WO2019167621A1 - Feuille adhésive thermoplastique et utilisation associée - Google Patents

Feuille adhésive thermoplastique et utilisation associée Download PDF

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Publication number
WO2019167621A1
WO2019167621A1 PCT/JP2019/005029 JP2019005029W WO2019167621A1 WO 2019167621 A1 WO2019167621 A1 WO 2019167621A1 JP 2019005029 W JP2019005029 W JP 2019005029W WO 2019167621 A1 WO2019167621 A1 WO 2019167621A1
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WIPO (PCT)
Prior art keywords
adhesive sheet
thermoplastic adhesive
adhesive
weight
adhesive layer
Prior art date
Application number
PCT/JP2019/005029
Other languages
English (en)
Japanese (ja)
Inventor
祥平 和田
逸大 畑中
裕行 椿
直幸 西山
Original Assignee
日東電工株式会社
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 日東電工株式会社 filed Critical 日東電工株式会社
Priority to KR1020207027436A priority Critical patent/KR20200125657A/ko
Priority to CN201980015498.XA priority patent/CN111770973B/zh
Publication of WO2019167621A1 publication Critical patent/WO2019167621A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • C09J11/08—Macromolecular additives
    • 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
    • C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02—Vinyl aromatic monomers and conjugated dienes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • 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
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/35—Heat-activated
    • 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
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • 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
    • C09J2301/304—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 the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
    • 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 thermoplastic adhesive sheet and a fabric joined by the thermoplastic adhesive sheet.
  • Patent Document 1 proposes a fabric bonding tape in which a pressure-sensitive adhesive layer is provided on the surface of a hot-melt adhesive in order to obtain temporary adhesion.
  • a pressure-sensitive adhesive hereinafter referred to as “pressure-sensitive adhesive” which exhibits a soft solid (viscoelastic body) state in a temperature range near room temperature and has a property of easily adhering to an adherend by pressure. It is also referred to as an “adhesive”.
  • pressure-sensitive adhesive which exhibits a soft solid (viscoelastic body) state in a temperature range near room temperature and has a property of easily adhering to an adherend by pressure. It is also referred to as an “adhesive”.
  • a pressure-sensitive adhesive containing a styrene block copolymer.
  • thermoplastic adhesives as described in Patent Document 1.
  • Such a thermoplastic adhesive is aligned with the joint location of the fabric and then impregnated into the fabric by hot pressing to join the fabrics together.
  • the thermoplastic adhesive as described above usually has no tack and does not adhere to a rough surface such as a fabric at room temperature. Therefore, another means such as the surface pressure-sensitive adhesive layer used in Patent Document 1 is necessary for temporary adhesion for alignment and the like.
  • an adhesive obtained by impregnating a stretchable material such as a fabric by hot pressing is difficult to follow the stretch of the adherend material because of its hardness at normal temperature. For this reason, the stretchability of the adherend material can be reduced at the joint location by the adhesive. Such a change causes a feeling of discomfort in the clothing using the fabric.
  • the present invention was created in view of the above circumstances, and has an object to provide a thermoplastic adhesive sheet having temporary adhesiveness and deformation recovery and capable of exhibiting a good adhesive function. And Another object of the present invention is to provide a fabric joined by a thermoplastic adhesive sheet.
  • thermoplastic adhesive sheet (hereinafter also simply referred to as “adhesive sheet”) having a thermoplastic adhesive (hereinafter also simply referred to as “adhesive”) layer is provided.
  • This thermoplastic adhesive sheet has the following characteristics: (A) The thermoplastic adhesive sheet was bonded to a polyester urethane foam having a thickness of 10 mm in an environment of 23 ° C. and 50% RH by reciprocating a 2 kg roller, and left in the same environment for 30 minutes.
  • a peel strength measured under the conditions of 300 mm / min and a peel angle of 180 degrees is 2N / 10 mm or more; and (B) a thermoplastic adhesive sheet measurement sample having a measurement length of 100 mm is prepared, When stretched 50% at a speed of 300 mm / min at 23 ° C., held for 3 seconds, and then shrunk at a speed of 300 mm / min, the shrinkage strength F S30% with respect to the stretch strength F E30% at 30% stretch length The hysteresis determined from the ratio [ FS30% / FE30% ] is 35% or more; Satisfied.
  • the adhesive sheet has a tack at room temperature (about 23 ° C.), for example, good temporary adhesion to a rough surface of a fabric or the like by hand-bonding at room temperature. Showing gender.
  • the adhesive sheet bonded to the adherend material by temporary adhesion is joined to the adherend with high positional accuracy by subsequent adhesion by hot pressing or the like (also referred to as “main adhesion”).
  • main adhesion good adhesion and fixation can be realized by utilizing the thermoplastic properties of the thermoplastic adhesive sheet.
  • the adherend surface is rough or the adherend is an impregnated material, the adhesive sheet spreads by heating or penetrates into the adherend and exhibits good adhesion performance.
  • the impregnated material refers to a material having a property that allows impregnation of a fluid (typically a liquid).
  • the adhesive sheet is deformed in accordance with the deformation (for example, expansion / contraction) of the material in an aspect in which the material is attached to a material having deformation recovery properties such as an elastic material, a rubber elastic material, etc. After that, the original shape can be recovered together with the adherend material. That is, the adhesive sheet does not interfere with the shape recovery (for example, stretchability) of the adherend material.
  • Such deformation recovery ability that can follow the deformation recovery (for example, stretchability) of the adherend may be one that does not impair the comfort of clothing (particularly underwear).
  • a thermoplastic adhesive sheet satisfying the above characteristics can exhibit a good adhesive function while having both temporary adhesiveness and deformation recovery property.
  • the thermoplastic adhesive sheet according to a preferred embodiment has the following characteristics: (C) For a thermoplastic adhesive sheet measurement sample having a measurement length of 100 mm, a 30% modulus measured at a rate of 300 mm / min at 23 ° C. is 0.6 MPa or less; To be more satisfied. Since the adhesive sheet satisfying the above property (C) is excellent in flexibility, the flexibility of the material is not impaired when used for bonding a material having flexibility such as a fabric. For example, when the adhesive sheet is used in such a manner that the adherend material is impregnated, it is advantageous that flexibility can be secured in the material. As an example of the effect by this structure, reduction of the hardness (strength) which the adhesive agent provided to the conventional fabric had was mentioned.
  • thermoplastic adhesive sheet has the following characteristics: (D) The thermoplastic adhesive sheet was pressure-bonded to a stainless steel plate under the conditions of 120 ° C., 0.2 MPa, and 10 seconds, left at 23 ° C. for 30 minutes, and then measured under the conditions of a tensile speed of 300 mm / min and a peeling angle of 180 degrees. The peel strength is 15 N / 10 mm or more; To be more satisfied. Since the thermoplastic adhesive sheet satisfying the above property (D) can be firmly bonded to an adherend having a rough surface such as a fabric by thermocompression bonding, it has excellent adhesion reliability.
  • the thermoplastic adhesive layer is a rubber adhesive layer containing a rubber polymer as a base polymer.
  • the thermoplastic adhesive layer more preferably contains a block copolymer of a monovinyl-substituted aromatic compound and a conjugated diene compound as a base polymer.
  • the thermoplastic adhesive layer contains a tackifying resin T LOH having a hydroxyl value of 30 mgKOH / g or less as a tackifying resin.
  • a tackifier resin having a hydroxyl value of a predetermined value or less By using a tackifier resin having a hydroxyl value of a predetermined value or less, deterioration of the adhesive sheet is preferably suppressed.
  • thermoplastic adhesive layer is a non-crosslinkable adhesive layer.
  • a non-crosslinkable adhesive is likely to obtain good adhesive force by thermocompression bonding.
  • the thermoplastic adhesive sheet has a thickness of 0.03 mm to 1 mm.
  • the thickness of the adhesive sheet By setting the thickness of the adhesive sheet to a predetermined value or more, the temporary adhesive property and the main adhesive property tend to be improved. Moreover, the deformation
  • thermoplastic adhesive sheet is configured as a base material-less adhesive sheet composed only of an adhesive layer.
  • said each characteristic can be satisfied preferably, and the effect by the technique disclosed here can be exhibited preferably.
  • thermoplastic adhesive sheet disclosed herein Since the thermoplastic adhesive sheet disclosed herein has temporary adhesiveness and can exhibit a good adhesive function, it is preferably used for joining fabrics that require alignment by temporary adhesion. The adhesive sheet is also excellent in deformation recovery. Therefore, it is preferable for the use of joining a stretchable fabric (preferably underwear).
  • the adhesive sheet By applying the technology disclosed here to fabric bonding, the adhesive sheet is accurately aligned using the temporary adhesive property, and then the fabric is impregnated into the fabric through main bonding by heating. Thus, it exhibits a good adhesive force and further follows the stretchability of the fabric. This leads to, for example, not impairing the comfort of clothing made using the fabric.
  • a fabric joined by any of the thermoplastic adhesive sheets disclosed herein is provided.
  • the joining of the fabrics may be a joining of one fabric and another cloth, or may be a joining of a part of one cloth and another part.
  • thermoplastic adhesive sheet baseless double-sided adhesive sheet
  • thermoplastic adhesive sheet double-sided adhesive sheet with a base material
  • thermoplastic adhesive sheet single-sided adhesive sheet with a base material
  • thermoplastic adhesive refers to an adhesive that softens and plastically deforms by heating at a predetermined temperature or higher.
  • the thermoplastic adhesive is a material having a property of being cured again when cooled to a melting temperature or lower, and reversibly softening and curing by heat.
  • the thermoplastic adhesive disclosed herein may exhibit fluidity at a temperature of about 80 ° C. or higher (eg, about 100 ° C. or higher, typically about 120 ° C. or higher).
  • the thermoplastic properties are usually controlled by appropriately setting conditions (temperature, pressure, time, etc.) during main bonding.
  • the thermoplastic adhesive has a weight fraction (gel fraction) of an organic solvent insoluble matter measured by immersing in an organic solvent such as toluene for 1 week (approximately 0%, for example, 0). ⁇ 1%).
  • the gel fraction is measured using a porous polytetrafluoroethylene membrane (for example, trade name “Nitoflon NTF1122” manufactured by Nitto Denko Corporation, average pore diameter 0.2 ⁇ m, porosity 75%).
  • the “pressure-sensitive adhesive” is a material that exhibits a soft solid (viscoelastic body) state in the temperature range near room temperature and has a property of easily adhering to an adherend by pressure as described above.
  • Pressure sensitive adhesive referred to here, "C A. Dahlquist,.” Adhesion: Fundamental and Practice “, McLaren & Sons, (1966) P. 143 ,” as defined in the, in general, the complex tensile modulus E * ( 1 Hz) ⁇ 10 7 dyne / cm 2 (typically a material having the above properties at 25 ° C.).
  • the pressure-sensitive adhesive in the technology disclosed herein can also be grasped as a solid component of the adhesive composition or a constituent component of the adhesive layer.
  • an adhesive and an adhesive layer that satisfy the following property (A) are typical examples of the pressure-sensitive adhesive and the pressure-sensitive adhesive layer.
  • a block copolymer of a monovinyl-substituted aromatic compound and a conjugated diene compound refers to a monovinyl-substituted aromatic compound as a main monomer (more than 50% by weight of a copolymer component; the same applies hereinafter).
  • a segment a segment
  • B segment a segment having a conjugated diene compound as a main monomer
  • the glass transition temperature of the A segment is higher than the glass transition temperature of the B segment.
  • a triblock copolymer having an A segment (hard segment) at each end of a B segment (soft segment), one A
  • examples thereof include a copolymer having a diblock structure composed of a segment and one B segment (diblock body having an AB structure).
  • the “styrene block copolymer” means a polymer having at least one styrene block.
  • the styrene block refers to a segment having styrene as a main monomer.
  • a segment consisting essentially of styrene is a typical example of a styrene block as used herein.
  • the “styrene isoprene block copolymer” refers to a polymer having at least one styrene block and at least one isoprene block (a segment having isoprene as a main monomer).
  • styrene isoprene block copolymers are triblock copolymer (triblock body) having styrene blocks (hard segment) at both ends of isoprene block (soft segment), one isoprene block and one styrene. Examples thereof include a diblock copolymer (diblock body) composed of blocks.
  • the “styrene butadiene block copolymer” refers to a polymer having at least one styrene block and at least one butadiene block (a segment containing butadiene as a main monomer).
  • the “styrene content” of the styrenic block copolymer refers to the weight ratio of the styrene component to the total weight of the block copolymer.
  • the styrene content can be measured by NMR (nuclear ceramic resonance spectrum method).
  • the ratio of the diblock body in the styrene block copolymer (hereinafter sometimes referred to as “diblock body ratio” or “diblock ratio”) is determined by the following method.
  • a styrene block copolymer is dissolved in tetrahydrofuran (THF), and GS5000H and G4000H liquid chromatograph columns manufactured by Tosoh Corporation are connected in two stages, for a total of four stages, and THF is used as the mobile phase. Then, high performance liquid chromatography is performed under conditions of a temperature of 40 ° C. and a flow rate of 1 mL / min. The peak area corresponding to the diblock body is measured from the obtained chart. And the diblock body ratio is calculated
  • the adhesive sheet disclosed herein (which may be in a long form such as a tape shape) is, for example, a substrate-less (that is, no substrate) double-sided adhesive sheet 1 as shown in FIG. It can be in form.
  • the adhesive sheet 1 is a base material-less adhesive sheet made of a thermoplastic adhesive layer 11.
  • the adhesive layer 11 typically has a single layer structure.
  • the double-sided adhesive sheet 1 before use (before being attached to an adherend) is such that the first adhesive surface 11A and the second adhesive surface 11B of the adhesive layer 11 are peeled off at least on the surface (front surface) on the adhesive layer side. It may be in a form protected by the release liners 21 and 22 as surfaces.
  • the release liner 22 is omitted, the release liner 21 having both surfaces as release surfaces is used, and this and the adhesive layer 11 are overlapped and wound in a spiral shape so that the second adhesive surface 11B is the release liner. 21 may be in contact with the back surface of 21 and protected.
  • the technique disclosed herein can be preferably applied to a base-less double-sided adhesive sheet as shown in FIG. 1 as well as a double-sided adhesive sheet 2 with a base as shown in FIG.
  • the double-sided adhesive sheet 2 includes a base material (for example, polyurethane film) 15 and a first adhesive layer 11 and a second adhesive layer 12 supported on both sides of the base material 15, respectively. More specifically, the first adhesive layer 11 and the second adhesive layer 12 are respectively provided on the first surface 15A and the second surface 15B (both non-peelable) of the substrate 15.
  • the double-sided adhesive sheet 2 before use has at least the surface (adhesive surface) 11A of the first adhesive layer 11 and the surface (adhesive surface) 12A of the second adhesive layer 12 at least
  • the adhesive layer side surface (front surface) may be in a form protected by a release liner having a release surface.
  • the first adhesive layer is formed by using a release liner 21 whose both surfaces are release surfaces, and superimposing this on the first adhesive layer 11 and winding it in a spiral shape.
  • the surface 11A of 11 may be in contact with the back surface of the release liner 21 and protected.
  • the technology disclosed herein also includes a base material 15 and a single-sided adhesive type base material including an adhesive layer 11 supported on a first surface (non-peeling surface) 15 ⁇ / b> A of the base material.
  • the adhesive sheet 3 can also be applied.
  • the adhesive sheet 3 before use has a release liner in which the surface (adhesive surface) 11A of the adhesive layer 11 is at least the surface (front surface) on the adhesive layer side. 21 may be the protected form.
  • the release liner 21 is omitted, and the first adhesive surface 11A is the second of the base material 15 by winding the adhesive sheet 3 with the base material 15 using the base material 15 having the second surface 15B as the release surface. It may be in a form protected against the surface 15B.
  • the total thickness of the adhesive sheet disclosed herein is not particularly limited, and is suitably about 3 mm or less, preferably about 1 mm, from the viewpoint of thinning, miniaturization, weight reduction, resource saving, and the like. Hereinafter, it is more preferably about 0.7 mm or less, and still more preferably about 0.5 mm or less (for example, about 0.4 mm or less).
  • the adhesive layer with a limited thickness is also limited in the amount of impregnation of the adherend such as fabric during thermocompression bonding, for example, so that the influence of the impregnation on the deformation recovery property (for example, stretchability) of the adherend is also affected. There is a small tendency.
  • the total thickness is suitably about 0.01 mm or more, preferably about 0.03 mm or more, more preferably about 0.05 mm or more, More preferably, it is about 0.1 mm or more.
  • the thickness of an adhesive bond layer and a base material is included in the total thickness of an adhesive sheet, the thickness of a release liner is not included.
  • the adhesive sheet disclosed herein is characterized by having an adhesive force to the foam (vs. foam adhesive force) of about 2 N / 10 mm or more. Since the foam surface is a rough surface, an adhesive sheet satisfying the above characteristics exhibits good temporary adhesion by hand-bonding at a normal temperature to a rough surface such as a fabric. Thereby, accurate alignment with respect to the adherend surface is possible.
  • the adhesive strength with respect to foam is preferably about 3 N / 10 mm or more, more preferably about 4 N / 10 mm or more.
  • the adhesive force to the foam may be about 5 N / 10 mm or more, but is appropriate to be about 10 N / 10 mm or less, preferably about 8 N / 10 mm or less (eg, about 6N / 10 mm or less).
  • the property (A) is specifically measured by the following method. That is, a thermoplastic adhesive sheet is cut into a size of 100 mm ⁇ 10 mm to prepare a measurement sample. When the object to be measured is a double-sided adhesive sheet, one side (non-measurement adhesive surface) is attached to a polyethylene terephthalate (PET) film having a thickness of 25 ⁇ m and backed. Next, in an environment of 23 ° C. and 50% RH, the surface of the thermoplastic adhesive layer to be measured is exposed, and the exposed adhesive surface is 2 kg on the surface of a polyester urethane foam having a thickness of 10 mm as an adherend. The roller is reciprocated once and bonded together (crimping).
  • PET polyethylene terephthalate
  • the peel strength (adhesive strength to foam) [N / 10 mm] was measured under the conditions of a tensile speed of 300 mm / min and a peel angle of 180 degrees. taking measurement.
  • a polyester-based flexible urethane foam (trade name “SC” (gray), density 31 kg / m 3 manufactured by Inoac Corporation) is used.
  • the universal tensile / compression tester a commercially available device (for example, a device name “Tensile / Compression Tester, TG-1kN” manufactured by Minebea Co., Ltd.) can be used. In the examples described later, the same method is used.
  • the adhesive sheet disclosed herein is characterized by having a hysteresis (30% hysteresis at 50% elongation) measured by the following method of about 35% or more.
  • a hysteresis (30% hysteresis at 50% elongation) measured by the following method of about 35% or more.
  • the 30% hysteresis at 50% elongation is preferably about 40% or more, more preferably about 50% or more (for example, 55% or more).
  • the hysteresis is ideally 100%, but may be about 80% or less, for example, about 70% or less from the viewpoint of compatibility with other characteristics such as temporary adhesion.
  • the characteristic (B) (30% hysteresis at 50% elongation) is specifically measured by the following method. That is, the thermoplastic adhesive sheet is cut into a width of 50 mm so as to have a measurement length of 100 mm, and wound in the width direction to form a measurement sample as a column. Although this measurement depends on the length of the measurement sample, since it does not depend on the cross-sectional area (that is, thickness and width), a width other than 50 mm may be adopted as long as the measurement is not hindered. For the same reason, it is not necessary to form a winding or a column if it does not interfere with the measurement.
  • the prepared measurement sample is set in a tensile / compression tester so that the distance between chucks (measurement length) is 100 mm, and is stretched by 50% at a speed of 300 mm / min at 23 ° C. (thus stretching to 150 mm). After holding for 3 seconds in the stretched state, the shrinking operation is performed at a speed of 300 mm / minute, and the stretching is returned to 0% (distance between chucks: 100 mm).
  • the extension strength F E30% [N] at 30% extension length (130 mm) and the contraction strength F S30% [N] at 30% extension length are recorded, and the extension strength F E30% [N] is recorded.
  • the hysteresis value (%) is obtained from the following formula from the ratio of shrinkage strength F S30% to [F S30% / F E30% ].
  • Hysteresis value (%) F S30% / F E30% ⁇ 100
  • a commercially available apparatus for example, apparatus name “Tensile / Compression Tester, TG-1kN” manufactured by Minebea Co., Ltd.
  • TG-1kN manufactured by Minebea Co., Ltd.
  • the adhesive sheet according to a preferred embodiment has a 30% modulus of 0.6 MPa or less.
  • the 30% modulus is more preferably about 0.5 MPa or less, and still more preferably about 0.45 MPa or less (for example, 0.4 MPa or less).
  • the 30% modulus is usually about 0.1 MPa or more, preferably about 0.2 MPa or more, more preferably about 0.3 MPa, from the viewpoint of compatibility with other characteristics such as deformation recovery. It can be above (for example, 0.35 MPa or more).
  • Property (C) (30% modulus) is measured at a rate of 300 mm / min at 23 ° C. for a thermoplastic adhesive sheet measurement sample having a measurement length of 100 mm. Specifically, in the measurement of the above characteristic (B), 30% modulus is obtained by dividing the tensile strength F E30% [N] at 30% stretch length (130 mm) by the cross-sectional area [mm 2 ] of the adhesive sheet. [MPa] can be obtained. Since the 30% modulus does not depend on the length of the measurement sample, the distance between chucks of the tension / compression tester may be appropriately changed during measurement. Moreover, since it is divided by the cross-sectional area, the width and thickness can be changed within a range that does not hinder measurement. For the same reason, there is no need to make a winding or a column as long as the measurement is not hindered. Other measurement conditions are basically the same as the measurement of the characteristic (B). In the examples described later, the same method is used.
  • the adhesive sheet according to a preferred embodiment has a thermocompression adhesive force (relative to SUS thermocompression adhesive force) to stainless steel of about 15 N / 10 mm or more measured under the thermocompression bonding conditions of 120 ° C., 0.2 MPa, and 10 seconds.
  • the adhesive strength against SUS thermocompression bonding is highly correlated with the thermocompression bonding strength against a rough surface such as fabric, although the absolute value is different. Since the thermoplastic adhesive sheet satisfying this characteristic tends to exhibit a thermocompression bonding force of a predetermined level or more even on a rough surface such as a fabric, the adherend having the rough surface in the main bonding after temporary fixing. It can be firmly bonded to.
  • the adhesive strength against SUS thermocompression bonding is more preferably about 18 N / 10 mm or more, more preferably about 20 N / 10 mm or more, and particularly preferably about 22 N / 10 mm or more, for example, about 25 N / 10 mm or more. It may be about 28 N / 10 mm or more, or about 30 N / 10 mm or more.
  • the upper limit of the adhesive strength against SUS thermocompression bonding is not particularly limited, and may be, for example, about 50 N / 10 mm or less.
  • the characteristic (D) (vs. SUS thermocompression bonding strength) is specifically measured by the following method. That is, a thermoplastic adhesive sheet is cut into a size of 100 mm ⁇ 10 mm to prepare a measurement sample. When the object to be measured is a double-sided adhesive sheet, one side (non-measurement adhesive surface) is attached to a 50 ⁇ m thick PET film and backed. Next, in an environment of 23 ° C. and 50% RH, the surface of the thermoplastic adhesive layer to be measured is exposed, and the exposed adhesive surface is 120 ° C. on the surface of a stainless steel plate (SUS304 plate) as an adherend. Thermocompression bonding is performed at 0.2 MPa for 10 seconds.
  • SUS304 plate stainless steel plate
  • peel strength [N / 10 mm under conditions of a tensile speed of 300 mm / min and a peel angle of 180 degrees] ]
  • a commercially available apparatus for example, apparatus name “Tensile / Compression Tester, TG-1kN” manufactured by Minebea Co., Ltd.
  • TG-1kN tensile speed
  • the type of adhesive constituting the thermoplastic adhesive layer disclosed herein is not particularly limited.
  • the adhesive layer is, for example, acrylic, polyester, urethane, polyether, olefin, rubber, silicone, polyamide, fluorine, vinyl acetate, vinyl chloride, vinyl alcohol, vinyl acetal.
  • the technique disclosed here can be preferably implemented in the form of an adhesive sheet including an adhesive layer including, for example, an acrylic polymer, a polyester polymer, a urethane polymer, or a rubber polymer as a base polymer. Especially, it can implement especially preferably in the form of the adhesive sheet provided with the rubber-type adhesive layer which contains a rubber-type polymer as a base polymer.
  • Examples of the base polymer contained in the rubber-based adhesive layer include natural rubber; styrene butadiene rubber; polyisoprene; acrylonitrile butadiene rubber; chloroprene rubber; butene (1-butene and cis- or trans-2-butene.
  • butene-based polymers having 2-methylpropene (isobutylene) as the main monomer; AB type and ABA type block copolymer rubbers and their hydrides, such as styrene-butadiene-styrene blocks Copolymer rubber (SBS), Styrene-isoprene-styrene block copolymer rubber (SIS), SBS hydride styrene-ethylene-butylene-styrene block copolymer rubber, SIS hydride styrene-ethylene -Propylene-styrene block co-weight Body rubber; various rubber polymers and the like. These rubber polymers can be used singly or in combination of two or more.
  • SBS styrene-butadiene-styrene blocks Copolymer rubber
  • SIS Styrene-isoprene-styrene block copolymer rubber
  • the adhesive layer which concerns on one preferable aspect contains the block copolymer of a monovinyl substituted aromatic compound and a conjugated diene compound as a base polymer.
  • the monovinyl substituted aromatic compound refers to a compound in which one functional group having a vinyl group is bonded to an aromatic ring.
  • a typical example of the aromatic ring is a benzene ring (which may be a benzene ring substituted with a functional group having no vinyl group (for example, an alkyl group)).
  • Specific examples of the monovinyl substituted aromatic compound include styrene, ⁇ -methylstyrene, vinyl toluene, vinyl xylene and the like.
  • Specific examples of the conjugated diene compound include 1,3-butadiene and isoprene.
  • Such a block copolymer can be used for a base polymer individually by 1 type or in combination of 2 or more types.
  • the A segment (hard segment) in the block copolymer has a copolymerization ratio of the monovinyl-substituted aromatic compound (two or more can be used in combination) of about 70% by weight or more (more preferably about 90% by weight or more). And it may be substantially 100% by weight.)
  • the B segment (soft segment) in the block copolymer has a copolymerization ratio of the conjugated diene compound (two or more can be used in combination) of about 70% by weight or more (more preferably about 90% by weight or more). It may be substantially 100% by weight). With such a block copolymer, a higher performance adhesive sheet can be realized.
  • the block copolymer may be in the form of a diblock body, a triblock body, a radial body, a mixture thereof, and the like.
  • an A segment for example, a styrene block
  • the block copolymer in the technique disclosed herein it is appropriate to use a block copolymer having a diblock ratio of about 30% by weight or more from the viewpoint of adhesive strength (peel strength) to the adherend.
  • the block body ratio is preferably about 40% by weight or more, more preferably about 50% by weight or more, still more preferably about 60% by weight or more, and particularly preferably about 65% by weight or more. From the viewpoint of peel strength, a block copolymer having a diblock ratio of about 70% by weight or more is most preferable. From the viewpoint of cohesiveness and the like, a block copolymer having a diblock body ratio of about 90% by weight or less (more preferably about 85% by weight or less, for example, about 80% by weight or less) can be preferably used.
  • the base polymer is a styrenic block copolymer.
  • the base polymer includes at least one of a styrene isoprene block copolymer and a styrene butadiene block copolymer is preferable.
  • the proportion of the styrene isoprene block copolymer is about 70% by weight or more, the proportion of the styrene butadiene block copolymer is 70% by weight or more, or
  • the total ratio of the styrene isoprene block copolymer and the styrene butadiene block copolymer is preferably about 70% by weight or more.
  • substantially all (for example, about 95 to 100% by weight) of the styrenic block copolymer is a styrene isoprene block copolymer.
  • the styrene content of the styrenic block copolymer can be, for example, about 5 to 40% by weight. From the viewpoint of cohesiveness, usually, a styrene block copolymer having a styrene content of about 10% by weight or more (more preferably more than 10% by weight, for example, 12% by weight or more) is preferable. From the viewpoint of peel strength, the styrene content is preferably about 35% by weight or less (typically about 30% by weight or less, more preferably about 25% by weight or less), and about 20% by weight or less (typically Less than 20% by weight, for example 18% by weight or less) is particularly preferred.
  • a rubber-like polymer other than the block copolymer is used. 1 type or 2 types or more may be contained.
  • Such rubbery polymers are acrylic, polyester, urethane, polyether, olefin, rubber, silicone, polyamide, fluorine, vinyl acetate, vinyl chloride, vinyl, which are well known in the adhesive field.
  • Various polymers such as alcohol, vinyl acetal, and vinyl butyral may be used.
  • the rubber-based rubbery polymer examples include natural rubber, acrylonitrile butadiene rubber, isoprene rubber, chloroprene rubber, polyisobutylene, butyl rubber, recycled rubber and the like.
  • the amount of the rubbery polymer used is usually about 50 parts by weight or less per 100 parts by weight of the block copolymer. Preferably, it is about 30 parts by weight or less, more preferably about 10 parts by weight or less (for example, about 5 parts by weight or less).
  • the technique disclosed herein is an embodiment in which the adhesive layer does not substantially contain a rubbery polymer other than the block copolymer (for example, the content per 100 parts by weight of the block copolymer is 0 to 1 weight). Part of the embodiment).
  • the adhesive layer disclosed herein preferably contains a tackifying resin in addition to the base polymer.
  • the tackifying resin is selected from various known tackifying resins such as petroleum resins, styrene resins, coumarone / indene resins, terpene resins, modified terpene resins, rosin resins, rosin derivative resins, and ketone resins. Species or two or more can be used.
  • Examples of petroleum resins include aliphatic (C5) petroleum resins, aromatic (C9) petroleum resins, aliphatic / aromatic copolymer (C5 / C9) petroleum resins, and hydrogenated products thereof ( Examples thereof include alicyclic petroleum resins obtained by hydrogenating aromatic petroleum resins.
  • styrenic resins include those based on homopolymers of styrene, those based on homopolymers of ⁇ -methylstyrene, those based on homopolymers of vinyltoluene, styrene, Those containing as a main component a copolymer containing at least two of ⁇ -methylstyrene and vinyltoluene in the monomer composition (for example, ⁇ -methylstyrene / styrene copolymer containing ⁇ -methylstyrene / styrene copolymer as the main component) Polymer resin) and the like.
  • a resin containing coumarone and indene can be used as a monomer component constituting the resin skeleton (main chain).
  • monomer components that can be included in the resin skeleton other than coumarone and indene include styrene, ⁇ -methylstyrene, methylindene, and vinyltoluene.
  • terpene resin examples include ⁇ -pinene polymer, ⁇ -pinene polymer, dipentene polymer and the like.
  • modified terpene resin examples include those obtained by modifying the terpene resin (phenol modification, styrene modification, hydrogenation modification, hydrocarbon modification, etc.). Specific examples include terpene phenol resins, styrene-modified terpene resins, hydrogenated terpene resins, and the like.
  • terpene phenol resin refers to a polymer containing a terpene residue and a phenol residue.
  • a copolymer of terpene and a phenol compound (terpene-phenol copolymer resin) and a terpene homopolymer or copolymer It is a concept that includes both a combination (terpene resin, typically unmodified terpene resin) and phenol-modified (phenol-modified terpene resin).
  • terpene constituting the terpene phenol resin include monoterpenes such as ⁇ -pinene, ⁇ -pinene and limonene (including d-form, l-form and d / l-form (dipentene)).
  • rosin resin examples include unmodified rosins such as gum rosin, wood rosin and tall oil rosin (raw rosin); modified rosins modified by hydrogenation, disproportionation, polymerization, etc. (hydrogenation) Rosin, disproportionated rosin, polymerized rosin, and other chemically modified rosins).
  • rosin derivative resins include those obtained by esterifying unmodified rosin with alcohols (that is, rosin esterified products) and modified rosins (hydrogenated rosin, disproportionated rosin, polymerized rosin, etc.) with alcohols.
  • Rosin esters such as esterified products (ie, esterified products of modified rosin); Unmodified rosin or modified rosin (hydrogenated rosin, disproportionated rosin, polymerized rosin, etc.) modified with unsaturated fatty acid Rosins; Unsaturated fatty acid-modified rosin esters obtained by modifying rosin esters with unsaturated fatty acids; Unmodified rosin, modified rosin (hydrogenated rosin, disproportionated rosin, polymerized rosin, etc.), unsaturated fatty acid-modified rosin or Rosin alcohols with reduced carboxyl groups in saturated fatty acid-modified rosin esters; unmodified rosin, modified Metal salts of rosins (particularly rosin esters) such as gin and various rosin derivatives; obtained by adding phenol to an rosin (unmodified rosin, modified rosin, various rosin derivatives, etc.) with an acid catalyst and thermal poly
  • the adhesive layer may contain a tackifying resin TLOH having a hydroxyl value of about 30 mgKOH / g or less.
  • a tackifier resin having a hydroxyl value of a predetermined value or less deterioration of the adhesive sheet is preferably suppressed.
  • Tackifying resin TLOH can be used individually by 1 type or in combination of 2 or more types.
  • the hydroxyl value of the tackifier resin T LOH is preferably about 20 mgKOH / less than g, and more preferably about less than 15 mgKOH / g, more preferably about less than 10 mgKOH / g, particularly preferably about less than 5 mgKOH / g (e.g., less than 3 mgKOH / g ).
  • hydroxyl value or is less than 1 mgKOH / g, or hydroxyl group may be used preferably undetectable tackifier resin T LOH.
  • a value measured by a potentiometric titration method defined in JIS K0070: 1992 can be adopted.
  • the specific measurement method is as follows. [Measurement method of hydroxyl value] 1.
  • Reagent (1) As an acetylating reagent, about 12.5 g (about 11.8 mL) of acetic anhydride is taken, and pyridine is added thereto to make a total volume of 50 mL, and the mixture is sufficiently stirred. Alternatively, about 25 g (about 23.5 mL) of acetic anhydride is taken, and pyridine is added thereto to make a total volume of 100 mL, and the mixture is sufficiently stirred.
  • Hydroxyl value [(BC) ⁇ f ⁇ 28.05] / S + D here, B: Amount of 0.5 mol / L potassium hydroxide ethanol solution used for the blank test (mL), C: The amount of 0.5 mol / L potassium hydroxide ethanol solution used for the sample (mL), f: factor of 0.5 mol / L potassium hydroxide ethanol solution, S: weight of the sample (g), D: Acid value, 28.05: 1/2 of the molecular weight of potassium hydroxide 56.11, It is.
  • Adhesive layer as the tackifier resin T LOH, softening point containing tackifier resin T LOH1 above 120 ° C..
  • the softening point of the tackifier resin T LOH1 is more preferably about 130 ° C. or more, more preferably about 140 ° C. or more. Particularly preferred is about 145 ° C. or higher (eg, 150 ° C. or higher).
  • the softening point of the tackifying resin T LOH1 is usually about 200 ° C. or less, preferably about 180 ° C. or less, more preferably about 170 ° C. or less (for example, 160 ° C.). The following).
  • the softening point of the tackifier resin is defined as a value measured based on the softening point test method (ring ball method) defined in JIS K5902 and JIS K2207. Specifically, the sample is melted as quickly as possible, and is carefully filled so that no bubbles are formed in the ring placed on a flat metal plate. After cooling, cut off the raised part from the plane including the upper end of the ring with a slightly heated sword. Next, a supporter (ring stand) is put in a glass container (heating bath) having a diameter of 85 mm or more and a height of 127 mm or more, and glycerin is poured until the depth becomes 90 mm or more.
  • ring ball method softening point test method
  • the steel ball (diameter 9.5 mm, weight 3.5 g) and the ring filled with the sample are immersed in glycerin so as not to contact each other, and the temperature of glycerin is maintained at 20 ° C. plus or minus 5 ° C. for 15 minutes. .
  • a steel ball is placed on the center of the surface of the sample in the ring, and this is placed in a fixed position on the support.
  • the distance from the upper end of the ring to the glycerin surface is maintained at 50 mm, a thermometer is placed, the position of the center of the mercury bulb of the thermometer is set to the same height as the center of the ring, and the container is heated.
  • the flame of the Bunsen burner used for heating is placed between the center and the edge of the bottom of the container so that the heating is even. It should be noted that the rate at which the bath temperature rises after reaching 40 ° C. after heating has started must be 5.0 plus or minus 0.5 ° C. per minute.
  • the temperature at the time when the sample gradually softens and flows down from the ring and finally comes into contact with the bottom plate is read and used as the softening point. Two or more softening points are measured simultaneously, and the average value is adopted.
  • tackifying resin TLOH what has an aromatic ring is used preferably.
  • the tackifying resin TLOH having an aromatic ring include the above-described aromatic petroleum resins, aliphatic / aromatic copolymer petroleum resins, styrene resins, coumarone-indene resins, styrene-modified terpene resins, phenol-modified terpenes Examples thereof include resins and rosin phenol resins. Among them, it is more preferable to use a tackifying resin T LOH1 having a softening point of 120 ° C. or higher as the tackifying resin T LOH having an aromatic ring.
  • the tackifying resin TLOH1 having an aromatic ring is particularly preferably used for an adhesive layer containing a base polymer having a monovinyl-substituted aromatic compound such as styrene as a main monomer.
  • the tackifying resin TLOH1 generally has a high softening point that tends to decrease the compatibility with the base polymer, but the hydroxyl value is limited to 30 mgKOH / g or less. It is easy to be compatible with a hard domain composed of compound units, and the heat resistance of pseudo-crosslinking by the hard domain can be improved.
  • Preferable examples of the material having a hydroxyl value of 30 mg KOH / g or less, a softening point of 120 ° C. or more and usable as a tackifying resin T LOH1 having an aromatic ring include aromatic petroleum resins, aliphatic / aromatic Examples include copolymer petroleum resins, styrene resins, and coumarone-indene resins. Aliphatic / aromatic copolymer petroleum resins having a C5 fraction copolymerization ratio of less than 15% by weight (more preferably less than 10% by weight, more preferably less than 5% by weight, for example less than 3% by weight) Is preferred.
  • the copolymerization ratio of C9 fraction is 55% by weight or more (more preferably 60% by weight or more, more preferably 65% by weight or more).
  • Particularly preferred tackifying resins TLOH1 include aromatic petroleum resins and styrene resins (for example, ⁇ -methylstyrene / styrene copolymer resins).
  • the amount of tackifying resin T LOH1 used is not particularly limited. From the viewpoints of deterioration suppression, high temperature cohesiveness, etc., the amount of tackifying resin TLOH1 used is preferably about 5 parts by weight or more, preferably about 10 parts by weight or more, more preferably 100 parts by weight of the base polymer. Is about 15 parts by weight or more, more preferably about 20 parts by weight or more, and particularly preferably about 25 parts by weight or more. Further, from the viewpoint of achieving both high adhesion reliability and temporary adhesion in the main adhesion, the amount of the tackifier resin T LOH1 used relative to 100 parts by weight of the base polymer can be, for example, about 100 parts by weight or less.
  • the amount of tackifying resin T LOH1 used is preferably about 40 parts by weight or less, and may be about 35 parts by weight or less with respect to 100 parts by weight of the base polymer.
  • Adhesive layer as the tackifier resin T LOH, softening point containing tackifier resin T LOH2 below 120 ° C..
  • the lower limit of the softening point of the tackifying resin T LOH2 is not particularly limited. Usually, those having a softening point of about 40 ° C. or higher (typically about 60 ° C. or higher) can be preferably used. From the viewpoint of achieving both high adhesion reliability and temporary adhesion in the main adhesion, a tackifying resin TLOH2 having a softening point of about 80 ° C.
  • tackifying resin TLOH2 whose softening point is 110 degreeC or more and less than 120 degreeC is preferable.
  • the tackifying resin TLOH2 has a hydroxyl value of 30 mgKOH / g or less and is not particularly limited except that the softening point is less than 120 ° C., and its structure (for example, presence or absence of an aromatic ring, presence or absence of an isoprene unit, The presence or absence of a terpene skeleton or the presence or absence of a rosin skeleton is not particularly limited.
  • various tackifying resins petroleum resin, styrene resin, coumarone / indene resin, terpene resin, modified terpene resin, rosin resin, rosin derivative resin, ketone resin, etc.
  • the adhesive layer includes at least one of a petroleum resin and a terpene resin as the tackifying resin T LOH2 .
  • a composition in which the main component of the tackifying resin TLOH2 (that is, a component occupying more than 50% by weight of the tackifying resin TLOH2 ) is a petroleum resin, a composition that is a terpene resin, a petroleum resin and a terpene resin
  • a composition or the like that is a combination can be preferably employed.
  • the main component of the tackifying resin T LOH2 is a terpene resin (for example, ⁇ -pinene polymer or ⁇ -pinene polymer) is preferable.
  • the terpene resin may be substantially all of the tackifying resin T LOH2 (for example, 95% by weight or more).
  • the amount of tackifying resin T LOH2 used is not particularly limited. From the standpoint of deterioration prevention, temporary adhesion, etc., the amount of tackifying resin TLOH2 used relative to 100 parts by weight of the base polymer is suitably about 10 parts by weight or more, preferably about 20 parts by weight or more. Preferably it is about 30 parts by weight or more, more preferably about 40 parts by weight or more (for example, 45 parts by weight or more). In addition, from the viewpoint of achieving both high adhesion reliability and temporary adhesion in the main adhesion, the amount of the tackifier resin T LOH2 used relative to 100 parts by weight of the base polymer can be, for example, approximately 120 parts by weight or less. Usually, about 90 parts by weight or less is preferable, and about 70 parts by weight or less (for example, about 60 parts by weight or less) is more preferable.
  • the tackifier resin T LOH hydroxyl value is not more than 30 mgKOH / g, a tackifier resin T LOH1 softening point of 120 ° C. or higher, tackifier resin T LOH2 softening point is lower than 120 ° C. Use together.
  • Its content ratio is not particularly limited, and adhesion reliability and the temporary adhesive in the adhesive from the viewpoint of achieving both a high level, the ratio of the content of the tackifier resin T LOH2 to the content of the tackifier resin T LOH1 (T LOH2 / T LOH1 ) is suitably about 0.5 or more, preferably about 0.8 or more, more preferably about 1.2 or more, and still more preferably about 1.5 or more.
  • the ratio (T LOH2 / T LOH1 ) is suitably about 3 or less, preferably about 2.5 or less, more preferably about 2 or less, and still more preferably about 1.8 or less.
  • the amount of tackifier resin T LOH (when used in combination with a tackifier resin T LOH1 a tackifier resin T LOH2 its total amount) is not particularly limited. From the viewpoint of preferably exhibiting the effects of the technology disclosed herein, the amount of the tackifying resin TLOH used relative to 100 parts by weight of the base polymer is suitably about 15 parts by weight or more, preferably about 35 parts by weight. More preferably, it is about 50 parts by weight or more, more preferably about 65 parts by weight or more (for example, about 70 parts by weight or more).
  • the amount of the tackifying resin TLOH used relative to 100 parts by weight of the base polymer can be, for example, about 220 parts by weight or less, usually about 170 parts by weight or less, preferably about 120 parts by weight or less (for example, about 100 parts by weight). Part or less) is more preferable.
  • tackifying resin THOH in place of the hydroxyl value is not more than 30 mgKOH / g tackifier resin T LOH, or in combination with tackifier resins T LOH, tackifying resin hydroxyl value exceeds 30 mgKOH / g T HOH can be used.
  • the hydroxyl value of the tackifier resin THOH may be, for example, about 40 mgKOH / g or more, or about 50 mgKOH / g or more.
  • the tackifier resin T HOH also in a manner that includes a tackifying resin having a hydroxyl value of about 80 mg KOH / g or more (e.g.
  • the hydroxyl value of the tackifying resin TLOH is typically about 200 mgKOH / g or less, preferably about 150 mgKOH / g or less (for example, 120 mgKOH / g or less).
  • the tackifying resin T HOH is not particularly limited, and the above-described various tackifying resins, and a tackifying resin having a hydroxyl value of more than 30 mgKOH / g can be used.
  • terpene phenol resin, rosin phenol resin, polymerized rosin, esterified product of polymerized rosin and the like can be used.
  • Typical examples include phenolic resins having a phenol structure in the molecule (including terpene phenol resins and rosin phenol resins).
  • Such tackifying resin THOH can be used individually by 1 type or in combination of 2 or more types.
  • the usage-amount of tackifying resin THOH is not restrict
  • the amount of the tackifying resin THOH used with respect to 100 parts by weight of the base polymer can be, for example, about 100 parts by weight or less, preferably about 60 parts by weight or less, About 30 parts by weight or less, more preferably 10 parts by weight or less.
  • the deterioration of the adhesive is preferably suppressed by limiting the amount of the phenolic resin used as the tackifying resin THOH .
  • the technique disclosed herein can also be implemented in an embodiment where the amount of tackifying resin THOH used is about 5 parts by weight or less (eg, about 1 part by weight or less) with respect to 100 parts by weight of the base polymer.
  • An embodiment that substantially does not contain the tackifying resin THOH can also be preferably implemented.
  • an adhesive bond layer does not contain tackifying resin THOH substantially means that the quantity of tackifying resin THOH with respect to 100 weight part of base polymers is less than 0.1 weight part.
  • the base polymer includes an adhesive layer made of an adhesive that is non-crosslinked (non-crosslinkable adhesive).
  • the “adhesive layer composed of a non-crosslinkable adhesive” refers to an intentional treatment (that is, a cross-linking treatment such as a cross-linking treatment) for forming a chemical bond between base polymers when the adhesive layer is formed. It refers to an adhesive layer that has not been mixed with a crosslinking agent.
  • Such an adhesive layer and the adhesive composition used to form the adhesive layer may be substantially free of a crosslinking agent such as an isocyanate compound.
  • the adhesive composition contains substantially no crosslinking agent means that the content of the crosslinking agent contained in the adhesive composition is less than 0.1% by weight (for example, 0 to 0.05% by weight). .
  • the adhesive composition disclosed herein includes a leveling agent, a crosslinking aid, a plasticizer, a softening agent, a filler (typically inorganic particles), a colorant (pigment, dye, etc.), a charging agent, if necessary. It may contain various additives generally used in the field of adhesives such as an inhibitor, an anti-aging agent, an ultraviolet absorber, an antioxidant, and a light stabilizer. About such various additives, a conventionally well-known thing can be used by a conventional method.
  • the adhesive composition disclosed herein is about 0.1 to 10 parts by weight (preferably about 1 to 7 parts by weight, preferably about 1 to 7 parts by weight) with respect to 100 parts by weight of the base polymer from the viewpoint of preventing deterioration, aging and the like. It is preferable to contain an anti-aging agent (about 5 to 5 parts by weight).
  • the adhesive disclosed herein does not substantially contain liquid rubber such as polybutene (for example, the content per 100 parts by weight of the base polymer is 1 part by weight or less, and may be 0 parts by weight). .) Embodiment may be preferably implemented. According to such an adhesive, an adhesive sheet having excellent adhesion reliability at the time of main adhesion can be realized.
  • the adhesive composition has a total amount of base polymer and tackifying resin of 90% by weight of the total weight of the adhesive (that is, the weight of the adhesive layer constituted by the adhesive).
  • the composition may occupy the above.
  • an embodiment in which the total amount of the base polymer and the tackifying resin is 90 to 99.8% by weight (typically, for example, 95 to 99.5% by weight) of the total weight of the adhesive can be preferably employed.
  • the adhesive composition may be a composition substantially free of a chelate compound.
  • the chelate compound is, for example, a chelate compound of an alkaline earth metal oxide and a resin (alkylphenol resin or the like) having a functional group (hydroxyl group, methylol group or the like) capable of coordinating the oxide.
  • a resin alkylphenol resin or the like
  • the technique disclosed here can be preferably implemented in an embodiment in which the adhesive composition does not contain such a chelate compound at all or the content of the chelate compound is 1% by weight or less. According to such an embodiment, an adhesive sheet with better adhesive strength can be realized.
  • the adhesive composition disclosed herein is not particularly limited.
  • the adhesive composition or adhesive in a form (solvent type) containing the adhesive (adhesive component) having the above composition in an organic solvent May be an adhesive composition in a form dispersed in an aqueous solvent (water dispersion type, typically an aqueous emulsion type), a hot melt type adhesive composition, or the like.
  • a solvent-type adhesive composition is particularly preferable.
  • Such a solvent-type adhesive composition is typically prepared in the form of a solution containing the above-described components in an organic solvent.
  • the organic solvent can be appropriately selected from known or commonly used organic solvents.
  • aromatic compounds such as toluene and xylene (typically aromatic hydrocarbons); acetates such as ethyl acetate and butyl acetate; aliphatic or alicyclic hydrocarbons such as hexane, cyclohexane, and methylcyclohexane
  • halogenated alkanes such as 1,2-dichloroethane
  • ketones such as methyl ethyl ketone and acetylacetone
  • a mixed solvent of two or more it is usually appropriate to adjust the solvent-based adhesive composition to a solid content (NV) of 30 to 65% by weight (for example, 40 to 55% by weight).
  • NV solid content
  • a method for obtaining the adhesive sheet from the adhesive composition various conventionally known methods can be applied.
  • a method (direct method) in which an adhesive layer is formed by directly applying (typically applying) the adhesive composition to a substrate and drying it can be preferably employed.
  • the adhesive composition is applied to a surface having good releasability (for example, the surface of a release liner, the back surface of a release support substrate, etc.) and dried to form an adhesive layer on the surface.
  • the method is preferably employed for the production of a substrate-less adhesive sheet.
  • a method of transferring the adhesive layer to the substrate may be employed.
  • the adhesive composition can be carried out using a known or conventional coater such as a gravure roll coater, reverse roll coater, kiss roll coater, dip roll coater, bar coater, knife coater, spray coater and the like.
  • the adhesive composition is preferably dried under heating.
  • a drying temperature typically 40 ° C. to 150 ° C. (typically 40 ° C. to 120 ° C., for example 50 ° C. to 120 ° C., more preferably 70 ° C. to 100 ° C.) can be preferably used.
  • the drying time is not particularly limited, but may be about several tens of seconds to several minutes (for example, within about 5 minutes, preferably about 30 seconds to 2 minutes). Then, you may provide an additional drying process as needed.
  • the adhesive layer is typically formed continuously, but may be formed in a regular or random pattern such as a dot or stripe depending on the purpose and application.
  • the thickness of the adhesive layer is suitably about 3 mm or less, preferably about 1 mm or less, from the viewpoint of thinning, miniaturization, weight reduction, resource saving, and the like. More preferably, it is about 0.7 mm or less, and still more preferably about 0.5 mm or less (for example, about 0.4 mm or less).
  • the adhesive layer with a limited thickness also limits the amount of impregnation of the adherend such as fabric, so that the influence of the impregnation on the deformation recovery property (for example, stretchability) of the adherend is also reduced. .
  • the thickness is suitably about 0.01 mm or more, preferably about 0.03 mm or more, more preferably about 0.05 mm or more, Preferably it is about 0.1 mm or more.
  • the adhesive layer having the above thickness is preferably provided on each side of the base material.
  • ⁇ Base material> When the technology disclosed herein is applied to a double-sided adhesive sheet with a substrate or a single-sided adhesive sheet with a substrate, examples of the substrate include a polypropylene film, an ethylene-propylene copolymer film, a polyester film, a polyurethane film, Plastic films such as vinyl chloride films; Foam sheets made of foams such as polyurethane foam, polyethylene foam and polychloroprene foam; Various fibrous materials (natural fibers such as hemp and cotton; synthetic fibers such as polyester, vinylon and polyurethane) , Semi-synthetic fibers such as acetate, etc.) woven and non-woven fabrics (single or mixed paper, such as Japanese paper and fine paper) by single or mixed spinning, etc .; metals such as aluminum foil and copper foil Foil; etc.
  • the plastic film typically a non-porous plastic film, which is a concept distinguished from a woven fabric or a non-woven fabric
  • any of an unstretched film and a stretched (uniaxially stretched or biaxially stretched) film is used.
  • a surface of the substrate on which the adhesive layer is provided may be subjected to a surface treatment such as application of a primer and corona discharge treatment.
  • the thickness of the substrate can be appropriately selected according to the purpose, but is generally about 2 ⁇ m to 500 ⁇ m (typically 10 ⁇ m to 200 ⁇ m).
  • a conventional release paper or the like can be used as the release liner, and is not particularly limited.
  • a release liner having a release treatment layer on the surface of a substrate such as a plastic film or paper, or a release liner made of a low adhesive material such as a fluorine-based polymer (polytetrafluoroethylene, etc.) or a polyolefin-based resin (polyethylene, polypropylene, etc.) Etc.
  • the release treatment layer may be formed, for example, by surface-treating the substrate with a release treatment agent such as silicone-based, long-chain alkyl-based, fluorine-based, or molybdenum sulfide.
  • the adhesive sheet disclosed herein is useful for joining between members in various OA equipment, home appliances, automobiles, clothes, daily necessities, housewares, leisure goods, etc. (for example, for fixing various parts in such products). is there.
  • the adhesive sheet disclosed here can be used for joining hard members such as resin parts, but it is possible to use the temporary adhesive property, deformation recovery property, flexibility and adhesive reliability of a preferred embodiment, and fabric. It is preferably used for joining flexible materials such as leather, paper, rubber sheets and resin sheets.
  • fabric is a preferred application target of the technology disclosed herein.
  • the fabric includes natural fibers, synthetic fibers, semi-synthetic fibers, woven fabrics and knitted fabrics formed from these composite fibers, and includes all fabrics called fabrics.
  • the leather includes artificial leather, synthetic leather, and semi-synthetic leather.
  • the product including the flexible material include clothes such as coats, jackets, shirts, pants, underwear, household items such as shoes, bags, towels, household items such as curtains, carpets, sofas, bedding, and wets. Examples include sports equipment such as suits.
  • the adhesive sheet disclosed here is preferably used as a sewing alternative joining (seamless joining) means in the above applications. Joining (typically seamless joining) of stretchable fabrics such as underwear is a particularly preferred application of the technology disclosed herein.
  • stretchable materials can be formed from natural fibers such as cotton, various synthetic fibers such as acrylic, polyester, and urethane, and natural / synthetic composite fibers thereof.
  • the bonding mode of the fabric or the like by the adhesive sheet is not particularly limited.
  • a mode in which the layers are partially overlapped and bonded via an adhesive sheet can be appropriately employed.
  • the technique disclosed here can be preferably implemented in a mode in which adherends are partially overlapped and bonded via an adhesive sheet.
  • the adhesive sheet disclosed herein can be preferably used for joining fabrics (typically seamless joining). Therefore, according to the technique disclosed herein, a fabric bonded by a thermoplastic adhesive (adhesive bonded fabric) is provided.
  • a fabric bonded by a thermoplastic adhesive adheresive bonded fabric
  • Such an adhesive-bonded fabric is produced, for example, by placing a thermoplastic adhesive sheet between one fabric and another one fabric, temporarily bonding the fabric, and then performing a hot press.
  • thermoplastic adhesive sheet having a thermoplastic adhesive layer
  • a peel strength measured under the conditions of 300 mm / min and a peel angle of 180 degrees is 2N / 10 mm or more; and (B) a thermoplastic adhesive sheet measurement sample having a measurement length of 100 mm is prepared, When stretched 50% at a speed of 300 mm / min at 23 ° C., held for 3 seconds, and then shrunk at a speed of 300 mm / min, the shrinkage strength F S30% with respect to the stretch strength F E30% at 30% stretch length The hysteresis determined from the ratio [ FS30% / FE30% ] is 35% or more; Satisfying, thermoplastic adhesive sheet.
  • thermoplastic adhesive sheet measurement sample having a measurement length of 100 mm, a 30% modulus measured at a rate of 300 mm / min at 23 ° C. is 0.6 MPa or less;
  • thermoplastic adhesive sheet according to (1) further satisfying (3) The following characteristics:
  • the peel strength is 15 N / 10 mm or more;
  • the thermoplastic adhesive sheet according to (1) or (2), further satisfying (4) The thermoplastic adhesive sheet according to any one of (1) to (3), wherein the thermoplastic adhesive layer is a rubber-based adhesive layer containing a rubber-based polymer as a base polymer.
  • the thermoplastic adhesive layer, a tackifying resin, hydroxyl value comprises a tackifier resin T LOH or less 30 mgKOH / g, the (1) thermoplastic adhesive according to any one of (1) to (7) Sheet.
  • thermoplastic adhesive sheet according to any one of (8) to (10), wherein the tackifying resin T LOH contains a tackifying resin T LOH2 having a softening point of less than 120 ° C. (12) The content of the tackifying resin T LOH in the thermoplastic adhesive layer is 15 to 220 parts by weight with respect to 100 parts by weight of the base polymer contained in the thermoplastic adhesive layer.
  • thermoplastic adhesive sheet according to any one of (1) to (16) which is used for joining fabrics.
  • a thermoplastic adhesive sheet with a release liner comprising: the thermoplastic adhesive sheet according to any one of (1) to (17) above; and a release liner that protects the adhesive surface of the thermoplastic adhesive sheet.
  • Example 1 [Preparation of Thermoplastic Adhesive Composition] Styrene isoprene block copolymer (manufactured by ZEON Corporation, product name “Quintac 3520”, styrene content 15%, diblock body ratio 78%) as a base polymer 100 parts, terpene resin 50 parts (Yasuhara Chemical) Product name “YS Resin PX1150N”, softening point 115 ° C., hydroxyl value less than 1 mgKOH / g) and aromatic petroleum resin (manufactured by JX Nippon Mining & Energy, product name “Nisseki Neopolymer 150”, softening 30 parts by temperature of 155 ° C., hydroxyl value of less than 1 mg KOH / g), 3 parts of an anti-aging agent (product name “IRGANOX1010” manufactured by BASF) and toluene as a solvent are stirred and mixed to give a thermoplastic adhesive of NV 50% An
  • thermoplastic adhesive sheet The thermoplastic adhesive composition prepared above is applied to the release-treated surface of release liner A that has been subjected to a release treatment with a silicone-based release agent, followed by drying at 120 ° C. for 3 minutes, and a thermoplastic having a thickness of 0.2 mm. An adhesive layer was formed. A release liner B that had been subjected to a release treatment with a silicone release agent was bonded to the thermoplastic adhesive layer. Thus, the base material-less thermoplastic adhesive sheet which consists of a thermoplastic adhesive layer was produced.
  • thermoplastic adhesive sheet according to each example was prepared in the same manner as in Example 1 except that the thickness of the thermoplastic adhesive layer was changed to that shown in Table 1.
  • Example 4 The product name “No. 501K” manufactured by Nitto Denko Corporation was used as the adhesive sheet according to this example.
  • “No. 501K” is a double-sided pressure-sensitive adhesive tape with a base material having a thickness of 0.17 mm in which an acrylic pressure-sensitive adhesive layer is formed on both surfaces of the nonwoven fabric base material.
  • Example 5 100 parts of styrene butadiene block copolymer (product name “Saprene T-432” manufactured by Asahi Kasei Chemicals Co., Ltd., styrene content 30%) as base polymer and 120 parts of alicyclic hydrocarbon resin (manufactured by Arakawa Chemical Industries, Ltd. The name “Arcon M-115”, softening point 115 ° C.) and toluene as a solvent were mixed with stirring to prepare a 50% NV thermoplastic adhesive composition.
  • the thermoplastic adhesive composition prepared above is applied to the release-treated surface of release liner A that has been subjected to a release treatment with a silicone-based release agent, dried at 120 ° C.
  • thermoplastic adhesive sheet which consists of a thermoplastic adhesive layer was produced.
  • the adhesive sheet according to each example was cut into a strip shape having a width of 10 mm. Prepare two sheets of commercially available underwear cut into a 20 mm wide strip, and make two rounds of 2 kg rollers on each adhesive surface of the adhesive sheet piece in an environment of 23 ° C. and 50% RH. Then, a measurement sample was produced by pressure bonding. The obtained measurement sample was left in the same environment for 30 minutes, and then the measurement sample was peeled off into a T shape using a universal tensile / compression tester.
  • T-type peeling is such that when the plane of the measurement sample (the plane of the fabric joined by the adhesive sheet) is 0 degree, one cloth forms a T-shape at +90 degrees and the other cloth at -90 degrees. It is peeling to peel off.
  • the force required for this T-peeling was measured with the above-mentioned testing machine, and this was defined as a temporary adhesive force to fabric (preliminary adhesive force against fabric) [N / 10 mm].
  • the device name “Tensile / Compression Tester, TG-1kN” manufactured by Minebea Co., Ltd. was used, but an equivalent product or a commercially available device can be used.
  • the adhesive sheet according to each example was cut into a strip shape having a width of 10 mm so as to have a measurement length of 100 mm.
  • two commercially available skin-wearing fabrics cut into a 20 mm wide strip so as to have a measurement length of 100 mm are prepared, and each of the two fabrics is made of the adhesive sheet piece in an environment of 23 ° C. and 50% RH.
  • the measurement sample was produced by crimping
  • the obtained measurement sample was allowed to stand at room temperature (23 ° C.) for 1 hour, and then set in a tensile and compression tester so that the distance between chucks (measurement length) was 100 mm (L0), and at 23 ° C., 100 mm / min.
  • the film was stretched 50% at the speed (thus stretched to 150 mm), held in the stretched state of 50% for 3 seconds, then released and left for 30 minutes, and the measured length L1 [mm] was recorded. From the above operation, the strength (30% elongation strength) [N] when the measurement sample was stretched 30% and the residual strain (50% elongation residual strain) [%] after standing for 30 minutes were determined.
  • 3 shows a temporary adhesive force of 0.1 N / 10 mm or more (specifically, 0.4 to 0.6 N / 10 mm) to the fabric, and the residual fabric bonded with the adhesive sheet. The strain was 5% or less.
  • the double-sided pressure-sensitive adhesive sheet with a nonwoven fabric substrate according to Example 4 in which the hysteresis was not measured due to breakage had a residual strain exceeding 5%.
  • the adhesive sheet according to Example 5 having an adhesive force to foam of less than 2 N / 10 mm had a remarkably small temporary adhesive force to the fabric and did not have sufficient temporary adhesiveness.
  • the absolute value of the measured value differed from the said evaluation result with respect to foam adhesive force and cloth temporary adhesive force, since the both adherend surfaces were rough surfaces, the fixed correlation was shown.
  • Example 1 the fabric bonded with the adhesive sheet according to Example 1 having a thickness of 0.06 mm was the adhesive bonded fabric according to Example 5 (adhesion) Compared to the 30% modulus of the sheet exceeding 0.6 MPa and the thickness of 0.05 mm, the 30% elongation strength was suppressed to be low, and the original flexibility of the fabric was maintained. Furthermore, in Examples 1 to 3 where the adhesive strength against SUS thermocompression bonding is relatively high, a tendency to increase the adhesive strength against fabric is recognized. A relatively high correlation was observed.
  • thermoplastic adhesive sheet having an adhesive strength to foam of 2 N / 10 mm or more and a 30% hysteresis at 50% elongation of 35% or more, that is, a thermoplastic satisfying the characteristics (A) and (B) According to the adhesive sheet, it can be seen that the adhesive sheet has temporary adhesiveness and deformation recovery and can exhibit a good adhesive function. It can also be seen that the thermoplastic adhesive sheet having a 30% modulus of 0.6 MPa or less, that is, satisfying the characteristic (C) does not impair the flexibility of the adherend material. Furthermore, it can be seen that the thermoplastic adhesive sheet having a SUS thermocompression bonding adhesive strength of 15 N / 10 mm or more, that is, satisfying the characteristic (D), is excellent in adhesive reliability based on the strong adhesive force.

Landscapes

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

Abstract

L'invention concerne une feuille adhésive thermoplastique dotée de propriétés de collage temporaire et de propriétés de récupération de déformation, et apte à remplir une fonction de collage souhaitable. La feuille adhésive thermoplastique selon l'invention comprend une couche adhésive thermoplastique. Ladite feuille remplie les caractéristiques (A) et (B) suivantes. La feuille adhésive thermoplastique selon l'invention présente les caractéristiques suivantes : (A) une résistance au décollage d'au moins 2 N/10 mm par rapport à une mousse d'uréthane à base de polyester ; et (B) une hystérèse d'au moins 35 %, telle que déterminée à partir du rapport [FS30%/FE30%] d'une résistance au retrait FS30% par rapport à une résistance à l'allongement FE30%, à une longueur d'allongement de 30 %, après que la feuille a été étirée de 50 % à une vitesse de 300 mm/min, à 23 °C, maintenue dans cet état pendant 3 secondes, puis laissée se rétracter à une vitesse de 300 mm/min.
PCT/JP2019/005029 2018-02-27 2019-02-13 Feuille adhésive thermoplastique et utilisation associée WO2019167621A1 (fr)

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JP7246858B2 (ja) 2023-03-28
CN111770973B (zh) 2023-05-02

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