CN109096929B - Incompletely cured OCA optical cement with multilayer structure and preparation method thereof - Google Patents
Incompletely cured OCA optical cement with multilayer structure and preparation method thereof Download PDFInfo
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- CN109096929B CN109096929B CN201810700504.2A CN201810700504A CN109096929B CN 109096929 B CN109096929 B CN 109096929B CN 201810700504 A CN201810700504 A CN 201810700504A CN 109096929 B CN109096929 B CN 109096929B
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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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
- C09J7/403—Adhesives in the form of films or foils characterised by release liners characterised by the structure of the release feature
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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
- 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
Abstract
The invention discloses an incompletely cured OCA optical cement with a multilayer structure and a preparation method thereof. The invention is a product with low elastic rate, but has different physical properties, and has die cutting stability and environmental adaptability which are not possessed by a single-layer product in use and preservation; the invention also solves the problem of interface binding force among the multilayer OCAs, and ensures that the incompletely cured OCAs of the multilayer structure can not be layered and the like after being attached to an adherend before and after curing.
Description
Technical Field
The invention belongs to the technical field of optical cement, and particularly relates to incompletely cured OCA (optical clear adhesive) optical cement with a multilayer structure and a preparation method thereof.
Background
In a tsp (touch screen panel) assembly process recently applied to smart phones and tablet computers, a plurality of colors appear on a tempered glass cover plate, which causes the process of ink on the tempered glass to increase in the printing process, and the corresponding segment difference also increases. In order to overcome the increasing thickness of the ink step difference layer, a plurality of soft type OCA (optical clear adhesive) products are available on the market. Although the product can overcome the ink segment difference of the cover glass on the market, the OCA has a soft chemical structure, and other unstable physical characteristics can be caused in the using process.
In order to overcome the above problems, manufacturers like Mitsubishi plastics, 3M, TMS, etc. have introduced "incompletely cured" OCA products. Because of not curing type OCA completely in TSP assembly process, overcome the printing ink segment difference more easily, and then make the technology yields of equipment producer etc. to improve, and then more and more producers choose this not completely cured OCA product. The conventional process is to ship the incompletely cured and unstable-chemical-structure OCA product to an assembly manufacturer, and after the manufacturer assembles the TSP (after overcoming the printing step difference), add a post-curing process to ensure the stability of the physical properties. The method can easily overcome the ink segment difference (convenience of TSP assembly) and ensure the physical characteristics of the product. There are many incompletely cured OCAs on the market, for example: semi Liquid Type OCA and UV (Cure or curing) Type OCA; typical OCA products of this type are 3M 280X, Mitsubishi G6.2, and the like.
As early as 2013, the incompletely cured OCA was successfully developed by korean TMS corporation, and the post-curing process was required by the later assembly manufacturers by heating. Although the products do not need to be additionally provided with UV irradiation equipment by an assembly manufacturer, the products have some other disadvantages in practical application, such as easy flowing during long-distance transportation, seasonal variation and other external environmental factors, which cause the physical properties (curing degree) to change, thus making the TSP manufacturer difficult to set the production process standard and unstable the yield. Since 2015, post-UV irradiation process products began to emerge from incompletely cured OCAs, and once released for the most approval of TSP manufacturers, OCAs of this type have become mainstream and are becoming more prevalent in the TSP assembly market. The incompletely cured OCA is currently on the market, and due to its incompletely cured nature, care is particularly required during transportation and storage, as compared to the fully cured OCA that is already on the market. The incompletely cured OCA needs to be delivered with the following conditions: the extent of cure during shipment of the OCA product should remain stable with minimal die cutting stability. The OCA serving as the double-sided adhesive tape without the base material needs to be cut into the size required by a customer in the using process, and the important function of the good die cutting performance is the cohesive force of the adhesive. However, the incompletely cured OCA commonly found in the market is much poorer in cohesive force, so that the improvement of the die cutting performance of the incompletely cured OCA is a technical problem to be solved in the field.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an incompletely cured OCA optical cement with a multilayer structure and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a preparation method of incompletely cured OCA optical cement with a multilayer structure comprises the following steps:
the method comprises the following steps: preparation of OCA coating liquid
Preparing a monomer premix from 650 parts by weight of 2-ethylhexyl acrylate, 15 parts by weight of isobornyl acrylate, 20 parts by weight of 2-hydroxyethyl acrylate and 0.01 part by weight of 1-hydroxycyclohexyl benzophenone as a photoinitiator, and partially polymerizing the mixture by exposure to ultraviolet radiation under a nitrogen atmosphere to obtain a prepolymer having a viscosity of 300 cps; after the polymerization reaction, respectively adding 0.1%, 0.1% and 0.1% by mass of 1-hydroxycyclohexyl benzophenone, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate, stirring for 10 to 40 minutes, filtering with 480-mesh filter cloth, and vacuumizing for 20 to 60 minutes to obtain the OCA coating liquid;
step two: preparation of a fully cured first OCA layer
Pouring the OCA coating liquid between an upper release film and a lower release film, and irradiating and curing by UV light with the light quantity of 400mJ/cm2-800mJ/cm2 to obtain a completely cured first OCA layer, wherein the thickness of the first OCA layer is 50-250 mu m, and the curing time is 4-30 min;
step three: preparation of a second OCA layer that is not completely cured
Pouring the OCA coating liquid between an upper layer release film and a lower layer release film, and irradiating and curing the OCA coating liquid by UV light with the light quantity of 400mJ/cm2-800mJ/cm2 to obtain the second OCA layer which is not cured completely, wherein the thickness of the second OCA layer is 50-250 mu m, and the curing time is 1-30 min;
step four: and carrying out layer attachment on the first OCA layer and the second OCA layer to obtain the incompletely cured OCA optical cement with the multilayer structure.
Further, in the second step, the thickness of the first OCA layer is 50 μm, and the curing time is 8 min.
Further, in the third step, the thickness of the second OCA layer is 125 μm, and the curing time is 2 min.
Further, in step four, before carrying out the layer attached, first OCA layer with the surface that second OCA layer attached each other is through corona, plasma or primer treatment respectively.
The utility model provides a multilayer construction's not complete solidification type OCA optical cement, includes first OCA layer and second OCA layer, first OCA layer outside is pasted to have heavily from the type layer, second OCA layer outside is pasted to have lightly from the type layer.
The invention has the outstanding effects that: according to the incompletely cured OCA optical cement with a multilayer structure and the preparation method thereof, the completely cured first OCA layer and the incompletely cured second OCA layer are compounded, the incompletely cured second OCA layer is attached to cover glass, the filling of ink section difference is met, the whole cohesion is improved by the completely cured first OCA layer, and the excellent die cutting property is met to adapt to weather changes in all seasons and various problems in the transportation process. The invention is a product with low elastic rate, but has different physical properties, and has die cutting stability and environmental adaptability which are not possessed by a single-layer product in use and preservation; the invention also solves the problem of interface binding force among the multilayer OCAs, and ensures that the incompletely cured OCAs of the multilayer structure can not be layered and the like after being attached to an adherend before and after curing.
The following detailed description of the embodiments of the present invention is provided in connection with the accompanying drawings for the purpose of facilitating understanding and understanding of the technical solutions of the present invention.
Drawings
FIG. 1 is a schematic structural diagram of an incompletely cured OCA optical adhesive of multi-layer structure according to embodiments 1-3 of the present invention.
Detailed Description
The process of the present invention is illustrated below by means of specific examples, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
The preparation method of the incompletely cured OCA optical cement with a multilayer structure in the embodiment includes the following steps:
the method comprises the following steps: preparation of OCA coating liquid
Preparing a monomer premix from 650 parts by weight of 2-ethylhexyl acrylate, 15 parts by weight of isobornyl acrylate, 20 parts by weight of 2-hydroxyethyl acrylate and 0.01 part by weight of 1-hydroxycyclohexyl benzophenone as a photoinitiator, and partially polymerizing the mixture by exposure to ultraviolet radiation under a nitrogen atmosphere to obtain a prepolymer having a viscosity of 300 cps; after the polymerization reaction, adding 0.1%, 0.1% and 0.1% by mass of 1-hydroxycyclohexyl benzophenone, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate, stirring for 10 minutes, filtering with 480-mesh filter cloth, and vacuumizing for 20 minutes to obtain an OCA coating liquid;
step two: preparation of a fully cured first OCA layer
Pouring OCA coating liquid between the upper and lower release films, and controlling the light passing amount to be 400mJ/cm2The UV light is irradiated and cured to obtain a completely cured first OCA layer, the thickness of the first OCA layer is 50 microns, and the curing time is 8 min;
step three: preparation of a second OCA layer that is not completely cured
Pouring OCA coating liquid between the upper and lower release films, and passing light with a light quantity of 400mJ/cm2The UV light is irradiated and cured to obtain a second OCA layer which is not completely cured, the thickness of the second OCA layer is 50 mu m, and the curing time is 1 min;
step four: and carrying out layer attachment on the first OCA layer and the second OCA layer to obtain the incompletely cured OCA optical cement with a multilayer structure.
In step four, before carrying out the layer attached, the surface that first OCA layer and second OCA layer attached each other is through corona treatment respectively.
As shown in fig. 1, the incompletely cured OCA optical cement with a multilayer structure of the present embodiment includes a first OCA layer 1 and a second OCA layer 2, a heavy release layer 3 is attached to the outer side of the first OCA layer 1, and a light release layer 4 is attached to the outer side of the second OCA layer 2.
Example 2
The preparation method of the incompletely cured OCA optical cement with a multilayer structure in the embodiment includes the following steps:
the method comprises the following steps: preparation of OCA coating liquid
Preparing a monomer premix from 650 parts by weight of 2-ethylhexyl acrylate, 15 parts by weight of isobornyl acrylate, 20 parts by weight of 2-hydroxyethyl acrylate and 0.01 part by weight of 1-hydroxycyclohexyl benzophenone as a photoinitiator, and partially polymerizing the mixture by exposure to ultraviolet radiation under a nitrogen atmosphere to obtain a prepolymer having a viscosity of 300 cps; after the polymerization reaction, adding 0.1%, 0.1% and 0.1% by mass of 1-hydroxycyclohexyl benzophenone, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate, stirring for 40 minutes, filtering with 480-mesh filter cloth, and vacuumizing for 60 minutes to obtain an OCA coating liquid;
step two: preparation of a fully cured first OCA layer
Pouring OCA coating liquid between the upper and lower release films, and controlling the light passing amount to be 800mJ/cm2The UV light is irradiated and cured to obtain a completely cured first OCA layer, the thickness of the first OCA layer is 250 micrometers, and the curing time is 30 min;
step three: preparation of a second OCA layer that is not completely cured
Pouring OCA coating liquid between the upper and lower release films, and passing light amount of 800mJ/cm2The UV light is irradiated and cured to obtain a second OCA layer which is not completely cured, the thickness of the second OCA layer is 250 micrometers, and the curing time is 30 min;
step four: and carrying out layer attachment on the first OCA layer and the second OCA layer to obtain the incompletely cured OCA optical cement with a multilayer structure.
In the fourth step, before the layer attaching, the surfaces of the first OCA layer and the second OCA layer attached to each other are respectively subjected to plasma treatment.
As shown in fig. 1, the incompletely cured OCA optical cement with a multilayer structure of the present embodiment includes a first OCA layer 1 and a second OCA layer 2, a heavy release layer 3 is attached to the outer side of the first OCA layer 1, and a light release layer 4 is attached to the outer side of the second OCA layer 2.
Example 3
The preparation method of the incompletely cured OCA optical cement with a multilayer structure in the embodiment includes the following steps:
the method comprises the following steps: preparation of OCA coating liquid
Preparing a monomer premix from 650 parts by weight of 2-ethylhexyl acrylate, 15 parts by weight of isobornyl acrylate, 20 parts by weight of 2-hydroxyethyl acrylate and 0.01 part by weight of 1-hydroxycyclohexyl benzophenone as a photoinitiator, and partially polymerizing the mixture by exposure to ultraviolet radiation under a nitrogen atmosphere to obtain a prepolymer having a viscosity of 300 cps; after the polymerization reaction, adding 0.1%, 0.1% and 0.1% by mass of 1-hydroxycyclohexyl benzophenone, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate, stirring for 30 minutes, filtering with 480-mesh filter cloth, and vacuumizing for 50 minutes to obtain an OCA coating liquid;
step two: preparation of a fully cured first OCA layer
Pouring OCA coating liquid between the upper and lower release films, and controlling the light passing amount to be 600mJ/cm2The UV light is irradiated and cured to obtain a completely cured first OCA layer, the thickness of the first OCA layer is 100 microns, and the curing time is 4 min;
step three: preparation of a second OCA layer that is not completely cured
Pouring OCA coating liquid between the upper and lower release films, and allowing the light to pass through the release films at a rate of 600mJ/cm2The UV light is irradiated and cured to obtain a second OCA layer which is not completely cured, the thickness of the second OCA layer is 125 mu m, and the curing time is 2 min;
step four: and carrying out layer attachment on the first OCA layer and the second OCA layer to obtain the incompletely cured OCA optical cement with a multilayer structure.
In the fourth step, before the layer is attached, the surfaces of the first OCA layer and the second OCA layer which are attached to each other are respectively treated by primer.
As shown in fig. 1, the incompletely cured OCA optical cement with a multilayer structure of the present embodiment includes a first OCA layer 1 and a second OCA layer 2, a heavy release layer 3 is attached to the outer side of the first OCA layer 1, and a light release layer 4 is attached to the outer side of the second OCA layer 2.
In examples 1 to 3 of the present invention, a polymer was produced by bulk polymerization, and then a reaction additive was added to prepare an OCA coating liquid, and then the coating liquid was crosslinked and cured by UV irradiation to adjust the degree of curing by a method of adjusting brightness. The preparation method does not use solvent, is environment-friendly and has simple process. By utilizing the method, the incompletely cured OCA can be prepared by adjusting the illumination intensity and brightness of UV equipment, but the incompletely cured OCA prepared by the method has great defects in cohesive force, so that the OCA product has problems in die cutting, and the problems are solved by adopting a product structure with a multilayer structure in order to improve the die cutting processability.
The invention has various embodiments, and all technical solutions formed by adopting equivalent transformation or equivalent transformation are within the protection scope of the invention.
Claims (5)
1. A preparation method of incompletely cured OCA optical cement with a multilayer structure is characterized by comprising the following steps:
the method comprises the following steps: preparation of OCA coating liquid
Preparing a monomer premix from 650 parts by weight of 2-ethylhexyl acrylate, 15 parts by weight of isobornyl acrylate, 20 parts by weight of 2-hydroxyethyl acrylate and 0.01 part by weight of 1-hydroxycyclohexyl benzophenone as a photoinitiator, and partially polymerizing the mixture by exposure to ultraviolet radiation under a nitrogen atmosphere to obtain a prepolymer having a viscosity of 300 cps; after the polymerization reaction, respectively adding 0.1%, 0.1% and 0.1% by mass of 1-hydroxycyclohexyl benzophenone, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate, stirring for 10 to 40 minutes, filtering with 480-mesh filter cloth, and vacuumizing for 20 to 60 minutes to obtain the OCA coating liquid;
step two: preparation of a fully cured first OCA layer
Pouring the OCA coating liquid between an upper release film and a lower release film, wherein the light passing amount is 400mJ/cm2-800mJ/cm2The first OCA layer is completely cured by UV light irradiation, the thickness of the first OCA layer is 50-250 μm, and the curing time is 4-30 min;
step three: preparation of a second OCA layer that is not completely cured
Pouring the OCA coating liquid between an upper release film and a lower release film, wherein the light passing amount is 400mJ/cm2-800mJ/cm2The second OCA layer which is not completely cured is obtained by UV light irradiation curing, the thickness of the second OCA layer is 50-250 μm, and the curing time is 1-2 min;
step four: and carrying out layer attachment on the first OCA layer and the second OCA layer to obtain the incompletely cured OCA optical cement with the multilayer structure.
2. The method for preparing the incompletely cured OCA optical cement with a multi-layer structure according to claim 1, wherein the method comprises the following steps: in the second step, the thickness of the first OCA layer is 50 μm, and the curing time is 8 min.
3. The method for preparing the incompletely cured OCA optical cement with a multi-layer structure according to claim 1, wherein the method comprises the following steps: in the third step, the thickness of the second OCA layer is 125 μm, and the curing time is 2 min.
4. The method for preparing the incompletely cured OCA optical cement with a multi-layer structure according to claim 1, wherein the method comprises the following steps: in step four, before carrying out the layer attached, first OCA layer with the surface that second OCA layer attached to each other is through corona, plasma or priming paint processing respectively.
5. The incompletely cured OCA optical cement with a multilayer structure is characterized in that: including first OCA layer and second OCA layer of claim 1, first OCA layer outside is attached with heavy release layer, second OCA layer outside is attached with light release layer.
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| CN110305589A (en) * | 2019-07-23 | 2019-10-08 | 新纶科技（常州）有限公司 | A kind of acrylate adhesive of UV type water boiling resistance and its preparation method of adhesive tape |
| CN110481047B (en) * | 2019-08-20 | 2020-07-21 | 太仓展新胶粘材料股份有限公司 | Hob die cutting system and method for OCA optical cement with four-layer 1:1 structure |
| CN114836138B (en) * | 2022-03-28 | 2023-11-10 | 南方科技大学 | Super elastic glue, preparation method and application |
| CN114958241A (en) * | 2022-07-29 | 2022-08-30 | 江苏日久光电股份有限公司 | Optical film |
| CN115537124B (en) * | 2022-09-28 | 2024-04-05 | 新纶电子材料(常州)有限公司 | Post-curable optical adhesive, OCA optical adhesive and preparation method thereof |
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| JPH05105852A (en) * | 1991-10-14 | 1993-04-27 | Sekisui Chem Co Ltd | Double-coated self-adhesive tape and its production |
| JP4467388B2 (en) * | 2004-09-07 | 2010-05-26 | 三洋電機株式会社 | COMPOUND LENS, COMPOSITE LENS MANUFACTURING METHOD, AND LENS MODULE |
| KR101928727B1 (en) * | 2011-10-24 | 2018-12-13 | 오지 홀딩스 가부시키가이샤 | Pressure-sensitive adhesive sheet, method for using same, and laminate |
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| US9443751B2 (en) * | 2012-09-24 | 2016-09-13 | Lintec Corporation | Back grinding sheet |
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