CN111334219A - Release film for electronic optical adhesive and preparation method thereof - Google Patents
Release film for electronic optical adhesive and preparation method thereof Download PDFInfo
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- CN111334219A CN111334219A CN202010341521.9A CN202010341521A CN111334219A CN 111334219 A CN111334219 A CN 111334219A CN 202010341521 A CN202010341521 A CN 202010341521A CN 111334219 A CN111334219 A CN 111334219A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a release film for electronic optical adhesive, which comprises the following raw materials in parts by weight: 9-15 parts of silicone oil, 62-80 parts of solvent, 1-3 parts of catalyst, 1.5-3 parts of cross-linking agent, 2-7 parts of epoxy vinyl resin, 3-6 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 3-6 parts of nano zinc oxide, 2.5-5 parts of alumyte powder and 2.5-5 parts of nano tungsten carbide-cobalt. The release film for the electronic optical adhesive keeps the release force stable under the conditions of ultraviolet irradiation and high-temperature baking, and avoids the release film from falling off due to UV light irradiation or high-temperature heating, so that the quality of the electronic optical adhesive is ensured. The invention also provides a preparation method of the release film for the electronic optical adhesive.
Description
Technical Field
The invention relates to the technical field of release films, in particular to a release film for electronic optical adhesive and a preparation method thereof.
Background
The electronic optical adhesive (OCA) is a clean high-transparency substrate-free double-sided adhesive tape, has excellent transparency, has light transmittance of over 90 percent, and also has the advantages of high adhesion, high temperature resistance, ultraviolet resistance and the like. The adhesive is mainly used for adhering a touch screen substrate (a capacitive screen and a resistive screen) and a front panel, and has a wide market in the fields of smart phones, handwriting computers, touch screen multimedia machines and the like.
The electronic optical adhesive is formed by compounding a release film layer, an OCA adhesive layer and a release film layer. The release film layers are respectively attached to the upper surface and the lower surface of the OCA glue layer. The release film layer is obtained by coating a release liquid on the surface of the substrate and curing. In the preparation of the electronic optical adhesive, the OCA adhesive is coated on a release film and then is cured by UV or heat to form an OCA adhesive layer. When adopting high temperature thermocuring to prepare electron optical cement, traditional from type membrane from the type layer again through secondary high temperature (more than 150 ℃) toast the thermosetting back (carry out high temperature curing from type layer itself for the first time), often can local embrittlement from the type layer, not only can cause from type membrane from type power rising, do not have from the type effect, still can lead to coming off from the type layer of type membrane, the adhesion causes electron optical cement luminousness to descend on OCA glue film surface, be unfavorable for OCA to glue the combined use who laminates touch-sensitive screen base plate or TFT base plate, the luminousness of high-transparent display screen or touch-sensitive screen is influenced, the display screen can be fuzzy relatively, it is unclear. When UV is adopted to form the electronic optical adhesive, ultraviolet rays with a wave band of 365nm are mainly adopted, the release layer of the traditional release film is irradiated by a UV lamp with a wave band of 365nm, because the ultraviolet rays belong to high-energy short waves, the release layer of the release film can be accelerated to age under the irradiation of the ultraviolet rays, the ultraviolet rays damage-Si-O-or-C-O-covalent bonds of the release layer, and the release film can be cracked and speckled. When the release film is used, the silicon-oxygen bond of the release layer is damaged by ultraviolet rays through irradiation of UV light, so that aging and deterioration occur, the release force rises, and the release layer does not have a release effect.
Therefore, it is necessary to develop a release film for an electronic optical adhesive, which can maintain the release force thereof stable under the conditions of ultraviolet irradiation and high-temperature baking, so as to ensure the quality of the electronic optical adhesive.
Disclosure of Invention
The invention aims to provide a release film for an electronic optical adhesive, which keeps the release force stable under the conditions of ultraviolet irradiation and high-temperature baking, and avoids the release film from falling off under high-temperature heating so as to ensure the quality of the electronic optical adhesive.
The second purpose of the invention is to provide a preparation method of the release film for the electronic optical adhesive.
In order to achieve the purpose, the invention provides a release film for an electronic optical adhesive, which comprises the following preparation raw materials in parts by weight: 9-15 parts of silicone oil, 62-80 parts of solvent, 1-3 parts of catalyst, 1.5-3 parts of cross-linking agent, 2-7 parts of epoxy vinyl resin, 3-6 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 3-6 parts of nano zinc oxide, 2.5-5 parts of alumyte powder and 2.5-5 parts of nano tungsten carbide-cobalt.
Compared with the prior art, the release film for the electronic optical adhesive provided by the invention comprises raw materials of silicone oil, a solvent, a catalyst, a cross-linking agent, epoxy vinyl resin, bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, nano zinc oxide, alumyte powder and nano tungsten carbide-cobalt. Introducing a catalyst to carry out catalytic reaction quickly; the curing of the bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester and the silicone oil can effectively prevent a silicon-oxygen bond of a release layer from being damaged when the release film is irradiated by UV light with a wave band of 365nm in the using process, and the nano zinc oxide can shield ultraviolet light waves so that a silicone oil layer of the release film maintains effective and stable chemical properties; the bauxite powder and the silicone oil are combined and cured, so that the heat resistance of the release film for the electronic optical adhesive is improved, the release layer is prevented from being aged and falling off due to high-temperature baking, and the reduction of the light transmittance and the increase of the haze of the electronic optical adhesive are prevented; the nano tungsten carbide-cobalt improves the high-temperature resistance effect of the release film, and reduces the release layer from aging and falling off due to high-temperature baking; the epoxy vinyl resin can prevent alumina powder from falling off, and can especially improve the compounding performance of silicone oil and nanometer tungsten carbide-cobalt. Therefore, the release film for the electronic optical adhesive keeps the release force stable under the conditions of ultraviolet irradiation and high-temperature baking, and avoids the release film from falling off under the conditions of UV irradiation or high-temperature heating, so as to ensure the quality of the electronic optical adhesive.
Preferably, the silicone oil is at least one selected from the group consisting of methyldichlorosilane, allyltrimethylsilane, and trimethylethynylsilane.
Preferably, the solvent is at least one selected from ethanol, isopropyl ether, cyclohexanone and n-heptane. Preferably, the solvent is a mixture of ethanol, isopropyl ether, cyclohexanone and n-heptane, the dosage of the n-heptane is larger than that of the rest solvents, and the dosage ratio of the ethanol, the isopropyl ether, the cyclohexanone and the n-heptane is 2:1:5: 6.
Preferably, the catalyst is at least one selected from a platinum-carbon catalyst, a platinum-palladium-carbon bimetallic catalyst or [1, 3-bis (2,4, 6-trimethylphenyl) -2-imidazolidinylidene ] (2-isopropoxy-5-nitrobenzylidene) ruthenium dichloride.
Further, the average particle diameter (mum) of the platinum-carbon catalyst is 30-60 μm, and the platinum content is 0.5% -5%. The average grain diameter (mum) of the platinum-palladium carbon bimetallic catalyst is 35-60μm, and the platinum content is 2% -10%.
Preferably, the particle size of the nano tungsten carbide-cobalt is 80-200nm, and the tungsten content is 40-60%.
Preferably, the nano zinc oxide has a particle size of 30-50nm and a purity of 97-99 wt%.
Preferably, the particle size of the bauxite powder is 200-300 meshes.
The invention also provides a preparation method of the release film for the electronic optical adhesive, which comprises the following steps:
(1) adding silicone oil and a solvent into a container, and uniformly stirring at the stirring speed of 500-800 r/min;
(2) adding a cross-linking agent into a container, controlling the stirring speed to rise to 1000-;
(3) adding epoxy vinyl resin into the container and uniformly stirring to obtain a mixture A, wherein the stirring speed is increased to 1200-1500 r/min;
(4) filtering the mixture A by using a filter screen to obtain release liquid;
(5) and coating the release solution on the surface of the substrate, and baking and curing to obtain the release film for the electronic optical adhesive.
Preferably, a filter screen with 800 meshes and 1000 meshes is adopted in the step (4), so that the platinum-carbon catalyst, [1, 3-bis (2,4, 6-trimethylphenyl) -2-imidazolidinylidene ] (2-isopropoxy-5-nitrobenzylidene) ruthenium dichloride or platinum-palladium-carbon bimetallic catalyst particles selected from the mixture A can be effectively filtered out, and scratches or granular black spots caused by the particles are avoided.
Preferably, the substrate is selected from at least one of PE, PET, OPP or PBAT.
Preferably, the baking and curing are performed by using 5 sections of ovens, the temperature of the first section of oven is 60-70 ℃, the temperature of the second section of oven is 100-. Can let more abundant from type liquid solidification, avoid leading to the solvent lock to be in from type the layer inside because of violent solidification, produce the bubble, influence the performance.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but the present invention is not limited thereto.
Example 1
In this embodiment, the release film for the electronic optical adhesive comprises the following raw materials in parts by weight: 15 parts of methyl dichlorosilane, 10 parts of ethanol, 5 parts of isopropyl ether, 25 parts of cyclohexanone, 30 parts of n-heptane, 3 parts of platinum-carbon catalyst, 3 parts of silane coupling agent (manufacturer: Nanjing warp knitting chemical KH-560), 7 parts of epoxy vinyl resin, 6 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 4 parts of nano zinc oxide, 3 parts of aluminum bauxite powder and 4 parts of nano tungsten carbide-cobalt.
The method for preparing the release film by adopting the raw materials with the components and the contents comprises the following steps:
(1) adding methyl dichlorosilane, ethanol, isopropyl ether, cyclohexanone and n-heptane into a container, and uniformly stirring at the stirring speed of 800r/min for 5 min;
(2) then adding a silane coupling agent into a container, controlling the stirring speed to rise to 1200r/min, adding a platinum-carbon catalyst, nano zinc oxide, alumine powder, nano tungsten carbide-cobalt and bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester after 2min, and uniformly stirring for 3 min;
(3) then adding epoxy vinyl resin into the container and uniformly stirring to obtain a mixture A, wherein the stirring speed is increased to 1500r/min for 20 min;
(4) filtering the mixture A by using a 900-mesh filter screen, and taking out platinum-carbon catalyst particles to obtain a release solution;
(5) coating a release solution on the surface of a PE (polyethylene) substrate by a mirror-surface comma scraper, baking and curing by a suspension oven, and performing by using a 5-section oven, wherein the temperature of the first section oven is 70 ℃, the temperature of the second section oven is 110 ℃, the temperature of the third section oven is 130 ℃, the temperature of the fourth section oven is 110 ℃, the temperature of the fifth section oven is 100 ℃, and the curing time is 1.5min to prepare the rolled release film for the electron-optical adhesive.
Example 2
In this embodiment, the release film for the electronic optical adhesive comprises the following raw materials in parts by weight: 10 parts of allyl trimethylsilane, 18 parts of ethanol, 6 parts of isopropyl ether, 24 parts of cyclohexanone, 24 parts of n-heptane, 2 parts of platinum-palladium-carbon bimetallic catalyst, 2 parts of silane coupling agent (JS-D858 in Henchang chemical industry, manufacturer), 3 parts of epoxy vinyl resin, 4 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 3 parts of nano zinc oxide, 5 parts of aluminum bauxite powder and 5 parts of nano tungsten carbide-cobalt.
The preparation method of the release film for electronic optical adhesive in this embodiment is the same as that in embodiment 1, and therefore, the detailed description thereof is omitted.
Example 3
In this embodiment, the release film for the electronic optical adhesive comprises the following raw materials in parts by weight: 10 parts of allyl trimethylsilane, 5 parts of trimethylethynyl silane, 10 parts of ethanol, 5 parts of isopropyl ether, 24 parts of cyclohexanone, 28 parts of n-heptane, 1 part of platinum-palladium carbon bimetallic catalyst, 1.5 parts of silane coupling agent (manufacturer: Henchang chemical JS-D858), 5 parts of epoxy vinyl resin, 3 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 6 parts of nano zinc oxide, 4 parts of bauxite powder and 3 parts of nano tungsten carbide-cobalt.
The preparation method of the release film for electronic optical adhesive in this embodiment is the same as that in embodiment 1, and therefore, the detailed description thereof is omitted.
Example 4
The preparation method of the release film for the electronic optical adhesive in the embodiment is basically the same as that in the embodiment 1, and the difference is that: in example 4, 20 parts of ethanol, 20 parts of isopropyl ether and 40 parts of cyclohexanone are used as the solvent, while in example 1, 10 parts of ethanol, 5 parts of isopropyl ether, 25 parts of cyclohexanone and 30 parts of n-heptane are used as the solvent.
The preparation method of the release film for electronic optical adhesive in this embodiment is the same as that in embodiment 1, and therefore, the detailed description thereof is omitted.
Example 5
The preparation method of the release film for the electronic optical adhesive in the embodiment is basically the same as that in the embodiment 1, and the difference is that: in example 5, 10 parts of ethanol, 5 parts of isopropyl ether, 30 parts of cyclohexanone and 25 parts of n-heptane are used as the solvent, while in example 1, 10 parts of ethanol, 5 parts of isopropyl ether, 25 parts of cyclohexanone and 30 parts of n-heptane are used as the solvent.
The preparation method of the release film for electronic optical adhesive in this embodiment is the same as that in embodiment 1, and therefore, the detailed description thereof is omitted.
Comparative example 1
The preparation method of the release film for the electronic optical adhesive of the comparative example is basically the same as that of the release film of the example 1, and the difference is that: the raw material containing epoxy vinyl resin was prepared in example 1, while the epoxy vinyl resin was not contained in comparative example 1.
Comparative example 2
The preparation method of the release film for the electronic optical adhesive of the comparative example is basically the same as that of the release film of the example 1, and the difference is that: the starting material was prepared in example 1 containing bis {3- [3- (2H-benzotriazol-2-yl) -4-hydroxy-5-t-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, while comparative example 2 did not contain bis {3- [3- (2H-benzotriazol-2-yl) -4-hydroxy-5-t-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester.
Comparative example 3
The preparation method of the release film for the electronic optical adhesive of the comparative example is basically the same as that of the release film of the example 1, and the difference is that: the raw material prepared in example 1 contained nano tungsten carbide-cobalt, while comparative example 3 did not contain nano tungsten carbide-cobalt.
Comparative example 4
The preparation method of the release film for the electronic optical adhesive of the comparative example is basically the same as that of the release film of the example 1, and the difference is that: the raw material aluminum-containing alumina powder was prepared in example 1, while the aluminum-free alumina powder was prepared in comparative example 4.
The release films for electronic optical adhesives obtained in examples 1 to 5 and comparative examples 1 to 4 were subjected to an aging resistance test and an ultraviolet resistance test. The results of the aging resistance test are shown in Table 1, and the results of the ultraviolet resistance test are shown in Table 2.
The aging resistance detection method comprises the following steps:
(1) taking the release films prepared in the examples 1-5 and the comparative examples 1-4 as test objects, wherein the size of the release films is A4, and testing the release force L0 and the residual adhesion rate W0 of each release film according to GBT 25256-;
(2) then placing the release films in a high-temperature oven for baking, wherein the oven temperature is 170 ℃, and the heating time is 1 h;
(3) and taking out the release films baked by the high-temperature oven, and testing the release force L1 and the residual adhesion rate W1 of the release films respectively.
(4) The rate of change of the release force was calculated as (L1-L0)/(L0) × 100%, and the rate of change of the residual adhesion was calculated as W1-W0.
After high-temperature baking, the release force is higher, the residual adhesion rate is lower, and the release layer of the release film falls off more due to heating.
The ultraviolet resistance test method comprises the following steps:
(1) taking the release films prepared in the examples 1-5 and the comparative examples 1-4 as test objects, wherein the size of the release films is A4, and testing the release force H0 and the residual adhesion rate K0 of each release film according to GBT 25256-;
(2) then placing the release films in a UV curing box for irradiation, wherein the wavelength is 365nm, the light-emitting angle is 60 degrees, and the UV curing irradiation time is 1 h;
(3) and taking out the release films irradiated by the UV curing box, and testing the release force H1 and the residual adhesion rate K1 of the release films respectively.
(4) The release rate was calculated as (H1-H0)/(H0) × 100%, and the residual adhesion rate was calculated as K1-K0.
After UV light irradiation, the higher the release force is, the lower the residual adhesion rate is, which indicates that the release layer of the release film falls off more due to UV light irradiation.
TABLE 1 anti-aging Performance test results
TABLE 2 UV resistance test results
As can be seen from the data in tables 1-2, the release layer of the release film prepared by the raw materials and the method of the present application has less release layer peeling off under high temperature baking and UV light irradiation than that of the release film of comparative examples 1-4, which indicates that the release film of the present application has relatively stable release force. The composite curing of the bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester and the silicone oil can effectively prevent a silicon-oxygen bond of a release layer from being damaged when the release film is irradiated by 365 nm-waveband UV light in the using process, and the nano zinc oxide can shield ultraviolet light waves to maintain the effective and stable chemical performance of a silicone oil layer of the release film; the bauxite powder and the silicone oil are combined and cured, so that the heat resistance of the release film for the electronic optical adhesive is improved, the release layer is prevented from being aged and falling off due to high-temperature baking, and the reduction of the light transmittance and the increase of the haze of the electronic optical adhesive are prevented; the nano tungsten carbide-cobalt improves the high-temperature resistance effect of the release film, and reduces the release layer from aging and falling off due to high-temperature baking; the epoxy vinyl resin can prevent the alumina powder from falling off, and particularly can improve the composite performance of the silicone oil and the nano tungsten carbide-cobalt, so that the silicone oil and the nano tungsten carbide-cobalt are fully mixed, and the high-temperature resistant effect is improved. Therefore, the release film for the electronic optical adhesive keeps the release force stable under the conditions of ultraviolet irradiation and high-temperature baking, and avoids the release film from falling off under the conditions of UV irradiation or high-temperature heating, so as to ensure the quality of the electronic optical adhesive.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the best embodiments, the present invention is not limited to the above disclosed embodiments, but should cover various modifications, equivalent combinations, made according to the essence of the present invention.
Claims (9)
1. The release film for the electronic optical adhesive comprises the following preparation raw materials in parts by weight: 9-15 parts of silicone oil, 62-80 parts of solvent, 1-3 parts of catalyst, 1.5-3 parts of cross-linking agent, and is characterized by also comprising 2-7 parts of epoxy vinyl resin, 3-6 parts of bis {3- [3- (2H-benzotriazole-2-yl) -4-hydroxy-5-tert-butylphenyl ] -propionic acid } -polyethylene glycol 300 ester, 3-6 parts of nano zinc oxide, 2.5-5 parts of bauxite powder and 2.5-5 parts of nano tungsten carbide-cobalt.
2. The release film for an electronic optical adhesive according to claim 1, wherein the silicone oil is at least one selected from the group consisting of methyldichlorosilane, allyltrimethylsilane, and trimethylethynylsilane.
3. The release film for electronic optical adhesive according to claim 1, wherein the solvent is at least one selected from the group consisting of ethanol, isopropyl ether, cyclohexanone, and n-heptane.
4. The release film for an electronic optical adhesive according to claim 1, wherein the solvent is a mixture of ethanol, isopropyl ether, cyclohexanone and n-heptane, the amount of n-heptane used is greater than the amount of the remaining solvents, and the ratio of the amounts of ethanol, isopropyl ether, cyclohexanone and n-heptane used is 2:1:5: 6.
5. The release film for an electronic optical adhesive according to claim 1, wherein the catalyst is at least one selected from a platinum-carbon catalyst, a platinum-palladium-carbon bimetallic catalyst and ruthenium dichloride [1, 3-bis (2,4, 6-trimethylphenyl) -2-imidazolidinylidene ] (2-isopropoxy-5-nitrobenzylidene).
6. The release film for electronic optical cement according to claim 1, wherein the particle size of the nano tungsten carbide-cobalt is 80-200nm, and the tungsten content is 40-60%.
7. The method for preparing the release film for the electronic optical adhesive according to any one of claims 1 to 6, comprising the steps of:
(1) adding silicone oil and a solvent into a container, and uniformly stirring at the stirring speed of 500-800 r/min;
(2) adding a cross-linking agent into a container, controlling the stirring speed to rise to 1000-;
(3) adding epoxy vinyl resin into the container and uniformly stirring to obtain a mixture A, wherein the stirring speed is increased to 1200-1500 r/min;
(4) filtering the mixture A by using a filter screen to obtain release liquid;
(5) and coating the release solution on the surface of the substrate, and baking and curing to obtain the release film for the electronic optical adhesive.
8. The method for preparing a release film for an electronic optical adhesive according to claim 7, wherein the baking and curing are performed by using 5-section ovens, the temperature of the first section oven is 60-70 ℃, the temperature of the second section oven is 100-110 ℃, the temperature of the third section oven is 120-130 ℃, the temperature of the fourth section oven is 100-110 ℃, and the temperature of the fifth section oven is 80-100 ℃.
9. The method for preparing a release film for an electron optical adhesive according to claim 7, wherein the substrate is at least one selected from PE, PET, OPP and PBAT.
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