CN117229726A - High-performance double-layer-structured acrylic OCA optical adhesive and preparation method thereof - Google Patents
High-performance double-layer-structured acrylic OCA optical adhesive and preparation method thereof Download PDFInfo
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- CN117229726A CN117229726A CN202311242522.8A CN202311242522A CN117229726A CN 117229726 A CN117229726 A CN 117229726A CN 202311242522 A CN202311242522 A CN 202311242522A CN 117229726 A CN117229726 A CN 117229726A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 46
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- 238000007872 degassing Methods 0.000 claims description 8
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- 238000001029 thermal curing Methods 0.000 claims description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 7
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- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 6
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
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- DYJRZZRIXYRTMH-UHFFFAOYSA-N 2-methylnonyl prop-2-enoate Chemical compound CCCCCCCC(C)COC(=O)C=C DYJRZZRIXYRTMH-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
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- 238000012935 Averaging Methods 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- NSWXSZROIQNWCH-UHFFFAOYSA-N hexyl 2-methylidenebutanoate Chemical compound CCCCCCOC(=O)C(=C)CC NSWXSZROIQNWCH-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-performance acrylic OCA optical adhesive with a double-layer structure and a preparation method thereof. Compared with the prior art, the invention selects the most appropriate OCA optical adhesive formula for different bonding surfaces according to the characteristics of bonding base materials, and realizes the best bonding effect between two different bonding surfaces; when the OCA optical adhesive with the high-performance double-layer structure is attached to different base materials, the OCA optical adhesive has very good inhibition effect on bubble rebound phenomenon generated by stress or section difference; when the single-layer OCA optical adhesive is adhered to a resin plate and a film or glass, the problem of poor degree of fit of the single-layer OCA optical adhesive between different base materials can be well solved; the OCA optical adhesive with the high-performance double-layer structure can enable the display touch product to be less prone to generating colloid cracking, bubble rebound and other anomalies, and improves the product quality.
Description
Technical Field
The invention relates to the technical field of optical cement, in particular to an acrylic OCA optical cement with a high-performance double-layer structure and a preparation method thereof.
Background
The double-layer acrylic OCA optical adhesive is a material commonly used for bonding optical elements (such as display screens, touch screens, etc.). Currently, the related art about double-layer acrylic OCA optical adhesives mainly includes the following aspects: and (3) material selection: the preparation of the double-layer acrylic OCA optical cement mainly relates to the selection of materials. There are a number of different brands and models of acrylic OCA optical adhesives currently available on the market. The selection of a suitable material may take into account such factors as its optical clarity, bond strength, durability, thermal stability, and compatibility with the material being bonded. The preparation process comprises the following steps: the preparation of bilayer acrylic OCA optical adhesives typically involves coating and lamination processes. First, a first layer of acrylic OCA optical clear adhesive is coated onto a substrate by a coating technique, and then a second layer of acrylic OCA optical clear adhesive is coated on the surface of the first layer of optical clear adhesive. The coating can be roller coating, spray coating, knife coating, etc. After the coating is completed, appropriate heat and pressure treatment is required to ensure the curing and bonding effects of the optical cement. And (3) adhesive property test: it is necessary to test the adhesive properties of the double-layer acrylic OCA optical adhesive. The double-layer acrylic OCA optical adhesive is widely applied to the field of optical display, such as liquid crystal displays, touch screens, OLED displays and the like. They are used to bond transparent optical elements to provide excellent optical properties and mechanical support.
Coating-lamination process: this is the most common preparation process for double-layer acrylic OCA optical adhesives. First, a first layer of acrylic OCA optical adhesive is applied to a substrate, and a roll coating, spray coating, knife coating, or the like may be used. And then, coating a second layer of acrylic OCA optical adhesive on the surface of the first layer of optical adhesive. After coating, the optical cement is cured and bonded by heat and pressure treatment.
Adhesive film method: this preparation process uses an adhesive film as a carrier. First, a layer of acrylic OCA optical adhesive was coated on a substrate, and then an adhesive film was placed on the optical adhesive to form a three-layer structure of adhesive film/optical adhesive/substrate. Next, a second layer of acrylic OCA optical cement was applied over the adhesive film. Finally, the optical cement is solidified and bonded with the substrate by heating and pressure treatment.
Double tape method: this preparation process uses double-sided tape as a carrier. First, a double-sided tape was attached to a substrate, and then a first layer of acrylic OCA optical tape was attached to the tape. Next, a second layer of acrylic OCA optical cement was applied. Finally, the optical cement is solidified and bonded with the substrate by heating and pressure treatment.
The preparation processes have certain flexibility in practical application, and can be adjusted and optimized according to specific requirements and process conditions.
The Chinese patent application CN116463074A discloses a manufacturing method of an OCA optical cement sandwich structure and the OCA optical cement sandwich structure, and the manufacturing method of the OCA optical cement sandwich structure comprises the following steps: the heavy release film layer is tiled on a flat workbench surface; coating OCA optical adhesive on the upper surface of the heavy release film layer to form an OCA optical adhesive layer; curing the OCA optical adhesive layer; cutting the OCA optical adhesive layer to a preset size and shape by using a cutting device, and keeping the original size and shape of the heavy release film layer; attaching a light release film layer to the upper surface of the OCA optical adhesive layer; and the heavy release film layer and the light release film layer are cut to the preset size and shape simultaneously by using the cutting device, so that the size and shape of the heavy release film layer and the light release film layer after being cut are the same, and the size of the OCA optical adhesive layer after being cut is smaller than that of the heavy release film layer and the light release film layer. The OCA optical adhesive structure with the sandwich structure is formed by cutting in the laying process, so that the problem of film tearing and adhesive tape stripping caused when the OCA optical adhesive is applied to automatic attaching equipment is avoided. However, the OCA optical cement sandwich structure prepared by the method has poor light transmittance, high bubble rebound risk, poor water vapor blocking effect and unsatisfactory adhesive force and dynamic folding effect.
Disclosure of Invention
In view of the defects of poor light transmittance, high bubble rebound risk, poor water vapor barrier effect and unsatisfactory adhesive force and dynamic folding effect of the multilayer acrylic OCA optical adhesive in the prior art, the invention aims to provide the acrylic OCA optical adhesive with a high-performance double-layer structure and a preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical scheme:
the preparation method of the high-performance acrylic OCA optical adhesive with the double-layer structure comprises the following steps: the acrylic OCA optical adhesive with the double-layer structure comprises a PET light release film, an acrylic OCA optical adhesive with the double-layer structure and a PET heavy release film from top to bottom in sequence.
The acrylic OCA optical adhesive with the double-layer structure is divided into a lowest OCA optical adhesive layer and an uppermost OCA optical adhesive layer, wherein the lowest OCA optical adhesive layer is formed by coating resin glue on a layer of PET heavy release film through a doctor blade coating method and performing high-temperature thermal curing molding; the uppermost OCA optical adhesive is coated on the lowermost OCA optical adhesive by modified resin glue through a doctor blade coating method, and is obtained through high-temperature heat curing.
The PET light release film and the PET heavy release film are respectively positioned at the outer sides of the acrylic OCA optical cement with the double-layer structure, and the middle of the uppermost OCA optical cement film and the lowermost OCA optical cement film play a role in connection after being cured at high temperature.
The high-temperature curing temperature is 140-160 ℃, and the high-temperature curing time is 1-3 min.
The thickness of the lowest OCA optical adhesive layer is 5-1000 mu m, and the thickness of the uppermost OCA optical adhesive layer is 5-1000 mu m.
The thickness of the PET light release film is 40-60 mu m; the thickness of the PET heavy release film is 80-90 mu m.
The preparation method of the resin glue comprises the following steps of:
mixing 60-80 parts of 2-ethylhexyl acrylate and 20-40 parts of hydroxyethyl acrylate at 100-300 rpm for 20-40 min, adding 1-2 parts of 1-hydroxycyclohexyl phenyl ketone to obtain a prepolymer mixture, stirring the prepolymer mixture at 100-500 rpm at 15-25 ℃, simultaneously bubbling with nitrogen for degassing for 20-40 min, and irradiating with ultraviolet rays under nitrogen atmosphere by using an ultraviolet lamp with the power of 20-40W and the wavelength of 200-400 nm after the degassing is completed to obtain the resin glue.
The preparation method of the modified resin glue comprises the following steps of:
s1, mixing 10-20 parts of 2-acetamidofluorene and 0.05-0.1 part of dibutyl tin dioctadecanoate, stirring at 100-300 rpm under a nitrogen atmosphere at 40-60 ℃ for 10-20 min, then dropwise adding 40-60 parts of (methoxy triethylene glycol ether propyl) trimethoxysilane for 10-30 min, stirring at 100-500 rpm after the dropwise adding is completed for 30-50 min, then dropwise adding 1-5 parts of 2-methylpropan-2-enoate for 10-30 min, stirring at 100-500 rpm after the dropwise adding is completed for 30-50 min, and then cooling to room temperature to obtain a modifier;
s2, adding 60-80 parts of 2-methyl-2-acrylic acid nonyl ester, 4-6 parts of acrylic acid and 15-25 parts of pentaerythritol triacrylate into 130-150 parts of ethyl acetate, stirring at 100-500 rpm at 70-90 ℃ for 1-3 h, adding 4-6 parts of 4,4' -azobis (4-cyano valeric acid), slowly adding for 10-30 min, treating for 4-8 h, and cooling to room temperature to obtain a treating agent;
and S3, stirring and mixing 8-12 parts of the modifier prepared in the step S1 and 15-25 parts of the treating agent prepared in the step S2 at 100-500 rpm for 10-30 min to obtain the modified resin glue.
The main substances in the preparation of the resin glue have the functions of:
hexyl 2-ethylacrylate and hydroxyethyl acrylate: these two monomers are the main components of acrylic OCA optical adhesives, which polymerize in the reaction to form the polymer matrix of the adhesive.
1-hydroxycyclohexyl phenyl ketone: the photoinitiator is a photoinitiator, the activity of the photoinitiator is excited by ultraviolet irradiation, the polymerization reaction of the monomer is initiated, and the curing of the acrylic OCA optical adhesive is promoted.
The ultraviolet lamp provides ultraviolet irradiation, activates the photoinitiator, and enables the acrylic OCA optical adhesive to undergo polymerization reaction and be solidified into a solid state.
The main substances in the preparation method of the modified resin glue have the functions that:
2-acetamidofluorene and dibutyldioctadecanoic acid tin: these are components of the modifier. The addition of the acrylic OCA optical adhesive can improve the performance and performance stability of the acrylic OCA optical adhesive and enhance the crosslinking degree and adhesion performance of the adhesive.
(methoxy triethylene glycol ether propyl) trimethoxysilane: this is one of the components in the modifier. It plays roles of enhancing adhesion and improving adhesion between the adhesive and a base material in the modified resin glue.
2-methylprop-2-enoic acid 2-phosphinoxyethyl ester: this is one of the components in the modifier. It can raise the durability and mechanical performance of modified resin glue.
2-methyl-2-acrylic acid nonyl ester, acrylic acid and pentaerythritol triacrylate: these are the main components of the modified resin glue, which polymerize in the reaction to form the polymer matrix of the adhesive.
Ethyl acetate: as the reaction solvent, the environment of the reaction system is provided.
1, 4' -azobis (4-cyanovaleric acid): this is an initiator, which participates in the polymerization of the modified resin glue.
In general, in the process of preparing the acrylic OCA optical adhesive and the modified resin adhesive, the performance of the adhesive can be regulated and controlled by polymerization reaction and adding the modifier, and the adhesive performance, the optical performance and the mechanical performance are improved.
The acrylic OCA optical adhesive is modified by the modifier to improve the adhesive force and the dynamic folding property. The possible reasons and mechanisms of action are that the introduction of the modifier may alter the chemical structure and properties of the acrylic OCA, thereby improving its adhesive and mechanical properties. The cross-linking agent in the modifier can carry out cross-linking reaction with double bonds in the acrylic acid OCA to form a three-dimensional network structure. The crosslinked structure can enhance the strength and durability of the adhesive and improve the adhesive force and the dynamic folding property. The components of the modifier may interact with molecules in the acrylic OCA, such as hydrogen bonding, electrostatic forces, etc. These interactions can enhance the adsorption force and compatibility between molecules and improve the adhesion performance of the adhesive. And changes the morphology of acrylic OCA, such as increases the crosslink density, improves dispersibility, etc. These structural changes can enhance the strength and toughness of the adhesive and improve its dynamic folding properties.
The high-performance acrylic OCA optical adhesive with a double-layer structure prepared by the invention has no bubble rebound risk: it is possible that the resin glue of the present invention can effectively remove bubbles from the resin glue by using ultraviolet irradiation and nitrogen bubbling for degassing during the preparation process. In this way, the formation and aggregation of bubbles during the coating and curing process can be avoided, thereby reducing the risk of bubble rebound and enabling the optical cement to have higher quality and reliability. The water vapor barrier property is excellent: the acrylic OCA optical adhesive with the double-layer structure comprises a PET light release film and a PET heavy release film, and the films play a role in connection between the uppermost OCA optical adhesive and the lowermost OCA optical adhesive. The PET film has good water vapor barrier property, can effectively prevent water vapor from penetrating, and protects the optical device from being influenced and damaged by moisture, thereby improving the stability and the service life of the optical device. The acrylic OCA optical adhesive with the double-layer structure consists of a lowest OCA optical adhesive layer and an uppermost OCA optical adhesive layer. The lowest OCA optical cement is coated on a layer of PET heavy release film by resin glue, and is formed by high-temperature thermal curing. The uppermost OCA optical cement is coated on the lowermost OCA optical cement by the modified resin glue, and then thermally cured at high temperature. The double-layer structure can enhance the mechanical strength and durability of the optical cement, provide better protection and support, reduce the influence of external impact and stress on optical devices, reduce the risk of breakage, reduce the risk of bubble rebound and prevent the permeation of water vapor.
Compared with the traditional single-layer structure, the optical cement with the double-layer structure has the following obvious advantages:
1. improving the bonding strength: the double-layer structure can remarkably improve the bonding strength. By superposing the two layers of optical cement together to form a stronger bonding interface, the contact area and the bonding area can be increased, thereby improving the overall bonding strength and reliability.
2. Reduction of optical reflection and scattering: the double-layer structure can reduce interface reflection and scattering between the optical cement and the substrate. The second layer of optical cement can fill a tiny gap between the first layer of optical cement and the substrate, so that the possibility of interface reflection and scattering is reduced, and the optical transparency and the transmission efficiency are improved.
3. Increase durability and stability: the double layer structure can increase the durability and stability of the optical cement. The first layer of optical adhesive provides basic adhesive function and protection, while the second layer of optical adhesive further increases the resistance to shearing and external environmental factors, such as humidity, temperature, etc., thereby improving the durability and stability of the optical adhesive.
3. Optimizing stress distribution: the double-layer structure can optimize stress distribution and reduce stress concentration. The first layer of optical adhesive can absorb and relieve a part of stress, and disperse the stress into the second layer of optical adhesive, so that the possibility of stress concentration is reduced, and the reliability and stability of bonding are improved.
4. Better adaptability and adjustability: the double-layer structure can be designed and adjusted according to different requirements. By selecting different optical cement materials and thickness combinations, flexible adjustment of adhesion properties, optical properties and mechanical properties can be achieved to meet the requirements of specific applications.
In summary, the optical cement of the double-layer structure has obvious advantages over the conventional single-layer structure, including improved adhesion strength, reduced optical reflection and scattering, increased durability and stability, optimized stress distribution, and better adaptability and adjustability. These advantages make the optical cement with double-layer structure have wider application prospect in bonding and optical application.
Compared with the prior art, the invention has the beneficial effects that:
1) The preparation of the invention can improve the performance and performance stability of the acrylic OCA optical adhesive by introducing the modifier into the acrylic OCA optical adhesive. The modifier can enhance the crosslinking degree and the adhesion performance of the adhesive and improve the adhesive force between the adhesive and the base material.
2) The invention adopts a double-layer structure design, has a light release film and a heavy release film layer, can provide better mechanical support and protection, and enhances the stability and durability of the optical cement.
3) The optimized double-layer structure and the introduction of the modifier can obviously improve the bonding performance, including adhesion, shear strength and durability.
4) According to the high-performance acrylic OCA optical adhesive with a double-layer structure, the most appropriate OCA optical adhesive formula is selected for different bonding surfaces according to the characteristics of bonding base materials, so that the best bonding effect between two different bonding surfaces is realized; when the OCA optical adhesive with the high-performance double-layer structure is attached to different base materials, the OCA optical adhesive has very good inhibition effect on bubble rebound phenomenon generated by stress or section difference; when the single-layer OCA optical adhesive is adhered to a resin plate and a film or glass, the problem of poor degree of fit of the single-layer OCA optical adhesive between different base materials can be well solved; the OCA optical adhesive with the high-performance double-layer structure can enable the display touch product to be less prone to generating colloid cracking, bubble rebound and other anomalies, and improves the product quality.
5) The invention adopts two different OCA optical adhesives to prepare, which can simultaneously take the characteristic advantages of the two optical adhesives into consideration; the touch screen can be suitable for the lamination of cover plates of different material types and touch screen functional sheets, is also suitable for the full lamination of touch screens and liquid crystal screens, is mainly used for products such as consumer products, industrial control products, vehicle-mounted products, military products and the like, and has the advantages of excellent foam removal performance, high cyclicity, good physical properties and good optical properties.
Detailed Description
The main material sources are as follows:
2-methylprop-2-enoic acid 2-phosphinoxyethyl ester: CAS:125146-50-1, english name: 2-phosphoxynyl 2-methylprop-2-enoate, having the formula: c (C) 6 H 11 O 6 P。
2-methyl-2-acrylic acid nonyl ester: CAS:93804-46-7, english name: 2-methylnonyl acrylate, molecular formula: c (C) 13 H 24 O 2 。
PET light release film: brand number: matte PET release film, huizhou Yingbo New Material science and technology Co., ltd., thickness: 50 μm.
PET heavy release film: the Xuan paper Co Ltd in Suzhou, the material quality: PET film, model: YX, thickness: 85 μm.
Hydroxyl-terminated polydimethyl siloxane: huangshan City powerful chemical industry Co., ltd., model: QL-2311VDV.
Example 1
The preparation method of the high-performance acrylic OCA optical adhesive with the double-layer structure comprises the following steps:
the acrylic OCA optical adhesive with the double-layer structure comprises a PET light release film, an acrylic OCA optical adhesive with the double-layer structure and a PET heavy release film from top to bottom in sequence; the acrylic OCA optical adhesive with the double-layer structure is divided into a lowest OCA optical adhesive layer and an uppermost OCA optical adhesive layer, wherein the lowest OCA optical adhesive layer is formed by coating resin glue on a layer of PET heavy release film through a doctor blade coating method and performing high-temperature thermal curing molding; the uppermost OCA optical adhesive is coated on the lowermost OCA optical adhesive by a modified resin adhesive through a doctor blade coating method and is obtained through high-temperature thermal curing, wherein the temperature of the high-temperature thermal curing is 150 ℃, and the time of the high-temperature thermal curing is 2min; the PET light release film and the PET heavy release film are respectively positioned at the outer sides of the acrylic OCA optical cement with the double-layer structure, and the middle of the uppermost OCA optical cement film and the lowermost OCA optical cement film plays a role in connection after being thermally cured at high temperature; the thickness of the lowermost OCA optical adhesive is 300 mu m, and the thickness of the uppermost OCA optical adhesive is 500 mu m, so that the acrylic OCA optical adhesive with a high-performance double-layer structure is obtained.
The preparation method of the resin glue comprises the following steps:
70g of 2-ethylhexyl acrylate and 30g of hydroxyethyl acrylate are stirred and mixed for 30min at 200rpm, then 1.5g of 1-hydroxycyclohexyl phenyl ketone is added to obtain a prepolymer mixture, the prepolymer mixture is stirred and degassed for 30min at 300rpm at 20 ℃ while bubbling with nitrogen, and after the degassing is completed, ultraviolet irradiation is performed under nitrogen atmosphere by using an ultraviolet lamp with the power of 30W and the wavelength of 405nm, thereby obtaining the resin glue.
The preparation method of the modified resin glue comprises the following steps:
s1, adding 14g of 2-acetamidofluorene and 0.07g of dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring at 200rpm under a nitrogen atmosphere at 50 ℃ for 15min, then dropwise adding 50g of (methoxy triethylene glycol ether propyl) trimethoxysilane for 20min, stirring at 200rpm for 40min after dropwise adding, then dropwise adding 3g of 2-methylpropan-2-enoate 2-phosphinoethyl for 20min, stirring at 200rpm for 40min after dropwise adding, and cooling to room temperature to obtain a modifier;
s2, adding 70g of 2-methyl-2-acrylic acid nonyl ester, 5g of acrylic acid and 20g of pentaerythritol triacrylate into 140g of ethyl acetate, stirring at 300rpm at 80 ℃ for 2 hours, adding 5g of 4,4' -azobis (4-cyanovaleric acid), slowly adding for 20 minutes, and cooling to room temperature after 6 hours of treatment to obtain a treating agent;
and S3, stirring and mixing 10g of the modifier prepared in the step S1 and 20g of the treating agent prepared in the step S2 at 200rpm for 20min to obtain the modified resin glue.
Comparative example 1
The preparation method of the high-performance double-layer-structured acrylic OCA optical adhesive is basically the same as that of example 1, and the only difference is that: the preparation methods of the modified resin glue are different.
The preparation method of the modified resin glue comprises the following steps:
s1, adding 14g of isophorone diisocyanate and 0.07g of dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring at 200rpm under a nitrogen atmosphere at 50 ℃ for 15min, then dropwise adding 50g of (methoxy triethylene glycol ether propyl) trimethoxysilane for 20min, stirring at 200rpm for 40min after the dropwise adding, dropwise adding 3g of 2-methylpropan-2-enoate 2-phosphinoethyl for 20min, stirring at 200rpm for 40min after the dropwise adding, and cooling to room temperature to obtain a modifier;
s2, adding 70g of 2-methyl-2-acrylic acid nonyl ester, 5g of acrylic acid and 20g of pentaerythritol triacrylate into 140g of ethyl acetate, stirring at 300rpm at 80 ℃ for 2 hours, adding 5g of 4,4' -azobis (4-cyanovaleric acid), slowly adding for 20 minutes, and cooling to room temperature after 6 hours of treatment to obtain a treating agent;
and S3, stirring and mixing 10g of the modifier prepared in the step S1 and 20g of the treating agent prepared in the step S2 at 200rpm for 20min to obtain the modified resin glue.
The preparation method of the resin glue is the same as that of the example 1.
Comparative example 2
The preparation method of the high-performance double-layer-structured acrylic OCA optical adhesive is basically the same as that of example 1, and the only difference is that: the preparation methods of the modified resin glue are different.
The preparation method of the modified resin glue comprises the following steps:
s1, adding 14g of 2-acetamidofluorene and 0.07g of dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring at 200rpm under a nitrogen atmosphere at 50 ℃ for 15min, then dropwise adding 50g of hydroxyl-terminated polydimethylsiloxane for 20min, stirring at 200rpm for 40min after the dropwise adding, dropwise adding 3g of 2-methylpropan-2-enoate 2-phosphinoxyethyl ester for 20min, stirring at 200rpm for 40min after the dropwise adding, and cooling to room temperature to obtain a modifier;
s2, adding 70g of 2-methyl-2-acrylic acid nonyl ester, 5g of acrylic acid and 20g of pentaerythritol triacrylate into 140g of ethyl acetate, stirring at 300rpm at 80 ℃ for 2 hours, adding 5g of 4,4' -azobis (4-cyanovaleric acid), slowly adding for 20 minutes, and cooling to room temperature after 6 hours of treatment to obtain a treating agent;
and S3, stirring and mixing 10g of the modifier prepared in the step S1 and 20g of the treating agent prepared in the step S2 at 200rpm for 20min to obtain the modified resin glue.
The preparation method of the resin glue is the same as that of the example 1.
Comparative example 3
The preparation method of the high-performance double-layer-structured acrylic OCA optical adhesive is basically the same as that of example 1, and the only difference is that: the preparation methods of the modified resin glue are different.
The preparation method of the modified resin glue comprises the following steps:
s1, adding 14g of 2-acetamidofluorene and 0.07g of dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring at 200rpm under a nitrogen atmosphere at 50 ℃ for 15min, then dropwise adding 50g of (methoxy triethylene glycol ether propyl) trimethoxysilane for 20min, stirring at 200rpm for 40min after the dropwise adding, dropwise adding 3g of 2-hydroxyethyl methacrylate for 20min, stirring at 200rpm for 40min after the dropwise adding, and cooling to room temperature to obtain a modifier;
s2, adding 70g of 2-methyl-2-acrylic acid nonyl ester, 5g of acrylic acid and 20g of pentaerythritol triacrylate into 140g of ethyl acetate, stirring at 300rpm at 80 ℃ for 2 hours, adding 5g of 4,4' -azobis (4-cyanovaleric acid), slowly adding for 20 minutes, and cooling to room temperature after 6 hours of treatment to obtain a treating agent;
and S3, stirring and mixing 10g of the modifier prepared in the step S1 and 20g of the treating agent prepared in the step S2 at 200rpm for 20min to obtain the modified resin glue.
The preparation method of the resin glue is the same as that of the example 1.
Comparative example 4
The preparation method of the high-performance double-layer-structured acrylic OCA optical adhesive is basically the same as that of example 1, and the only difference is that: the preparation methods of the modified resin glue are different.
The preparation method of the modified resin glue comprises the following steps:
s1, adding 14g of isophorone diisocyanate and 0.07g of dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring at 200rpm under a nitrogen atmosphere at 50 ℃ for 15min, then dropwise adding 50g of hydroxyl-terminated polydimethylsiloxane for 20min, stirring at 200rpm for 40min after the dropwise adding, dropwise adding 3g of 2-hydroxyethyl methacrylate for 20min, stirring at 200rpm for 40min after the dropwise adding, and cooling to room temperature to obtain a modifier;
s2, adding 70g of 2-methyl-2-acrylic acid nonyl ester, 5g of acrylic acid and 20g of pentaerythritol triacrylate into 140g of ethyl acetate, stirring at 300rpm at 80 ℃ for 2 hours, adding 5g of 4,4' -azobis (4-cyanovaleric acid), slowly adding for 20 minutes, and cooling to room temperature after 6 hours of treatment to obtain a treating agent;
and S3, stirring and mixing 10g of the modifier prepared in the step S1 and 20g of the treating agent prepared in the step S2 at 200rpm for 20min to obtain the modified resin glue.
The preparation method of the resin glue is the same as that of the example 1.
Test example 1
Adhesion test
The samples prepared in the examples and comparative examples of the present invention were cut into 25mm wide and 400mm long, the light release film was removed and attached to PI, PI 50 μm thick and 300mm long was attached to the other side, and corona treated, the ends of each strip were clamped to the tensile clamps of the tensile machine, peeled off at a speed of 300mm/min, and the data of 5 groups were tested for averaging. See in particular table 1.
TABLE 1 adhesion test results
| Test protocol | Adhesive force (N/25 mm) |
| Example 1 | 13.7 |
| Comparative example 1 | 12.1 |
| Comparative example 2 | 11.6 |
| Comparative example 3 | 11.8 |
| Comparative example 4 | 9.5 |
Test example 2
Dynamic folding test
Samples prepared in the examples of the present invention and comparative examples were laminated between two 50 μm thick PIs to form a laminated structure. The laminate structure was then cut to a specification of 10cm by 5 cm. The sample was then mounted in a dynamic folding device with two folding stations that rotated from 180 ° (sample unbent) to 0 ° (sample folded) and 250000 folds were performed at a test frequency of about 3 seconds/time. The radius of curvature of 4mm is determined by the gap between the two rigid plates in the closed state (0 deg.). Folding was performed at room temperature. Observing whether bubbles, folds, layering and fracture occur after folding. Scoring was performed according to the criteria of table 2, each sample was tested 5 times, and the score average was obtained, and the test results are shown in table 3.
Table 2 scoring criteria
Table 3 dynamic fold test results
| Experimental protocol | Post-folding score |
| Example 1 | 96.4 |
| Comparative example 1 | 91.0 |
| Comparative example 2 | 89.8 |
| Comparative example 3 | 88.0 |
| Comparative example 4 | 76.0 |
Test example 3
Evaluation of aging test
The high-performance acrylic OCA optical adhesive/ITO glass with a double-layer structure is prepared according to the glass cover plate/the invention, and the structure is attached and defoamed, the defoamation process is 70 ℃,60min, the pressure is 3.5KG, and the size is 5 inches.
After aging for 1000 hours at 95 ℃, the sample of the invention has no foam return, no yellowing, no whitening and no warping.
After aging for 1000 hours at the temperature of 85 ℃ and the humidity of 85%, the samples of the invention have no water vapor permeation and no foaming, which indicates that the samples of the invention have better water vapor barrier property.
The sample provided by the invention has no bubble rebound risk and excellent water vapor barrier property. The adhesive force and the dynamic folding effect of the embodiment 1 of the invention are best probably because the embodiment 1 of the invention is obtained by firstly coating resin glue between two layers of release films through a doctor blade coating method and then coating modified resin glue on the lowest OCA optical glue layer which is coated in advance, and realizing integral bonding through high-temperature thermal curing and forming, thus obtaining the acrylic OCA optical glue with a high-performance double-layer structure. The resin glue is prepared by mixing 2-ethylhexyl acrylate and hydroxyethyl acrylate under stirring, adding 1-hydroxycyclohexyl phenyl ketone to obtain a prepolymer mixture, stirring, degassing, and irradiating with ultraviolet rays after degassing is completed. The preparation method of the modified resin glue comprises the steps of adding 2-acetamidofluorene and dibutyl tin dioctadecanoate into a double-neck flask equipped with a mechanical stirrer, stirring under a nitrogen atmosphere, then dropwise adding (methoxy triethylene glycol ether propyl) trimethoxysilane, then dropwise adding 2-methylpropan-2-enoate 2-phosphinoethyl ester, stirring, and then cooling to room temperature to obtain a modifier; adding 2-methyl-2-acrylic acid nonyl ester, acrylic acid and pentaerythritol triacrylate into ethyl acetate, stirring at high temperature, adding 4,4' -azobis (4-cyano valeric acid), and cooling to room temperature to obtain a treating agent; and stirring and mixing the modifier and the treating agent to obtain the modified resin glue.
In the preparation process of the resin glue, 1-hydroxy cyclohexyl phenyl ketone is used as a photoinitiator to react with 2-ethylhexyl acrylate and hydroxyethyl acrylate to form respective free radicals, and then the free radicals are polymerized to further form polymer chains. Thereby forming a copolymer having higher adhesion, strength and crosslinkability.
Example 1 contains an acetamido group in the molecule that can react with the carboxyl group in the modified resin glue molecule to form an amide bond, as compared with comparative example 1. The introduction of the amide bond can increase the crosslinking degree of the modified resin glue molecules, thereby improving the adhesion performance and mechanical performance of the modified resin glue molecules. And the introduction of 2-acetamidofluorene may change the structure and arrangement of the modified resin glue molecules. The structural change can increase the interaction force between molecules and improve the adhesion performance and dynamic folding performance of the adhesive. The 2-acetamidofluorene may have better stability and durability than isophorone diisocyanate. This ensures that the modifier maintains its modifying effect during long-term use and storage, thereby improving the performance stability of the modified resin glue optical adhesive.
Example 1 in comparison with comparative example 2 in the preparation of the modified resin glue, (methoxy-triethylene glycol ether-propyl) trimethoxysilane was introduced into the modified resin glue. (methoxy triethylene glycol ether propyl) trimethoxysilane is an organic silicon compound and has better surface activity and hydrophilicity. The modified resin glue can improve the coating performance and interface compatibility with a base material, and improve the adhesion and durability. The addition of the modifier may change the structure and arrangement of the modified resin glue molecules, so that the modified resin glue has better dynamic folding performance. This is important for coping with external influences such as temperature changes and mechanical stresses, and can improve the stability and reliability of the adhesive interface.
Example 1 in contrast to comparative example 3, 2-methylprop-2-enoate 2-phosphinoxyethyl ester contains a phosphate group in the molecule that can react with carboxyl groups in the modified resin glue to form ester bonds. Thus, additional crosslinking sites can be introduced, the crosslinking degree of the optical adhesive is enhanced, and the adhesion performance and the mechanical performance are improved. And the structure and arrangement mode of the modified resin glue molecules can be changed, so that the modified resin glue has better dynamic folding performance. This is important for coping with external influences such as temperature changes and mechanical stresses, and can improve the stability and reliability of the adhesive interface.
The modified resin glue is easy to spread on the substrate, so that the modified resin glue has higher adhesiveness and peeling strength. On the other hand, since the modified resin glue has more methacrylic groups, it has more crosslinked structure. The modifier improves the adhesion properties of the silicone unit-containing treatment. The specific reasons and mechanisms of action may be affected by the components and proportions of the modifier used, the reaction conditions, and the like.
Finally, the following is specifically described: the preparation method and implementation effect can be only used for the technical scheme of the invention, and are not limiting on the invention; corresponding changes, such as modification, addition or replacement, etc. made by those skilled in the art in the technical scheme of the present invention also belong to the protection scope of the technical scheme implemented by the present invention.
Claims (9)
1. The preparation method of the high-performance double-layer-structured acrylic OCA optical adhesive is characterized by comprising the following steps of: the acrylic OCA optical adhesive with the double-layer structure comprises a PET light release film, an acrylic OCA optical adhesive with the double-layer structure and a PET heavy release film from top to bottom in sequence.
2. The method for preparing the high-performance acrylic OCA optical adhesive with a double-layer structure according to claim 1, wherein the acrylic OCA optical adhesive with the double-layer structure is divided into a lowermost OCA optical adhesive and an uppermost OCA optical adhesive, and the lowermost OCA optical adhesive is coated on a layer of PET heavy release film by resin glue through a doctor blade coating method and is obtained through high-temperature thermal curing molding; the uppermost OCA optical adhesive is coated on the lowermost OCA optical adhesive by modified resin glue through a doctor blade coating method, and is obtained through high-temperature heat curing.
3. The method for preparing the high-performance acrylic OCA optical adhesive with the double-layer structure as claimed in claim 2, wherein the PET light release film and the PET heavy release film are respectively positioned at the outer sides of the acrylic OCA optical adhesive with the double-layer structure, and the middle part of the uppermost OCA optical adhesive film and the lowermost OCA optical adhesive film is subjected to high-temperature curing to play a role in connection.
4. The method for preparing high-performance double-layer structured acrylic OCA optical adhesive according to claim 3, wherein the high-temperature curing temperature is 140-160 ℃, and the high-temperature curing time is 1-3 min.
5. The method for preparing high-performance double-layer structured acrylic OCA optical adhesive according to claim 2, wherein the thickness of the lowest OCA optical adhesive is 5-1000 μm, and the thickness of the uppermost OCA optical adhesive is 5-1000 μm.
6. The method for preparing the high-performance double-layer structured acrylic OCA optical adhesive according to claim 1, wherein the thickness of the PET light release film is 40-60 μm; the thickness of the PET heavy release film is 80-90 mu m.
7. The preparation method of the high-performance double-layer structured acrylic OCA optical adhesive as claimed in claim 2, which is characterized in that the preparation method of the resin adhesive is as follows in parts by weight:
mixing 60-80 parts of 2-ethylhexyl acrylate and 20-40 parts of hydroxyethyl acrylate at 100-300 rpm for 20-40 min, adding 1-2 parts of 1-hydroxycyclohexyl phenyl ketone to obtain a prepolymer mixture, stirring the prepolymer mixture at 100-500 rpm at 15-25 ℃, simultaneously bubbling with nitrogen for degassing for 20-40 min, and irradiating with ultraviolet rays under nitrogen atmosphere by using an ultraviolet lamp with the power of 20-40W and the wavelength of 200-400 nm after the degassing is completed to obtain the resin glue.
8. The method for preparing the high-performance double-layer structured acrylic OCA optical adhesive according to claim 3, wherein the method for preparing the modified resin glue is as follows in parts by weight:
s1, mixing 10-20 parts of 2-acetamidofluorene and 0.05-0.1 part of dibutyl tin dioctadecanoate, stirring at 100-300 rpm under a nitrogen atmosphere at 40-60 ℃ for 10-20 min, then dropwise adding 40-60 parts of (methoxy triethylene glycol ether propyl) trimethoxysilane for 10-30 min, stirring at 100-500 rpm after the dropwise adding is completed for 30-50 min, then dropwise adding 1-5 parts of 2-methylpropan-2-enoate for 10-30 min, stirring at 100-500 rpm after the dropwise adding is completed for 30-50 min, and then cooling to room temperature to obtain a modifier;
s2, adding 60-80 parts of 2-methyl-2-acrylic acid nonyl ester, 4-6 parts of acrylic acid and 15-25 parts of pentaerythritol triacrylate into 130-150 parts of ethyl acetate, stirring at 100-500 rpm at 70-90 ℃ for 1-3 h, adding 4-6 parts of 4,4' -azobis (4-cyano valeric acid), slowly adding for 10-30 min, treating for 4-8 h, and cooling to room temperature to obtain a treating agent;
and S3, stirring and mixing 8-12 parts of the modifier prepared in the step S1 and 15-25 parts of the treating agent prepared in the step S2 at 100-500 rpm for 10-30 min to obtain the modified resin glue.
9. An acrylic OCA optical adhesive with a high-performance bilayer structure, which is characterized by being prepared by the preparation method according to any one of claims 1 to 8.
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