofuran acrylate, silyl acrylate, lauric acid acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, butyl acrylate, 4-(1-oxo-2-propenyl)morpholine, stearic acid acrylate, isooctyl acrylate, and isodecyl acrylate.
  • the acrylic monomer is isodecyl acrylate or a mixture containing isodecyl acrylate; the use of the long-chain monomer isodecyl acrylate SR395 provides a guarantee for tg, and further provides a guarantee of modulus and adhesion.
  • the antioxidant may be a hindered phenol, a phosphite, a carbon radical scavenger, a metal passivator, etc.
  • the antioxidant in order to ensure thermal stability, not affect light curing, and contain no metal ions, the antioxidant is a hindered phenol antioxidant.
  • the present invention also relates to a method for preparing an ultra-low-viscosity, sprayable OCR glue for a full film lamination set, comprising the following steps:
  • the mixed liquid is vacuum degassed for 15 minutes to form a final product, which is a touch screen OCR glue with high bonding strength, high elongation, good optical performance, stable modulus under heavy and high temperatures, low tg, and suitable viscosity for Inkjet spraying.
  • step S1 mixing is performed under conditions of light protection and humidity less than 50%; because the product is light sensitive and needs to be protected from light, water vapor will cause incomplete curing, and the reaction can proceed smoothly when the humidity is below 50.
  • step S1 acrylic resin, acrylic monomer, photoinitiator, antioxidant, and additive are weighed by weight and mixed, and a high-speed disperser is used to fully stir at a speed of 500 RPM for 30 minutes to obtain a uniform mixed solution.
  • the above OCR glue preparation method is used to prepare a glue composition as shown in Table 2 below, and then tested.
  • Examples 1-3 and Comparative Examples 1-8 were respectively subjected to ultraviolet irradiation at a wavelength of UV-LED 365, with a cumulative energy of not less than 5000 mj;
  • Test method multifunctional continuous induction viscometer method; test instrument: DV2T LV; calibration: silicone oil standard liquid; test rotor: 61-64 or SC4-18; torque range: 40-60%; measurement temperature: 25°C.
  • Test instrument Anton Paar MCR302; Specimen size: cylinder with 8mm diameter and 1mm thickness; Temperature range: -50-100°C; Heating rate: 3°C/min; Deformation mode: shear mode; Test frequency: 1Hz.
  • Examples 1-3 The various properties of Examples 1-3 in which the components are reasonably matched in the present invention are excellent.
  • the content of acrylic resin is too low, and the peel strength of the product is poor, which may be due to the reduction of the content of the characteristic group that promotes adhesion and the reduction of the density of hydrogen bonds;
  • the content of acrylic resin is relatively high, and the comprehensive performance is good, but the viscosity of the product is significantly increased, which is not conducive to Inkjet spraying; in Comparative Example 3, only a single photoinitiator 184 is used, and the peel strength of the product is low, which is due to the lack of the synergistic effect of the initiator.
  • Comparative Example 4 only a single photoinitiator TPO is used, and the modulus of the product is significantly reduced, which is due to the insufficient efficiency of the single initiator.
  • Comparative Example 5 a combination of photoinitiators 184 and 1173 is used, and the peel strength of the product is low, which is due to the single effect of the combination.
  • Comparative Example 6 a combination of photoinitiators TPO and 1173 is used, and the modulus of the product is significantly reduced, which is due to the insufficient curing effect of the combination.
  • Comparative Example 7 a combination of photoinitiators 651 and 1173 is used, and the optical YI of the product is significantly increased, which is due to the yellowing of 651 in the combination.

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

An ultra-low-viscosity sprayable OCR glue for a full-lamination module. The OCR glue is prepared from the following raw materials in parts by weight: 15-25 parts of an acrylic resin; 65-80 parts of an acrylic monomer; 0.5-4 parts of a photoinitiator; 0.1-0.5 parts of an antioxidant; and 0.1-0.5 parts of an auxiliary agent, wherein the auxiliary agent is a defoaming agent, a wetting dispersant, an adhesion promoter or a silane coupling agent; and the acrylic resin is one or a mixture of more than one of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate. The present invention further relates to a preparation method for the OCR glue. The OCR glue prepared thereby has a high bonding strength, high elongation, good optical performance, a stable heavy high-temperature modulus, and a low Tg, and is also suitable for Inkjet spraying viscosity.

Description

超低粘、可喷涂的用于全贴膜组的OCR胶水及其制备方法Ultra-low viscosity, sprayable OCR glue for full film lamination set and preparation method thereof 技术领域Technical Field
本发明涉及OCR胶领域，尤其涉及一种超低粘、可喷涂的用于全贴膜组的OCR胶水及其制备方法。The invention relates to the field of OCR glue, and in particular to an ultra-low-viscosity, sprayable OCR glue for a full film lamination set and a preparation method thereof.
背景技术Background technique
随着电子技术的发展，传统的按键方式已被逐渐淘汰，触控方式已广泛出现于我们的生产生活当中，电容式触控屏技术的发展使人们意识到电容式触摸屏技术的飞速发展将会彻底改变现有的生活方式，触控显示一体化模组更成为目前的主流趋势。With the development of electronic technology, the traditional button method has been gradually eliminated, and the touch method has been widely used in our production and life. The development of capacitive touch screen technology has made people realize that the rapid development of capacitive touch screen technology will completely change the existing lifestyle, and the touch display integrated module has become the current mainstream trend.
电容式触控屏是在玻璃屏幕上镀上一层透明的薄膜导电层，再在导电层外加上一块保护玻璃，双玻璃设计能彻底保护导电层及感应器，目前电容式触控屏的贴合主要采用光学级的压敏胶带(OCA)作为贴合的一种方式。Capacitive touch screens are made by coating a transparent thin-film conductive layer on a glass screen, and then adding a protective glass outside the conductive layer. The double-glass design can completely protect the conductive layer and the sensor. Currently, capacitive touch screens are mainly bonded using optical-grade pressure-sensitive adhesive tape (OCA).
触控显示一体化模组分为显示屏、触摸屏和保护玻璃三层结构，采用贴合的方法构成三层一体结构。可以采用全贴合或框贴两种方式进行贴合，其中框贴主要使用双面胶膜将四边固定贴合，层之间会存在着空气层。全贴合技术采用OCA胶膜或OCR胶水将屏屏之间无缝隙粘贴在一起，消除了屏幕间的空气间隙，大幅度降低光线的反射，减少透出光线的损耗进而提升亮度，增强了显示效果。全贴合屏比较普通贴合方式厚度降低100微米以上，使机身更轻薄。触摸屏与显示面板紧密结合不但能提高强度，更能有效降低噪声对触控学号所造成的影响，提升触控操作的流畅性。同时也有助于窄边框设计，使边框可以做到更窄。The touch display integrated module is divided into three layers: display screen, touch screen and protective glass. The three-layer integrated structure is formed by laminating. It can be laminated by full lamination or frame lamination. The frame lamination mainly uses double-sided adhesive film to fix the four sides together, and there will be an air layer between the layers. The full lamination technology uses OCA film or OCR glue to glue the screens together seamlessly, eliminating the air gap between the screens, greatly reducing the reflection of light, reducing the loss of transmitted light, and thus improving the brightness and enhancing the display effect. The thickness of the fully laminated screen is reduced by more than 100 microns compared to the ordinary lamination method, making the body thinner and lighter. The close combination of the touch screen and the display panel can not only improve the strength, but also effectively reduce the impact of noise on the touch screen, and improve the smoothness of the touch operation. It also helps with the narrow frame design, making the frame narrower.
光学透明压敏胶带(OCA)主要用于粘接透明光学元件，其具有光学透明、透过率高、粘接强度良好、对贴合产品基材无特殊要求、厚度均匀、生产效 率高、无溢胶问题、粘接区域可控、无腐蚀性问题等优点，特别适用于小尺寸的产品贴合；但存在着如不易返修、需要根据基材形状尺寸等原因进行裁切、容易产生胶材脱落、胶层与粘接面之间接触不充分或者在贴合面容易混入气泡或者出现凹痕等问题。Optically clear pressure-sensitive adhesive tape (OCA) is mainly used for bonding transparent optical components. It has the advantages of optical transparency, high transmittance, good bonding strength, no special requirements for the substrate of the bonding product, uniform thickness, high production efficiency, no glue overflow problem, controllable bonding area, no corrosion problem, etc. It is particularly suitable for bonding small-sized products; however, there are problems such as difficulty in rework, need to be cut according to the shape and size of the substrate, easy to cause the adhesive material to fall off, insufficient contact between the adhesive layer and the bonding surface, or easy mixing of bubbles or dents on the bonding surface.
液体光学透明胶水(OCR)具有无色透明、透过率高、粘接强度好、可在光或热条件下固化。可用于平面、曲面及不平整表面的贴合，尤其适用于大尺寸贴合；在贴合表面规则形状、大小和缝隙落差及综合成本上相对于OCA胶膜具有特别的优势，能解决OCA胶膜的局限性。Liquid optically clear adhesive (OCR) is colorless and transparent, has high transmittance, good bonding strength, and can be cured under light or heat conditions. It can be used for laminating flat, curved and uneven surfaces, especially for large-size lamination; it has special advantages over OCA film in terms of regular shapes, sizes, gaps and comprehensive costs of laminating surfaces, and can solve the limitations of OCA film.
现有的OCR胶水大都不能兼顾高粘合强度、高伸长率，良好的光学性能、中高温模量稳定、低tg同时粘度超低(可喷涂施工)。如专利CN 102426494 A，在丙烯酸树脂中引入嵌段烯烃极大的提高了OCR胶水的附着力，但缺点也很明显，产品的粘度过高无法喷涂；专利CN 114316895 A采用了硅胶体系制备OCR胶水，很好的改善了光学性能和耐化性，但高粘度仍是一个导致无法喷涂的重大缺陷。专利CN 113831848 A采用了丙烯酸体系，具备了可喷涂的低粘度，但只有tg<0℃的描述没有具体的数值体现，相对高的玻璃化温度对剥离强度显然是不利的，同时该专利产品并没有对剥离强度方面的描述和体现。Most of the existing OCR glues cannot take into account high bonding strength, high elongation, good optical properties, stable modulus at medium and high temperatures, low tg and ultra-low viscosity (can be sprayed). For example, patent CN 102426494 A introduces block olefins into acrylic resin to greatly improve the adhesion of OCR glue, but the disadvantage is also obvious. The viscosity of the product is too high to be sprayed; patent CN 114316895 A uses a silicone system to prepare OCR glue, which greatly improves the optical properties and chemical resistance, but the high viscosity is still a major defect that makes it impossible to spray. Patent CN 113831848 A uses an acrylic system and has a low viscosity that can be sprayed, but there is only a description of tg<0℃ without a specific numerical value. The relatively high glass transition temperature is obviously not conducive to peel strength. At the same time, the patented product does not describe or reflect the peel strength.
如此需要现有的OCR胶水进行改进，设计出一种粘合强度高、伸长率高，光学性能好、重高温模量稳定、低tg，同时具有适合Inkjet喷涂粘度的触摸屏OCR胶水。Therefore, it is necessary to improve the existing OCR glue and design a touch screen OCR glue with high bonding strength, high elongation, good optical performance, stable modulus under heavy and high temperature, low tg, and suitable viscosity for Inkjet spraying.
发明内容Summary of the invention
为了克服现有技术的不足，本发明的第一个目的是提供一种超低粘、可喷涂的用于全贴合模组的OCR胶水，由如下重量配比的原料组成：In order to overcome the shortcomings of the prior art, the first object of the present invention is to provide an ultra-low viscosity, sprayable OCR glue for a fully laminated module, which is composed of the following raw materials in weight ratio:
Figure PCTCN2022134939-appb-000001
Figure PCTCN2022134939-appb-000001
Figure PCTCN2022134939-appb-000002
Figure PCTCN2022134939-appb-000002
其中，所述助剂为消泡剂、润湿分散剂、附着力促进剂或硅烷偶联剂；Wherein, the auxiliary agent is a defoamer, a wetting and dispersing agent, an adhesion promoter or a silane coupling agent;
所述丙烯酸树脂为聚氨酯丙烯酸酯、环氧丙烯酸酯、聚酯丙烯酸酯及聚烯烃丙烯酸酯中的至少一种。The acrylic resin is at least one of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate.
优选地，Preferably,
丙烯酸树脂      15-25份。Acrylic resin      15-25 parts.
优选地，所述光引发剂为2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮、安息香双甲醚、2，4，6-三甲基苯甲酰基-二苯基氧化膦、2，4，6-三甲基苯甲酰基苯基膦酸乙酯中的至少一种。Preferably, the photoinitiator is at least one of 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, benzoin dimethyl ether, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, and 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester.
优选地，光引发剂为1-羟基环己基苯基甲酮(184)、光引发剂2，4，6-三甲基苯甲酰基-二苯基氧化膦(TPO)的组合。Preferably, the photoinitiator is a combination of 1-hydroxycyclohexyl phenyl ketone (184) and photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO).
优选地，所述丙烯酸单体为丙烯酸异冰片酯、四氢呋喃丙烯酸酯、丙烯酸基硅烷酯、月桂酸丙烯酸酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、丙烯酸丁酯、4-(1-氧代-2-丙烯基)吗啡啉、硬脂酸丙烯酸酯、丙烯酸异辛酯、丙烯酸异癸酯中的至少一种。Preferably, the acrylic monomer is at least one of isobornyl acrylate, tetrahydrofuran acrylate, silane acrylate, lauric acid acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, butyl acrylate, 4-(1-oxo-2-propenyl)morpholine, stearic acid acrylate, isooctyl acrylate, and isodecyl acrylate.
优选地，所述丙烯酸单体为丙烯酸异癸酯或包含丙烯酸异癸酯的混合物。Preferably, the acrylic monomer is isodecyl acrylate or a mixture comprising isodecyl acrylate.
优选地，所述抗氧剂为受阻酚类抗氧剂。Preferably, the antioxidant is a hindered phenol antioxidant.
本发明还涉及一种如上所述的超低粘、可喷涂的用于全贴膜组的OCR胶水的制备方法，包括以下步骤：The present invention also relates to a method for preparing the ultra-low viscosity, sprayable OCR glue for a full lamination set as described above, comprising the following steps:
S1：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合以形成混合液；S1: Weigh acrylic resin, acrylic monomer, photoinitiator, antioxidant, and additive according to weight to form a mixed solution;
S2：将所述混合液真空脱泡15分钟，以形成最终成品。S2: vacuum degassing the mixed solution for 15 minutes to form a final product.
9.如权利要求8所述的超低粘、可喷涂的用于全贴膜组的OCR胶水的制 备方法，其特征在于，步骤S1中：混合在避光、湿度小于50％的条件下进行。9. The method for preparing the ultra-low viscosity, sprayable OCR glue for the full film lamination set according to claim 8, characterized in that in step S1: mixing is performed under the conditions of being protected from light and having a humidity of less than 50%.
优选地，步骤S1中：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合，使用高速分散机，在500RPM速度下充分搅拌30分钟，以得到的均一混合液。Preferably, in step S1: acrylic resin, acrylic monomer, photoinitiator, antioxidant and auxiliary agent are weighed in parts by weight and mixed, and stirred at a speed of 500 RPM for 30 minutes using a high-speed disperser to obtain a uniform mixed solution.
相比现有技术，本发明的有益效果在于：本发明提供一种超低粘、可喷涂的用于全贴合模组的OCR胶水，由如下重量配比的原料组成：丙烯酸树脂15-25份；丙烯酸单体65-80份；光引发剂0.5-4份；抗氧剂0.1-0.5份；助剂0.1-0.5份；其中，助剂为消泡剂、润湿分散剂、附着力促进剂或硅烷偶联剂；丙烯酸树脂为聚氨酯丙烯酸酯、环氧丙烯酸酯、聚酯丙烯酸酯及聚烯烃丙烯酸酯中的一种或一种以上的混合物。本发明还涉及该OCR胶水的制备方法，由此制备的OCR胶水粘合强度高、伸长率高，光学性能好、重高温模量稳定、低tg，同时适合Inkjet喷涂粘度。Compared with the prior art, the beneficial effect of the present invention is that the present invention provides an ultra-low viscosity, sprayable OCR glue for full lamination modules, which is composed of the following raw materials in weight ratio: 15-25 parts of acrylic resin; 65-80 parts of acrylic monomer; 0.5-4 parts of photoinitiator; 0.1-0.5 parts of antioxidant; 0.1-0.5 parts of auxiliary agent; wherein the auxiliary agent is a defoamer, a wetting dispersant, an adhesion promoter or a silane coupling agent; the acrylic resin is one or more of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate. The present invention also relates to a preparation method of the OCR glue, and the OCR glue prepared thereby has high bonding strength, high elongation, good optical properties, stable modulus under heavy and high temperature, low tg, and is suitable for Inkjet spraying viscosity.
本上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例详细说明如后。本发明的具体实施方式由以下实施例详细给出。The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention. The specific implementation of the present invention is given in detail by the following embodiments.
具体实施方式Detailed ways
下面，结合具体实施方式，对本发明做进一步描述，需要说明的是，在不相冲突的前提下，以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。The present invention is further described below in conjunction with specific implementation methods. It should be noted that, under the premise of no conflict, the various embodiments or technical features described below can be arbitrarily combined to form a new embodiment.
本发明涉及一种超低粘、可喷涂的用于全贴合模组的OCR胶水，由如下重量配比的原料组成：The present invention relates to an ultra-low-viscosity, sprayable OCR glue for a fully-fitted module, which is composed of the following raw materials in the following weight ratio:
Figure PCTCN2022134939-appb-000003
Figure PCTCN2022134939-appb-000003
其中，助剂为消泡剂、润湿分散剂、附着力促进剂或硅烷偶联剂；具体地，助剂可为BYK-088、BYK A530、BYK DISPER 163，BYK 3550、BYK 4500、BYK 4510、A187、A1120、A174等；The additive is a defoamer, a wetting and dispersing agent, an adhesion promoter or a silane coupling agent; specifically, the additive can be BYK-088, BYK A530, BYK DISPER 163, BYK 3550, BYK 4500, BYK 4510, A187, A1120, A174, etc.;
丙烯酸树脂为聚氨酯丙烯酸酯、环氧丙烯酸酯、聚酯丙烯酸酯及聚烯烃丙烯酸酯中的一种或一种以上的混合物；丙烯酸树脂的分子中含有多种特征官能团，使固化后的OCR胶水具有优秀的耐磨性、粘附力、柔韧性、剥离强度、耐低温性能、光学性能和耐候性。具体地，丙烯酸树脂可为SARTOMER公司的CN9004、CN152、CN153、CN2273、CN9023、CN9021、CN9018等；本发明足足分相互配合，取长补短，制得的OCR胶水各项性能均很优异；而且在触摸屏制作过程中可以高效喷涂全贴合，不会有屏间空气残留，固化速度快、生产效率高、粘度极低、剥离强度高、透光性好、雾度低、中高温模量稳定、耐黄变性能好，具有优异的使用性和固化性能。Acrylic resin is a mixture of one or more of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate; the molecules of acrylic resin contain a variety of characteristic functional groups, so that the cured OCR glue has excellent wear resistance, adhesion, flexibility, peel strength, low temperature resistance, optical properties and weather resistance. Specifically, the acrylic resin can be CN9004, CN152, CN153, CN2273, CN9023, CN9021, CN9018, etc. of SARTOMER; the present invention fully cooperates with each other, takes the advantages and makes up for the shortcomings, and the OCR glue obtained has excellent properties; and in the process of touch screen production, it can be sprayed and fully bonded efficiently, and there will be no air residue between the screens, fast curing speed, high production efficiency, extremely low viscosity, high peel strength, good light transmittance, low haze, stable medium and high temperature modulus, good yellowing resistance, and has excellent usability and curing performance.
应当理解，在一定程度上使用有机硅体系理论也可制备OCR胶水，但是过高的粘度始终是一个高效喷涂需要解决的问题。It should be understood that OCR glue can be prepared using silicone system theory to a certain extent, but excessive viscosity is always a problem that needs to be solved for efficient spraying.
在一些实施例中，In some embodiments,
丙烯酸树脂      15-25份。该重量范围内的丙烯酸树脂含量对剥离强度起着非常重要的作用，过低会导致剥离强度急剧下降，过高会引起粘度上升。Acrylic resin      15-25 parts. The acrylic resin content within this weight range plays a very important role in peel strength. Too low will cause a sharp drop in peel strength, and too high will cause an increase in viscosity.
光引发剂为2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮、安息香双甲醚、2，4，6-三甲基苯甲酰基-二苯基氧化膦、2，4，6-三甲基苯甲酰基苯基膦酸乙酯中的一种或一种以上的混合物。在一些实施例中，为了保证固化的快速性且保证具有一定的漂白性，进而提高OCR胶水的耐黄变性，光引发剂为1-羟基环己基苯基甲酮(184)、光引发剂2，4，6-三甲基苯甲酰基-二苯基氧化膦(TPO)的组合。The photoinitiator is one or a mixture of 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexylphenyl ketone, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, benzoin dimethyl ether, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester. In some embodiments, in order to ensure rapid curing and certain bleaching properties, thereby improving the yellowing resistance of the OCR glue, the photoinitiator is a combination of 1-hydroxycyclohexylphenyl ketone (184) and photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO).
丙烯酸单体为丙烯酸异冰片酯、四氢呋喃丙烯酸酯、丙烯酸基硅烷酯、月桂酸丙烯酸酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、丙烯酸丁 酯、4-(1-氧代-2-丙烯基)吗啡啉、硬脂酸丙烯酸酯、丙烯酸异辛酯、丙烯酸异癸酯中的一种或一种以上的混合物。在一些实施例中，丙烯酸单体为丙烯酸异癸酯或包含丙烯酸异癸酯的混合物；该长链单体丙烯酸异癸酯SR395的使用为tg提供了保障，进一步提供了模量保证和粘接性。The acrylic monomer is one or a mixture of one or more of isobornyl acrylate, tetrahydrofuran acrylate, silyl acrylate, lauric acid acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, butyl acrylate, 4-(1-oxo-2-propenyl)morpholine, stearic acid acrylate, isooctyl acrylate, and isodecyl acrylate. In some embodiments, the acrylic monomer is isodecyl acrylate or a mixture containing isodecyl acrylate; the use of the long-chain monomer isodecyl acrylate SR395 provides a guarantee for tg, and further provides a guarantee of modulus and adhesion.
抗氧剂可为受阻酚、亚磷酸酯、碳自由基捕捉剂、金属钝化剂等。在一些实施例中，为了保证热稳定、不影响光固化、不含金属离子，抗氧剂为受阻酚类抗氧剂。The antioxidant may be a hindered phenol, a phosphite, a carbon radical scavenger, a metal passivator, etc. In some embodiments, in order to ensure thermal stability, not affect light curing, and contain no metal ions, the antioxidant is a hindered phenol antioxidant.
本发明还涉及一种超低粘、可喷涂的用于全贴膜组的OCR胶水的制备方法，包括以下步骤：The present invention also relates to a method for preparing an ultra-low-viscosity, sprayable OCR glue for a full film lamination set, comprising the following steps:
S1：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合以形成混合液；S1: Weigh acrylic resin, acrylic monomer, photoinitiator, antioxidant, and additive according to weight to form a mixed solution;
S2：将混合液真空脱泡15分钟，以形成最终成品，该最终成品为粘合强度高、伸长率高，光学性能好、重高温模量稳定、低tg，同时具有适合Inkjet喷涂粘度的触摸屏OCR胶水。S2: The mixed liquid is vacuum degassed for 15 minutes to form a final product, which is a touch screen OCR glue with high bonding strength, high elongation, good optical performance, stable modulus under heavy and high temperatures, low tg, and suitable viscosity for Inkjet spraying.
在一些实施例中，步骤S1中：混合在避光、湿度小于50％的条件下进行；因为产品对光敏感-需要避光，水汽会导致固化不完全-湿度50以下反应可以平稳进行。In some embodiments, in step S1: mixing is performed under conditions of light protection and humidity less than 50%; because the product is light sensitive and needs to be protected from light, water vapor will cause incomplete curing, and the reaction can proceed smoothly when the humidity is below 50.
在一些实施例中，为了提高反应效率，保证反应的均一性，步骤S1中：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合，使用高速分散机，在500RPM速度下充分搅拌30分钟，以得到的均一混合液。In some embodiments, in order to improve the reaction efficiency and ensure the uniformity of the reaction, in step S1: acrylic resin, acrylic monomer, photoinitiator, antioxidant, and additive are weighed by weight and mixed, and a high-speed disperser is used to fully stir at a speed of 500 RPM for 30 minutes to obtain a uniform mixed solution.
以下为用不同方法制备OCR胶水的实施例及对比例，不同实施例及对比例中所用原料如表1所示：The following are examples and comparative examples of preparing OCR glue using different methods. The raw materials used in the different examples and comparative examples are shown in Table 1:
表1原料明细表Table 1 Raw materials list
聚氨酯丙烯酸酯CN9004Polyurethane acrylate CN9004 SARTOMERSARTOMER
环氧丙烯酸酯CN152Epoxy acrylate CN152 SARTOMERSARTOMER
丙烯酸异癸酯SR395Isodecyl acrylate SR395 SARTOMERSARTOMER
丙烯酸丁酯BAButyl acrylate BA 济南普莱华Jinan Pulaihua
丙烯酸羟丁酯HBAHydroxybutyl acrylate HBA 日本三菱Mitsubishi
月桂酸丙烯酸酯LALauric Acid Acrylate LA 广东三旺化工Guangdong Sanwang Chemical
光引发剂1-羟基环己基苯基甲酮(184)Photoinitiator 1-Hydroxycyclohexylphenyl ketone (184) 常州强力新材Changzhou Qiangli New Materials
2-羟基-2-甲基-1-苯基丙酮(1173)2-Hydroxy-2-methyl-1-phenylpropanone(1173) 常州强力新材Changzhou Qiangli New Materials
安息香双甲醚(651)Benzoin dimethyl ether (651) 常州强力新材Changzhou Qiangli New Materials
光引发剂2，4，6-三甲基苯甲酰基-二苯基氧化膦(TPO)Photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO) 常州强力新材Changzhou Qiangli New Materials
抗氧剂1010Antioxidant 1010 青岛杰得佳Qingdao Jiedejia
附着力促进剂BYK 4510Adhesion promoter BYK 4510 大连连晟Dalian Liansheng
硅烷偶联剂A187Silane coupling agent A187 广东迈图Guangdong Maitu
实施例一Embodiment 1
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量14份、CN152重量7.6份，丙烯酸单体SR395重量26份、BA重量15份、HBA重量15份、LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 14 parts by weight of acrylic resin CN9004, 7.6 parts by weight of CN152, 26 parts by weight of acrylic monomer SR395, 15 parts by weight of BA, 15 parts by weight of HBA, 10 parts by weight of LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed liquid for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-fit modules.
实施例二Embodiment 2
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed solution for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
实施例三Embodiment 3
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量15份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 15 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed solution for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
对比例一Comparative Example 1
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量5份、CN152重量7.6份，丙烯酸单体SR395重量35份、BA重量15份、HBA重量15份、LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 5 parts by weight of acrylic resin CN9004, 7.6 parts by weight of CN152, 35 parts by weight of acrylic monomer SR395, 15 parts by weight of BA, 15 parts by weight of HBA, 10 parts by weight of LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed liquid for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
对比例二Comparative Example 2
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量20份、CN152重量7.6份，丙烯酸单体SR395重量20份、BA重量15份、HBA重量15份、LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 20 parts by weight of acrylic resin CN9004, 7.6 parts by weight of CN152, 20 parts by weight of acrylic monomer SR395, 15 parts by weight of BA, 15 parts by weight of HBA, 10 parts by weight of LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed liquid for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-fit modules.
对比例三Comparative Example 3
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂184重量2份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重 量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 2 parts by weight of photoinitiator 184, 0.1 parts by weight of antioxidant 1010, 0.1 parts by weight of auxiliary agent BYK4510 and 0.2 parts by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at a speed of 500RPM for 30 minutes, vacuum degas the obtained uniform mixed solution for 15 minutes, and prepare a sprayable, ultra-low viscosity OCR glue for full-fit modules.
对比例四Comparative Example 4
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂TPO重量2份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 2 parts by weight of photoinitiator TPO, 0.1 parts by weight of antioxidant 1010, 0.1 parts by weight of auxiliary agent BYK4510 and 0.2 parts by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed liquid for 15 minutes to prepare a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
对比例五Comparative Example 5
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂184重量1份、2-羟基-2-甲基-1-苯基丙酮(1173)重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator 184, 1 part by weight of 2-hydroxy-2-methyl-1-phenylpropanone (1173), 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187 were accurately weighed and added into the container in sequence, and the mixture was stirred thoroughly at 500RPM for 30 minutes using a high-speed disperser, and the obtained uniform mixed solution was vacuum degassed for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
对比例六Comparative Example 6
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂TPO重量1份、2-羟基-2-甲基-1-苯基丙酮重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速 分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator TPO, 1 part by weight of 2-hydroxy-2-methyl-1-phenylpropanone, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, add them into the container in sequence, use a high-speed disperser, stir thoroughly at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed solution for 15 minutes, and prepare a sprayable, ultra-low viscosity OCR glue for full-fit module.
对比例七Comparative Example 7
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体SR395重量30份、丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂TPO重量1份、2-羟基-2-甲基-1-苯基丙酮重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 30 parts by weight of acrylic monomer SR395, 15 parts by weight of butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator TPO, 1 part by weight of 2-hydroxy-2-methyl-1-phenylpropanone, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, add them into the container in sequence, use a high-speed disperser, stir thoroughly at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed solution for 15 minutes, and prepare a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
对比例八Comparative Example 8
在避光、湿度小于50％的条件下，准确称量丙烯酸树脂CN9004重量10份、CN152重量5份、丙烯酸单体丙烯酸丁酯BA重量15份、丙烯酸羟丁酯HBA重量15份、月桂酸丙烯酸酯LA重量10份，光引发剂184重量1份、TPO重量1份，抗氧剂1010重量0.1份，助剂BYK4510重量0.1份、A187重量0.2份依次加入容器内，使用高速分散机，在500RPM速度下充分搅拌30分钟，将得到的均一混合液真空脱泡15分钟，制得可喷涂、超低粘的用于全贴合模组的OCR胶水。Under the conditions of avoiding light and keeping humidity less than 50%, accurately weigh 10 parts by weight of acrylic resin CN9004, 5 parts by weight of CN152, 15 parts by weight of acrylic monomer butyl acrylate BA, 15 parts by weight of hydroxybutyl acrylate HBA, 10 parts by weight of lauric acid acrylate LA, 1 part by weight of photoinitiator 184, 1 part by weight of TPO, 0.1 part by weight of antioxidant 1010, 0.1 part by weight of auxiliary agent BYK4510 and 0.2 part by weight of A187, and add them into the container in sequence. Use a high-speed disperser to fully stir at 500RPM for 30 minutes, vacuum degas the obtained uniform mixed liquid for 15 minutes to obtain a sprayable, ultra-low viscosity OCR glue for full-lamination modules.
上述OCR胶水制备方法制作如下表2配方的胶水组合物，并测试。The above OCR glue preparation method is used to prepare a glue composition as shown in Table 2 below, and then tested.
表2不同实施例原料表Table 2 Raw materials of different embodiments
Figure PCTCN2022134939-appb-000004
Figure PCTCN2022134939-appb-000004
Figure PCTCN2022134939-appb-000005
Figure PCTCN2022134939-appb-000005
测试方法：Test Methods:
对实施例1-3及对比例1-8分别在UV-LED 365波长下进行紫外照射，累计能量不小于5000mj；Examples 1-3 and Comparative Examples 1-8 were respectively subjected to ultraviolet irradiation at a wavelength of UV-LED 365, with a cumulative energy of not less than 5000 mj;
OCR胶水粘度测试：OCR glue viscosity test:
测试方法：多功能连续感应粘度计法；测试仪器：DV2T LV；校准：硅油标准液；测试转子：61-64或SC4-18；扭矩范围：40-60％；测量温度：25℃。Test method: multifunctional continuous induction viscometer method; test instrument: DV2T LV; calibration: silicone oil standard liquid; test rotor: 61-64 or SC4-18; torque range: 40-60%; measurement temperature: 25℃.
储能模量和Tg的测试：Storage modulus and Tg test:
测试仪器：Anton Paar MCR302；试片尺寸：直径8mm、厚度1mm的圆柱体；温度范围：-50-100℃；升温速率：3℃/min；变形模式：剪切模式；测试频率：1Hz。Test instrument: Anton Paar MCR302; Specimen size: cylinder with 8mm diameter and 1mm thickness; Temperature range: -50-100℃; Heating rate: 3℃/min; Deformation mode: shear mode; Test frequency: 1Hz.
剥离强度测试方法：GB/T 2790Peel strength test method: GB/T 2790
断裂伸长率测试方法：GB/T 528Elongation at break test method: GB/T 528
透过率、雾度、YI：GB/T 2410Transmittance, haze, YI: GB/T 2410
测试结果如表3所示：The test results are shown in Table 3:
表3不同实施例测试结果表Table 3 Test results of different embodiments
Figure PCTCN2022134939-appb-000006
Figure PCTCN2022134939-appb-000006
Figure PCTCN2022134939-appb-000007
Figure PCTCN2022134939-appb-000007
数据分析：data analysis:
本发明中各组分合理搭配的实施例1-3的各项性能均较优异。对比例1中丙烯酸树脂的含量过低，产品的剥离强度较差，可能是由于促进粘附特征基团含量减少，形成氢键密度降低导致；对比例2中丙烯酸树脂的含量相对偏高，综合性能较好，但产品的粘度明显增加，不利于Inkjet喷涂；对比例3中只使用了单一的光引发剂184，产品的剥离强度较低，是由于缺少引发剂的协同效应导致。对比例4中只使用了单一的光引发剂TPO，产品的模量明显降低，是由于单一引发剂的效率不够导致。对比例5中使用了光引发剂184和1173组合，产品的剥离强度较低，是由于该组合效应单一导致。对比例6中使用了光引发剂TPO和1173组合，产品的模量明显降低，是由于该组合的固化效应不足导致。对比例7中使用了光引发剂651和1173组合，产品的光学YI明显增大，是由于该组合中的651易黄变导致。对比例8中没有使用软单体SR395，产品的粘度、断裂伸长率、Tg、模量均较大幅度变差，是次组合固化后的产品链段中缺少足够的软段、软弹性不佳导致。The various properties of Examples 1-3 in which the components are reasonably matched in the present invention are excellent. In Comparative Example 1, the content of acrylic resin is too low, and the peel strength of the product is poor, which may be due to the reduction of the content of the characteristic group that promotes adhesion and the reduction of the density of hydrogen bonds; in Comparative Example 2, the content of acrylic resin is relatively high, and the comprehensive performance is good, but the viscosity of the product is significantly increased, which is not conducive to Inkjet spraying; in Comparative Example 3, only a single photoinitiator 184 is used, and the peel strength of the product is low, which is due to the lack of the synergistic effect of the initiator. In Comparative Example 4, only a single photoinitiator TPO is used, and the modulus of the product is significantly reduced, which is due to the insufficient efficiency of the single initiator. In Comparative Example 5, a combination of photoinitiators 184 and 1173 is used, and the peel strength of the product is low, which is due to the single effect of the combination. In Comparative Example 6, a combination of photoinitiators TPO and 1173 is used, and the modulus of the product is significantly reduced, which is due to the insufficient curing effect of the combination. In Comparative Example 7, a combination of photoinitiators 651 and 1173 is used, and the optical YI of the product is significantly increased, which is due to the yellowing of 651 in the combination. In Comparative Example 8, the soft monomer SR395 was not used, and the viscosity, elongation at break, Tg, and modulus of the product deteriorated significantly. This was due to the lack of sufficient soft segments in the product chain segments after the combination was cured and the poor soft elasticity.
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和这里示出的实施例。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, and 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 the specific details and the embodiments shown here.

Claims (10)

  1. 一种超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，由如下重量配比的原料组成：An ultra-low viscosity, sprayable OCR glue for full lamination modules, characterized in that it is composed of the following raw materials in weight ratio:
    Figure PCTCN2022134939-appb-100001
    Figure PCTCN2022134939-appb-100001
    其中，所述助剂为消泡剂、润湿分散剂、附着力促进剂或硅烷偶联剂；Wherein, the auxiliary agent is a defoamer, a wetting and dispersing agent, an adhesion promoter or a silane coupling agent;
    所述丙烯酸树脂为聚氨酯丙烯酸酯、环氧丙烯酸酯、聚酯丙烯酸酯及聚烯烃丙烯酸酯中的至少一种。The acrylic resin is at least one of polyurethane acrylate, epoxy acrylate, polyester acrylate and polyolefin acrylate.
  2. 如权利要求1所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，The ultra-low viscosity, sprayable OCR glue for full lamination modules as claimed in claim 1, characterized in that:
    丙烯酸树脂    15-25份。Acrylic resin    15-25 parts.
  3. 如权利要求1所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，所述光引发剂为2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮、安息香双甲醚、2，4，6-三甲基苯甲酰基-二苯基氧化膦、2，4，6-三甲基苯甲酰基苯基膦酸乙酯中的至少一种。The ultra-low viscosity, sprayable OCR glue for full-fit modules according to claim 1, characterized in that the photoinitiator is at least one of 2-hydroxy-2-methyl-1-phenylpropanone, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, benzoin dimethyl ether, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, and 2,4,6-trimethylbenzoylphenylphosphonic acid ethyl ester.
  4. 如权利要求3所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，光引发剂为1-羟基环己基苯基甲酮(184)、光引发剂2，4，6-三甲基苯甲酰基-二苯基氧化膦(TPO)的组合。The ultra-low viscosity, sprayable OCR glue for full-lamination modules as described in claim 3 is characterized in that the photoinitiator is a combination of 1-hydroxycyclohexyl phenyl ketone (184) and photoinitiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO).
  5. 如权利要求1所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，所述丙烯酸单体为丙烯酸异冰片酯、四氢呋喃丙烯酸酯、丙烯酸基硅烷酯、月桂酸丙烯酸酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、丙烯酸丁酯、4-(1-氧代-2-丙烯基)吗啡啉、硬脂酸丙烯酸酯、丙烯酸 异辛酯、丙烯酸异癸酯中的至少一种。The ultra-low viscosity, sprayable OCR glue for full-fit modules according to claim 1, characterized in that the acrylic monomer is at least one of isobornyl acrylate, tetrahydrofuran acrylate, silyl acrylate, lauric acid acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, butyl acrylate, 4-(1-oxo-2-propenyl)morpholine, stearic acid acrylate, isooctyl acrylate, and isodecyl acrylate.
  6. 如权利要求5所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，所述丙烯酸单体为丙烯酸异癸酯或包含丙烯酸异癸酯的混合物。The ultra-low viscosity, sprayable OCR glue for full-lamination modules according to claim 5, characterized in that the acrylic monomer is isodecyl acrylate or a mixture containing isodecyl acrylate.
  7. 如权利要求1所述的超低粘、可喷涂的用于全贴合模组的OCR胶水，其特征在于，所述抗氧剂为受阻酚类抗氧剂。The ultra-low viscosity, sprayable OCR glue for full-fit modules according to claim 1, wherein the antioxidant is a hindered phenol antioxidant.
  8. 一种如权利要求1所述的超低粘、可喷涂的用于全贴合模组的OCR胶水的制备方法，其特征在于，包括以下步骤：A method for preparing the ultra-low viscosity, sprayable OCR glue for full lamination modules as claimed in claim 1, characterized in that it comprises the following steps:
    S1：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合以形成混合液；S1: Weigh acrylic resin, acrylic monomer, photoinitiator, antioxidant and additive according to weight to form a mixed solution;
    S2：将所述混合液真空脱泡15分钟，以形成最终成品。S2: vacuum degassing the mixed solution for 15 minutes to form a final product.
  9. 如权利要求8所述的超低粘、可喷涂的用于全贴合模组的OCR胶水的制备方法，其特征在于，步骤S1中：混合在避光、湿度小于50％的条件下进行。The method for preparing the ultra-low viscosity, sprayable OCR glue for the fully-fitted module according to claim 8 is characterized in that in step S1: mixing is carried out under conditions of light avoidance and humidity less than 50%.
  10. 如权利要求8所述的超低粘、可喷涂的用于全贴合模组的OCR胶水的制备方法，其特征在于，步骤S1中：按重量份称取丙烯酸树脂、丙烯酸单体、光引发剂、抗氧剂、助剂混合，使用高速分散机，在500RPM速度下充分搅拌30分钟，以得到的均一混合液。The method for preparing an ultra-low viscosity, sprayable OCR glue for a fully-fitted module according to claim 8, characterized in that in step S1: acrylic resin, acrylic monomer, photoinitiator, antioxidant, and additive are weighed in parts by weight, and mixed, and a high-speed disperser is used to fully stir at a speed of 500RPM for 30 minutes to obtain a uniform mixed solution.
PCT/CN2022/134939 2022-11-16 2022-11-29 Ultra-low-viscosity sprayable ocr glue for full-lamination module, and preparation method therefor WO2024103441A1 (en)

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