WO2017010501A1 - Feuille adhésive, stratifié, et leur procédé de production - Google Patents

Feuille adhésive, stratifié, et leur procédé de production Download PDF

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Publication number
WO2017010501A1
WO2017010501A1 PCT/JP2016/070648 JP2016070648W WO2017010501A1 WO 2017010501 A1 WO2017010501 A1 WO 2017010501A1 JP 2016070648 W JP2016070648 W JP 2016070648W WO 2017010501 A1 WO2017010501 A1 WO 2017010501A1
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Prior art keywords
pressure
sensitive adhesive
adhesive sheet
monomer
meth
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PCT/JP2016/070648
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English (en)
Japanese (ja)
Inventor
山本　真之
苑平 郭
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王子ホールディングス株式会社
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Priority to JP2017528699A priority Critical patent/JPWO2017010501A1/ja
Publication of WO2017010501A1 publication Critical patent/WO2017010501A1/fr

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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
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • 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

Definitions

  • the present invention relates to a pressure-sensitive adhesive sheet and laminate suitable for bonding a pair of optical members, and a method for manufacturing the same.
  • display device modules such as a liquid crystal display (LCD) and input device modules such as a touch panel have been widely used in various fields.
  • LCD liquid crystal display
  • input device modules such as a touch panel
  • a transparent double-sided pressure-sensitive adhesive sheet is used for the purpose of bonding optical members.
  • a transparent double-sided pressure-sensitive adhesive sheet is also used for bonding the display device module and the input device module (for example, Patent Documents 1 to 3).
  • LCD liquid crystal display
  • various optical films and optical members have been developed.
  • miniaturization and thinning of LCDs have progressed, and it has been considered to reduce the thickness of an optical film constituting the LCD.
  • thinning of the LCD it is also required to reduce the thickness of a double-sided pressure-sensitive adhesive sheet used for bonding optical films constituting the LCD (for example, Patent Document 4).
  • the present inventors provide a pressure-sensitive adhesive sheet that is excellent in handling properties when bonding an optical film or the like, and is made into a thin film, in order to solve the problems of the conventional technology.
  • the study was advanced for the purpose.
  • the present inventors have used a pressure-sensitive adhesive sheet composed of a dual-cure pressure-sensitive adhesive containing a specific component for bonding optical films and the like.
  • the inventors have found that the pressure-sensitive adhesive sheet can be made thinner.
  • the present inventors have found that even a pressure-sensitive adhesive sheet having such a thin film can maintain good adhesion and durability, and have completed the present invention.
  • the present invention has the following configuration.
  • [5] A method for producing a laminate comprising a step of bringing the pressure-sensitive adhesive sheet according to any one of [1] to [4] into contact with the surface of an adherend and heating in that state or irradiating active energy rays.
  • [6] A laminate produced by the method according to [5].
  • [7] The laminate according to [6], which has optical members on both surfaces of the pressure-sensitive adhesive sheet.
  • the pressure-sensitive adhesive sheet can be formed into a thin film by forming the pressure-sensitive adhesive sheet from a dual-cure pressure-sensitive adhesive containing a specific component.
  • a pressure-sensitive adhesive sheet is preferably used, for example, when a pair of optical films and the like are bonded, and can exhibit good adhesiveness and durability.
  • FIG. 1 is a cross-sectional view showing a laminate as an embodiment of the present invention.
  • a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
  • the pressure-sensitive adhesive sheet of the present invention comprises a base polymer (A) containing a non-crosslinkable (meth) acrylic acid ester unit (a1) and an acrylic monomer unit (a2) having a crosslinkable functional group, and a polymerizable unsaturated group.
  • a pressure-sensitive adhesive composition containing the agent (D) and the solvent (E) is included and includes a pressure-sensitive adhesive that is semi-cured by heating or irradiation with active energy rays.
  • the thickness of the pressure-sensitive adhesive sheet of the present invention is 1 to 10 ⁇ m.
  • the pressure-sensitive adhesive sheet of the present invention comprises a non-crosslinkable (meth) acrylic acid ester unit (a1) and a base polymer (A) containing an acrylic monomer unit (a2) having a crosslinkable functional group, and a polymerizable unsaturated group.
  • a pressure-sensitive adhesive composition containing (D) and a solvent (E) contains a pressure-sensitive adhesive that is semi-cured by heating or irradiation with active energy rays, and the pressure-sensitive adhesive sheet exhibits a soft semi-cured state.
  • the semi-cured state means that the gel fraction is less than 20%, and the gel fraction may be less than 15% or less than 10%.
  • the pressure-sensitive adhesive sheet of the present invention exhibits semi-curability, but the pressure-sensitive adhesive sheet is completely cured by applying heat or active energy rays after the pressure-sensitive adhesive sheet is bonded to the adherend surface. That is, the pressure-sensitive adhesive sheet of the present invention is in a state where it is semi-cured only by heating or irradiation with active energy rays before bonding, but is completely cured by heating or active energy rays after bonding.
  • the same method may be sufficient as the hardening method in a semi-hardening process and a complete hardening process, it is preferable to harden
  • thermosetting when heat curing is performed in the semi-curing process, it is preferable to irradiate active energy rays in the complete curing process, and when active energy rays are irradiated in the semi-curing process, It is preferable to perform thermosetting.
  • such a two-stage-cured pressure-sensitive adhesive sheet may be referred to as a dual-cure pressure-sensitive adhesive sheet.
  • the “semi-cured state” means a state in which one of heat and active energy rays is cured, and means a soft state before the second stage curing.
  • the “fully cured state” means a state where the semi-cured adhesive sheet is cured by heating or irradiating with active energy rays.
  • the storage elastic modulus of the dynamic viscoelasticity measured by shear stress or tensile stress at a frequency of 1 Hz is at least Tg (glass transition point). ) 1.5 times or more in the range from higher temperature to 60 ° C.
  • the dynamic viscoelasticity is preferably 1.5 to 1000 times, and more preferably 2 to 100 times.
  • the storage elastic modulus of dynamic viscoelasticity measured by shear stress or tensile stress at 1 Hz frequency of the pressure-sensitive adhesive constituting the pressure-sensitive adhesive sheet in the semi-cured state in the present invention is a temperature region higher than Tg (glass transition point) or 50 It is preferably 1.0 ⁇ 10 6 Pa or less, more preferably 8.0 ⁇ 10 5 Pa or less, and even more preferably 5.0 ⁇ 10 5 Pa or less in the region of 0 ° C. or higher.
  • the thickness of the pressure-sensitive adhesive sheet may be 1 to 10 ⁇ m, preferably 2 to 8 ⁇ m, and more preferably 3 to 7 ⁇ m. Even when the pressure-sensitive adhesive sheet of the present invention is thinned so as to be within the above range, excellent adhesiveness and durability can be maintained over a long period of time.
  • the distance of displacement after 60 minutes, measured according to the holding power measurement method of JIS Z0237, is preferably 10 mm or more, more preferably 20 mm or more, by pressure-bonding the adhesive sheet to a SUS plate.
  • difference mentioned above is the adhesive sheet of the state before irradiating an active energy ray to an adhesive sheet, Comprising: It is a measured value in the adhesive sheet of a semi-hardened state.
  • the distance of deviation after 60 minutes measured according to the holding power measurement method of JIS Z0237 is It is preferably less than 10 mm.
  • the pressure-sensitive adhesive constituting the pressure-sensitive adhesive sheet aggregates after the second-stage curing, and exhibits strong adhesiveness. By setting it as such a structure, a pressure sensitive adhesive sheet can be made into a thin film and, after complete curing, good adhesiveness and durability are exhibited.
  • the Young's modulus of the pressure-sensitive adhesive sheet may be 0.01 to 0.30 N / mm 2 or 0.03 to 0.20 N / mm 2 . If the Young's modulus is within the above range, the semi-cured adhesive sheet tends to have a desirable hardness. In addition, Young's modulus can be made into a desired range by adjusting the addition amount etc. of the monomer mentioned later.
  • the Young's modulus in this specification is a value obtained from a stress-strain diagram measured using Shimadzu Corporation Autograph AGS-X at a pulling speed of 10 (mm / min).
  • the pressure-sensitive adhesive sheet of the present invention may be a single-sided pressure-sensitive adhesive sheet or a double-sided pressure-sensitive adhesive sheet, but is preferably a double-sided pressure-sensitive adhesive sheet.
  • a single-sided adhesive sheet the multilayer sheet which laminated
  • the double-sided pressure-sensitive adhesive sheet include a single-layer sheet comprising only a pressure-sensitive adhesive sheet, a multilayer pressure-sensitive adhesive sheet in which a plurality of pressure-sensitive adhesive layers are laminated, and a multilayer sheet in which pressure-sensitive adhesive layers are laminated on both sides of a support.
  • the pressure-sensitive adhesive composition comprises a base polymer (A) containing a non-crosslinkable (meth) acrylic acid ester unit (a1) and an acrylic monomer unit (a2) having a crosslinkable functional group, and a polymerizable unsaturated group.
  • A a base polymer
  • A1 a non-crosslinkable acrylic acid ester unit
  • a2 acrylic monomer unit
  • a2 a polymerizable unsaturated group
  • At least one monomer (B), a crosslinking agent (C) that reacts with the base polymer (A) by heat, and a polymerization initiator that initiates the polymerization reaction of the monomer (B) by irradiation with active energy rays (D) and a solvent (E) are contained.
  • the monomer (B) in the pressure-sensitive adhesive composition may have a vapor pressure at 25 ° C. of 300 Pa or less, and the surface tension of the solvent (E) at 25 ° C. should be 20 mN / m or more and less than 40 mN / m. Can do.
  • the coating suitability at the time of producing an adhesive sheet improves, and when an adhesive composition is applied and thermosetted, an adhesive sheet with a smooth surface can be formed. This is considered to be due to the following reason.
  • First, by containing the solvent (E), the problem that the end portion becomes thick during coating when the pressure-sensitive adhesive sheet is produced is less likely to occur.
  • the concentration of the solvent (E), which is likely to cause popping, is low by containing the monomer (B) that functions as a liquid medium for reducing the viscosity of the coating agent. It can be suppressed.
  • the solvent (E) selectively evaporates, but the rapid increase in the surface tension of the coating film is suppressed by containing the monomer (B) that is difficult to volatilize.
  • the selective evaporation of the solvent (E) increases the viscosity as the solid content concentration in the pressure-sensitive adhesive sheet increases, and the flow of the substance in the pressure-sensitive adhesive sheet is suppressed. It is considered that the synergistic action of these can suppress production problems such as the occurrence of thick end portions and side walls, and can form an adhesive sheet having a smooth surface.
  • the monomer (B) and the solvent (E) in the pressure-sensitive adhesive composition may satisfy at least one or all of the following conditions (1) and (2).
  • fusing point of a monomer (B) is 25 degrees C or less.
  • (2) The solvent (E) does not have a polymerizable unsaturated group and has a higher vapor pressure at 25 ° C. than the monomer (B).
  • the solvent (E) should have a difference in solubility parameter between the solvent (E) and the monomer (B) within 2 [(cal / cm 3 ) 1/2 ]. Can do. Thereby, the coating suitability at the time of producing an adhesive sheet improves, and when an adhesive composition is applied and thermosetted, an adhesive sheet with a smooth surface can be formed. This is considered to be due to the following reason. First, by containing the solvent (E), it is difficult to cause a coating defect in which the end portion becomes thick during coating when the pressure-sensitive adhesive sheet is produced. Further, when the difference in solubility parameter between the solvent (E) and the monomer (B) is within 2 [(cal / cm 3 ) 1/2 ], the adhesive composition is thermally cured.
  • the solvent (E) does not have a polymerizable unsaturated group, and the surface tension at 25 ° C. may be 20 mN / m or more and less than 40 mN / m. That is, in the pressure-sensitive adhesive composition, the monomer (B) has a vapor pressure at 25 ° C. of 300 Pa or less, and the surface tension at 25 ° C. of the solvent (E) is 20 mN / m or more and less than 40 mN / m, Furthermore, the solvent (E) may be composed of a solvent having a solubility parameter difference within 2 [(cal / cm 3 ) 1/2 ] with respect to the monomer (B).
  • the pressure-sensitive adhesive composition contains a non-crosslinkable (meth) acrylic acid ester unit (a1) and an acrylic monomer unit (a2) having a crosslinkable functional group as the base polymer (A).
  • the “unit” is a repeating unit (monomer unit) constituting the polymer.
  • the non-crosslinkable (meth) acrylic acid ester unit (a1) is derived from a (meth) acrylic acid alkyl ester.
  • (meth) acrylic acid alkyl esters include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, (meth) Isobutyl acrylate, t-butyl (meth) acrylate, n-pentyl (meth) acrylate, n-hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, ( Isooctyl (meth) acrylate, n-nonyl (meth) acrylate, isononyl (meth) acrylate, n-decyl
  • (meth) acrylate means containing both “acrylate” and “methacrylate”
  • (meth) acrylic acid means “acrylic acid” and “methacrylic acid”. Is meant to include both.
  • Examples of the acrylic monomer unit (a2) having a crosslinkable functional group include a hydroxy group-containing monomer unit, an amino group-containing monomer unit, a glycidyl group-containing monomer unit, and a carboxy group-containing monomer unit. It is done. These monomer units may be one type or two or more types.
  • the ratio of the carboxy group-containing monomer unit contained in the acrylic monomer unit (a2) may be 1% by mass or less based on the total mass of the acrylic monomer unit (a2). It may be less than or equal to 0% by mass or 0% by mass.
  • the hydroxy group-containing monomer unit is derived from a hydroxy group-containing monomer.
  • the hydroxy group-containing monomer include hydroxyalkyl (meth) acrylates such as 2-hydroxyethyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, (Meth) acrylic acid lactones such as (meth) acrylic acid mono (diethylene glycol) (meth) acrylic acid [(mono, di or poly) alkylene glycol] and (meth) acrylic acid monocaprolactone.
  • the amino group-containing monomer unit include those derived from amino group-containing monomers such as (meth) acrylamide and allylamine.
  • Examples of the glycidyl group-containing monomer unit include those derived from glycidyl group-containing monomers such as glycidyl (meth) acrylate.
  • Examples of the carboxy group-containing monomer unit include those derived from acrylic acid and methacrylic acid.
  • the content of the crosslinkable acrylic monomer unit (a2) in the base polymer (A) may be 0.01 to 20% by mass, may be 0.5 to 15% by mass, It may be 10% by mass. If the content of the crosslinkable acrylic monomer unit (a2) is not less than the above lower limit value, it has sufficient crosslinkability necessary to maintain a semi-cured state, and if not more than the above upper limit value, Necessary adhesion can be maintained.
  • the base polymer (A) has a monomer unit other than the non-crosslinkable (meth) acrylic acid ester unit (a1) and the acrylic monomer unit (a2) having a crosslinkable functional group, if necessary. May be.
  • the other monomer may be any one that can be copolymerized with a non-crosslinkable (meth) acrylic acid ester and an acrylic monomer having a crosslinkable functional group.
  • (meth) acrylonitrile, vinyl acetate, styrene examples include vinyl chloride, vinyl pyrrolidone, and vinyl pyridine.
  • the content of other monomer units in the base polymer (A) may be 0 to 20% by mass or 0 to 15% by mass.
  • the weight average molecular weight of the base polymer (A) can be 100,000 to 2,000,000, and may be 300,000 to 1,500,000.
  • the weight average molecular weight of a base polymer (A) is a value before bridge
  • the weight average molecular weight is a value determined by size exclusion chromatography (SEC) and determined on a polystyrene basis.
  • SEC size exclusion chromatography
  • the monomer (B) contains at least one of a monofunctional monomer (B1) having at least one polymerizable unsaturated group and a polyfunctional monomer (B2) having two or more polymerizable unsaturated groups. May be.
  • the polymerizable unsaturated group include a group containing an ethylenic double bond, and examples thereof include a (meth) acryloyl group and a vinyl group.
  • the monomer (B) may contain either the monofunctional monomer (B1) or the polyfunctional monomer (B2).
  • the monofunctional monomer (B1) and the polyfunctional monomer Both of (B2) may be included.
  • thermosetting pressure-sensitive adhesive sheet By containing the monomer (B), when the pressure-sensitive adhesive composition is heat-cured in the first stage (semi-curing step), the thermosetting pressure-sensitive adhesive sheet is in a semi-cured state and is cured with active energy rays. Can have sex. When the pressure-sensitive adhesive composition is cured by irradiation with active energy rays in the first stage, the pressure-sensitive adhesive sheet is in a semi-cured state and has thermosetting properties. In addition, in this invention, after making it harden
  • the monomer (B) one having a vapor pressure at 25 ° C. of 300 Pa or less may be used.
  • the vapor pressure at 25 ° C. of the monomer (B) may be 200 Pa or less, or 100 Pa or less.
  • the lower limit of the vapor pressure is not particularly limited in terms of the coating suitability of the pressure-sensitive adhesive composition.
  • the vapor pressure of the monomer (B) can be measured according to JIS-K2258 “Crude oil and fuel oil—Vapor pressure test method—Reed method” and the like, for example, http: // www. chemspider.
  • the predicted value can be obtained by a website such as com / or software such as ACD / PhysChem Suite.
  • the melting point of the monomer (B) may be 25 ° C. or lower. Thereby, transparency (haze etc.) etc. of the adhesive sheet formed improve. Further, the melting point of the monomer (B) may be 20 ° C. or less, or 15 ° C. or less. The lower limit of the melting point is not particularly limited.
  • the melting point of the monomer (B) can be measured according to JIS K 0064: 1992 “Measuring method of melting point and melting range of chemical product”.
  • a monomer having an alkyl group with a chain length of 10 or more or a monomer having a polycyclic structure is used as the monomer (B), a more excellent holding force can be exhibited after complete curing. Can do.
  • the monomer as described above promotes the entanglement of the monomer and the base polymer. Thereby, it is thought that an adhesive composition is hardened
  • Examples of the monomer having an alkyl group having 10 or more chain length atoms include alkyl acrylates having an alkyl group having 10 or more chain length atoms. As long as the alkyl group has 10 or more chain-length atoms, it may have a side chain or a substituent. Examples of such side chains and substituents include alkyl groups. The number of chain length atoms of the alkyl group may be 10 to 27, 10 to 25, or 15 to 22. Isostearyl acrylate can be mentioned as a particularly preferred alkyl acrylate from the viewpoint of holding power.
  • the monomer having a polycyclic structure may be a polycyclic aliphatic monomer or a polycyclic aromatic monomer.
  • polycyclic structure examples include a bicyclo structure and a tricyclo structure.
  • a substituent such as an alkyl group may be bonded to these polycyclic structures.
  • Specific examples of the polycyclic structure include a norbornene ring and an adamantane ring.
  • monofunctional monomer (B1) examples include pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, and n-octyl (meth) acrylate.
  • the monofunctional monomer (B1) is preferably lauryl (meth) acrylate.
  • polyfunctional monomer (B2) examples include ethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, 1,3-butylene glycol di (meth) acrylate, and di (meth) acryl. 1,4-butylene glycol acid, 1,9-nonanediol di (meth) acrylate, 1,6-hexanediol diacrylate, polybutylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, Tetraethylene glycol di (meth) acrylate, tripropylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, tetra ( Many such as (meth) acrylic acid pentaerythritol (Meth) acrylic acid esters of alcohols, and
  • the monomer (B) may not have a functional group that is reactive with the functional group of the acrylic monomer unit (a2).
  • the monomer (B) may have the same functional group (for example, a hydroxy group) as the acrylic monomer unit (a2) or may not have a functional group.
  • the monomer (B) is a monofunctional monomer (B1) or a polyfunctional monomer (B2) alone, or a monofunctional monomer (B1) and / or a polyfunctional monomer ( Two or more types of B2) may be used in combination.
  • the content of the monomer (B) is appropriately selected according to the composition, molecular weight, crosslinking density, etc. of the base polymer (A), and is not particularly limited, but 100 parts by mass of the base polymer (A) On the other hand, it can be 5 to 150 parts by mass, 10 to 120 parts by mass, or 15 to 90 parts by mass. Further, the content of the monomer (B) may be 1 to 60% by mass, 2 to 50% by mass, or 5 to 35% by mass with respect to the total mass of the pressure-sensitive adhesive composition. It may be.
  • the monomer (B) contains both the monofunctional monomer (B1) and the polyfunctional monomer (B2), it is appropriately selected according to the composition, molecular weight, crosslinking density, etc. of the polymer (A).
  • the monofunctional monomer (B1) can be 4 to 120 parts by mass, 8 to 100 parts by mass with respect to 100 parts by mass of the base polymer (A), It can be -80 mass parts.
  • the polyfunctional monomer (B2) can be 1 to 30 parts by mass, 2 to 20 parts by mass, or 3 to 10 parts by mass.
  • the mass ratio of the monofunctional monomer (B1) to the polyfunctional monomer (B2) can be 2: 1, 3: 1, or 5: 1.
  • Cross-linking agent (C) examples include cross-linkable functional groups possessed by the base polymer (A) among known cross-linking agents such as isocyanate compounds, epoxy compounds, oxazoline compounds, aziridine compounds, metal chelate compounds and butylated melamine compounds. Can be selected as appropriate in consideration of the reactivity. For example, when a hydroxy group is included as a crosslinkable functional group, an isocyanate compound can be used from the reactivity of the hydroxy group. From the viewpoint that the acrylic monomer unit (a2) having a crosslinkable functional group can be easily crosslinked, an isocyanate compound and an epoxy compound can be used.
  • Examples of the isocyanate compound include tolylene diisocyanate, xylylene diisocyanate, hexamethylene diisocyanate, and isophorone diisocyanate.
  • Examples of the epoxy compound include ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, propylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, glycerin diglycidyl ether, neopentyl glycol diglycidyl ether, and 1,6-hexanediol diester.
  • Glycidyl ether tetraglycidyl xylenediamine, 1,3-bis (N, N-diglycidylaminomethyl) cyclohexane, trimethylolpropane polyglycidyl ether, diglycerol polyglycidyl ether, polyglycerol polyglycidyl ether, sorbitol polyglycidyl ether, etc. Can be mentioned.
  • crosslinking agent (C) 1 type may be used independently or 2 or more types may be used together.
  • the content of the crosslinking agent (C) is appropriately selected according to the desired adhesive properties and the like, and is not particularly limited, but is 0.01 to 5 with respect to 100 parts by mass of the base polymer (A). The mass may be 0.03 to 3 parts by mass.
  • the content of the crosslinking agent (C) can be 0.01 to 5.0% by mass and 0.02 to 2.0% by mass with respect to the total mass of the pressure-sensitive adhesive composition. it can.
  • any polymerization initiator may be used as long as it can initiate the polymerization reaction of the monomer (B) by irradiation with active energy rays.
  • active energy rays mean those having energy quanta among electromagnetic waves or charged particle beams, and examples include ultraviolet rays, electron beams, visible rays, X-rays, ion rays and the like. Among these, from the viewpoint of versatility, ultraviolet rays or electron beams are preferable, and ultraviolet rays are particularly preferable.
  • Examples of the polymerization initiator (D) include acetophenone-based initiators, benzoin ether-based initiators, benzophenone-based initiators, hydroxyalkylphenone-based initiators, thioxanthone-based initiators, and amine-based initiators.
  • Specific examples of the acetophenone initiator include diethoxyacetophenone and benzyldimethyl ketal.
  • Specific examples of the benzoin ether initiator include benzoin and benzoin methyl ether.
  • Specific examples of the benzophenone initiator include benzophenone and methyl o-benzoylbenzoate.
  • Specific examples of the hydroxyalkylphenone initiator include 1-hydroxy-cyclohexyl-phenyl-ketone and the like.
  • thioxanthone initiator examples include 2-isopropylthioxanthone and 2,4-dimethylthioxanthone.
  • amine initiator examples include triethanolamine and ethyl 4-dimethylbenzoate.
  • the polymerization initiator (D) one type may be used alone, or two or more types may be used in combination.
  • the content of the polymerization initiator (D) is appropriately selected according to the content of the monomer (B), the irradiation amount of active energy rays when semi-cured or completely cured, and the like. Although not limited, it can be 0.05 to 10% by mass and 0.1 to 5.0% by mass with respect to the total mass of the monomer (B).
  • the content of the polymerization initiator (D) can be 0.1 to 10 parts by mass with respect to 100 parts by mass of the base polymer (A), and can be 1 to 5 parts by mass.
  • the solvent (E) is used for improving the coating suitability of the pressure-sensitive adhesive composition.
  • a solvent (E) include hydrocarbons such as hexane, heptane, octane, toluene, xylene, ethylbenzene, cyclohexane, and methylcyclohexane; halogenated hydrocarbons such as dichloromethane, trichloroethane, trichloroethylene, tetrachloroethylene, and dichloropropane.
  • Alcohols such as methanol, ethanol, propanol, isopropyl alcohol, butanol, isobutyl alcohol and diacetone alcohol; ethers such as diethyl ether, diisopropyl ether, dioxane and tetrahydrofuran; acetone, methyl ethyl ketone, methyl isobutyl ketone, isophorone and cyclohexanone Ketones; methyl acetate, ethyl acetate, butyl acetate, isobutyl acetate, amyl acetate, ethyl butyrate Esters; ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monomethyl ether acetate, propylene glycol monomethyl ether, propylene glycol monoethyl ether, polyols and derivatives thereof such as propylene glycol monomethyl ether acetate.
  • ethers such as die
  • the solvent (E) examples include a solvent having no polymerizable unsaturated group and having a higher vapor pressure at 25 ° C. than that of the monomer (B). Since the larger the difference in vapor pressure between the monomer (B) and the solvent (E), the fewer the coating defects and the easier the production, the vapor pressure of the solvent (E) can be 2000 Pa or higher. This can be done. Although an upper limit is not specifically limited, It is 50000 Pa or less practically.
  • the vapor pressure of the solvent (E) can be measured according to JIS-K2258-2 “Crude oil and petroleum products—Determination of vapor pressure—Part 2: Three-time expansion method”, for example, http: // www. chemspider. com / and software such as ACD / PhysChem Suite.
  • Solvents that have no polymerizable unsaturated groups and have a higher vapor pressure at 25 ° C. than monomer (B) include hexane, heptane, cyclohexane, benzene, toluene, ethanol, isopropyl alcohol, diisopropyl ether, tetrahydrofuran, and acetone. , Methyl ethyl ketone, methyl isobutyl ketone, ethyl acetate and the like.
  • the said solvent can be suitably selected according to the kind of monomer (B).
  • the solvent (E) may have a surface tension at 25 ° C. of 20 mN / m or more and less than 40 mN / m, or 22 mN / m or more and less than 36 N / m. If the surface tension is not less than the above lower limit value, it is possible to suppress the formation of a yuzu skin (orange peel), and if it is less than the above upper limit value, coating defects such as occurrence of thick end portions (framing) are unlikely to occur.
  • the difference in solubility parameter between the solvent (E) and the monomer (B) may be within 2 [(cal / cm 3 ) 1/2 ], or 1.5 [(cal / cm 3 ) 1 / 2 ].
  • ⁇ is a solubility parameter
  • ⁇ E is molar evaporation energy (cal / mol)
  • V molar volume (cm 3 / mol).
  • Those having a similar solubility parameter ⁇ dissolve well. It agrees with the rule of thumb that similar things melt well.
  • the solubility parameter can be determined by various methods, but in the present specification, the solubility parameter is calculated from the chemical composition by the method of Fedors.
  • a solvent (E) may be used individually by 1 type, and may use 2 or more types together.
  • the content of the solvent (E) is not particularly limited, but can be 25 to 500 parts by mass, and 30 to 400 parts by mass with respect to 100 parts by mass of the base polymer (A). Can do.
  • the content of the solvent (E) can be 10 to 90% by mass and 20 to 80% by mass with respect to the total mass of the pressure-sensitive adhesive composition.
  • the pressure-sensitive adhesive composition may contain a plasticizer.
  • a plasticizer is included, the content of the plasticizer can be 50 parts by mass or less, 100 parts by mass or less, and 10 parts by mass or less with respect to 100 parts by mass of the base polymer (A). It can also be.
  • a non-functional acrylic polymer can be used as the plasticizer.
  • a non-functional acrylic polymer is a polymer consisting only of an acrylic monomer unit having no functional group other than an acrylate group, or an acrylic monomer unit having no functional group other than an acrylate group and no functional group. It means a polymer composed of non-acrylic monomer units.
  • an acrylic monomer unit which does not have functional groups other than an acrylate group the thing similar to a non-crosslinkable (meth) acrylic acid ester unit (a1) is mentioned, for example.
  • Non-acrylic monomer units having no functional group include, for example, vinyl acetate, vinyl propionate, vinyl butyrate, vinyl caproate, vinyl caprylate, vinyl caprate, vinyl laurate, vinyl myristate, vinyl palmitate, stearin.
  • Examples thereof include carboxylic acid vinyl esters such as vinyl acid vinyl, vinyl cyclohexanecarboxylate, and vinyl benzoate, and styrene.
  • the pressure-sensitive adhesive composition may contain components other than those described above as long as the effects of the present invention are not impaired.
  • Other components include components known as additives for pressure-sensitive adhesives, such as antioxidants, metal corrosion inhibitors, tackifiers, silane coupling agents, ultraviolet absorbers, light stabilizers such as hindered amine compounds, etc. You can select from among them as needed.
  • antioxidants include phenolic antioxidants, amine-based antioxidants, lactone-based antioxidants, phosphorus-based antioxidants, sulfur-based antioxidants, and the like. These antioxidants may be used alone or in combination of two or more.
  • the metal corrosion inhibitor include benzoriazol resins.
  • Examples of the tackifier include rosin resin, terpene resin, terpene phenol resin, coumarone indene resin, styrene resin, xylene resin, phenol resin, and petroleum resin.
  • Examples of the silane coupling agent include mercaptoalkoxysilane compounds (for example, mercapto group-substituted alkoxy oligomers).
  • Examples of the ultraviolet absorber include benzotriazole compounds and benzophenone compounds. However, when ultraviolet rays are used for the active energy rays during complete curing, it is necessary to add them in a range that does not inhibit the polymerization reaction.
  • the pressure-sensitive adhesive sheet of the present invention is obtained by semi-curing the pressure-sensitive adhesive composition by heating or irradiation with active energy rays, containing at least a part of the monomer (B) in an unreacted state, and a crosslinking agent ( Among at least one selected from C) and the polymerization initiator (D), at least a part thereof is contained in an unreacted state. That is, the manufacturing method of the adhesive sheet of this invention includes the process of heating an adhesive composition or irradiating an active energy ray.
  • the pressure-sensitive adhesive sheet of the present invention may be composed of a pressure-sensitive adhesive layer and other layers, but is preferably composed of only a pressure-sensitive adhesive layer.
  • other layers include a pressure-sensitive adhesive layer formed from a pressure-sensitive adhesive composition other than the above, a support, a release sheet, and the like.
  • the support include polystyrene, styrene-acrylic copolymer, acrylic resin, polyethylene terephthalate, polycarbonate, polyetheretherketone, triacetylcellulose, and other plastic films; antireflection films, optical films such as electromagnetic wave shielding films, etc. Is mentioned.
  • the production process of the pressure-sensitive adhesive sheet of the present invention includes a step of applying a pressure-sensitive adhesive composition on a release sheet to form a coating film, a step of heating the coating film to a semi-cured product, or activating the coating film And a step of forming a semi-cured product by irradiation with energy rays.
  • the step of coating the pressure-sensitive adhesive composition on the release sheet to form a coating film and the step of heating the coating film to make a semi-cured product will be described as a representative.
  • the reaction of the base polymer (A) and the crosslinking agent (C) proceeds to form a semi-cured product (adhesive sheet). That is, during heating, the polymerization reaction of the monomer (B) by the polymerization initiator (D) does not proceed or is slight in the coating film, so that in the resulting semi-cured product (adhesive sheet)
  • the monomer (B) and polymerization initiator (D) contained in the pressure-sensitive adhesive composition remain. Therefore, the pressure-sensitive adhesive sheet of the present invention has active energy ray curability.
  • an aging treatment may be performed in which the pressure-sensitive adhesive sheet is allowed to stand for a certain period at a certain temperature.
  • the aging treatment can be performed, for example, by standing at 23 ° C. for 7 days.
  • a release sheet a peelable laminate sheet having a release sheet substrate and a release agent layer provided on one side of the release sheet substrate, or a polyolefin film such as a polyethylene film or a polypropylene film as a low polarity substrate Is mentioned. Papers and polymer films are used as the release sheet substrate in the peelable laminate sheet.
  • a release agent constituting the release agent layer for example, a general-purpose addition type or condensation type silicone release agent or a long-chain alkyl group-containing compound is used.
  • Specific examples of silicone release agents include BY24-4527 and SD-7220 manufactured by Toray Dow Corning Silicone, KS-3600, KS-774, and X62-2600 manufactured by Shin-Etsu Chemical Co., Ltd.
  • the silicone release agent contains a silicone resin which is an organosilicon compound having a SiO 2 unit and a (CH 3 ) 3 SiO 1/2 unit or CH 2 ⁇ CH (CH 3 ) SiO 1/2 unit. Also good.
  • Specific examples of the silicone resin include BY24-843, SD-7292, SHR-1404 manufactured by Toray Dow Corning Silicone, KS-3800, X92-183 manufactured by Shin-Etsu Chemical Co., Ltd., and the like.
  • release sheet two types of release sheets having different peelability can be used in order to facilitate peeling. That is, when the peelability from one side and the peelability from the other are different, it becomes easy to peel only the release sheet having the higher peelability first. In that case, what is necessary is just to adjust the peelability of each peeling sheet according to the bonding method and the bonding order.
  • the pressure-sensitive adhesive composition forming the pressure-sensitive adhesive sheet can be performed using a known coating apparatus.
  • the coating apparatus include a blade coater, an air knife coater, a roll coater, a bar coater, a gravure coater, a micro gravure coater, a rod blade coater, a lip coater, a die coater, and a curtain coater.
  • the solvent may be contained in the coating liquid.
  • the solvent include methanol, ethanol, isopropanol, acetone, methyl ethyl ketone, toluene, n-hexane, n-butyl alcohol, methyl isobutyl ketone, methyl butyl ketone, ethyl butyl ketone, cyclohexanone, ethyl acetate, butyl acetate, propylene glycol monomethyl.
  • Ether acetate, ethylene glycol monoethyl ether, propylene glycol monomethyl ether, N-methyl-2-pyrrolidone and the like are used. These may be used alone or in combination of two or more.
  • the coating film can be heated using a known heating device such as a heating furnace or an infrared lamp.
  • the first optical member (optical film) and the second optical member (optical film) are bonded together when the pressure-sensitive adhesive sheet is in a semi-cured state, and heating or active energy rays are used. There is a method of completely curing an adhesive sheet by irradiation.
  • the adherend is preferably an optical member (optical film).
  • the first optical member (optical film) may be a retardation film
  • the second optical member (optical film) may be a polarizing plate.
  • the pressure-sensitive adhesive sheet of the present invention is preferably attached so as to be in direct contact with the TAC film (triacetyl cellulose film).
  • the pressure-sensitive adhesive sheet is bonded to the surface of the adherend in a semi-cured state, it is completely cured by heating or irradiation with an active energy ray, whereby the cohesive force of the pressure-sensitive adhesive sheet is increased and the adhesiveness is improved.
  • active energy rays include ultraviolet rays, electron beams, visible rays, X-rays, ion rays and the like, and can be appropriately selected according to the polymerization initiator (D) contained in the pressure-sensitive adhesive sheet.
  • ultraviolet rays or electron beams are preferable, and ultraviolet rays are particularly preferable.
  • the ultraviolet light source for example, a high pressure mercury lamp, a low pressure mercury lamp, an ultrahigh pressure mercury lamp, a metal halide lamp, a carbon arc, a xenon arc, an electrodeless ultraviolet lamp, or the like can be used.
  • the electron beam for example, an electron beam emitted from various electron beam accelerators such as a cockloftwald type, a bandecraft type, a resonant transformation type, an insulating core transformer type, a linear type, a dynamitron type, and a high frequency type can be used.
  • the present invention also relates to a method for producing a laminate including a step of bringing a pressure-sensitive adhesive sheet into contact with an adherend surface and heating in that state or a step of irradiating active energy rays. Moreover, this invention relates also to the laminated body manufactured with such a manufacturing method.
  • the pressure-sensitive adhesive sheet is preferably brought into contact with a pair of adherend surfaces in a semi-cured state, and the pair of adherends are a first optical member (optical film) and a second optical member (optical film). This is good. That is, it is preferable to bond an optical member (optical film) to both surfaces of the pressure-sensitive adhesive sheet.
  • a roll-to-roll method can be used in the step of bringing the pressure-sensitive adhesive sheet into contact with the adherend surface.
  • the production speed of the process of bringing the pressure-sensitive adhesive sheet into contact with the adherend surface can be increased, and the production efficiency of the laminate can be increased.
  • FIG. 1 is a cross-sectional view illustrating an example of the structure of the laminate of the present invention.
  • the laminate 100 of the present invention preferably has a pressure-sensitive adhesive sheet 10, and has optical members (optical films 22 and 24) on both surfaces of the pressure-sensitive adhesive sheet 10.
  • the optical member include a polarizing plate (polarizing film), a retardation film, and a brightness enhancement film used for a liquid crystal display device.
  • the adhesive sheet of this invention can also be used for bonding with a scattering prevention film and a glass base material other than an optical member, and can also be used for bonding with a surface protection film.
  • AIBN azobisisobutyronitrile
  • the solution was heated to 60 ° C. and random copolymerized to obtain a base polymer (A).
  • the solution viscosity at 23 ° C. of a 35 mass% solution of this base polymer (A) was 5500 mPa ⁇ s.
  • the pressure-sensitive adhesive solution prepared as described above was used as a 38 ⁇ m-thick polyethylene terephthalate film (separator film) having a release agent layer treated with a silicone release agent (38RL-07 (2), manufactured by Oji F-Tex Co., Ltd.). On the surface of the film, uniformly apply with an applicator so that the coating amount after drying is 3 ⁇ m / m 2, and dry for 3 minutes in a 100 ° C. air-circulating constant temperature oven. Formed. Next, a 38 ⁇ m-thick separator film (manufactured by Oji F-Tex Co., Ltd., 38RL-07 (L)) was bonded to the surface of the pressure-sensitive adhesive layer.
  • the double-sided adhesive sheet provided with the structure of the separator film / adhesive layer / separator film in which the adhesive layer was pinched
  • the pressure-sensitive adhesive sheet was cured for 7 days at 23 ° C. and a relative humidity of 50%.
  • the thickness of the adhesive sheet was 3 ⁇ m.
  • Example 2 A double-sided PSA sheet was obtained in the same manner as in Example 1 except that the PSA sheet was prepared using the PSA solution of Example 1 so that the coating amount was 8 ⁇ m / m 2 .
  • the pressure-sensitive adhesive sheet was cured for 7 days at 23 ° C. and a relative humidity of 50%. The thickness of the adhesive sheet was 8 ⁇ m.
  • Example 1 In ⁇ Preparation of pressure-sensitive adhesive solution> in Example 1, isostearyl acrylate as the monomer (B1) having one polymerizable unsaturated group, trimethylolpropane ethylene oxide-modified triacrylate as the polyfunctional monomer (B2), A pressure-sensitive adhesive solution was prepared in the same manner as in Example 1 except that 1-hydroxy-cyclohexyl-phenyl-ketone was not blended as the polymerization initiator (D). A double-sided PSA sheet was obtained in the same manner as in Example 1 except that the PSA sheet was prepared using the PSA solution so that the coating amount was 3 ⁇ m / m 2 . The pressure-sensitive adhesive sheet was cured for 7 days at 23 ° C. and a relative humidity of 50%. The thickness of the adhesive sheet was 3 ⁇ m.
  • Example 2 A double-sided PSA sheet was obtained in the same manner as in Example 1 except that the PSA sheet was prepared using the PSA solution of Comparative Example 1 so that the coating amount was 8 ⁇ m / m 2 .
  • the pressure-sensitive adhesive sheet was cured for 7 days at 23 ° C. and a relative humidity of 50%. The thickness of the adhesive sheet was 8 ⁇ m.
  • the separator on the heavy release side was peeled off, and the adhesive surface was bonded to a SUS plate so that the area of the exposed bonding portion was 25 mm ⁇ 25 mm, and JIS According to the holding power measuring method of Z0237, a 1 kg weight was suspended and the amount of deviation after 60 minutes was measured.
  • the film thickness reduction was achieved.
  • the pressure-sensitive adhesive sheets obtained in the examples had a semi-cured state and appropriate holding power after irradiation with active energy rays, and were also excellent in durability.

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

Abstract

La présente invention vise à fournir une feuille adhésive amincie qui présente d'excellentes propriétés de manipulation lors de la stratification un film optique ou similaire. La présente invention concerne une feuille adhésive qui a une épaisseur de 1 à 10 µm et qui contient un adhésif partiellement durci par chauffage d'une composition adhésive ou irradiation de la composition adhésive avec des rayons d'énergie active, ladite composition adhésive comprenant : un polymère de base (A) contenant un motif ester d'acide (méth)acrylique non réticulable (a1) et un motif monomère acrylique (a2) ayant un groupe fonctionnel réticulable ; un monomère (B) ayant au moins un groupe insaturé polymérisable ; un agent de réticulation (C) qui réagit avec le polymère de base (A) en résultat de la chaleur ; un initiateur de polymérisation (D) qui amène la réaction de polymérisation du monomère (B) à démarrer en résultat de l'irradiation avec des rayons d'énergie active ; et un solvant (E).
PCT/JP2016/070648 2015-07-13 2016-07-13 Feuille adhésive, stratifié, et leur procédé de production WO2017010501A1 (fr)

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JP2020164714A (ja) * 2019-03-29 2020-10-08 アイカ工業株式会社 粘着剤組成物
WO2020226169A1 (fr) * 2019-05-08 2020-11-12 王子ホールディングス株式会社 Feuille adhésive, procédé de production d'un corps multicouche, et corps multicouche
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WO2020241619A1 (fr) * 2019-05-28 2020-12-03 王子ホールディングス株式会社 Feuille adhésive, procédé de production de corps stratifié et corps stratifié
JP2020193278A (ja) * 2019-05-28 2020-12-03 王子ホールディングス株式会社 粘着シート、積層体の製造方法および積層体
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JP2020023656A (ja) * 2018-02-05 2020-02-13 日東電工株式会社 粘着シートおよび粘着シート剥離方法
JP2020164714A (ja) * 2019-03-29 2020-10-08 アイカ工業株式会社 粘着剤組成物
JP7286376B2 (ja) 2019-03-29 2023-06-05 アイカ工業株式会社 粘着剤組成物
WO2020226169A1 (fr) * 2019-05-08 2020-11-12 王子ホールディングス株式会社 Feuille adhésive, procédé de production d'un corps multicouche, et corps multicouche
JP2020193279A (ja) * 2019-05-28 2020-12-03 王子ホールディングス株式会社 粘着シート、積層体の製造方法および積層体
WO2020241619A1 (fr) * 2019-05-28 2020-12-03 王子ホールディングス株式会社 Feuille adhésive, procédé de production de corps stratifié et corps stratifié
JP2020193278A (ja) * 2019-05-28 2020-12-03 王子ホールディングス株式会社 粘着シート、積層体の製造方法および積層体
WO2021167091A1 (fr) * 2020-02-21 2021-08-26 日東電工株式会社 Couche de composition adhésive, produit stratifié, produit stratifié optique, dispositif optique et procédé de production de produit stratifié optique

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