CN114196353A - High-filling-property SCA optical adhesive and preparation method and application thereof - Google Patents

High-filling-property SCA optical adhesive and preparation method and application thereof Download PDF

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Publication number
CN114196353A
CN114196353A CN202111588762.4A CN202111588762A CN114196353A CN 114196353 A CN114196353 A CN 114196353A CN 202111588762 A CN202111588762 A CN 202111588762A CN 114196353 A CN114196353 A CN 114196353A
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Prior art keywords
optical cement
sca
sca optical
photoinitiator
eva resin
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CN202111588762.4A
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Inventor
孙仕兵
顾孔胜
周双荣
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Shenzhen Gaoren Electronic New Material Co ltd
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Shenzhen Gaoren Electronic New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853Vinylacetate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a high-filling SCA optical cement and a preparation method thereof. The SCA optical cement comprises the following components in percentage by mass: 95-98% of EVA resin, 0.2-1% of cross-linking agent, 0.2-1% of coupling agent, 0.1-1% of photoinitiator and 1-3% of microcrystalline wax. The segment difference coverage rate of the SCA optical cement provided by the invention can reach 50%, and the environment measurement is stable and has no risk. According to the invention, the VA content and MI in the EVA resin are controlled, so that the flow property of the optical adhesive is improved, a certain amount of microcrystalline wax is added, and the flow property of the optical adhesive is further improved, so that the filling property of the optical adhesive is improved after a display screen or a functional sheet is attached. When the reliability test is carried out, the problems of air bubbles and the like can not occur. In the whole laminating process, the flow property of the optical cement is excellent, and the filling property is greatly improved.

Description

High-filling-property SCA optical adhesive and preparation method and application thereof
Technical Field
The invention relates to the field of optical cement, in particular to a high-filling SCA optical cement and a preparation method and application thereof.
Background
At present, the optical cement is widely applied to the laminating of the touch screen and the full laminating of the liquid crystal screen and the touch screen. The LOCA process of the liquid glue is complex and the production efficiency is low; the solid glue has high production efficiency, but has the fatal problems of low coverage rate of section difference, instable circular measurement and bubble rebound during the high-section difference lamination. The solid glue in the current market has the best segment difference coverage rate of about 20 percent, and still has the problem of unstable environment measurement.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the SCA optical cement with high filling property. The segment difference coverage rate of the SCA optical cement can reach 50%, and the environmental measurement is stable and has no risk.
The high-filling SCA optical cement provided by the invention comprises the following components in percentage by mass: 95-98% of EVA resin (ethylene-vinyl acetate copolymer), 0.2-1% of cross-linking agent, 0.2-1% of coupling agent, 0.1-1% of photoinitiator and 1-3% of microcrystalline wax.
Further, the SCA optical cement comprises the following components in percentage by mass: 95-98% of EVA resin (ethylene-vinyl acetate copolymer), 0.2-1% of cross-linking agent, 0.2-1% of coupling agent, 0.1-1% of photoinitiator and 1.5-2.5% of microcrystalline wax.
In the invention, the EVA resin generally has 5-40% of VA (vinyl acetate) content and 10-400g/(10min) of MI (melt index). Preferably, the EVA resin has a VA content of 28% and an MI of 15g/(10 min).
Specifically, the higher the VA content of the EVA resin is, the higher its elasticity, flexibility, compatibility, transparency, and the like are; when the content of VA is reduced, the performance of VA is close to that of Polyethylene (PE), the rigidity is increased, and the wear resistance and the electrical insulation are improved. The content of VA is constant, the dissolved MI is increased, the softening point is reduced, the processability and the surface gloss are improved, but the strength is reduced, otherwise, the molecular weight is increased along with the reduction of the MI, and the impact property and the environmental stress cracking resistance are improved.
The cross-linking agent can be selected from one or more of tert-butyl peroxy-2-ethylhexanoate, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane, tert-amyl peroxy (2-ethylhexyl) carbonate and tert-butyl peroxy-2-ethylhexanoate. The simultaneous use of two or more crosslinking agents produces a synergistic effect and results in superior performance to single component applications.
The coupling agent is a silane coupling agent, and can be selected from one or more of vinyltris (methoxyethoxy) silane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane. More specifically, the following are: the mass ratio of the gamma-methacryloxypropyltrimethoxysilane to the N- (2-aminoethyl) -3-aminopropyltrimethoxysilane is 1: 1.
The photoinitiator can have certain light absorption capacity in an ultraviolet region (250-400 nm) or a visible light region (400-800 nm), and initiator molecules are transited from a ground state to an excited singlet state and transited from a system to an excited triplet state after directly or indirectly absorbing light energy; after the excited singlet or triplet state undergoes unimolecular or bimolecular chemical action, active fragments capable of initiating the polymerization of the monomers are generated, which can be radicals, cations, anions, etc. The invention selects the composite photoinitiator, and the initiation efficiency is higher. Specifically, the photoinitiator may be one or more selected from 1-hydroxycyclohexyl phenyl ketone (photoinitiator 184), 2-hydroxy-2-methyl-1-phenyl-1-propanone (photoinitiator 1713), photoinitiator TP0 and 4-phenylbenzophenone; more specifically, such as: the mixed photoinitiator consists of 1-hydroxycyclohexyl phenyl ketone and 2-hydroxy-2-methyl-1-phenyl-1-acetone in a mass ratio of 2: 1.
The microcrystalline wax acts as a plasticizer. The EVA resin contains strong polar groups, has strong intermolecular action, and can reduce the interaction between molecular chains by the interaction between the EVA resin and a polymer by adding a plasticizer under the premise of increasing the processing temperature, thereby achieving the purpose of improving the processing fluidity.
According to one embodiment of the invention, the SCA optical cement comprises the following components in percentage by mass: 95% of EVA resin (ethylene-vinyl acetate copolymer), 1% of cross-linking agent, 1% of coupling agent, 0.5% of photoinitiator and 2.5% of microcrystalline wax.
According to one embodiment of the invention, the SCA optical cement comprises the following components in percentage by mass: 98% of EVA resin (ethylene-vinyl acetate copolymer), 0.2% of cross-linking agent, 0.2% of coupling agent, 0.1% of photoinitiator and 1.5% of microcrystalline wax.
According to one embodiment of the invention, the SCA optical cement comprises the following components in percentage by mass: 95% of EVA resin (ethylene-vinyl acetate copolymer), 1% of cross-linking agent, 1% of coupling agent, 1% of photoinitiator and 2% of microcrystalline wax.
According to one embodiment of the invention, the SCA optical cement comprises the following components in percentage by mass: 96% of EVA resin (ethylene-vinyl acetate copolymer), 0.5% of cross-linking agent, 0.5% of coupling agent, 0.5% of photoinitiator and 2.5% of microcrystalline wax.
The invention also provides a preparation method of the high-filling SCA optical cement.
The preparation method of the SCA optical cement provided by the invention comprises the following steps:
1) uniformly mixing the EVA resin, the cross-linking agent, the coupling agent and the photoinitiator according to respective proportions to obtain a mixed ingredient; preparing microcrystalline wax into powder, adding the powder into the mixed ingredients, and uniformly mixing again;
2) and (2) introducing the mixture prepared in the step 1) into a double-screw extruder, extruding the mixture at the tail end of the double-screw extruder through a melt pump, filtering and extruding the mixture through a screen, and calendering to form a film to obtain the SCA optical adhesive layer.
In the step 2), the twin-screw extruder is usually preheated for 20-30min at 80 ℃.
Furthermore, a layer of protective release film can be attached to the front surface and the back surface of the SCA optical adhesive layer respectively to prepare the SCA optical adhesive film. The SCA optical glue layer can be made into different thicknesses (such as 200 μm) according to requirements.
The invention also provides an application of the SCA optical cement.
The invention provides an application of an SCA optical adhesive in preparation of a touch screen laminating film, and particularly relates to laminating of a functional sheet and a cover plate.
The high-filling optical adhesive provided by the invention improves the self-flowing property of the optical adhesive by controlling the VA content and MI in the EVA resin, and further improves the flowing property of the optical adhesive by adding a certain amount of microcrystalline wax, so that the filling property of the optical adhesive is improved after a display screen or a functional sheet is attached. When the reliability test is carried out, the problems of air bubbles and the like can not occur. In the whole laminating process, the flow property of the optical cement is excellent, and the filling property is greatly improved.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
The invention provides a high-filling SCA optical adhesive which comprises, by mass, 95% -98% of EVA resin (ethylene-vinyl acetate copolymer), 0.2% -1% of cross-linking agent, 0.2% -1% of coupling agent, 0.1% -1% of photoinitiator and 1% -3% of microcrystalline wax.
The preparation method of the high-filling SCA optical cement comprises the following steps:
(1) uniformly mixing the EVA resin, the cross-linking agent, the coupling agent and the photoinitiator according to respective proportions, preparing the microcrystalline wax into powder, adding the powder into the mixed ingredients, and uniformly mixing again.
(2) Introducing the prepared mixture into a double-screw extruder, extruding the mixture at the tail end of the extruder through a melt pump, filtering and extruding the mixture through a screen, calendering the mixture into a film, and attaching a layer of protective release film on the front surface and the back surface of the adhesive film respectively to prepare an optical adhesive film; wherein, the thickness of the optical adhesive layer can be 200 μm.
The EVA resin used in the following examples had a VA content of 28% and an MI of 15g/(10 min).
Example 1: SCA optical cement with high filling property
The high-filling SCA optical cement comprises the following components in percentage by mass: the EVA resin content is 95%, the tert-butyl peroxy-2-ethylhexanoate content is 1%, the contents of gamma-methacryloxypropyltrimethoxysilane and N- (2-aminoethyl) -3-aminopropyltrimethoxysilane (mass ratio is 1:1) are 1%, the contents of 1-hydroxycyclohexyl phenyl ketone and 2-hydroxy-2-methyl-1-phenyl-1-propanone (mass ratio is 2:1) are 0.5%, and the microcrystalline wax content is 2.5%.
The preparation method comprises the following steps:
(1) uniformly mixing EVA resin, a cross-linking agent, a coupling agent and a photoinitiator according to respective proportions, preparing microcrystalline wax into powder, adding the powder into the mixed ingredients, and uniformly mixing again;
(2) introducing the prepared mixture into a double-screw extruder, extruding the mixture at the tail end of the extruder through a melt pump, filtering and extruding the mixture through a screen, and calendering to form a film to obtain an optical adhesive layer; meanwhile, the front and back surfaces of the adhesive film are respectively attached with a layer of protective release film to obtain the optical adhesive film.
Example 2: SCA optical cement with high filling property
The high-filling SCA optical cement comprises the following components in percentage by mass: the EVA resin content is 98%, the tert-butyl peroxy-2-ethylhexanoate content is 0.2%, the gamma-methacryloxypropyltrimethoxysilane content is 0.2%, the 1-hydroxycyclohexyl phenyl ketone content is 0.1%, and the microcrystalline wax content is 1.5%.
The preparation method is the same as example 1.
Example 3: SCA optical cement with high filling property
The high-filling SCA optical cement comprises the following components in percentage by mass: the EVA resin content is 95%, the tert-butyl peroxy-2-ethylhexanoate content is 1%, the N- (2-aminoethyl) -3-aminopropyltrimethoxysilane content is 1%, the 1-hydroxycyclohexyl phenyl ketone and 2-hydroxy-2-methyl-1-phenyl-1-propanone (mass ratio is 2:1) content is 1%, and the microcrystalline wax content is 2%.
The preparation method is the same as example 1.
Example 4: SCA optical cement with high filling property
The high-filling SCA optical cement comprises the following components in percentage by mass: the content of EVA resin is 96%, the content of tert-butyl peroxy-2-ethylhexanoate is 0.5%, the content of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane is 0.5%, the content of 1-hydroxycyclohexyl phenyl ketone and 2-hydroxy-2-methyl-1-phenyl-1-acetone (mass ratio is 2:1) is 0.5%, and the content of microcrystalline wax is 2.5%.
The preparation method is the same as example 1.
The high-filling optical adhesive film prepared in the above examples can achieve 50% of step coverage, and the test results are shown in table 1 below. The high-filling optical adhesive films prepared in the examples are subjected to an environment resistance test according to the standard, the yellowing test data are averaged, and the test results are shown in the following table 2.
TABLE 1 Filability test
Figure BDA0003428447330000051
Table 1 segment coverage is 100% ink segment difference/adhesive layer thickness.
TABLE 2 environmental resistance test
Figure BDA0003428447330000052
As shown in tables 1 and 2, the high-filling optical cement prepared by the invention has excellent flow property, the coverage rate of the film segment difference can reach more than 50%, and the high-filling optical cement has excellent humidity resistance, heat resistance and aging resistance.

Claims (9)

1. A high-filling SCA optical cement comprises the following components in percentage by mass: 95-98% of EVA resin, 0.2-1% of cross-linking agent, 0.2-1% of coupling agent, 0.1-1% of photoinitiator and 1-3% of microcrystalline wax.
2. An SCA optical cement according to claim 1, characterized in that: the VA content of the EVA resin is 5-40%, and the MI is 10-400g/(10 min); preferably, the EVA resin has a VA content of 28-33% and an MI of 15-30 g/(10 min).
3. An SCA optical cement according to claim 1 or 2, characterized in that: the cross-linking agent is selected from one or more of tert-butyl peroxy-2-ethylhexanoate, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane, tert-amyl peroxy (2-ethylhexyl) carbonate and tert-butyl peroxy-2-ethylhexanoate.
4. An SCA optical cement according to any one of claims 1-3, characterized in that: the coupling agent is a silane coupling agent, and is specifically selected from one or a mixture of more of vinyl tri (methoxyethoxy) silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-methacryloxypropyl trimethoxy silane, N- (2-aminoethyl) -3-aminopropyl trimethoxy silane and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane.
5. An SCA optical cement according to any one of claims 1-4, characterized in that: the photoinitiator has light absorption capacity in an ultraviolet region (250-400 nm) or a visible light region (400-800 nm), and initiator molecules are transited from a ground state to an excited singlet state and transited from a system to an excited triplet state after directly or indirectly absorbing light energy; after the excited singlet or triplet state undergoes unimolecular or bimolecular chemical action, active fragments are generated which are capable of initiating the polymerization of the monomer.
6. An SCA optical cement according to claim 5, characterized in that: the photoinitiator is a composite photoinitiator and is one or a mixture of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, a photoinitiator TP0 and 4-phenyl benzophenone.
7. A process for the preparation of an SCA optical cement according to any one of claims 1 to 6, comprising the following steps:
1) uniformly mixing the EVA resin, the cross-linking agent, the coupling agent and the photoinitiator in proportion to obtain a mixed ingredient; preparing microcrystalline wax into powder, adding the powder into the mixed ingredients, and uniformly mixing again;
2) and (2) introducing the mixture prepared in the step 1) into a double-screw extruder, extruding the mixture at the tail end of the double-screw extruder through a melt pump, filtering and extruding the mixture through a screen, and calendering to form a film to obtain the SCA optical adhesive layer.
8. The method of claim 7, wherein: the method also comprises the step of attaching a layer of release film to the front surface and the back surface of the SCA optical adhesive layer respectively to prepare the SCA optical adhesive film.
9. Use of the SCA optical cement of any one of claims 1-6 in the preparation of a touch screen adhesive film.
CN202111588762.4A 2021-12-23 2021-12-23 High-filling-property SCA optical adhesive and preparation method and application thereof Pending CN114196353A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304332A (en) * 2011-08-25 2012-01-04 詹显光 Ultraviolet-ray-blocking and anti-aging ethylene-vinyl acetate (EVA) adhesive film and preparation method thereof
CN106366979A (en) * 2016-08-30 2017-02-01 陈广汉 Blue ray resistant OHA optical cement
CN107746693A (en) * 2017-09-28 2018-03-02 江苏斯瑞达新材料科技有限公司 Moisture-proof yellowing-resistant liquid optical clear adhesive and preparation method thereof
CN108164801A (en) * 2017-11-23 2018-06-15 广州鹿山新材料股份有限公司 A kind of no xanthochromia, UV mercury lamps curing EVA optical adhesive films and preparation method thereof of easily doing over again
CN111944455A (en) * 2020-07-07 2020-11-17 深圳市高仁电子新材料有限公司 High-weather-resistance blue-light-proof optical adhesive and film forming preparation method thereof
US20210230128A1 (en) * 2018-05-03 2021-07-29 Eutec New Materials Technology (Suzhou) Co., Ltd. Anti-blue light compound, preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304332A (en) * 2011-08-25 2012-01-04 詹显光 Ultraviolet-ray-blocking and anti-aging ethylene-vinyl acetate (EVA) adhesive film and preparation method thereof
CN106366979A (en) * 2016-08-30 2017-02-01 陈广汉 Blue ray resistant OHA optical cement
CN107746693A (en) * 2017-09-28 2018-03-02 江苏斯瑞达新材料科技有限公司 Moisture-proof yellowing-resistant liquid optical clear adhesive and preparation method thereof
CN108164801A (en) * 2017-11-23 2018-06-15 广州鹿山新材料股份有限公司 A kind of no xanthochromia, UV mercury lamps curing EVA optical adhesive films and preparation method thereof of easily doing over again
US20210230128A1 (en) * 2018-05-03 2021-07-29 Eutec New Materials Technology (Suzhou) Co., Ltd. Anti-blue light compound, preparation method and application thereof
CN111944455A (en) * 2020-07-07 2020-11-17 深圳市高仁电子新材料有限公司 High-weather-resistance blue-light-proof optical adhesive and film forming preparation method thereof

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