WO2016084123A1 - 粘着剤組成物及び粘着テープ - Google Patents
粘着剤組成物及び粘着テープ Download PDFInfo
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- WO2016084123A1 WO2016084123A1 PCT/JP2014/081012 JP2014081012W WO2016084123A1 WO 2016084123 A1 WO2016084123 A1 WO 2016084123A1 JP 2014081012 W JP2014081012 W JP 2014081012W WO 2016084123 A1 WO2016084123 A1 WO 2016084123A1
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- sensitive adhesive
- pressure
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- adhesive tape
- resistance
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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
- 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
- C09J133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
-
- 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
-
- 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
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
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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
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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
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/245—Vinyl resins, e.g. polyvinyl chloride [PVC]
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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
- 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 composition excellent in rebound resistance, load resistance, narrow frame moisture heat resistance, processability, impact resistance and waterproofness, and an adhesive tape using the same.
- Display screens of portable electronic devices such as smartphones and tablet terminals generally have a structure in which a touch panel and a liquid crystal module are combined. And in recent years, the enlargement of the display screen and the thinning of the case are progressing.
- the FPC Flexible Printed Circuits
- the FPC is incorporated in the liquid crystal module, and the FPC is bent at a sharper angle along with the enlargement of the display screen and the thinning of the housing, and the structure is constantly applied with a strong repulsive force.
- the impact resistant waterproof double-sided pressure-sensitive adhesive tape used to fix the housing and the top panel has been narrowed along with the increase in the size of the LCD screen.
- the adhesive tape needs to have adhesion that can withstand the repulsive force of the FPC from the inside and can withstand external forces such as impact resistance and waterproofness. Become. If the adhesion is insufficient, peeling of the top panel due to strong internal stress, falling off due to external stress or flooding may occur, resulting in breakage of the device. Moreover, in processing aptitude, while the narrowing of the tape progresses, when the adhesive is soft when punching into a strip shape, a frame shape, etc., glue breaks, glue balls, etc. adhere to the blade and cutting can not be performed well, The yield will be worse.
- a pressure-sensitive adhesive having a high theoretical Tg and a pressure-sensitive adhesive for rebound resistance generally has no problem in processability.
- the rebound resistance may be improved by adding a high softening point tackifying resin in an amount of 10 to 30% based on the solid content of the adhesive.
- the load resistance, impact resistance, and waterproofness are inferior.
- Patent Document 1 discloses an acrylic copolymer having a (meth) acrylate having 4 to 12 carbon atoms and a vinyl monomer having a carboxyl group as a monomer component on both sides of a foam base, and a polymerized rosin ester tackifying resin And a double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer comprising an acrylic pressure-sensitive adhesive composition containing
- Patent Document 2 describes a double-sided pressure-sensitive adhesive tape in which a pressure-sensitive adhesive layer containing an acrylic copolymer and a tackifying resin is provided on both sides of a substrate made of a polyethylene foam.
- Patent Document 3 shows a double-sided pressure-sensitive adhesive tape used for fixing a member of an electronic device, comprising: a substrate, a first pressure-sensitive adhesive layer provided on one surface of the substrate, and the other of the substrate And a second pressure-sensitive adhesive layer provided on the surface of at least one of the first pressure-sensitive adhesive layer and the second pressure-sensitive adhesive layer, and an acrylic polymer, having a weight average molecular weight of 20000 or less
- An acrylic polymer is described as a double-sided pressure-sensitive adhesive tape characterized in that it contains an acrylic oligomer different in monomers.
- Patent Document 4 50 to 90% by mass of (meth) acrylic acid alkyl ester (A1) having an alkyl group having 4 to 12 carbon atoms, 3 to 20% by mass of carboxyl group-containing monomer (A2), hydroxyl group-containing monomer (A3) 3 to 20% by mass, and 3 to 15% by mass of (meth) acrylic acid alkyl ester (A4) having an alkyl group having 1 to 3 carbon atoms are contained as a component, and the weight average molecular weight is 700,000 to A pressure-sensitive adhesive composition is described which contains an acrylic copolymer (A) having a hydroxyl group and a carboxyl group and a crosslinking agent (B) and having a molecular weight of 2,000,000 and a theoretical Tg of ⁇ 40 ° C. or less.
- a pressure-sensitive adhesive composition is described which contains an acrylic copolymer (A) having a hydroxyl group and a carboxyl group and a crosslinking agent (B) and having a molecular weight of 2
- the object of the present invention is to provide a pressure-sensitive adhesive composition excellent in various properties such as waterproofness, load resistance, processability, impact resistance, narrow frame moisture heat load resistance, artificial sebum resistance, artificial sweat resistance etc.
- a pressure-sensitive adhesive composition excellent in various properties such as waterproofness, load resistance, processability, impact resistance, narrow frame moisture heat load resistance, artificial sebum resistance, artificial sweat resistance etc.
- the present invention is an alkyl (meth) acrylate having an alkyl group having 1 to 3 carbon atoms and containing 10 to 20% by mass of (meth) acrylic acid alkyl ester (A1) and having 4 to 12 carbon atoms. 50 to 80% by mass of ester (A2), 10 to 15% by mass of carboxyl group-containing monomer (A3), 0.01 to 0.5% by mass of hydroxyl group-containing monomer (A4), and 1 to 5% of vinyl acetate (A5) %, An acrylic copolymer having a weight average molecular weight of 950,000 to 2,000,000 and a theoretical Tg of ⁇ 55 ° C. or less obtained by using a peroxide type polymerization initiator It is an adhesive composition containing a combination (A), a crosslinking agent (B), a silane coupling agent (C), and an antioxidant (D).
- the present invention is a pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer formed of the pressure-sensitive adhesive composition of the present invention on one side or both sides of a polyolefin resin substrate, wherein the MD direction and the TD direction of the polyolefin resin substrate
- the bending moment of the adhesive tape is 5 gf / cm or more
- the shear deformation rate at heating of the pressure-sensitive adhesive tape is 150% or less
- the splitting force is 70 N / cm 2 or more.
- the present invention is also a pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer formed of the pressure-sensitive adhesive composition of the present invention on one side or both sides of a polyester resin substrate.
- the pressure-sensitive adhesive composition of the present invention is resistant to low temperature even though it contains a relatively large amount of (meth) acrylic acid alkyl ester (A1) having an alkyl group having 1 to 3 carbon atoms, which is a high Tg monomer. It is excellent in impact resistance, and is also excellent in various properties such as load resistance, narrow frame moisture heat resistance, processability, waterproofness, artificial sebum resistance, artificial sweat oil resistance and the like. And since the single-sided or double-sided pressure-sensitive adhesive tape of the present invention is excellent in each of the above-mentioned properties, it can be used for various applications in a field requiring such properties.
- the pressure-sensitive adhesive composition of the present invention is a composition containing an acrylic copolymer (A), a crosslinking agent (B), a silane coupling agent (C) and an antioxidant (D).
- the acrylic copolymer (A) is a (meth) acrylic acid alkyl ester (A1) having an alkyl group having 1 to 3 carbon atoms, and (meth) acrylic acid having an alkyl group having 4 to 12 carbon atoms. It is an acrylic copolymer containing an alkyl ester (A2), a carboxyl group-containing monomer (A3), a hydroxyl group-containing monomer (A4) and a vinyl acetate (A5) as a component of a polymer chain.
- (Meth) acrylic acid alkyl ester (A1) is a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 3 carbon atoms, and has impact resistance, load resistance, processability, narrow frame moisture heat resistance load It is a component to improve the quality. Specific examples include methyl (meth) acrylate, ethyl (meth) acrylate and propyl (meth) acrylate. Among them, methyl (meth) acrylate is preferable.
- the content of the (meth) acrylic acid alkyl ester (A1) is 10 to 20% by mass, preferably 12 to 16 in 100% by mass of the constituent component (monomer unit) of the acrylic copolymer (A). It is mass%. The lower limits of these ranges are significant in terms of characteristics such as rebound resistance, load resistance, processability, and narrow frame heat resistance. The upper limit is significant in terms of characteristics such as narrow frame low temperature impact resistance and waterproofness.
- the (meth) acrylic acid alkyl ester (A2) is a (meth) acrylic acid alkyl ester having an alkyl group having 4 to 12 carbon atoms. Specific examples include butyl (meth) acrylate, isobutyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, octyl (meth) acrylate, isooctyl (meth) acrylate, isononyl (meth) acrylate and lauryl (meth) acrylate. Be Among them, 2-ethylhexyl (meth) acrylate is preferable.
- the content of the (meth) acrylic acid alkyl ester (A2) is 50 to 80% by mass, preferably 65 to 79% in 100% by mass of the constituent component (monomer unit) of the acrylic copolymer (A). It is mass%.
- the carboxyl group-containing monomer (A3) is a component for improving impact resistance, load resistance, processability, narrow frame low temperature impact resistance, and waterproofness.
- acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, 2-carboxy-1-butene, 2-carboxy-1-pentene, 2-carboxy-1-hexene, 2-carboxy -1- heptene is mentioned.
- the content of the carboxyl group-containing monomer (A3) is 10 to 15% by mass, preferably 10 to 12% by mass, in 100% by mass of the constituent component (monomer unit) of the acrylic copolymer (A). is there.
- the lower limits of these ranges are significant in terms of characteristics such as rebound resistance, load resistance, processability, narrow frame moisture heat load resistance, narrow frame low temperature impact resistance, waterproofness, and the like.
- the hydroxyl group-containing monomer (A4) is a component for improving impact resistance, load resistance, processability, and narrow frame low temperature impact resistance. Specific examples include 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate and 4-hydroxybutyl (meth) acrylate.
- the content of the hydroxyl group-containing monomer (A4) is 0.01 to 0.5 mass% in 100 mass% of the constituent component (monomer unit) of the acrylic copolymer (A), and preferably 0.05 It is ⁇ 0.15 mass%.
- the upper limit value of these ranges is to suppress the change with time of the adhesive tape in a heating and moist heat atmosphere, and to have characteristics such as sufficient resilience resistance, load resistance, processability, narrow frame low temperature resistance and waterproofness. It is significant to maintain.
- Vinyl acetate (A5) is a component for improving resilience, load resistance, processability, and narrow frame moisture heat load resistance.
- the content of vinyl acetate (A5) is 1 to 5% by mass, preferably 2 to 4% by mass, in 100% by mass of the constituent component (monomer unit) of the acrylic copolymer (A).
- the lower limits of these ranges are significant in terms of characteristics such as rebound resistance, load resistance, processability, and narrow frame heat resistance.
- the upper limit value is significant in terms of characteristics such as load resistance, narrow frame moisture heat load resistance, and narrow frame low temperature impact resistance.
- the acrylic copolymer (A) is obtained by copolymerizing at least the components (A1) to (A5) described above.
- the polymerization method is not particularly limited, but radical solution polymerization is preferable in terms of easy polymer design.
- an acrylic syrup comprising the acrylic copolymer (A) and the monomer thereof may be prepared first, and the acrylic syrup may be polymerized by blending a crosslinking agent (B) and an additional photopolymerization initiator.
- monomers other than the components (A1) to (A5) may be copolymerized within the range not impairing the effects of the present invention.
- the weight average molecular weight of the acrylic copolymer (A) is 950,000 to 2,000,000, and preferably 100 to 1.5 million. The lower limits of these ranges are significant in terms of characteristics such as load resistance, narrow frame heat resistance, and processability. The upper limit is significant in terms of the properties such as the coatability of the pressure-sensitive adhesive composition. This weight average molecular weight is a value measured by GPC method.
- the theoretical Tg of the acrylic copolymer (A) is ⁇ 55 ° C. or less, preferably ⁇ 55 to ⁇ 75 ° C. This theoretical Tg is a value calculated by the formula of FOX.
- the acrylic copolymer (A) described above is used as a resin component
- other types of additive components may be used in combination as long as the effects of the present invention are not impaired.
- the tackifying resin is used in combination, the low molecular weight component in the pressure-sensitive adhesive is increased, and the properties such as load resistance, resistance to artificial sebum resistance, and narrow frame moisture resistance and heat resistance decrease.
- the crosslinking agent (B) used in the present invention is a compound blended to react with the acrylic copolymer (A) to form a crosslinked structure.
- a compound capable of reacting with the carboxyl group and / or the hydroxyl group of the acrylic copolymer (A) is preferable.
- isocyanate crosslinking agents are preferred.
- Specific examples of the isocyanate crosslinking agent include tolylene diisocyanate, xylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate and modified prepolymers thereof. Two or more of these may be used in combination.
- the compounding amount of the crosslinking agent (B) is preferably 0.02 to 1 part by mass, more preferably 0.3 to 0.6 parts by mass with respect to 100 parts by mass of the acrylic copolymer (A).
- the silane coupling agent (C) is a component for improving the resilience resistance and the narrow frame moisture heat load resistance.
- silane coupling agents containing a glycidyl group are preferred. Specific examples include 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltriethoxysilane And tris- (trimethoxysilylpropyl) isocyanurate. Two or more of these may be used in combination.
- the compounding amount of the silane coupling agent (C) is preferably 0.01 to 0.05 parts by mass, more preferably 0.02 to 0.5 parts by mass with respect to 100 parts by mass of the acrylic copolymer (A). And particularly preferably 0.05 to 0.3 parts by mass.
- the antioxidant (D) is a component for improving the resilience resistance and the narrow frame moisture heat load resistance.
- hindered phenolic antioxidants are preferred.
- the blending amount of the antioxidant (D) is preferably 0.02 to 1.0 parts by mass, more preferably 0.07 to 0.7 parts by mass with respect to 100 parts by mass of the acrylic copolymer (A). is there.
- the pressure-sensitive adhesive composition of the present invention may further contain a light-shielding filler or a pigment.
- a light shielding filler include carbon black, carbon nanotubes, and black inorganic fillers.
- Specific examples of the pigment include carbon black, aniline black, acetylene black and ketjen black.
- the polyolefin-based pressure-sensitive adhesive tape of the present invention has a pressure-sensitive adhesive layer formed of the pressure-sensitive adhesive composition of the present invention on one side or both sides of a polyolefin resin substrate.
- the thickness of the pressure-sensitive adhesive layer is preferably 5 to 100 ⁇ m, more preferably 10 to 80 ⁇ m.
- the pressure-sensitive adhesive layer may be formed only on one side of the substrate, but is preferably formed on both sides to form a double-sided pressure-sensitive adhesive tape.
- the pressure-sensitive adhesive layer can be formed by crosslinking the pressure-sensitive adhesive composition of the present invention.
- the pressure-sensitive adhesive composition can be coated on a substrate and crosslinked by heating to form a pressure-sensitive adhesive layer on the substrate.
- the pressure-sensitive adhesive composition may be coated on a release paper or other film and crosslinked by heating to form a pressure-sensitive adhesive layer, and the pressure-sensitive adhesive layer may be bonded to one side or both sides of a substrate.
- a coating apparatus such as a roll coater, a die coater, or a lip coater can be used.
- the solvent in the pressure-sensitive adhesive composition can be removed together with the crosslinking reaction by heating.
- the polyolefin resin base is particularly preferably made of a polyolefin resin foam.
- Polyethylene and polypropylene are mentioned as a specific example of polyolefin resin.
- the thickness of the polyolefin resin substrate is preferably 0.05 to 2.0 mm.
- the bending moment in the MD direction (longitudinal direction) and the TD direction (width direction) of the polyolefin resin substrate is 5 gf / cm or more, preferably 7 gf / cm or more.
- the heating shear deformation rate of the pressure-sensitive adhesive tape is 150% or less, preferably 130% or less.
- the pressure-sensitive adhesive tape has such a shear deformation rate at the time of heating, it becomes difficult to deform, and excellent impact resistance, load resistance and narrow frame moisture resistance heat load resistance are developed.
- Split ⁇ of adhesive tape is at 70N / cm 2 or more, preferably 90 N / cm 2 or more.
- the pressure-sensitive adhesive tape has such a splitting force, excellent impact resistance, load resistance and narrow frame moisture heat resistance can be exhibited.
- the polyester-based pressure-sensitive adhesive tape of the present invention has a pressure-sensitive adhesive layer formed of the pressure-sensitive adhesive composition of the present invention on one side or both sides of a polyester-based resin base.
- the method of forming the pressure-sensitive adhesive layer is the same as that of the polyolefin-based pressure-sensitive adhesive tape described above.
- the polyester resin substrate may be crystalline, amorphous or foamable.
- the polyester resin substrate is usually used in the form of a resin film.
- the thickness is 0.002 to 0.05 mm, preferably 0.006 to 0.038 mm.
- a polyethylene terephthalate is mentioned as a specific example of polyester-based resin.
- the weight average molecular weight (Mw) and theoretical Tg of each acrylic copolymer are shown in Table 1.
- the weight average molecular weight (Mw) is a value obtained by measuring the molecular weight of the acrylic copolymer in terms of standard polystyrene by the GPC method using the following measuring apparatus and conditions.
- ⁇ Device LC-2000 series (manufactured by JASCO Corporation)
- Column Shodex KF-806M x 2 pcs, Shodex KF-802 x 1 pc ⁇
- Eluent Tetrahydrofuran (THF) Flow rate: 1.0 mL / min Column temperature: 40 ° C.
- Injection volume 100 ⁇ L ⁇ Detector: Refractometer (RI) Measurement sample: A solution obtained by dissolving an acrylic polymer in THF to prepare a solution having a concentration of 0.5 wt% of an acrylic polymer, and removing dust by filtration with a filter.
- the theoretical Tg is a value calculated by the formula of FOX.
- the pressure-sensitive adhesive composition was applied onto a silicone-treated release paper to a dry thickness of 0.075 mm. Next, the solvent was removed and dried at 110 ° C. and a crosslinking reaction was carried out to form a pressure-sensitive adhesive layer.
- This pressure-sensitive adhesive layer was bonded to both sides of a 0.15 mm thick polyolefin-based foamed resin substrate (electron beam crosslinked polyethylene foamed resin, foaming ratio: 1.8 to 2 times) having a bending moment of 12 gf / cm. Then, it was aged at 40 ° C. for 3 days to obtain a polyolefin-based foamed resin base double-sided pressure-sensitive adhesive tape.
- Example 20 A polyolefin-based foamed resin substrate having a bending moment of 6.0 gf / cm and having a thickness of 0.1 mm (electron beam crosslinked polyethylene foamed resin, foaming ratio 1.5 to 2.2 times) Pasted on both sides of the Then, it was aged at 40 ° C. for 3 days to obtain a polyolefin-based foamed resin base double-sided pressure-sensitive adhesive tape.
- Example 21 A polyolefin-based foamed resin substrate having a bending moment of 14.0 gf / cm and a 0.2 mm-thick polyolefin-based foamed resin substrate (electron-beam crosslinked polyethylene foamed resin, foaming ratio: 2.5 to 3.5 times) according to the pressure-sensitive adhesive composition of Example 1 Pasted on both sides of the Then, it was aged at 40 ° C. for 3 days to obtain a polyolefin-based foamed resin base double-sided pressure-sensitive adhesive tape.
- Example 1 (Production of Adhesive Tape)>
- the pressure-sensitive adhesive composition of Example 1 was bonded to both sides of a 0.15 mm thick polyolefin-based foamed resin substrate (electron beam crosslinked polyethylene foamed resin, foaming ratio 3 times) having a bending moment of 1.0 gf / cm. . Then, it was aged at 40 ° C. for 3 days to obtain a polyolefin-based foamed resin base double-sided pressure-sensitive adhesive tape.
- Example 2 (Production of Adhesive Tape)>
- the pressure-sensitive adhesive composition of Example 1 is applied to both sides of a 0.15 mm thick polyolefin-based foamed resin substrate (electron beam crosslinked polyethylene foamed resin, foaming ratio 2.5 times) having a bending moment of 2.5 gf / cm. I put it together. Then, it was aged at 40 ° C. for 3 days to obtain a polyolefin-based foamed resin base double-sided pressure-sensitive adhesive tape.
- Example 22 0.45 parts of a crosslinking agent (B1), 0.15 parts of a silane coupling agent (C1), and an antioxidant (D1) based on 100 parts of the solid content of the acrylic copolymer (A) obtained in Production Example 1 0.07 parts were added and mixed to prepare a pressure-sensitive adhesive composition.
- the pressure-sensitive adhesive composition was applied onto a silicone-treated release paper to a dry thickness of 0.019 mm. Next, the solvent was removed and dried at 100 ° C. and a crosslinking reaction was performed to form a pressure-sensitive adhesive layer. This pressure-sensitive adhesive layer was bonded to both sides of a 0.012 mm thick biaxially stretched polyester film (polyethylene terephthalate film). Then, it was aged at 40 ° C. for 3 days to obtain a polyester film substrate double-sided pressure-sensitive adhesive tape.
- Comparative Example 11 (Production of Adhesive Tape)> A pressure-sensitive adhesive composition was prepared in the same manner as in Example 22 except that the acrylic copolymer (A) obtained in Production Example 19 was used, to obtain a polyester film base material double-sided pressure-sensitive adhesive tape.
- Table 2 The abbreviations in Table 2 are as follows. “B1”: Isocyanate crosslinker (Nippon Polyurethane Co., Ltd., trade name Coronate L-45E) “C1”: Silane coupling agent (Shin-Etsu Chemical Co., Ltd., trade name KBM-403) "C2”: Silane coupling agent (Shin-Etsu Chemical Co., Ltd., trade name KBM-402) "C3”: Silane coupling agent (Shin-Etsu Chemical Co., Ltd., trade name KBE-403) "C4": Silane coupling agent (Shin-Etsu Chemical Co., Ltd., trade name KBE-402) "D1”: Antioxidant (manufactured by BASF, trade name Irganox 1010)
- the double-sided adhesive tape is cut into a 63 mm ⁇ 118 mm frame with a width of 1 mm, one release paper is peeled off and bonded to a 2.0 mm thick glass plate, and the other release paper is peeled off to a 2.0 mm thick
- the glass plate of was pasted together.
- the sample was subjected to pressure treatment (0.5 MPa) for 1 minute at 23 ° C. using an autoclave. Then, this sample was temporarily submerged in water based on JIS IPX 7 (waterproof standard), and the waterproofness was evaluated according to the following criteria.
- a sample is prepared in the same manner as above, and is immersed in water at a depth of 10 cm based on JIS IPX 8 (waterproof standard) and subjected to pressure treatment at 23 ° C., 0.5 MPa for 1 hour using an autoclave using the following criteria. The waterproofness was evaluated. " ⁇ ”: Water did not penetrate into the frame. "X”: Water infiltrated into the frame.
- the double-sided adhesive tape is cut into a 63 mm ⁇ 118 mm frame with a width of 1 mm, one release paper is peeled off and bonded to a 2.0 mm thick glass plate, and the other release paper is peeled off to a 2.0 mm thick
- the glass plate of was pasted together.
- the sample was subjected to pressure treatment at 23.degree. C. and 0.5 MPa for 1 minute using an autoclave.
- the double-sided pressure-sensitive adhesive tape was cut into a size of 25 mm ⁇ 25 mm, and one release paper was peeled off. Then, as shown in FIG. 1, the double-sided adhesive tape 1 (base material 1a, adhesive layer 1b) was attached to the SUS304 hook 2 and then the other release paper was peeled off and attached to the adherend 3.
- adherend 3 As the adherend 3, SUS304, a polycarbonate plate, an acrylic plate, an EGI steel plate, a gal barium steel plate, and a glass plate were used. Then, a load (weight 4) of 700 gf was applied to the SUS 2 hook 2 and held at 85 ° C. for 24 hours, and the load resistance was evaluated based on the following criteria. "O”: Hook 2 did not fall for 24 hours. "X”: Hook 2 fell within 60 minutes.
- the double-sided adhesive tape is cut into a 63 mm ⁇ 118 mm frame with a width of 0.6 mm, one release paper is peeled off, and it is attached to the adherend 3 (polycarbonate plate of 1.5 mm thickness), and the other is separated.
- the template was peeled off and attached to an adherend 7 (tempered glass plate of 1.9 mm thickness).
- this bonded member was adjusted with a 2.0 mm thick SUS 304 plate 8 so as to have a weight of 160 gf, and then cured for 60 minutes.
- the sample was freely dropped in the shear direction from a height of 1.5 M in an atmosphere of ⁇ 20 ° C., and the impact resistance was evaluated according to the following criteria.
- the double-sided pressure-sensitive adhesive tape was cut into a size of 25 mm ⁇ 25 mm, and one release paper was peeled off. Then, as shown in FIG. 3, the double-sided adhesive tape 1 (substrate 1a, adhesive layer 1b) is attached to the SUS304 hook 2 and then the other release paper is peeled off, and the adherend 3 (2.0 mm thick) It bonded to a SUS304BA board), and it aged for 60 minutes in 23 degreeC and the atmosphere of 50% RH. Then, the SUS304 hook 2 was pulled upward at a speed of 300 mm / min, and the strength [N / cm 2 ] when the foam was broken was measured.
- the double-sided pressure-sensitive adhesive tape was cut into a size of 25 mm ⁇ 25 mm, and one release paper was peeled off. Then, as shown in FIG. 6, the double-sided adhesive tape 1 (substrate 1a, adhesive layer 1b) is bonded to a SUS304BA plate 9 0.5 mm thick, 30 mm wide and 100 mm long, and then the other release paper is peeled off. , It bonded to the SUS304BA board 9 of the same size, and it aged for 60 minutes in 23 degreeC and the atmosphere of 50% RH.
- a weight 10 of 1 kgf is hung at the lower end, heated at 120 ° C for 30 minutes, heated at 135 ° C for 30 minutes, its deformation is visually measured with a loupe, and the shear deformation rate ( ⁇ Sr) at heating is given by the following equation Calculated with.
- ⁇ Sr (Xi + Xt) / Xi ⁇ 100
- ⁇ Sr Shear deformation rate at heating (%)
- Xt sample deformation (mm)
- the double-sided pressure-sensitive adhesive tape was cut into a frame of 63 mm ⁇ 118 mm with widths of 0.5 mm, 0.6 mm, 0.8 mm, and 1.0 mm, and one of the release papers was peeled off. Then, as shown in FIG. 7, the double-sided adhesive tape 1 is attached to a 1.5 mm thick hook 6 made of polycarbonate, and then the other release paper is peeled off to form an adherend 3 (glass plate of 2.0 mm thick). It bonded, and it aged for 60 minutes in 23 degreeC and the atmosphere of 50% RH.
- Comparative Example 8 used Comparative Example 9 using a composition not containing the component (C), and Comparative Example 10 using a composition not containing the component (D), any of the properties was inferior.
- Examples 1 to 21 are examples of producing the pressure-sensitive adhesive tape of the present invention, all the characteristics were excellent.
- Reference Examples 1 and 2 although the pressure-sensitive adhesive composition of the present invention was used, since the substrate was different from that of the pressure-sensitive adhesive tape of the present invention, any of the properties was inferior.
- evaluation items of evaluation test A and evaluation test B, sample size and test conditions are different because the application and required performance of the polyolefin foam resin base adhesive tape and the polyester film base double-sided adhesive tape are slightly different from each other. It is.
- a polyolefin-based foamed resin base adhesive tape is used to fix a base having a foamed elastic property, for example, a portion where a housing and a top panel are fixed, and narrowing according to its size is required, and waterproof And adhesion are also required.
- polyester-based film substrate double-sided adhesive tape is used, for example, to fix the LCD panel and the back light unit, and it is required to narrow according to its size, and the repulsive force or fall of the FPC is always applied. Adhesiveness that can withstand the impact of time is required. If the adhesion is insufficient, peeling of the LCD panel and the backlight unit may occur, resulting in light leakage. (Waterproof)
- the size of the double-sided adhesive tape is a frame of 45 mm ⁇ 65 mm with a width of 1 mm, and the conditions of JIS IPX 8 (waterproof standard) are 23 ° C, 0.2 MPa, 30 minutes of pressure treatment, except for ⁇ Evaluation Test A>
- the test was conducted in the same manner as the waterproofness, and the waterproofness was evaluated according to the following criteria. " ⁇ ”: Water did not penetrate into the frame. "X”: Water infiltrated into the frame.
- the size of the double-sided adhesive tape is 1 mm in width and 45 mm ⁇ 65 mm in a frame shape, and after being immersed in artificial sebum or artificial finger fat for 24 hours, the sample is allowed to stand in an atmosphere of 85 ° C and 85% RH for 72 hours.
- a test was conducted in the same manner as the artificial sebo-resistance and artificial finger-resistance of the evaluation test A>, and the artificial sebo-resistance and the artificial finger-lipid resistance were evaluated based on the following criteria.
- “(Circle)” Artificial sebum fluid and artificial finger fat fluid did not infiltrate into a frame.
- "X” Artificial sebum fluid and artificial finger fat fluid infiltrated into the frame.
- a shock of 10 gf of stainless steel ball 11 was freely dropped from a height of 0.5 M to the adherend 3 (polycarbonate plate of 1.5 mm thickness) side of this sample to give an impact, and the ball impact resistance was evaluated according to the following criteria. . " ⁇ ”: No peeling of members due to impact. "X”: Exfoliation of members due to impact.
- the narrow frame of ⁇ Evaluation Test A> except that the size of the double-sided adhesive tape is a frame of 45 mm x 65 mm with a width of 1 mm, a load of 50 gf (weight 4), and the test environment is 85 ° C and 85% RH for 24 hours.
- the test was conducted in the same manner as the heat resistance to moisture resistance, and the narrow frame heat resistance to moisture resistance was evaluated according to the following criteria. "O”: The hook 6 did not fall for 24 hours. "X”: The hook 6 fell within 60 minutes.
- Example 22 using the pressure-sensitive adhesive composition of the present invention all the properties were excellent.
- Comparative Example 11 in which the acrylic copolymer 19 in which the amount of the component (A3) is too small was used each property was inferior.
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Abstract
Description
本発明の粘着剤組成物は、アクリル系共重合体(A)と架橋剤(B)とシランカップリング剤(C)と酸化防止剤(D)を含有する組成物である。
アクリル系共重合体(A)の製造には、本発明の効果を損なわない範囲内で、成分(A1)~(A5)以外のモノマーを共重合させても良い。
アクリル系共重合体(A)の理論Tgは-55℃以下であり、好ましくは-55~-75℃である。この理論TgはFOXの式により算出される値である。
本発明のポリオレフィン基材粘着テープは、ポリオレフィン系樹脂基材の片面又は両面に、本発明の粘着剤組成物により形成された粘着剤層を有する。粘着剤層の厚さは、好ましくは5~100μm、より好ましくは10~80μmである。粘着剤層は基材の片面だけに形成しても良いが、両面に形成して両面粘着テープとすることが好ましい。
本発明のポリエステル基材粘着テープは、ポリエステル系樹脂基材の片面又は両面に、本発明の粘着剤組成物により形成された粘着剤層を有する。粘着剤層の形成方法は、先に説明したポリオレフィン基材粘着テープの場合と同様である。ポリエステル系樹脂基材は結晶性、アモルファス状または発泡性の何れであってもよい。
攪拌機、温度計、還流冷却器及び窒素ガス導入管を備えた反応装置に、表1に示す量(%)の成分(A1)~(A5)と、酢酸エチル、連鎖移動剤としてn-ドデカンチオール及び過酸化物系ラジカル重合開始剤としてラウリルパーオキサイド0.1部を仕込んだ。反応装置内に窒素ガスを封入し、攪拌しながら窒素ガス気流下で68℃、3時間、その後78℃、3時間で重合反応させた。その後、室温まで冷却し、酢酸エチルを添加した。これにより、固形分濃度30%のアクリル系共重合体(A)を得た。
・装置:LC-2000シリーズ(日本分光株式会社製)
・カラム:Shodex KF-806M×2本、Shodex KF-802×1本
・溶離液:テトラヒドロフラン(THF)
・流速:1.0mL/分
・カラム温度:40℃
・注入量:100μL
・検出器:屈折率計(RI)
・測定サンプル:アクリル系ポリマーをTHFに溶解させ、アクリル系ポリマーの濃度が0.5重量%の溶液を作製し、フィルターによるろ過でゴミを除去したもの。
理論Tgは、FOXの式により算出した値である。
表2に示す通り、製造例1~20で得たアクリル系共重合体(A)の固形分100部に対して、架橋剤(B)、シランカップリング剤(C)、酸化防止剤(D)を加えて混合し、粘着剤組成物を調製した。
実施例1の粘着剤組成物を、曲げモーメントが6.0gf/cmである0.1mm厚のポリオレフィン系発泡樹脂基材(電子線架橋ポリエチレン発泡樹脂、発泡倍率1.5~2.2倍)の両面に貼り合せた。そして40℃で3日間養生して、ポリオレフィン系発泡樹脂基材両面粘着テープを得た。
実施例1の粘着剤組成物を、曲げモーメントが14.0gf/cmである0.2mm厚のポリオレフィン系発泡樹脂基材(電子線架橋ポリエチレン発泡樹脂、発泡倍率2.5~3.5倍)の両面に貼り合せた。そして40℃で3日間養生して、ポリオレフィン系発泡樹脂基材両面粘着テープを得た。
実施例1の粘着剤組成物を、曲げモーメントが1.0gf/cmである0.15mm厚のポリオレフィン系発泡樹脂基材(電子線架橋ポリエチレン発泡樹脂、発泡倍率3倍)の両面に貼り合せた。そして40℃で3日間養生して、ポリオレフィン系発泡樹脂基材両面粘着テープを得た。
実施例1の粘着剤組成物を、曲げモーメントが2.5gf/cmである0.15mm厚のポリオレフィン系発泡樹脂基材(電子線架橋ポリエチレン発泡樹脂、発泡倍率2.5倍)の両面に貼り合せた。そして40℃で3日間養生して、ポリオレフィン系発泡樹脂基材両面粘着テープを得た。
製造例1で得たアクリル系共重合体(A)の固形分100部に対して、架橋剤(B1)0.45部、シランカップリング剤(C1)0.15部、酸化防止剤(D1)0.07部を加えて混合し、粘着剤組成物を調製した。
製造例19で得たアクリル系共重合体(A)を用いたこと以外は実施例22と同様にして粘着剤組成物を調製し、ポリエステル系フィルム基材両面粘着テープを得た。
「MA」:メチルアクリレート
「2-EHA」:2-エチルヘキシルアクリレート
「BA」:n-ブチルアクリレート
「AA」:アクリル酸
「4-HBA」:4-ヒドロキシブチルアクリレート
「Vac」:酢酸ビニル
「B1」:イソシアネート系架橋剤(日本ポリウレタン社製、商品名コロネートL-45E)
「C1」:シランカップリング剤(信越化学工業社製、商品名KBM-403)
「C2」:シランカップリング剤(信越化学工業社製、商品名KBM-402)
「C3」:シランカップリング剤(信越化学工業社製、商品名KBE-403)
「C4」:シランカップリング剤(信越化学工業社製、商品名KBE-402)
「D1」:酸化防止剤(BASF社製、商品名イルガノックス1010)
実施例1~21、比較例1~10及び参考例1~2で得たポリオレフィン系発泡樹脂基材両面粘着テープを、以下の方法で評価した。結果を表3~6に示す。
両面粘着テープを幅1mmで63mm×118mmの枠状に裁断し、一方の離型紙を剥離して2.0mm厚のガラス板に貼り合せ、更にもう一方の離型紙を剥離して2.0mm厚のガラス板を貼り合せた。このサンプルに対して、オートクレーブを用いて23℃、1分間の加圧処理(0.5MPa)を行った。そして、このサンプルをJIS IPX7(防水規格)に基づき一時的に水没させて、以下の基準で防水性を評価した。また、上記と同様にサンプルを作製し、JIS IPX8(防水規格)に基づき水深10cmの水中下に沈めて23℃、0.5MPa、1時間の加圧処理をオートクレーブを用いて行い以下の基準で防水性を評価した。
「○」:枠内に水が浸入しなかった。
「×」:枠内に水が浸入した。
両面粘着テープを幅1mmで63mm×118mmの枠状に裁断し、一方の離型紙を剥離して2.0mm厚のガラス板に貼り合せ、更にもう一方の離型紙を剥離して2.0mm厚のガラス板を貼り合せた。このサンプルに対して、オートクレーブを用いて23℃、0.5MPa、1分間の加圧処理を行った。そして、このサンプルを人工皮脂(トリオレイン33.3%、オレイン酸20.0%、スクワレン13.3%、ミリスチルオクタドデシレート33.4%)又は人工指脂(林純薬工業株式会社製)に72時間浸漬した。サンプルを取り出し、85℃、85%RHの雰囲気下で24時間静置し、その後通常の雰囲気下に24時間放置した。そのサンプルを目視観察し、以下の基準で耐人工皮脂性、耐人工指脂性を評価した。
「○」:枠内に人工皮脂液、人工指脂液が浸入しなかった。
「×」:枠内に人工皮脂液、人工指脂液が浸入した。
基材を幅38mm、長さ50mmの短冊状に裁断し、JIS P 8125に基づき、東洋精機製作所社製テーバー剛性度試験機を用いて、10gの重りを振り子へ取り付け、曲げ速度3°/sec、曲げ角度15°の時の目盛を読み、これを測定値とした。そしてこの測定値を以下の計算式に代入し、MD方向及びTD方向の曲げモーメント(M)を算出した。
M=38.0nk/w
M:曲げモーメント(gf/cm)
n:目盛の読み(10gの重りの時は1)
k:一目盛当りのモーメント(gf/cm)
w:試験片の幅
両面粘着テープを25mm×25mmのサイズに裁断し、一方の離型紙を剥離した。そして図1に示すように、SUS304製フック2に両面粘着テープ1(基材1a、粘着層1b)を貼り合せ、次いでもう一方の離型紙を剥離し、被着体3に貼り合せた。この被着体3としては、SUS304、ポリカーボネート板、アクリル板、EGI鋼板、ガルバリウム鋼板、ガラス板を用いた。そしてSUS304製フック2に700gfの荷重(錘4)をかけ、85℃で24時間保持し、以下の基準で耐荷重性を評価した。
「○」:24時間フック2は落下しなかった。
「×」:60分以内にフック2が落下した。
両面粘着テープを5mm×125mmのサイズで10本に細断した状態を維持したまま(すなわち細断した各々の粘着テープが細断時の隣接した状態を維持したまま)、65℃、80%RH雰囲気下に1日放置した。その後1本毎に180°方向に離型紙ごと剥離し、隣接した部分との癒着を目視にて確認し、以下の基準で加工性を評価した。
「○」:隣接した部分との癒着がほとんど無く、隣接部分を剥がすことなく剥離できた。
「×」:隣接した部分に著しい癒着があり、隣接部分が同時に剥がれてしまった。
両面粘着テープを幅0.6mmで63mm×118mmの枠状に裁断し、一方の離型紙を剥離して、被着体3(1.5mm厚のポリカーボネート板)に貼り合せ、更にもう一方の離型紙を剥離し、被着体7(1.9mm厚の強化ガラス板)に貼り合せた。この貼り合せした部材を図2に示すように、重さが160gfになるように2.0mm厚のSUS304板8で調整した後、60分間養生した。このサンプルを-20℃の雰囲気下で、1.5Mの高さからせん断方向に自由落下させ、以下の基準で耐衝撃性を評価した。
「○」:20回落下後、接着部分の剥がれ及び基材の層間破壊無し。
「×」:20回落下後、接着部分の剥がれ及び基材の層間破壊有り。
両面粘着テープを25mm×25mmにサイズに裁断し、一方の離型紙を剥離した。そして図3に示すように、SUS304製フック2に両面粘着テープ1(基材1a、粘着層1b)を貼り合せ、次いでもう一方の離型紙を剥離し、被着体3(2.0mm厚のSUS304BA板)に貼り合せ、23℃、50%RHの雰囲気下で60分養生した。そしてSUS304製フック2を上方向に300mm/minの速度で引張り、発泡体が切れた時の強度[N/cm2]を測定した。
1mm×20mmに裁断した両面粘着テープ1の一方の離型紙を剥離し、厚さ125μmで20mm×60mmのポリイミドフィルム5の一方に図4に示すように貼り付け、23℃、50%RHの雰囲気下で60分間養生した。その後、ポリイミドフィルム5を図5に示すように折り曲げて粘着テープ1を被着体3(1.5mm厚のポリカーボネート板)に貼り合せ、85℃、85%RHの雰囲気下で72時間放置し、接着部分の剥がれを目視にて確認し、以下の基準で耐反発性を評価した。
「○」:72時間後に接着部分の剥がれ無し。
「×」:72時間後に接着部分の剥がれ有り。
両面粘着テープを25mm×25mmのサイズに裁断し、一方の離型紙を剥離した。そして図6示すように、厚さ0.5mm、幅30mm、長さ100mmのSUS304BA板9に両面粘着テープ1(基材1a、粘着層1b)を貼り合せ、次いでもう一方の離型紙を剥離し、同じサイズのSUS304BA板9に貼り合せ、23℃、50%RHの雰囲気下で60分間養生した。次いで、その下端に1kgfの錘10を吊るし、120℃で30分、135℃で30分加熱し、その変形量をルーペにて目視測定し、加熱時せん断変形率(△Sr)を下記の式にて算出した。
△Sr=(Xi+Xt)/Xi×100
△Sr:加熱時せん断変形率(%)
Xi:仕込みサンプル長(mm)=25(mm)
Xt:サンプル変形量(mm)
両面粘着テープを幅0.5mm、0.6mm、0.8mm、1.0mmで63mm×118mmの枠状に裁断し、一方の離型紙を剥離した。そして図7に示すように、1.5mm厚のポリカーボネート製フック6に両面粘着テープ1を貼り合せ、次いでもう一方の離型紙を剥離し、被着体3(2.0mm厚のガラス板)に貼り合せ、23℃、50%RHの雰囲気下で60分間養生した。そしてガラス製フック6に200gfの荷重(錘4)をかけ、40℃、90%RHの雰囲気下で24時間保持し、以下の基準で耐荷重性を評価した。
「○」:24時間フック6は落下しなかった。
「×」:60分以内にフック6が落下した。
実施例22及び比較例11で得たポリエステル系フィルム基材両面粘着テープを、以下の方法で評価した。結果を表7~8に示す。
(防水性)
「○」:枠内に水が浸入しなかった。
「×」:枠内に水が浸入した。
両面粘着テープのサイズを幅1mmで45mm×65mmの枠状とし、人工皮脂又は人工指脂に24時間浸漬後、サンプルを85℃、85%RHの雰囲気下で72時間静置した他は、<評価試験A>の耐人工皮脂性、耐人工指脂性と同様の方法にて試験を行い、以下の基準で耐人工皮脂性、耐人工指脂性を評価した。
「○」:枠内に人工皮脂液、人工指脂液が浸入しなかった。
「×」:枠内に人工皮脂液、人工指脂液が浸入した。
両面粘着テープを1mm×125mmのサイズで10本に細断した他は、<評価試験A>の加工性と同様の方法にて試験を行い、以下の基準で加工性を評価した。
「○」:隣接した部分との癒着がほとんど無く、隣接部分を剥がすことなく剥離できた。
「×」:隣接した部分に著しい癒着があり、隣接部分が同時に剥がれてしまった。
両面粘着テープを1mm×50mmのサイズで2本裁断し、一方の離型紙を剥離した。そして図8に示すように、被着体3(1.5mm厚のポリカーボネート板)に65mmの間隔で平行に貼り合せ、更にもう一方の離型紙を剥離し、被着体7(1.9mm厚の強化ガラス板)に貼り合せた。この貼り合せした部材を85℃、85%RHの雰囲気下で72時間静置し、その後23℃、50%RH下に1時間放置した。このサンプルの被着体3(1.5mm厚のポリカーボネート板)側に0.5Mの高さから10gfのステンレス球11を自由落下させて衝撃を与え、以下の基準で落球耐衝撃性を評価した。
「○」:衝撃による部材の剥がれ無し。
「×」:衝撃による部材の剥がれ有り。
上記落球耐衝撃性において、23℃、50%RH下に1時間放置した後、更に-20℃環境下に1時間放置した。そして-20℃環境下で、このサンプルの被着体3(1.5mm厚のポリカーボネート板)側に0.3Mの高さから10gfのステンレス球を自由落下させて衝撃を与え、以下の基準で低温落球耐衝撃性を評価した。
「○」:衝撃による部材の剥がれ無し。
「×」:衝撃による部材の剥がれ有り。
1mm×10mmに裁断した両面粘着テープ1の一方の離型紙を剥離し、厚さ75μmで10mm×30mmのポリイミドフィルム5の一方に図4に示すように貼り付け、23℃、50%RHの雰囲気下で60分間養生した。その後、ポリイミドフィルム5を図5に示す形で、折り返し部分(図5で20mmと記載した部分)を4mmとなるように折り曲げて粘着テープ1を被着体3(1.5mm厚のポリカーボネート板)に貼り合せ、85℃の雰囲気下で72時間放置し、接着部分の剥がれを目視にて確認し、以下の基準で耐反発性を評価した。
「○」:72時間後に接着部分の剥がれ無し。
「×」:72時間後に接着部分の剥がれ有り。
両面粘着テープのサイズを幅1mmで45mm×65mmの枠状とし、200gfの荷重(錘4)、試験環境を85℃で24時間とした他は、<評価試験A>の狭額縁耐湿熱荷重性と同様の方法にて試験を行い、以下の基準で狭額縁耐荷重性を評価した。
「○」:24時間フック6は落下しなかった。
「×」:60分以内にフック6が落下した。
両面粘着テープのサイズを幅1mmで45mm×65mmの枠状とし、50gfの荷重(錘4)、試験環境を85℃、85%RHで24時間とした他は、<評価試験A>の狭額縁耐湿熱荷重性と同様の方法にて試験を行い、以下の基準で狭額縁耐湿熱荷重性を評価した。
「○」:24時間フック6は落下しなかった。
「×」:60分以内にフック6が落下した。
1a 基材
1b 粘着剤層
2 SUS304製フック
3 被着体
4 錘
5 ポリイミドフィルム
6 1.5mm厚ポリカーボネート製フック
7 1.9mm厚強化ガラス板
8 2.0mm厚SUS304板
9 0.5mm厚SUS304BA板
10 1kgf錘
11 10gfステンレス球
Claims (7)
- 炭素原子数が1~3のアルキル基を有する(メタ)アクリル酸アルキルエステル(A1)10~20質量%、炭素原子数が4~12のアルキル基を有する(メタ)アクリル酸アルキルエステル(A2)50~80質量%、カルボキシル基含有モノマー(A3)10~15質量%、水酸基含有モノマー(A4)0.01~0.5質量%、及び、酢酸ビニル(A5)1~5質量%をポリマー鎖の構成成分として含み、過酸化物系重合開始剤を用いて得られる共重合体の重量平均分子量が95万~200万、理論Tgが-55℃以下である、アクリル系共重合体(A)と、
架橋剤(B)と、
シランカップリング剤(C)と、
酸化防止剤(D)
を含有する粘着剤組成物。 - シランカップリング剤(C)がグリシジル基を含み、その配合量がアクリル系共重合体(A)100質量部に対して0.01~0.05質量部である請求項1記載の粘着剤組成物。
- 架橋剤(B)が、少なくともイソシアネート系架橋剤を含む請求項1記載の粘着剤組成物。
- 酸化防止剤(D)が、ヒンダードフェノール系酸化防止剤を含む請求項1記載の粘着剤組成物。
- ポリオレフィン系樹脂基材の片面又は両面に、請求項1記載の粘着剤組成物により形成された粘着剤層を有する粘着テープであって、
前記ポリオレフィン系樹脂基材のMD方向及びTD方向の曲げモーメントが5gf/cm以上であり、前記粘着テープの加熱時せん断変形率が150%以下であり、割裂力が70N/cm2以上である粘着テープ。 - 粘着剤層の厚さが5~100μmである請求項5記載の粘着テープ。
- ポリエステル系樹脂基材の片面又は両面に、請求項1記載の粘着剤組成物により形成された粘着剤層を有する粘着テープ。
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CN201480083756.5A CN107001889B (zh) | 2014-11-25 | 2014-11-25 | 粘着剂组合物及粘着带 |
JP2016561106A JP6307175B2 (ja) | 2014-11-25 | 2014-11-25 | 粘着剤組成物及び粘着テープ |
PCT/JP2014/081012 WO2016084123A1 (ja) | 2014-11-25 | 2014-11-25 | 粘着剤組成物及び粘着テープ |
KR1020177003097A KR102316411B1 (ko) | 2014-11-25 | 2014-11-25 | 점착제 조성물 및 점착 테이프 |
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WO2019131166A1 (ja) * | 2017-12-25 | 2019-07-04 | Dic株式会社 | 粘着テープ及び物品 |
WO2020004056A1 (ja) * | 2018-06-28 | 2020-01-02 | Dic株式会社 | 粘着テープ及び物品 |
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TW201623522A (zh) | 2016-07-01 |
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