WO2018230323A1 - 粘着シート及び電子機器 - Google Patents

粘着シート及び電子機器 Download PDF

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Publication number
WO2018230323A1
WO2018230323A1 PCT/JP2018/020479 JP2018020479W WO2018230323A1 WO 2018230323 A1 WO2018230323 A1 WO 2018230323A1 JP 2018020479 W JP2018020479 W JP 2018020479W WO 2018230323 A1 WO2018230323 A1 WO 2018230323A1
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WIPO (PCT)
Prior art keywords
pressure
sensitive adhesive
adhesive sheet
foam
mass
Prior art date
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PCT/JP2018/020479
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
祐也 北出
岩崎　剛
佑輔 高橋
秀晃 武井
Original Assignee
Dic株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Dic株式会社 filed Critical Dic株式会社
Priority to CN201880034093.6A priority Critical patent/CN110662812A/zh
Priority to KR1020197034593A priority patent/KR102518118B1/ko
Priority to JP2019525279A priority patent/JP6687160B2/ja
Publication of WO2018230323A1 publication Critical patent/WO2018230323A1/ja

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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
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • 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
    • C09J201/00—Adhesives based on unspecified macromolecular compounds
    • 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
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/26—Porous or cellular plastics
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature

Definitions

  • the present invention relates to a pressure-sensitive adhesive sheet that can be used in the production of various articles including electronic devices such as car navigation systems, personal computers, televisions, and smartphones.
  • the pressure-sensitive adhesive sheet using a foam as a base material is widely used, for example, in the case of fixing two or more housings, rechargeable batteries, circuit boards, and the like constituting an electronic device.
  • the pressure-sensitive adhesive sheet is, for example, a resin foam obtained by foaming a resin composition containing a polyolefin resin and a non-compatible resin with respect to the polyolefin resin in a ratio of 90:10 to 60:40,
  • a pressure-sensitive adhesive sheet based on a foamed sheet characterized in that an average major axis of an island part of a sea-island structure formed by an incompatible resin is 1 ⁇ m or more see, for example, Patent Document 1).
  • a pressure-sensitive adhesive sheet used for fixing a member has been required to have followability to a stepped portion such as a housing or a circuit board and high adhesive strength in order to prevent water from entering.
  • a curved surface or a complicated panel is frequently used from the viewpoint of design, and the pressure-sensitive adhesive sheet is more desired to have the ability to follow irregularities and high steps.
  • use of information display devices made of organic EL is in progress. Since such an organic EL display device is expensive, it is required to be reused when repairing an electronic device.
  • the pressure-sensitive adhesive sheet used for fixing the information display device a re-peeling performance that can be easily peeled without destroying the organic EL information display device at the time of disassembly for repair has been demanded.
  • the pressure-sensitive adhesive sheet using a high-strength foam is a step portion of the adherend.
  • the followability to the water is not sufficient, and it is easy to cause inundation from the outside.
  • the problem to be solved by the present invention is that the organic EL information display device and the like can be easily peeled when the electronic device is disassembled, etc., and has a high step portion on the adherend. It is providing the adhesive sheet which has favorable followable
  • the present inventors have a specific configuration for the foam base material used for the adhesive tape. It has been found that the above-mentioned problems can be solved when components are contained, a specific apparent density range is selected, a specific tensile modulus is selected, and they are combined.
  • the present invention is a pressure-sensitive adhesive sheet having a pressure-sensitive adhesive layer on one side or both sides of a foam base material directly or via another layer, wherein the foam base material is an ethylene vinyl acetate copolymer (EVA) and And / or 30 to 90% by mass of an ethylene acrylic acid copolymer (EAA), the apparent density of the foam substrate is 0.20 g / cm 3 to 0.60 g / cm 3, and the tensile modulus in the flow direction is
  • EAA ethylene vinyl acetate copolymer
  • EAA ethylene acrylic acid copolymer
  • the apparent density of the foam substrate is 0.20 g / cm 3 to 0.60 g / cm 3
  • the tensile modulus in the flow direction is
  • the present invention relates to an adhesive sheet having a pressure of 10 MPa to 35 MPa.
  • the pressure-sensitive adhesive sheet of the present invention can be peeled off without destroying the organic EL information display device or the like when the electronic device is disassembled, etc., and has good followability to a high step portion.
  • the pressure-sensitive adhesive sheet can be used in various scenes including the manufacture of electronic devices such as portable electronic terminals, the fixing of automobile parts, the fixing of interior and exterior of buildings, and the like.
  • the pressure-sensitive adhesive sheet of the present invention is a pressure-sensitive adhesive sheet having a pressure-sensitive adhesive layer on one side or both sides of a foam base material directly or via another layer, and the foam base material is an ethylene vinyl acetate copolymer (EVA). And / or 30 to 90% by mass of an ethylene acrylic acid copolymer (EAA), the apparent density of the foam substrate is 0.20 g / cm 3 to 0.60 g / cm 3, and the tensile modulus in the flow direction Is 10 MPa to 35 MPa.
  • EAA ethylene vinyl acetate copolymer
  • the pressure-sensitive adhesive sheet of the present invention is a foam containing 30 to 90% by mass of an ethylene vinyl acetate copolymer (EVA) and / or an ethylene acrylic acid copolymer (EAA) as a constituent of the base material (core).
  • EVA ethylene vinyl acetate copolymer
  • EAA ethylene acrylic acid copolymer
  • core base material
  • Use body substrate The content of the ethylene vinyl acetate copolymer and / or ethylene acrylic acid copolymer is more preferably 40 to 80% by mass, and most preferably 50 to 70% by mass.
  • the ethylene vinyl acetate copolymer preferably has a vinyl acetate content (copolymerization ratio) of 20% by mass or less and 5% by mass to 15% by mass.
  • the foam base material has an apparent density in the range of 0.20 g / cm 3 to 0.60 g / cm 3 .
  • the apparent density of the foam substrate is preferably in the range of 0.25g / cm 3 ⁇ 0.55g / cm 3, a range of 0.30g / cm 3 ⁇ 0.50g / cm 3 is more preferable.
  • the apparent density is an apparent density measured according to JISK6767. A foam cut into a rectangle of 4 cm ⁇ 5 cm is prepared for about 15 cm 3 minutes, and its mass is measured. Based on the mass and the volume, The value calculated by
  • the foam base material preferably has a thickness in the range of 50 ⁇ m to 300 ⁇ m, more preferably in the range of 70 ⁇ m to 300 ⁇ m, and most preferably in the range of 100 ⁇ m to 250 ⁇ m.
  • the thickness of the foam base is too small, it is difficult to ensure a foam strength that does not break during re-peeling.
  • the thickness of the foam is too large, the thickness of the electronic device itself is increased, which is not desirable from the viewpoint of the design and portability of the electronic device.
  • the foam has a tensile elastic modulus in the flow direction of 10 MPa to 35 MPa.
  • the tensile elastic modulus in the flow direction is preferably 12 MPa to 33 MPa, and most preferably 14 MPa to 29 MPa.
  • the tensile elasticity modulus of the flow direction of the said foam refers to the value measured according to JISK7161. Specifically, a foam having a distance between grips (L) of 20 mm and a width of a test piece (W) of 10 mm was measured using a Tensilon tensile tester in an environment of 23 ° C. and 50% RH at a tensile speed of 10 mm / min.
  • the tensile elastic modulus is calculated by the following method. This evaluation method is an evaluation suitable as an index of whether or not the foam can be peeled without tearing when the tape is peeled again.
  • the foam may further contain at least one selected from the group consisting of polyolefins, polyurethanes and acrylic polymers.
  • Polyolefin, polypropylene, and ethylene-propylene copolymer are preferred as the polyolefin, and acrylic rubber and other elastomers are preferred as the acrylic polymer.
  • acrylic polymer in order to increase the tensile strength at the time of re-peeling, at least one selected from linear low density polyethylene (LLDPE), low density polyethylene (LDPE), medium density polyethylene (MDPE), and high density polyethylene (HDPE) is used. It is preferable to contain.
  • the content thereof is preferably 5 to 60% by mass, more preferably 10 to 50% by mass, and most preferably 20 to 40% by mass.
  • the elastomer for improving followable
  • ethylene / propylene rubber EPDM
  • the elastomer content is preferably 5 to 40% by mass, more preferably 10 to 30% by mass.
  • the foam for example, one having a crosslinked structure can be used.
  • the method for producing the foam is not particularly limited.
  • a polyolefin resin such as a polyethylene resin is used.
  • a foamable resin composition containing a pyrolytic foaming agent, a foaming aid, and a colorant is supplied to an extruder, melted and kneaded, and then foamed by extruding into a sheet from the extruder.
  • crosslinking the said foamed resin sheet as needed, and the process of foaming a foamable resin sheet is mentioned.
  • the foam obtained by the above method may be melted or softened as necessary, and may be stretched in one or both of the flow direction and the width direction. The stretching may be performed a plurality of times as necessary.
  • the foamable resin composition can be produced by coating or casting a foamable resin composition on the surface of a release liner or the like and drying.
  • the step of cross-linking the foamable resin sheet obtained by the above method includes, for example, a method of irradiating the foamable resin sheet with ionizing radiation, a foamable resin composition containing an organic peroxide, and using it. It can be performed by a method of heating the obtained expandable resin sheet.
  • the ionizing radiation examples include electron beams, ⁇ rays, ⁇ rays, and ⁇ rays.
  • the dose of ionizing radiation is appropriately adjusted so that the gel fraction of the resin foam is within the above-mentioned preferable range, but a range of 5 to 200 kGy is preferable.
  • organic peroxide examples include 1,1-bis (t-butylperoxy) 3,3,5-trimethylcyclohexane, 1,1-bis (t-butylperoxy) cyclohexane, 2,2-bis ( t-butylperoxy) octane, n-butyl-4,4-bis (t-butylperoxy) valerate, di-t-butyl peroxide, t-butylcumyl peroxide, dicumyl peroxide, ⁇ , ⁇ ′ -Bis (t-butylperoxy-m-isopropyl) benzene, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, 2,5-dimethyl-2,5-di (t-butyl) Peroxy) hexyne-3, benzoyl peroxide, cumyl peroxyneodecanate, t-butyl peroxybenzoate, 2,5
  • the amount of the organic peroxide added is preferably 0.01 to 5 parts by mass, more preferably 0.1 to 3 parts by mass with respect to 100 parts by mass of the base resin.
  • the step of foaming the foamable resin sheet can be performed by, for example, a method of heating with hot air, a method of heating with infrared rays, a method using a salt bath, a method using an oil bath, or the like. Of these, a method of heating with hot air or a method of heating with infrared rays is preferable.
  • a foamable resin sheet containing a pyrolytic foaming agent When foaming the foamable resin sheet, a foamable resin sheet containing a pyrolytic foaming agent can be used.
  • the pyrolytic foaming agent may be appropriately determined according to the foaming ratio of the foam, but is preferably used in the range of 1 to 40 parts by weight with respect to 100 parts by weight of the base resin. More preferably, it is used in the range of 1 to 30 parts by mass.
  • the stretching step may be performed on the foam obtained by the above method, or may be performed in parallel with the step of foaming the foamable resin sheet.
  • the stretching step may be continued while maintaining the melted state in the foaming step, or may be performed after the foaming step by cooling and heating the foam again.
  • the molten state of the foam means a state of being heated to a melting point or higher of a resin such as a base resin constituting the foam.
  • the softening of the foam means a state where the foam is heated to a temperature not lower than the melting point and lower than the melting point of the base resin constituting the foam.
  • a colored product can be used for the purpose of imparting design properties, light shielding properties, concealing properties, light reflectivity, and light resistance.
  • a black colorant can be used as the colorant that can be used for the coloring.
  • carbon black, graphite, copper oxide, manganese dioxide, aniline black, perylene black, titanium black, cyanine black, Activated carbon, ferrite, magnetite, chromium oxide, iron oxide, molybdenum disulfide, chromium complex, complex oxide black pigment, anthraquinone organic black pigment and the like can be used.
  • carbon black graphite, copper oxide, manganese dioxide, aniline black, perylene black, titanium black, cyanine black, Activated carbon, ferrite, magnetite, chromium oxide, iron oxide, molybdenum disulfide, chromium complex, complex oxide black pigment, anthraquinone organic black pigment and the like can be used.
  • a colorant it is preferable to use
  • a white colorant can be used.
  • the foam of the present invention includes a foaming aid such as a plasticizer, an antioxidant, and zinc oxide, a cell nucleus adjusting material, a heat stabilizer, and aluminum hydroxide as necessary, as long as the physical properties are not impaired.
  • a foaming aid such as a plasticizer, an antioxidant, and zinc oxide, a cell nucleus adjusting material, a heat stabilizer, and aluminum hydroxide as necessary, as long as the physical properties are not impaired.
  • Containing additives such as flame retardants such as magnesium hydroxide, antistatic agents, glass and plastic hollow balloons / beads, fillers such as metal powders, metal compounds, conductive fillers, thermal conductive fillers, etc. Can be used.
  • the foam is preferably 0.1% by mass to 10% by mass, preferably 1% by mass to 7% by mass, with respect to the base resin, in order to maintain appropriate followability and cushioning properties. Is preferred.
  • a foamable resin composition is used to prevent color unevenness, partial excessive foaming, insufficient foaming, and the like. It is preferable to use a master batch obtained by kneading a thermoplastic resin having high compatibility with the additive and the additive in advance.
  • the foam it is preferable to use a foam having a surface with a wetting index of 36 mN / m or more by a wetting reagent for the purpose of improving the adhesiveness with the pressure-sensitive adhesive layer or other layers. It is more preferable to use a material having a surface of m or more, and it is more preferable to use a material having a surface of 48 mN / m or more.
  • Examples of the method for adjusting the wetness index of the surface of the foam to the above range include surface treatment methods such as corona treatment, flame treatment, plasma treatment, hot air treatment, ozone treatment, ultraviolet treatment, and application of an easy adhesion treatment agent. .
  • the pressure-sensitive adhesive sheet As the pressure-sensitive adhesive sheet, a sheet having a pressure-sensitive adhesive layer on one side or both sides of the foam directly or via another layer can be used.
  • Examples of the adhesive that can be used for forming the adhesive layer include acrylic adhesives, urethane adhesives, synthetic rubber adhesives, natural rubber adhesives, and silicone adhesives. , Containing an acrylic polymer obtained by polymerizing a monomer component containing a (meth) acrylic monomer, and using an acrylic pressure-sensitive adhesive containing a tackifier resin, a crosslinking agent or the like as required Is preferred.
  • Examples of the (meth) acrylic monomer that can be used in the production of the acrylic polymer include methyl (meth) acrylate, ethyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, t- Carbon such as butyl (meth) acrylate, n-hexyl (meth) acrylate, n-octyl (meth) acrylate, isooctyl (meth) acrylate, isononyl (meth) acrylate, cyclohexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, etc.
  • a (meth) acrylate having an alkyl group having 1 to 12 atoms can be used.
  • the (meth) acrylic monomer it is preferable to use a (meth) acrylate having an alkyl group having 4 to 12 carbon atoms, and having an alkyl group having 4 to 8 carbon atoms. It is more preferable to use (meth) acrylate, and it is particularly preferable to use either one or both of n-butyl acrylate and 2-ethylhexyl acrylate in order to achieve both excellent adhesion and excellent followability. .
  • the (meth) acrylate having an alkyl group having 1 to 12 carbon atoms is preferably used in an amount of 60% by mass or more, based on the total amount of monomers used in the production of the acrylic polymer. More preferably, it is used in the range of 98.5% by mass, and more preferably in the range of 90% by mass to 98.5% by mass in order to achieve both excellent adhesive strength and excellent followability.
  • a highly polar vinyl monomer can be used as a monomer.
  • a vinyl monomer having a hydroxyl group, a vinyl monomer having a carboxyl group, a vinyl monomer having an amide group, or the like can be used alone or in combination.
  • Examples of the monomer having a hydroxyl group include a hydroxyl group such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and 6-hydroxyhexyl (meth) acrylate. (Meth) acrylates can be used.
  • acrylic acid for example, acrylic acid, methacrylic acid, itaconic acid, maleic acid, (meth) acrylic acid dimer, crotonic acid, ethylene oxide-modified oxalic acid acrylate, etc.
  • acrylic acid is preferably used.
  • the monomer having an amide group for example, N-vinylpyrrolidone, N-vinylcaprolactam, acryloylmorpholine, acrylamide, N, N-dimethylacrylamide and the like can be used.
  • vinyl acetate vinyl acetate, ethylene oxide-modified succinic acid acrylate, 2-acrylamido-2-methylpropane sulfonic acid, and the like can be used in addition to those described above.
  • the high-polarity vinyl monomer is preferably used in a range of 1.5% by mass to 20% by mass with respect to the total amount of monomers used for the production of the acrylic polymer. More preferably, it is used in the range of ⁇ 10% by mass, and more preferably in the range of 2% by mass to 8% by mass in order to achieve both excellent adhesive force and excellent followability.
  • the adhesive containing a crosslinking agent described later it is preferable to use an acrylic polymer having a functional group that reacts with a functional group of the crosslinking agent as the acrylic polymer.
  • the functional group that the acrylic polymer may have include a hydroxyl group.
  • the hydroxyl group can be introduced into the acrylic polymer by using, for example, a vinyl monomer having a hydroxyl group as the monomer.
  • the vinyl monomer having a hydroxyl group is preferably used in the range of 0.01% by mass to 1.0% by mass with respect to the total amount of monomers used for the production of the acrylic polymer. More preferably, it is used in the range of mass% to 0.3 mass%.
  • the acrylic polymer can be produced by polymerizing the monomer by a method such as a solution polymerization method, a bulk polymerization method, a suspension polymerization method, an emulsion polymerization method, etc., and adopting a solution polymerization method Is preferable for improving the production efficiency of the acrylic polymer.
  • Examples of the solution polymerization method include a method in which the monomer, a polymerization initiator, and an organic solvent are mixed and stirred at a temperature of preferably 40 ° C. to 90 ° C. for radical polymerization.
  • polymerization initiator examples include peroxides such as benzoyl peroxide and lauryl peroxide, azo thermal polymerization initiators such as azobisisobutylnitrile, acetophenone photopolymerization initiators, benzoin ether photopolymerization initiators, benzyl A ketal photopolymerization initiator, an acyl phosphine oxide photopolymerization initiator, a benzoin photopolymerization initiator, a benzophenone photopolymerization initiator, or the like can be used.
  • peroxides such as benzoyl peroxide and lauryl peroxide
  • azo thermal polymerization initiators such as azobisisobutylnitrile
  • acetophenone photopolymerization initiators benzoin ether photopolymerization initiators
  • benzoin ether photopolymerization initiators benzyl A ketal photopolymerization initiator
  • the acrylic polymer obtained by the above method may be in a state of being dissolved or dispersed in an organic solvent, for example, when it is produced by a solution polymerization method.
  • acrylic polymer those having a weight average molecular weight of 400,000 to 3 million are preferably used, and those having a weight average molecular weight of 700,000 to 2.5 million are more preferably used.
  • the weight average molecular weight is a value measured by gel permeation chromatography (GPC method) and calculated in terms of standard polystyrene. Specifically, the weight average molecular weight can be measured using a GPC apparatus (HLC-8320GPC) manufactured by Tosoh Corporation under the following conditions.
  • the pressure-sensitive adhesive that can be used for forming the pressure-sensitive adhesive layer, it is possible to use a material containing a tackifying resin in order to achieve both excellent adhesion to an adherend and foam and excellent followability. preferable.
  • the tackifying resin examples include a rosin tackifying resin, a polymerized rosin tackifying resin, a polymerized rosin ester tackifying resin, a rosin phenol tackifying resin, a stabilized rosin ester tackifying resin, and a disproportionated rosin ester.
  • -Based tackifier resins hydrogenated rosin ester-based tackifier resins, terpene-based tackifier resins, terpene phenol-based tackifier resins, petroleum resin-based tackifier resins, (meth) acrylate resin-based tackifier resins, and the like.
  • an emulsion-type pressure-sensitive adhesive it is preferable to use an emulsion-type tackifying resin as the tackifying resin.
  • tackifying resin examples include disproportionated rosin ester tackifying resin, polymerized rosin ester tackifying resin, rosin phenol tackifying resin, hydrogenated rosin ester tackifying resin, (meth) acrylate, among others. It is preferable to use one or a combination of two or more of resins, terpene phenol resins, and petroleum resins.
  • the tackifier resin those having a softening point in the range of 30 ° C. to 180 ° C. are preferably used, and those having a softening point in the range of 70 ° C. to 140 ° C. are preferably used. ) Is more preferable for achieving both excellent adhesive strength and excellent followability.
  • the (meth) acrylate tackifying resin preferably has a glass transition temperature of 30 ° C. to 200 ° C., and preferably has a glass transition temperature of 50 ° C. to 160 ° C. It is more preferable.
  • the tackifying resin is preferably used in the range of 5 to 65 parts by weight, and in the range of 8 to 55 parts by weight, based on 100 parts by weight of the acrylic polymer. It is more preferable for achieving both excellent adhesion to the body and foam and excellent followability.
  • the pressure-sensitive adhesive used for forming the pressure-sensitive adhesive layer it is preferable to use a cross-linking agent in order to ensure excellent adhesion to the adherend and foam.
  • crosslinking agent for example, an isocyanate crosslinking agent, an epoxy crosslinking agent, a metal chelate crosslinking agent, an aziridine crosslinking agent, or the like can be used.
  • said crosslinking agent it is preferable to use any one or both of the isocyanate type crosslinking agent and epoxy-type crosslinking agent which are rich in the reactivity with an acrylic polymer, and using an isocyanate type crosslinking agent is preferable. More preferred.
  • isocyanate-based crosslinking agent examples include tolylene diisocyanate, naphthylene-1,5-diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate, xylylene diisocyanate, trimethylolpropane-modified tolylene diisocyanate, and the like. It is preferable to use trimethylolpropane-modified tolylene diisocyanate.
  • the crosslinking agent is preferably selected and used in such an amount that the gel fraction of the pressure-sensitive adhesive layer is 40 to 80% with respect to toluene, and is selected and used in such an amount that the gel fraction is 30 to 70% by mass. More preferably, it is possible to select and use an amount with a gel fraction of 35% by mass to 65% by mass, which achieves both excellent adhesion to the adherend and foam substrate and excellent followability. It is further preferable when obtaining an adhesive sheet.
  • the said gel fraction points out the value measured by the method shown below.
  • the pressure-sensitive adhesive coated on the release treatment surface of the release liner so that the thickness after drying is 50 ⁇ m is dried for 3 minutes in an environment of 100 ° C., and then 2 in an environment of 40 ° C.
  • the pressure-sensitive adhesive layer was formed by aging for a day.
  • the test piece was prepared by cutting the pressure-sensitive adhesive layer into a square having a length of 50 mm and a width of 50 mm.
  • test piece After measuring the mass (G1) of the test piece, the test piece was immersed in toluene in a 23 ° C. environment for 24 hours.
  • the insoluble component in toluene was extracted by filtering the mixture of the test piece and toluene using a 300 mesh wire net.
  • the mass (G2) of the insoluble component dried at 110 ° C. for 1 hour was measured.
  • the gel fraction was calculated based on the mass (G1), mass (G2) and the following formula.
  • the pressure-sensitive adhesive examples include plasticizers, softeners, antioxidants, flame retardants, glass and plastic fibers and balloons, beads, metals, metal oxides, metal nitride fillers, pigments, dyes, and the like. What contains additives, such as a coloring agent, a leveling agent, a thickener, a water repellent, an antifoamer, can be used.
  • the pressure-sensitive adhesive layer that can be formed using the pressure-sensitive adhesive preferably has a temperature that exhibits a peak value of loss tangent (tan ⁇ ) at a frequency of 1 Hz, preferably -40 ° C. to 15 ° C.
  • a pressure-sensitive adhesive layer formed to a thickness of about 2 mm was used using a viscoelasticity testing machine (trade name: ARES G2 manufactured by T.A. Instruments Japan).
  • a test piece is sandwiched between parallel disks having a diameter of 8 mm, which is a measuring part, and a storage elastic modulus (G ′) and a loss elastic modulus (G ′′) from ⁇ 50 ° C. to 150 ° C. are measured at a frequency of 1 Hz.
  • the thickness of the pressure-sensitive adhesive layer used in the present invention is preferably 5 ⁇ m to 100 ⁇ m, and preferably 15 ⁇ m to 80 ⁇ m in order to achieve both excellent adhesion to an adherend and foam and excellent followability. More preferably, it is particularly preferably from 25 ⁇ m to 75 ⁇ m.
  • the pressure-sensitive adhesive sheet of the present invention preferably has a strength value of 40 N / cm 2 or more, preferably 50 N / cm 2 or more, and 60 N / cm 2 when the indentation adhesive strength is measured in a 1 mm width frame shape. Most preferably, it is 2 or more.
  • the pressure-sensitive adhesive sheet of the present invention is formed by, for example, a direct method in which the pressure-sensitive adhesive is directly applied to the foam and dried, or after a pressure-sensitive adhesive layer is formed by applying a pressure-sensitive adhesive to the release sheet and then drying. It can be manufactured by a transfer method that is bonded to the body.
  • an adhesive containing an acrylic polymer and a crosslinking agent is used as the adhesive that forms the adhesive layer
  • the adhesive layer is laminated on one or both sides of the foam by the direct method or the transfer method.
  • aging in an environment of preferably 20 ° C. to 50 ° C., more preferably 23 ° C. to 45 ° C. for about 2 days to 7 days has excellent adhesion to adherends and foam substrates, and excellent This is preferable for achieving both the following ability.
  • the pressure-sensitive adhesive sheet of the present invention preferably has a thickness of 400 ⁇ m or less because it easily contributes to thinning of the electronic device, more preferably 100 ⁇ m to 300 ⁇ m, further preferably 150 ⁇ m to 300 ⁇ m, and more preferably 200 ⁇ m. Most preferably, it is ⁇ 300 ⁇ m. Since the pressure-sensitive adhesive sheet uses a foam having the specific apparent density and tensile elastic modulus, the foam has a total thickness of the pressure-sensitive adhesive sheet, as described above, even when it is peeled off during re-peeling. It is difficult to tear off, and it is possible to achieve both good followability to the stepped portion.
  • the pressure-sensitive adhesive sheet a sheet having other layers as required in addition to the foam and the pressure-sensitive adhesive layer can be used.
  • the other layer for example, when imparting dimensional stability, good tensile strength, re-peelability, etc. of the pressure-sensitive adhesive sheet, heat conduction such as a laminate layer such as a polyester film, a light shielding layer, a light reflecting layer, a metal layer, etc. Layer.
  • a release sheet may be laminated on the surface of the pressure-sensitive adhesive layer.
  • the release sheet for example, a film obtained by using a synthetic resin such as polyethylene, polypropylene, polyester, paper, non-woven fabric, cloth, foamed sheet, metal substrate, and at least one side of a laminate thereof is treated with silicone.
  • a peeling treatment such as a long-chain alkyl treatment or a fluorine treatment can be used.
  • the pressure-sensitive adhesive sheet of the present invention is particularly preferably used for fixing, for example, which is required to be adhesively fixed to a portion having unevenness or a large step and which is required not to break the adherend when re-peeling. it can.
  • the members having unevenness and large steps are often used as members in industrial applications such as electronic terminals such as car navigation systems and smartphones, automobiles, building materials, OA, and home appliance industries.
  • the member include two or more casings and lens members constituting an electronic terminal.
  • An article such as an electronic terminal in which two or more cases and lens members are fixed using the pressure-sensitive adhesive sheet of the present invention has excellent adhesive strength, can be re-peeled at the time of disassembly, and the like. It is waterproof.
  • Preparation Example 1 Production method of acrylic polymer (A-1) In a reaction vessel equipped with a stirrer, a reflux condenser, a nitrogen introduction tube, and a thermometer, 95.9 parts by mass of n-butyl acrylate, 4 parts by mass of acrylic acid 2-hydroxyethyl acrylate 0.1 and 200 parts by mass of ethyl acetate were charged, and the temperature was raised to 72 ° C. while blowing nitrogen under stirring.
  • Preparation Example 2 Production method of acrylic polymer (A-2) In a reaction vessel equipped with a stirrer, a reflux condenser, a nitrogen inlet tube, and a thermometer, 63.9 parts by mass of n-butyl acrylate, 2-ethylhexyl acrylate 32 Part by weight, 4 parts by weight of acrylic acid, 0.1 part by weight of 4-hydroxybutyl acrylate, and 200 parts by weight of ethyl acetate were charged, and the temperature was raised to 72 ° C. while blowing nitrogen under stirring.
  • Adhesive composition (A) In a container, with respect to 100 parts by mass of the acrylic polymer (A-1), 10 parts by mass of polymerized rosin ester-based tackifier resin D-125 (Arakawa Chemical Co., Ltd.) and disproportionated rosin ester-based tackifier resin After 15 parts by mass of A-100 (Arakawa Chemical Industries, Ltd.) were mixed and stirred, ethyl acetate was added to obtain a pressure-sensitive adhesive composition (A) having a solid content of 31% by mass.
  • Adhesive composition (B) In a container, with respect to 100 parts by mass of the acrylic polymer (A-2), 10 parts by mass of a polymerized rosin ester-based tackifier resin D-125 (Arakawa Chemical Industries, Ltd.) and a disproportionated rosin ester-based tackifier resin After 15 parts by mass of A-100 (Arakawa Chemical Industries, Ltd.) were mixed and stirred, ethyl acetate was added to obtain a pressure-sensitive adhesive composition (B) having a solid content of 31% by mass.
  • Adhesive (A1) Vernock D-40 (manufactured by DIC Corporation, trimethylolpropane adduct of tolylene diisocyanate, isocyanate group content 7 mass%, nonvolatile content 40 mass with respect to 100 parts by mass of the pressure-sensitive adhesive composition (A) %) 1.4 parts by mass was added, and the mixture was stirred and mixed to be uniform, and then filtered through a 100 mesh wire netting to obtain an adhesive (A1) having a gel fraction of 50%.
  • Adhesive (A2) The gel fraction was obtained by adding 0.7 parts by weight of Bernock D-40 as a crosslinking agent to 100 parts by weight of the pressure-sensitive adhesive composition (A), stirring and mixing the mixture uniformly, and then filtering through a 100-mesh wire mesh. A 30% pressure-sensitive adhesive (A2) was obtained.
  • Adhesive (A3) The gel fraction was obtained by adding 2.1 parts by weight of Bernock D-40 as a crosslinking agent to 100 parts by weight of the pressure-sensitive adhesive composition (A), stirring and mixing the mixture uniformly, and then filtering through a 100-mesh wire mesh. A 70% pressure-sensitive adhesive (A3) was obtained.
  • Adhesive (B) Next, 1.4 parts by mass of Bernock D-40 as a cross-linking agent is added to 100 parts by mass of the pressure-sensitive adhesive composition (B), and the mixture is stirred and mixed uniformly, and then filtered through a 100-mesh wire mesh. An adhesive (B) having a gel fraction of 50% was obtained.
  • Example 1 The adhesive (A1) is coated on the surface of the release liner using a bar coater so that the thickness of the adhesive layer after drying is 50 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both sides of the foam 1 adjusted in Table 1 by corona treatment and adjusted to a wetness index of 50 mN / m, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 2 A pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 2 shown in Table 1 was used instead of the foam 1.
  • Example 3 A pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 3 shown in Table 1 was used instead of the foam 1.
  • Example 4 instead of the foam 1, an adhesive sheet was obtained in the same manner as in Example 1 except that the foam 4 shown in Table 1 was used.
  • Example 5 instead of the foam 1, a pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 5 shown in Table 1 was used.
  • Example 6 instead of the foam 1, an adhesive sheet was obtained in the same manner as in Example 1 except that the foam 6 shown in Table 1 was used.
  • Example 7 instead of the foam 1, a pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 7 shown in Table 1 was used.
  • Example 8 A pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 8 shown in Table 1 was used instead of the foam 1.
  • Example 9 instead of the foam 1, a pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that the foam 9 shown in Table 1 was used.
  • Example 10 The pressure-sensitive adhesive (A1) is applied to the surface of the release liner using a bar coater so that the thickness of the pressure-sensitive adhesive layer after drying is 15 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 10 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 10 shown in Table 1, and cured under an environment of 40 ° C. for 48 hours.
  • the pressure-sensitive adhesive (A1) is applied to the surface of the release liner using a bar coater so that the thickness of the pressure-sensitive adhesive layer after drying is 15 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 11 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 11 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 12 By applying the pressure-sensitive adhesive (A1) to the surface of the release liner using a bar coater so that the thickness of the pressure-sensitive adhesive layer after drying is 25 ⁇ m, and drying at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 12 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 12 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 13 The adhesive (A1) is coated on the surface of the release liner using a bar coater so that the thickness of the adhesive layer after drying is 50 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both sides of the foam 13 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 13 shown in Table 1, and cured under an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 14 The adhesive (A1) is coated on the surface of the release liner using a bar coater so that the thickness of the adhesive layer after drying is 50 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 14 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 14 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 15 The adhesive (A2) is applied to the surface of the release liner using a bar coater so that the thickness of the adhesive layer after drying is 50 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 5 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 5 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 16 By applying the pressure-sensitive adhesive (A3) to the surface of the release liner using a bar coater so that the thickness of the pressure-sensitive adhesive layer after drying is 50 ⁇ m, and drying at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 5 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 5 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • Example 17 The pressure-sensitive adhesive is coated on the surface of the release liner with the use of a bar coater so that the thickness of the pressure-sensitive adhesive layer after drying is 50 ⁇ m, and is dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is affixed to both surfaces of the foam 5 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 5 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • the adhesive (A1) is coated on the surface of the release liner using a bar coater so that the thickness of the adhesive layer after drying is 50 ⁇ m, and dried at 80 ° C. for 3 minutes. A layer was made.
  • the pressure-sensitive adhesive layer is applied to both surfaces of the foam 15 having a wettability index adjusted to 50 mN / m by corona treatment on the surface of the foam 15 shown in Table 1, and cured in an environment of 40 ° C. for 48 hours.
  • an adhesive sheet was prepared.
  • A No voids such as bubbles existed at the interface between the step portion and the pressure-sensitive adhesive sheet up to a step of 60 ⁇ m.
  • Air gaps such as bubbles were not present at the interface between the step portion and the pressure-sensitive adhesive sheet up to a step of 50 ⁇ m, but voids such as bubbles were present at the interface between the step portion and the pressure-sensitive adhesive sheet at a step of 60 ⁇ m.
  • Air gaps such as bubbles were not present at the interface between the step portion and the pressure-sensitive adhesive sheet up to a step of 40 ⁇ m. However, air gaps such as air bubbles were present at the interface between the step portion and the pressure-sensitive adhesive sheet when the level difference was 50 ⁇ m or more.
  • E Gaps such as bubbles existed at the interface between the step portion and the adhesive sheet at a step of 30 ⁇ m.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesive Tapes (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Laminated Bodies (AREA)
PCT/JP2018/020479 2017-06-14 2018-05-29 粘着シート及び電子機器 WO2018230323A1 (ja)

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EP3720699A4 (en) * 2017-12-06 2021-08-04 3M Innovative Properties Company GRAPHIC SHEET, GRAPHIC SHEET PRODUCTION PROCESS AND CONSTRUCTION STRUCTURE

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EP3720699A4 (en) * 2017-12-06 2021-08-04 3M Innovative Properties Company GRAPHIC SHEET, GRAPHIC SHEET PRODUCTION PROCESS AND CONSTRUCTION STRUCTURE
US11530339B2 (en) 2017-12-06 2022-12-20 3M Innovative Properties Company Graphic sheet, method of producing graphic sheet, and building structure

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JP6687160B2 (ja) 2020-04-22
CN110662812A (zh) 2020-01-07
TW201905137A (zh) 2019-02-01

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