High-adhesion optical adhesive, OCA (Optical Clear Adhesive) optical cement as well as preparation method and application of high-adhesion optical adhesive and OCA optical cement

Abstract

The invention relates to a high-adhesion optical adhesive, an OCA (Optical Clear Adhesive) and a preparation method and application of the high-adhesion optical adhesive. The optical adhesive is prepared from the following components in parts by mass: 20 to 40 parts of vinyl silicone resin, 15 to 30 parts of vinyl silicone oil, 15 to 60 parts of a hydrogen-containing cross-linking agent, 1 to 3 parts of a boron-containing organic silicon tackifier, 0.1 to 3 parts of a nitrogen-containing polymer, 0.01 to 0.5 part of a catalyst and 0.2 to 1 part of an inhibitor. And by adding the boron-containing organic silicon tackifier, B-O-Si weak bond links are formed between B atoms and adjacent molecules of various substrates, so that the problem of insufficient bonding force can be effectively improved. The introduction of the boron element can destroy the regularity of the chain segment, thereby lowering the glass transition temperature (Tg) of the polymer and improving the low temperature resistance of the optical cement. By further adding a nitrogen-containing polymer, an N: B dynamic coordination bond is formed between N and B, so that the problem of hydrolysis resistance degradation caused by adding a boron-containing organic silicon tackifier is solved.

Description

Technical Field

[0001] The present invention relates to the technical field of adhesives, and in particular to a high-adhesion optical adhesive, an OCA optical adhesive, and a preparation method and application thereof. Background Art

[0002] Optical Clear Adhesive (OCA) refers to a non-substrate material with a release film attached to the upper and lower layers of the adhesive layer. It is a solid double-sided adhesive tape and a type of pressure-sensitive adhesive. OCA optical adhesive is widely used in the field of optical display, such as for bonding display modules, glass cover plates, touch screens and other display units. It has the characteristics of high light transmittance and good bonding strength.

[0003] At present, OCA optical adhesives can be divided into acrylate OCA, silicone OCA, polyurethane OCA, epoxy resin OCA, etc. according to the type of materials used. Compared with the other types of OCA, silicone OCA has better weather resistance, yellowing resistance, aging resistance, easy repair and other advantages. However, silicone OCA currently generally has poor initial adhesion, and the peel strength is much lower than other resins. The initial adhesion is too low, and it cannot be transferred immediately after the bonding is completed, resulting in low production efficiency, and the bonding components are prone to fall off and cause losses during the transfer of the display.

[0004] At present, adding tackifiers to silicone materials is a common method to solve the problem of adhesion between materials and substrates. However, in the actual production process, conventional tackifiers have poor compatibility with silicone materials and have little effect on the adhesion of substrates. Under certain temperature and humidity, the adhesion force decreases significantly, which will cause serious separation between silicone resin materials and substrates.

[0005] CN104774333A discloses a thickener for addition-type silicone rubber prepared by catalytic reaction of vinyl hydroxy silicone oil, glycidyl ether alkoxy silane and titanate. However, titanate, especially titanate complex, is generally yellow or even dark brown. The prepared thickener is colored, which may have an adverse effect on the preparation of colorless or light-colored addition-type organic silicone adhesives.

[0006] CN109824899A discloses an addition type silica gel thickener formed by catalytic reaction of epoxydialkoxysilane, boric acid, vinyldialkoxysilane and alkaline anion exchange resin, but the ion exchange resin may break during the reaction, and there is a risk of incomplete filtration when the catalyst is removed by subsequent decompression filtration. The prior art has the defects of poor compatibility between the thickener and the organosilicon material, insignificant thickening effect, and poor hydrolysis resistance. Therefore, how to provide a thickener with good compatibility, excellent thickening effect, and good hydrolysis resistance has become a problem that needs to be solved urgently. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides a highly adhesive, hydrolysis-resistant optical adhesive, OCA optical adhesive and its preparation method and application, aiming to improve the bonding performance of the tackifier while maintaining good hydrolysis resistance. The present invention effectively improves the problem of insufficient adhesion by adding a boron-containing organosilicon tackifier to the organosilicon OCA; the introduction of boron element in the organosilicon tackifier can also reduce the glass transition temperature (Tg) of the polymer and improve the low temperature resistance of the optical adhesive. Further addition of nitrogen-containing polymers solves the problem of hydrolysis resistance degradation caused by the addition of boron-containing organosilicon tackifiers. Moreover, the synthesis process involving the boron-containing organosilicon tackifier is catalyst-free, which to a certain extent avoids the adverse effects of the residue of the previous catalyst on the color, curing and other aspects of the adhesive during use. Moreover, the present invention introduces epoxy groups into the boron-containing silicone tackifier, which is suitable for different substrates. The prepared optical adhesive OCA has good initial bonding properties to glass, ink, polarizer, polyethylene terephthalate (PET) substrate, polycarbonate (PC), and polymethyl methacrylate (PMMA).

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides an optical adhesive, wherein the optical adhesive comprises the following components in parts by weight:

[0010] Vinyl silicone resin 20-40 parts

[0011] Vinyl silicone oil 15-30 parts

[0012] 15-60 parts of hydrogen-containing crosslinking agent

[0013] 1-3 parts of boron-containing silicone tackifier

[0014] 0.1-3 parts of nitrogen-containing polymer

[0015] Catalyst 0.01-0.5 parts

[0016] Inhibitor 0.2-1 part.

[0017] The present invention adds a boron-containing organosilicon tackifier to the optical adhesive. Since the B atom has an electron vacancy, it can serve as an acceptor of unpaired electrons on the polysiloxane chain segment or the surface of the substrate, forming a BO-Si weak bond link with adjacent molecules, which can effectively improve the problem of insufficient adhesion. The introduction of boron elements in the organosilicon tackifier can also destroy the regularity of the chain segment, thereby reducing the glass transition temperature (Tg) of the polymer and improving the low temperature resistance of the optical adhesive.

[0018] BO-Si is highly sensitive to water and is easily broken by hydrolysis, resulting in decreased adhesion and increased haze. The present invention further adds a nitrogen-containing polymer to form an N:B dynamic coordination bond between N and B, thereby solving the problem of hydrolysis resistance degradation caused by the addition of a boron-containing silicone thickener.

[0019] The present invention adds a boron-containing organosilicon tackifier and a nitrogen-containing polymer to the optical adhesive, and cooperates with other components to achieve good hydrolysis resistance while increasing the viscosity.

[0020] The mass fraction of the vinyl silicone resin is 20-40 parts, for example, it can be 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, 32 parts, 34 parts, 36 parts, 38 parts, and specific values ​​between the above points.

[0021] The mass fraction of the vinyl silicone oil is 15-30 parts, for example, 18 parts, 21 parts, 24 parts, 27 parts, and specific values ​​between the above values.

[0022] The mass fraction of the hydrogen-containing crosslinking agent is 15-60 parts, for example, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, and specific values ​​between the above values.

[0023] The mass fraction of the boron-containing organosilicon tackifier is 1-3 parts, for example, it can be 1.3 parts, 1.6 parts, 1.9 parts, 2.2 parts, 2.5 parts, 2.8 parts, and specific values ​​between the above values.

[0024] The mass fraction of the nitrogen-containing polymer is 0.1-3 parts, for example, 0.5 parts, 1 parts, 1.5 parts, 2 parts, 2.5 parts, and specific values ​​between the above values.

[0025] The mass fraction of the catalyst is 0.01-0.5 parts, for example, it can be 0.05 parts, 0.1 parts, 0.15 parts, 0.2 parts, 0.25 parts, 0.3 parts, 0.35 parts, 0.4 parts, 0.45 parts, and specific values ​​between the above points.

[0026] The mass fraction of the inhibitor is 0.2-1 part, for example, it can be 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, and specific values ​​between the above points.

[0027] Preferably, the vinyl silicone resin includes any one of vinyl MQ silicone resin, vinyl MDT silicone resin, vinyl MTQ silicone resin or vinyl DT silicone resin, or a combination of at least two thereof.

[0028] Preferably, the viscosity of the vinyl silicone resin at 25° C. is 5000-50000 mPa·s, for example, it may be 10000 mPa·s, 15000 mPa·s, 20000 mPa·s, 25000 mPa·s, 30000 mPa·s, 35000 mPa·s, 40000 mPa·s, 45000 mPa·s, and specific values ​​between the above points.

[0029] Preferably, the vinyl mass content of the vinyl silicone resin is 0.3-1.0 mmol / g, for example, it may be 0.4 mmol / g, 0.5 mmol / g, 0.6 mmol / g, 0.7 mmol / g, 0.8 mmol / g, 0.9 mmol / g, and specific values ​​between the above values.

[0030] Preferably, the vinyl silicone oil includes any one of silicone oil containing vinyl groups at the terminal, silicone oil containing vinyl groups at the side groups, and silicone oil containing vinyl groups at both the terminal and the side groups, or a combination of at least two of them.

[0031] Preferably, the viscosity of the vinyl silicone oil at 25° C. is 100-20000 mPa·s, for example, 3000 mPa·s, 6000 mPa·s, 9000 mPa·s, 12000 mPa·s, 15000 mPa·s, 18000 mPa·s, and specific values ​​between the above values.

[0032] Preferably, the vinyl content of the vinyl silicone oil is 0.1-0.75 mmol / g, for example, it may be 0.2 mmol / g, 0.3 mmol / g, 0.4 mmol / g, 0.5 mmol / g, 0.6 mmol / g, 0.7 mmol / g, and specific values ​​between the above values.

[0033] Preferably, the hydrogen-containing cross-linking agent includes at least one of hydrogen-containing silicone resin or hydrogen-containing silicone oil.

[0034] Preferably, the hydrogen-containing cross-linking agent includes hydrogen-containing silicone resin and hydrogen-containing silicone oil.

[0035] Preferably, the mass ratio of the hydrogen-containing silicone resin to the hydrogen-containing silicone oil is 1:0.8-1.2, for example, it can be 1:0.85, 1:0.90, 1:0.95, 1:1.00, 1:1.05, 1:1.10, 1:1.15, and specific values ​​between the above points.

[0036] Preferably, the structural formula of the hydrogen-containing silicone resin is (R 1 R 2 R 3 3SiO 1 / 2 ) x (R4 R 5 SiO 2 / 2 ) y (R 6 SiO 3 / 2 ) z , where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 are independently selected from hydrogen atoms or C1-C5 alkyl groups, such as C2, C3, C4, etc., and R 1 , R 2 , R 3 , R 4 , R 5 and R 6 At least one is a hydrogen atom; x, y, z are the molar ratios of each unit chain, x:y:z=1:(0.2-0.3):(2-3), (0.2-0.3) can be, for example, 0.21, 0.22, 0.23, 0.24, 0.25, 0.26, 0.27, 0.28, 0.29 and specific values ​​between the above point values, (2-3) can be, for example, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9 and specific values ​​between the above point values.

[0037] Preferably, the viscosity of the hydrogenated silicone resin at 25° C. is 10000-40000 mPa·s, for example, 15000 mPa·s, 20000 mPa·s, 25000 mPa·s, 30000 mPa·s, 35000 mPa·s, and specific values ​​between the above values.

[0038] Preferably, the silicon hydrogen content of the hydrogen-containing silicone resin is 0.1-1.2 mmol / g, for example, 0.3 mmol / g, 0.5 mmol / g, 0.7 mmol / g, 0.9 mmol / g, 1.1 mmol / g, and specific values ​​between the above values.

[0039] Preferably, the structural formula of the hydrogen-containing silicone oil is (R 7 R 8 R 9 3SiO 1 / 2 )p(R 10 R 11 SiO 2 / 2 )m(R 12 R 13 SiO 2 / 2 )n, where R 7 , R 8 , R 9, R 10 , R 11 , R 12 , R 13 are independently selected from hydrogen atoms or C1-C5 alkyl groups, such as C2, C3, C4, etc., and R 10 , R 11 , R 12 , R 13 at least one of them is a hydrogen atom; 1≤p≤2, for example, p is 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, and specific values ​​between the above points; 0≤m≤50, for example, m is 5, 10, 15, 20, 25, 30, 35, 40, 45, and specific values ​​between the above points; 0≤n≤50, for example, n is 5, 10, 15, 20, 25, 30, 35, 40, 45, and specific values ​​between the above points.

[0040] Preferably, the viscosity of the hydrogen-containing silicone oil at 25° C. is 100-3000 mPa·s, for example, 500 mPa·s, 1000 mPa·s, 1500 mPa·s, 2000 mPa·s, 2500 mPa·s, and specific values ​​between the above values.

[0041] Preferably, the silicon hydrogen content of the hydrogen-containing silicone oil is 0.05-0.5 mmol / g, for example, it can be 0.1 mmol / g, 0.15 mmol / g, 0.2 mmol / g, 0.25 mmol / g, 0.3 mmol / g, 0.35 mmol / g, 0.4 mmol / g, 0.45 mmol / g, and specific values ​​between the above points.

[0042] Preferably, the boron-containing organosilicon tackifier is prepared from hydroxy silicone oil, epoxysiloxane monomer and a boron-containing compound.

[0043] The boron-containing organosilicon tackifier of the present invention is prepared without a catalyst, thereby avoiding adverse effects on the color, curing and other aspects of the adhesive during use caused by the residue of the previous catalyst.

[0044] Although traditional polyborosiloxane can improve the adhesion between optical adhesives and substrates, it is not suitable for all substrates and has a poor adhesion effect on PET substrates. The present invention uses hydroxy silicone oil, epoxysilicone monomer and boron-containing compound to polymerize to form a boron-containing silicone thickener, introduces epoxy groups into the boron-containing thickener, broadens the application range of the boron-containing silicone thickener, and is suitable for different substrates. The prepared optical adhesive OCA has good initial adhesion properties to glass, ink, polarizer, polyethylene terephthalate (PET), polycarbonate (PC), and polymethyl methacrylate (PMMA).

[0045] Preferably, the viscosity of the hydroxy silicone oil at 25° C. is 40-2000 mPa·s, for example, it may be 200 mPa·s, 400 mPa·s, 600 mPa·s, 800 mPa·s, 1000 mPa·s, 1200 mPa·s, 1400 mPa·s, 1600 mPa·s, 1800 mPa·s, and specific values ​​between the above points.

[0046] Preferably, the hydroxyl mass content of the hydroxyl silicone oil is 0.9-4.5%, for example, it may be 1.5%, 2.1%, 2.7%, 3.3%, 3.9%, and specific values ​​between the above values.

[0047] Preferably, the epoxysiloxane monomer includes γ-glycidyloxypropyltrimethoxysilane and / or 3-glycidyloxypropylmethyldiethoxysilane.

[0048] Preferably, the boron-containing compound includes any one of boric acid, phenylboric acid or tetrahydroxyboron, or a combination of at least two thereof.

[0049] Preferably, the molar ratio of N to B in the optical adhesive is 0.2-0.6:1, for example, it can be 0.25:1, 0.3:1, 0.35:1, 0.4:1, 0.45:1, 0.5:1, 0.55:1, and specific values ​​between the above points.

[0050] The molar ratio of N to B in the optical adhesive is controlled within the range of 0.2-0.6:1. The OCA optical adhesive obtained by coating and die-cutting has good bonding effect on substrates such as ink, glass, polarizer, PET, PC, PMMA, etc., and has excellent hydrolysis resistance. When the molar ratio of N to B is higher than 0.6:1, the viscosity increasing effect is poor; when it is lower than 0.2:1, the hydrolysis resistance is poor.

[0051] Preferably, the preparation method of the boron-containing organosilicon thickener comprises the following steps: reacting hydroxy silicone oil, epoxysilicone monomer and boron-containing compound at 90-100°C, for example, 91°C, 92°C, 93°C, 94°C, 95°C, 96°C, 97°C, 98°C, 99°C, and specific values ​​between the above points; reacting for 5-6h, for example, 5.1h, 5.2h, 5.3h, 5.4h, 5.5h, 5.6h, 5.7h, 5.8h, 5.9h, and specific values ​​between the above points; obtaining the boron-containing organosilicon thickener.

[0052] Preferably, the added amount of the epoxysilicone monomer accounts for 5-20wt% of the total mass of the hydroxy silicone oil, epoxysilicone monomer and the boron-containing compound, for example, it can be 7wt%, 9wt%, 11wt%, 13wt%, 15wt%, 17wt%, 19wt%, and specific point values ​​between the above point values.

[0053] The amount of epoxysiloxane monomer added to the boron-containing organosilicon tackifier is controlled within the range of 5-20wt%, added to the optical adhesive, coated and die-cut to obtain the OCA optical adhesive, which has good bonding effect on substrates such as ink, glass, polarizer, PET, PC, PMMA, etc., and has excellent hydrolysis resistance. Too little addition of epoxysiloxane monomer will reduce the bonding effect of the adhesive on the substrate; too much addition of epoxysiloxane monomer will cause the refractive index of the boron-containing organosilicon tackifier to be much higher than that of conventional polysiloxane, thereby reducing the compatibility between the components.

[0054] Preferably, the reaction is carried out in an organic solvent, and the organic solvent is selected from any one or a combination of at least two of N,N-dimethylformamide, dimethyl sulfoxide, methanol, acetonitrile, isopropanol, 1,4-dioxane or cyclohexanone.

[0055] Preferably, the amount of the organic solvent is 10%-50% of the total mass of the feed in the reaction system, for example, it can be 15%, 20%, 25%, 30%, 35%, 40%, 45%, and specific values ​​between the above points.

[0056] Preferably, after the reaction is completed, the step of removing the solvent by distillation under reduced pressure is further included.

[0057] Preferably, the structure of the nitrogen-containing polymer is as follows:

[0058]

[0059] Wherein, R1', R2', R3', R4', R5' are independently selected from C1~C5 alkyl groups, for example, C2, C3, C4 alkyl groups; m1 is an integer of 1-5, for example, m1 is 2, 3, 4; m2 is an integer of 0-5, for example, m2 is 1, 2, 3, 4; n is an integer of 60~350, for example, n is 100, 150, 200, 230, 300, and specific point values ​​between the above point values.

[0060] Preferably, the nitrogen-containing polymer is obtained by addition reaction of divinyl silicone oil and amine compounds. In the present invention, the vinyl group in the nitrogen-containing polymer can participate in the curing of the optical adhesive and connect to the cross-linked network, thereby preventing the nitrogen-containing polymer from volatilizing due to thermal breakage of the N:B dynamic coordination bond, maintaining long-term hydrolysis resistance, and meeting the use requirements of different environments.

[0061] Preferably, in the raw material for preparing the nitrogen-containing polymer, the molar ratio of the amino group of the amine compound to the vinyl group of the divinyl silicone oil is 1:2 to 2.2; for example, it can be 1:2.03, 1:2.06, 1:2.09, 1:2.12, 1:2.15, 1:2.18, and specific values ​​between the above points.

[0062] Preferably, the viscosity of the double-ended vinyl silicone oil is 200-1000 mPa·s, for example, it may be 300 mPa·s, 400 mPa·s, 500 mPa·s, 600 mPa·s, 700 mPa·s, 800 mPa·s, 900 mPa·s, and specific values ​​between the above points.

[0063] Preferably, the amine compound is a secondary amine compound.

[0064] Preferably, the amine compound includes at least one of diethylamine or dipropylamine.

[0065] Preferably, the temperature of the addition reaction is 40-50°C, for example, it can be 41°C, 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C, 49°C, and specific values ​​between the above points; the reaction time is 3-6h, for example, it can be 3.5h, 4h, 4.5h, 5h, 5.5h, and specific values ​​between the above points.

[0066] Preferably, the method for preparing the nitrogen-containing polymer comprises the following steps:

[0067] S1, adding double-terminal vinyl silicone oil into the reactor, and heating to 40-50°C, for example, 41°C, 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C, 49°C, and specific values ​​between the above points;

[0068] S2, dropwise adding a mixture of an amine compound and a solvent, and keeping the mixture warm for reaction for 3 to 6 hours, for example, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, and specific hours between the above-mentioned hours, to obtain the nitrogen-containing polymer.

[0069] Preferably, the solvent includes any one of methanol, ethanol, dichloromethane, tetrahydrofuran or 1,4-dioxane, or a combination of at least two thereof.

[0070] Preferably, the catalyst comprises any one of chloroplatinic acid, Karstedt platinum catalyst or Willing platinum catalyst, or a combination of at least two thereof.

[0071] Preferably, the inhibitor comprises any one of acetylenic alcohol and a small molecule polymer inhibitor containing polyvinyl groups, or a combination of at least two of them.

[0072] Preferably, the inhibitor includes any one of 1,4-butynediol, ethynylcyclohexanol, tetramethyltetravinylcyclotetrasiloxane or 2-methyl-3-butyn-2-ol, or a combination of at least two thereof.

[0073] Preferably, the molar ratio of vinyl to silicon-hydrogen bonds in the optical adhesive is 0.95-1.05:1, for example, it can be 0.96:1, 0.97:1, 0.98:1, 0.99:1, 1:1, 1.01:1, 1.02:1, 1.03:1, 1.04:1, and specific values ​​between the above points.

[0074] In a second aspect, the present invention provides an OCA optical adhesive, which includes a light release film, an optical adhesive layer, and a heavy release film, wherein the optical adhesive layer is located between the light release film and the heavy release film, and the optical adhesive layer is obtained by curing the optical adhesive described in the first aspect.

[0075] In a third aspect, the present invention provides a use of the optical adhesive as described in the first aspect or the OCA optical adhesive as described in the second aspect in display bonding.

[0076] Compared with the prior art, the present invention has at least the following beneficial effects:

[0077] The present invention prepares boron-containing organosilicon polymer macromolecules (i.e., boron-containing organosilicon tackifiers) by using epoxysilicone monomers, hydroxy silicone oils, and boron-containing compounds. By adding the boron-containing organosilicon tackifiers to the optical adhesive, the B atoms can be used as acceptors of unpaired electrons on the polysiloxane segments or on the substrate surface due to the electron vacancies on the B atoms, forming BO-Si with adjacent molecules, thereby forming weak bond links, which can effectively improve the problem of insufficient adhesion. The boron-containing organosilicon tackifier of the present invention is added to the basic organosilicon resin composition to prepare organosilicon OCA, which can give the cured organosilicon OCA good initial bonding properties with various substrates.

[0078] The introduction of boron element in boron-containing silicone thickener can also destroy the regularity of the chain segments, thereby reducing the glass transition temperature (Tg) of the polymer and improving the low-temperature resistance of the optical adhesive.

[0079] BO-Si is highly sensitive to water and is easily broken by hydrolysis, resulting in decreased adhesion and increased haze. The present invention prepares a nitrogen-containing polymer by reacting an amine compound with vinyl silicone oil. With the addition of the nitrogen-containing polymer, N and B form an N:B dynamic coordination bond, thereby enhancing the hydrolysis resistance of the silicone tackifier and the silicone OCA. In addition, the nitrogen-containing silicone polymer is connected in the main cross-linked network during the curing process and will not migrate or volatilize. DETAILED DESCRIPTION

[0080] For the convenience of understanding the present invention, the present invention lists the following embodiments. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0081] The sources of the raw materials used in the embodiments of the present invention are as follows:

[0082] (A) Vinyl silicone oil

[0083]

[0084] (B) Vinyl silicone resin

[0085] Code supplier model Viscosity (mPa·s) Vinyl content (mmol / g) B-1 Delta Silicone DT-10050 10000 0.4444

[0086] (C) Hydrogenated silicone oil

[0087] Code Manufacturer Brand Silicon-hydrogen bond content (mmol / g) C-1 Anhui Iyota Silicone Oil Co., Ltd. IOTA203 0.18

[0088] (D) Hydrogenated silicone resin

[0089] The general structural formula is: (HMe2SiO 1 / 2 ) x (HMeSiO 2 / 2 ) y (MeSiO 3 / 2 ) z , wherein Me is methyl.

[0090] Code supplier x:y:z Silicon-hydrogen bond content (mmol / g) Viscosity (mPa·s) D-1 Hangzhou Silicon-based Materials 1：0.25：3 0.8 38000

[0091] (E) Catalyst

[0092] Code supplier model E-1 Anhui Iyota Silicone Oil Co., Ltd. IOTAPC16

[0093] (F) Inhibitors

[0094] Code supplier model F-1 Guangzhou Xiyi Chemical CEY

[0095] Coating equipment

[0096] Code Manufacturer model Coating Machine Shangwang Printing Machinery Co., Ltd. THVG-1100 Electric roller machine Beidou Instrument PT-509

[0097] Preparation Example 1

[0098] Preparation of boron-containing organosilicon tackifier G-1:

[0099] A dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device was placed in an oil bath, and 100 g of hydroxy silicone oil (viscosity 100 mPa.s, hydroxyl mass content 2.4%), 1.3 g of boric acid, 5.5 g of 3-glycidyloxypropylmethyldiethoxysilane, and 50 g of 1,4-dioxane were added to the round-bottom flask. After the materials were stirred evenly by mechanical stirring at room temperature, the oil bath was heated to 90°C, the reaction time was 6 hours, and the solvent was subsequently distilled off under reduced pressure. The solvent was distilled off under reduced pressure to obtain 102 g of a colorless and transparent liquid product, which was recorded as boron-containing organosilicon tackifier G-1 (the amount of epoxysiloxane monomer added accounted for 5.1% of the total mass of hydroxysilicone oil, epoxysiloxane monomer and boron-containing compound, and the B content was 0.02061 mol / 100 g).

[0100] Preparation Example 2

[0101] Preparation of boron-containing organosilicon tackifier G-2:

[0102] A dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device was placed in an oil bath, and 100 g of hydroxy silicone oil (viscosity 100 mPa.s, hydroxyl mass content 2.4%), 1.3 g of boric acid, 15 g of 3-glycidyloxypropylmethyldiethoxysilane, and 50 g of 1,4-dioxane were added to the round-bottom flask. After the materials were stirred evenly by mechanical stirring at room temperature, the oil bath was heated to 90°C, the reaction time was 6 hours, and the solvent was subsequently distilled off under reduced pressure. The solvent was distilled off under reduced pressure to obtain 108 g of a colorless and transparent liquid product, which was recorded as boron-containing organosilicon tackifier G-2 (the amount of epoxysiloxane monomer added accounted for 12.9% of the total mass of hydroxysilicone oil, epoxysiloxane monomer and boron-containing compound, and the B content was 0.01947 mol / 100 g).

[0103] Preparation Example 3

[0104] Preparation of boron-containing organosilicon tackifier G-3:

[0105] A dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device was placed in an oil bath, and 100 g of hydroxy silicone oil (viscosity 100 mPa.s, hydroxyl mass content 2.4%), 1.3 g of boric acid, 25 g of 3-glycidyloxypropylmethyldiethoxysilane, and 50 g of 1,4-dioxane were added to the round-bottom flask. After the materials were stirred evenly by mechanical stirring at room temperature, the oil bath was heated to 90°C, the reaction time was 6 hours, and the solvent was subsequently distilled off under reduced pressure. The solvent was distilled off under reduced pressure to obtain 114 g of a colorless and transparent liquid product, which was recorded as boron-containing organosilicon tackifier G-3 (the amount of epoxysiloxane monomer added accounted for 19.8% of the total mass of hydroxysilicone oil, epoxysiloxane monomer and boron-containing compound, and the B content was 0.01844 mol / 100 g).

[0106] Preparation Example 4

[0107] Preparation of boron-containing organosilicon tackifier G-4:

[0108] A dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device was placed in an oil bath, and 100 g of hydroxy silicone oil (viscosity 100 mPa.s, hydroxyl mass content 2.4%), 1.3 g of boric acid, 4 g of 3-glycidyloxypropylmethyldiethoxysilane, and 50 g of 1,4-dioxane were added to the round-bottom flask. After the materials were stirred evenly by mechanical stirring at room temperature, the oil bath was heated to 90°C, the reaction time was 6 hours, and the solvent was subsequently distilled off under reduced pressure. The solvent was distilled off under reduced pressure to obtain 102 g of a colorless and transparent liquid product, which was recorded as boron-containing organosilicon tackifier G-4 (the amount of epoxysiloxane monomer added accounted for 3.8% of the total mass of hydroxysilicone oil, epoxysiloxane monomer and boron-containing compound, and the B content was 0.02061 mol / 100 g).

[0109] Preparation Example 5

[0110] Preparation of boron-containing silicone tackifier G-5:

[0111] Place a dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device in an oil bath, add 100g of hydroxy silicone oil (viscosity 100mPa.s, hydroxyl mass content 2.4%), 1.3g of boric acid, 27g of 3-glycidyloxypropylmethyldiethoxysilane, and 50g of 1,4-dioxane into the round-bottom flask, stir the materials evenly by mechanical stirring at room temperature, heat the oil bath to 90°C, react for 6h, and then remove the solvent by vacuum distillation. Vacuum distillation to remove the solvent to obtain 114g of a colorless, transparent liquid product, recorded as boron-containing organosilicon tackifier G-5 (the amount of epoxysiloxane monomer added accounts for 21.0% of the total mass of hydroxy silicone oil, epoxysiloxane monomer, and boron-containing compound, and the B content is 0.01844mol / 100g)

[0112] Preparation Example 6

[0113] Preparation of nitrogen-containing polymers:

[0114] A dry round-bottom flask equipped with a mechanical stirrer, a thermometer, and a vacuum device is placed in an oil bath, 200 g of double-ended vinyl silicone oil (viscosity 250 mPa.s, vinyl mass content 0.70%) is placed in the round-bottom flask, the temperature is adjusted to 40°C, a mixed solution of 1.76 g of diethylamine dissolved in 50 g of methanol is added dropwise within 30 min, and the reaction is subsequently carried out for 4 h to obtain a nitrogen-containing polymer (N content is 0.012 mol / 100 g, vinyl content is 0.01389 mol / 100 g).

[0115] Example 1

[0116] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0117] Vinyl silicone oil A-1 20 parts

[0118] Vinyl silicone resin B-1 35 parts

[0119] Hydrogenated silicone oil C-1 21 parts

[0120] Hydrogenated silicone resin D-1 19.7 parts

[0121] Boron-containing silicone tackifier G-1 2 parts

[0122] 1.7 parts of nitrogen-containing polymer

[0123] Catalyst E-1 0.1 part

[0124] Inhibitor F-1 0.5 parts.

[0125] The preparation method of the optical adhesive is as follows:

[0126] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.57:1.

[0127] Example 2

[0128] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0129] Vinyl silicone oil A-1 20 parts

[0130] Vinyl silicone resin B-1 36 parts

[0131] Hydrogenated silicone oil C-1 19.3 parts

[0132] Hydrogen-containing silicone resin D-1 20.5 parts

[0133] Boron-containing silicone tackifier G-2 2 parts

[0134] 1.6 parts of nitrogen-containing polymer

[0135] Catalyst E-1 0.1 part

[0136] Inhibitor F-1 0.5 parts.

[0137] The preparation method of the optical adhesive is as follows:

[0138] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.57:1.

[0139] Example 3

[0140] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0141] Vinyl silicone oil A-1 20 parts

[0142] Vinyl silicone resin B-1 36 parts

[0143] Hydrogenated silicone oil C-1 19.4 parts

[0144] Hydrogen-containing silicone resin D-1 20.5 parts

[0145] Boron-containing silicone tackifier G-3 2 parts

[0146] 1.5 parts of nitrogen-containing polymer

[0147] Catalyst E-1 0.1 part

[0148] Inhibitor F-1 0.5 parts.

[0149] The preparation method of the optical adhesive is as follows:

[0150] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.56:1.

[0151] Example 4

[0152] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0153] Vinyl silicone oil A-1 20 parts

[0154] Vinyl silicone resin B-1 36.4 parts

[0155] Hydrogenated silicone oil C-1 19.3 parts

[0156] Hydrogen-containing silicone resin D-1 20.5 parts

[0157] Boron-containing silicone tackifier G-2 2 parts

[0158] 1.2 parts of nitrogen-containing polymer

[0159] Catalyst E-1 0.1 part

[0160] Inhibitor F-1 0.5 parts.

[0161] The preparation method of the optical adhesive is as follows:

[0162] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.43:1.

[0163] Example 5

[0164] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0165] Vinyl silicone oil A-1 20 parts

[0166] Vinyl silicone resin B-1 35.5 parts

[0167] Hydrogenated silicone oil C-1 20.8 parts

[0168] Hydrogen-containing silicone resin D-1 20.5 parts

[0169] Boron-containing silicone tackifier G-2 2 parts

[0170] 0.6 parts of nitrogen-containing polymer

[0171] Catalyst E-1 0.1 part

[0172] Inhibitor F-1 0.5 parts.

[0173] The preparation method of the optical adhesive is as follows:

[0174] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.21:1.

[0175] Example 6

[0176] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0177] Vinyl silicone oil A-1 20 parts

[0178] Vinyl silicone resin B-1 35 parts

[0179] Hydrogenated silicone oil C-1 21 parts

[0180] Hydrogenated silicone resin D-1 19.7 parts

[0181] 2 parts of boron-containing silicone tackifier G-4

[0182] 1.7 parts of nitrogen-containing polymer

[0183] Catalyst E-1 0.1 part

[0184] Inhibitor F-1 0.5 parts.

[0185] The preparation method of the optical adhesive is as follows:

[0186] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.57:1.

[0187] Example 7

[0188] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0189] Vinyl silicone oil A-1 20 parts

[0190] Vinyl silicone resin B-1 36 parts

[0191] Hydrogenated silicone oil C-1 19.4 parts

[0192] Hydrogen-containing silicone resin D-1 20.5 parts

[0193] Boron-containing silicone tackifier G-5 2 parts

[0194] 1.5 parts of nitrogen-containing polymer

[0195] Catalyst E-1 0.1 part

[0196] Inhibitor F-1 0.5 parts.

[0197] The preparation method of the optical adhesive is as follows:

[0198] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.56:1.

[0199] Example 8

[0200] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0201] Vinyl silicone oil A-1 20 parts

[0202] Vinyl silicone resin B-1 35.5 parts

[0203] Hydrogenated silicone oil C-1 20.9 parts

[0204] Hydrogen-containing silicone resin D-1 20.5 parts

[0205] Boron-containing silicone tackifier G-2 2 parts

[0206] 0.5 parts of nitrogen-containing polymer

[0207] Catalyst E-1 0.1 part

[0208] Inhibitor F-1 0.5 parts.

[0209] The preparation method of the optical adhesive is as follows:

[0210] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.18:1.

[0211] Example 9

[0212] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0213] Vinyl silicone oil A-1 20 parts

[0214] Vinyl silicone resin B-1 36 parts

[0215] Hydrogenated silicone oil C-1 19.3 parts

[0216] Hydrogenated silicone resin D-1 20.3 parts

[0217] Boron-containing silicone tackifier G-2 2 parts

[0218] 1.8 parts of nitrogen-containing polymer

[0219] Catalyst E-1 0.1 part

[0220] Inhibitor F-1 0.5 parts.

[0221] The preparation method of the optical adhesive is as follows:

[0222] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.64:1.

[0223] Comparative Example 1

[0224] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0225] Vinyl silicone oil A-1 20 parts

[0226] Vinyl silicone resin B-1 35.6 parts

[0227] Hydrogenated silicone oil C-1 21.3 parts

[0228] Hydrogenated silicone resin D-1 20.484 parts

[0229] Boron-containing silicone tackifier G-2 2 parts

[0230] Nitrogen-containing organic matter: 0.016 parts of diethylamine

[0231] Catalyst E-1 0.1 part

[0232] Inhibitor F-1 0.5 parts.

[0233] The preparation method of the optical adhesive is as follows:

[0234] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, nitrogen-containing polymer, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive, wherein the molar ratio of N to B in the optical adhesive is 0.56:1.

[0235] Comparative Example 2

[0236] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0237] Vinyl silicone oil A-1 20.5 parts

[0238] Vinyl resin B-1 36.5 parts

[0239] Hydrogenated silicone oil C-1 22 parts

[0240] Hydrogen-containing silicone resin D-1 20.16 parts

[0241] KH-560 0.24 parts

[0242] Catalyst E-1 0.1 part

[0243] Inhibitor F-1 0.5 parts.

[0244] The preparation method of the optical adhesive is as follows:

[0245] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, KH-560, a catalyst and an inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive.

[0246] Comparative Example 3

[0247] This embodiment provides an optical adhesive, which includes the following components in parts by weight:

[0248] Vinyl silicone oil A-1 21 parts

[0249] Vinyl silicone resin B-1 36.6 parts

[0250] Hydrogenated silicone oil C-1 19.3 parts

[0251] Hydrogen-containing silicone resin D-1 20.5 parts

[0252] Boron-containing silicone tackifier G-2 2 parts

[0253] Catalyst E-1 0.1 part

[0254] Inhibitor F-1 0.5 parts.

[0255] The preparation method of the optical adhesive is as follows:

[0256] Vinyl silicone oil, vinyl silicone resin, hydrogen-containing silicone resin, hydrogen-containing silicone oil, boron-containing organosilicon tackifier, catalyst and inhibitor are mixed, stirred evenly, and vacuum degassed to obtain an optical adhesive.

[0257] Application Example 1-9, Comparative Application Example 1-3

[0258] The optical adhesives prepared in Examples 1-9 and Comparative Examples 1-3 are respectively used to prepare organic silicone OCA optical adhesives, and the preparation method is as follows:

[0259] The organic silicone adhesive is coated on a first release film (non-silicone release film, thickness 75 μm, release force 30 gf / 25 mm), coated at a thickness of 250 μm by a selected scraping coating method, thermally cured (curing conditions are 60° C., 10 min), and then a second release film (fluorine release film, thickness 50 μm, release force 12 gf / 25 mm) is attached to the side of the organic silicone adhesive away from the first release film to obtain the organic silicone OCA.

[0260] Test Method

[0261] (I) Silicone adhesive OCA bonding strength test

[0262] 1. Peel force test

[0263] One layer of the organic silicon OCA optical adhesive obtained in Application Examples 1-9 or Comparative Application Examples 1-3 is coated on different substrates (ink, glass, polarizer, PET, PC, PMMA), and the other layer is coated on the original PET film to form a combined structure of PET-organic silicon OCA-substrate, which is placed on an electric roller machine and rolled once with a 3kg roller at a speed of 10mm / s to obtain a peeling sample of the corresponding substrate. The 180° peeling force is tested according to GB / T2792-2014.

[0264] 2. Light transmittance and haze test: Test in accordance with GB / T 2410 7.1.

[0265] The test results are shown in Table 1.

[0266] Table 1

[0267]

[0268] The test results show that:

[0269] (1) It can be seen from Application Examples 1-5 that the present invention can effectively improve the problem of insufficient adhesion by adding a boron-containing organosilicon tackifier to the optical adhesive. The OCA optical adhesive prepared in Application Examples 1-5 has improved adhesion to ink, glass, polarizer, PET, PC, PMMA and other substrates to varying degrees, and the initial peeling force is greater than 4.0N / 25mm. In addition, the introduction of boron can also reduce the glass transition temperature (Tg) of the polymer and improve the low-temperature resistance of the optical adhesive. The glass transition temperature of the organosilicon OCA prepared in Application Examples 1-5 is below -42°C, and the low-temperature resistance is excellent, which can meet the use requirements of different scenarios. By further adding a nitrogen-containing polymer, the problem of hydrolysis resistance degradation caused by the addition of a boron-containing organosilicon tackifier is solved. The organosilicon OCA prepared in Application Examples 1-5 has a haze of less than 0.3 after aging at 65°C / 95%RH, and has excellent high temperature and humidity resistance.

[0270] (2) It can be seen from Application Examples 2, 6 and 7 that the present invention controls the addition amount of epoxysiloxane monomer in the boron-containing organosilicon tackifier to be within the range of 5-20wt%, adds it to the optical adhesive, and obtains the OCA optical adhesive through coating and die-cutting. The adhesive has good bonding effect on substrates such as ink, glass, polarizer, PET, PC, PMMA, etc., and has excellent hydrolysis resistance. Too little addition of epoxysiloxane monomer will reduce the bonding effect of the adhesive on PET / PC / PMMA substrates; too much addition of epoxysiloxane monomer will cause the refractive index of the boron-containing organosilicon tackifier to be much higher than that of conventional polysiloxane, thereby reducing the compatibility between the components and causing the optical adhesive to fog.

[0271] Application Example 6: The addition amount of epoxysiloxane monomer in the boron-containing silicone tackifier is 3.8%. The 180° peeling force of the adhesive on various substrates at room temperature is reduced, and the impact on PET, PC, and PMMA is particularly obvious.

[0272] In Application Example 7, the addition amount of epoxysilicone monomer in the boron-containing silicone tackifier is 21.0%, the light transmittance of the adhesive is significantly reduced, the compatibility of the boron-containing silicone tackifier with other components of the optical adhesive is reduced, and the haze is significantly increased.

[0273] (3) It can be seen from Application Examples 2 and 5 and Application Examples 8 and 9, and from the comparison of Application Example 3 that the present invention controls the molar ratio of N to B within the range of 0.2-0.6:1, adds it to the optical adhesive, and obtains the OCA optical adhesive through coating and die-cutting, which has good bonding effect on substrates such as ink, glass, polarizer, PET, PC, PMMA, etc., and has excellent hydrolysis resistance. However, when the molar ratio of N to B is not within the range of 0.2-0.6:1, it cannot simultaneously achieve the technical effects of high bonding and excellent hydrolysis resistance. The molar ratio of N to B of the boron-containing silicone tackifier used in Application Example 8 is 0.17:1, and the effect of improving the bonding performance of various substrates is particularly prominent, but the haze after aging at 65°C / 95%RH is significantly higher than that of Application Examples 1-5, which is 2-3 times that of Application Examples 1-5.

[0274] The boron-containing silicone thickener used in Application Example 9 has a molar ratio of N:B of 0.64:1. After aging at 65°C / 95%RH, the haze change is small, and it has excellent high temperature and humidity resistance. However, after more B:N coordination, the possibility of B:O coordination is reduced, resulting in a significant reduction in the bonding effect of OCA to substrates such as glass, ink, and polarizers.

[0275] In the boron-containing silicone thickener used in comparative application example 3, no nitrogen-containing polymer was used to compound with the boron-containing silicone thickener. Since BO is sensitive to water vapor, after aging at 65°C / 95%RH for 1000h, BO hydrolyzed and caused the optical adhesive to fog, and the haze increased significantly.

[0276] (4) It can be seen from Application Example 2 and Comparative Application Example 1 that the present invention solves the problem of hydrolysis resistance degradation caused by adding boron-containing organic silicone tackifiers by adding nitrogen-containing polymers to the optical adhesive. When the comparative application example 1 uses ordinary nitrogen-containing organic diethylamine as a functional auxiliary agent, the initial peeling force on the substrate is not much different from that of application example 2. However, due to the dissociation and volatilization of most of the diethylamine during the aging process at 65°C / 95%RH, the final haze is much higher than that of application example 2.

[0277] (5) It can be seen from Application Example 2 and Comparative Application Example 2 that the present invention can effectively improve the problem of insufficient adhesion by adding a boron-containing organosilicon tackifier to the optical adhesive, and can also reduce the glass transition temperature (Tg) of the polymer, thereby improving the low-temperature resistance of the optical adhesive. When Comparative Application Example 2 uses the silane coupling agent KH-560, which is a commonly used adhesion promoter for organosilicon OCA, the 180° peeling force on various substrates at room temperature is significantly reduced, the glass transition temperature is -40°C, and the low-temperature resistance is also deteriorated.

[0278] In summary, the present invention can effectively improve the problem of insufficient adhesion by adding a boron-containing organosilicon tackifier to the optical adhesive, and can also reduce the glass transition temperature (Tg) of the polymer to improve the low temperature resistance of the optical adhesive. By further adding a nitrogen-containing polymer, the problem of hydrolysis resistance degradation caused by the addition of a boron-containing organosilicon tackifier is solved.

[0279] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. An optical adhesive, characterized in that: The optical adhesive comprises the following components in parts by weight:

2. The optical adhesive according to claim 1, characterized in that: The vinyl silicone resin includes any one of vinyl MQ silicone resin, vinyl MDT silicone resin, vinyl MTQ silicone resin or vinyl DT silicone resin, or a combination of at least two thereof; Preferably, the viscosity of the vinyl silicone resin at 25° C. is 5000-50000 mPa·s; Preferably, the vinyl silicone resin has a vinyl content of 0.3-1.0 mmol / g.

3. The optical adhesive according to claim 1 or 2, characterized in that: The vinyl silicone oil includes any one or a combination of at least two of silicone oil containing vinyl at the terminal, silicone oil containing vinyl at the side group, and silicone oil containing vinyl at both the terminal and the side group; Preferably, the viscosity of the vinyl silicone oil at 25° C. is 100-20000 mPa·s; Preferably, the vinyl content of the vinyl silicone oil is 0.1-0.75 mmol / g.

4. The optical adhesive according to any one of claims 1 to 3, characterized in that: The hydrogen-containing cross-linking agent includes at least one of hydrogen-containing silicone resin or hydrogen-containing silicone oil; Preferably, the hydrogen-containing cross-linking agent comprises hydrogen-containing silicone resin and hydrogen-containing silicone oil, and the mass ratio of the hydrogen-containing silicone resin to the hydrogen-containing silicone oil is 1:0.8-1.

2.

5. The optical adhesive according to claim 4, characterized in that: The structural formula of the hydrogen-containing silicone resin is (R 1 R 2 R 3 3SiO 1 / 2 ) x (R 4 R 5 SiO 2 / 2 ) y (R 6 SiO 3 / 2 ) z , where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 are independently selected from hydrogen or C1-C5 alkyl groups, and R 1 , R 2 , R 3 , R 4 , R 5 and R 6 At least one of them is a hydrogen atom; x, y, z are the molar ratios of each unit chain, x:y:z=1:0.2-0.3:2-3; Preferably, the viscosity of the hydrogenated silicone resin at 25° C. is 10000-40000 mPa·s; Preferably, the silicon hydrogen content of the hydrogen-containing silicone resin is 0.1-1.2 mmol / g; Preferably, the structural formula of the hydrogen-containing silicone oil is (R 7 R 8 R 9 3SiO 1 / 2 )p(R 10 R 11 SiO 2 / 2 )m(R 12 R 13 SiO 2 / 2 )n, where R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , R 13 are independently selected from hydrogen or C1-C5 alkyl groups, and R 10 , R 11 , R 12 , R 13 At least one is a hydrogen atom; 1≤p≤2, 0≤m≤50, 0≤n≤50; Preferably, the viscosity of the hydrogen-containing silicone oil at 25° C. is 100-3000 mPa·s; Preferably, the hydrogen-containing silicone oil has a silyl content of 0.05-0.5 mmol / g.

6. The optical adhesive according to any one of claims 1 to 5, characterized in that: The boron-containing organosilicon tackifier is prepared from hydroxy silicone oil, epoxysiloxane monomer and boron-containing compound; Preferably, the viscosity of the hydroxy silicone oil at 25° C. is 40-2000 mPa·s; Preferably, the hydroxyl mass content of the hydroxyl silicone oil is 0.9-4.5%; Preferably, the epoxysiloxane monomer comprises γ-glycidyloxypropyltrimethoxysilane and / or 3-glycidyloxypropylmethyldiethoxysilane; Preferably, the boron-containing compound comprises any one of boric acid, phenylboric acid or tetrahydroxyboron or a combination of at least two thereof; Preferably, the molar ratio of N to B in the optical adhesive is 0.2-0.6:1; Preferably, the method for preparing the boron-containing organosilicon tackifier comprises the following steps: reacting hydroxy silicone oil, epoxysiloxane monomer and boron-containing compound at 90-100° C. for 5-6 hours to obtain the boron-containing organosilicon tackifier; Preferably, the epoxysilicone monomer is added in an amount of 5-20wt% of the total mass of the hydroxy silicone oil, epoxysilicone monomer and boron-containing compound; Preferably, the reaction is carried out in an organic solvent, and the organic solvent is selected from any one or a combination of at least two of N,N-dimethylformamide, dimethyl sulfoxide, methanol, acetonitrile, isopropanol, 1,4-dioxane or cyclohexanone; Preferably, the amount of the organic solvent used is 10%-50% of the total mass of the feed in the reaction system; Preferably, after the reaction is completed, the step of removing the solvent by distillation under reduced pressure is further included.

7. The optical adhesive according to any one of claims 1 to 6, characterized in that: The structure of the nitrogen-containing polymer is as follows: wherein R1', R2', R3', R4', R5', and R6' are independently selected from C1 to C5 alkyl groups, m1 is an integer of 1 to 5, m2 is an integer of 0 to 5, and n is an integer of 60 to 350; Preferably, the nitrogen-containing polymer is obtained by addition reaction of divinyl silicone oil and an amine compound; Preferably, in the raw material for preparing the nitrogen-containing polymer, the molar ratio of the amino group of the amine compound to the vinyl group of the divinyl silicone oil is 1:2 to 2.2; Preferably, the viscosity of the double-terminated vinyl silicone oil at 25° C. is 200-1000 mPa·s; Preferably, the amine compound is a secondary amine compound; Preferably, the amine compound includes at least one of diethylamine or dipropylamine; Preferably, the temperature of the addition reaction is 40-50°C, and the reaction time is 3-6h; Preferably, the method for preparing the nitrogen-containing polymer comprises the following steps: S1, add double-terminal vinyl silicone oil into the reactor and heat it to 40-50°C; S2, dropwise adding a mixture of an amine compound and a solvent, and keeping the mixture warm for 3 to 6 hours to obtain the nitrogen-containing polymer; Preferably, the solvent includes any one of methanol, ethanol, dichloromethane, tetrahydrofuran or 1,4-dioxane, or a combination of at least two thereof.

8. The optical adhesive according to any one of claims 1 to 7, characterized in that: The catalyst comprises any one or a combination of at least two of chloroplatinic acid, Karstedt platinum catalyst or Willing platinum catalyst; Preferably, the inhibitor comprises any one of acetylenic alcohol and small molecule polymer inhibitor containing polyvinyl groups, or a combination of at least two thereof; Preferably, the inhibitor comprises any one or a combination of at least two of 1,4-butynediol, ethynylcyclohexanol, tetramethyltetravinylcyclotetrasiloxane or 2-methyl-3-butyn-2-ol; Preferably, the molar ratio of vinyl groups to silicon-hydrogen bonds in the optical adhesive is 0.95-1.05:

1.

9. An OCA optical adhesive, comprising a light release film, an optical adhesive layer, and a heavy release film, wherein the optical adhesive layer is located between the light release film and the heavy release film, and the optical adhesive layer is obtained by curing the optical adhesive according to any one of claims 1 to 8.

10. Use of the optical adhesive according to any one of claims 1 to 8 or the OCA optical adhesive according to claim 9 in display bonding.

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