JP5801615B2 - Separator selection method and pressure-sensitive adhesive sheet using the separator selected by the selection method - Google Patents

Separator selection method and pressure-sensitive adhesive sheet using the separator selected by the selection method Download PDF

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JP5801615B2
JP5801615B2 JP2011131911A JP2011131911A JP5801615B2 JP 5801615 B2 JP5801615 B2 JP 5801615B2 JP 2011131911 A JP2011131911 A JP 2011131911A JP 2011131911 A JP2011131911 A JP 2011131911A JP 5801615 B2 JP5801615 B2 JP 5801615B2
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separator
pressure
sensitive adhesive
adhesive sheet
evaluation
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JP2013001738A (en
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勝利 亀井
勝利 亀井
生島 伸祐
伸祐 生島
剛志 土生
剛志 土生
文輝 浅井
文輝 浅井
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Nitto Denko Corp
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Nitto Denko Corp
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Priority to JP2011131911A priority Critical patent/JP5801615B2/en
Priority to PCT/JP2012/063871 priority patent/WO2012172975A1/en
Priority to KR1020127027326A priority patent/KR101427504B1/en
Priority to CN201280002198.6A priority patent/CN103038300B/en
Priority to TW101121209A priority patent/TWI546532B/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/06Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/32Layered products comprising a layer of synthetic resin comprising polyolefins
    • B32B27/327Layered products comprising a layer of synthetic resin comprising polyolefins comprising polyolefins obtained by a metallocene or single-site catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered 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
    • B32B7/04Interconnection of layers
    • B32B7/06Interconnection of layers permitting easy separation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered 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
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65HHANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
    • B65H41/00Machines for separating superposed webs
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/10Homopolymers or copolymers of propene
    • C09J123/14Copolymers of propene
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/20Adhesives in the form of films or foils characterised by their carriers
    • C09J7/21Paper; Textile fabrics
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/20Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22Plastics; Metallised plastics
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38Pressure-sensitive adhesives [PSA]
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/40Adhesives in the form of films or foils characterised by release liners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/70Other properties
    • B32B2307/748Releasability
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2405/00Adhesive articles, e.g. adhesive tapes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/10Peculiar tacticity
    • C08L2207/14Amorphous or atactic polypropylene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2314/00Polymer mixtures characterised by way of preparation
    • C08L2314/06Metallocene or single site catalysts
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/30Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/312Additional 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/40Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00Presence of polyolefin

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

Description

本発明は、セパレータの選定方法および該選定方法により選定されたセパレータを用いた粘着シートに関する。   The present invention relates to a separator selection method and an adhesive sheet using a separator selected by the selection method.

粘着剤層および基材層を有する粘着シートの製造方法として、生産効率およびコスト性に優れることから、基材層を構成する材料と粘着剤層を構成する材料を共押し出しする成形方法が知られている(例えば、特許文献1)。また、粘着シートは、通常、使用されるまでの保護材として粘着剤層と接するように、セパレータが配置されている。このような粘着シートにおいて、共押し出しにより粘着シートを成形する場合、粘着剤層とセパレータの間への異物の混入を抑えることができ、かつ、粘着剤層とセパレータとが接する面が平滑な粘着シートが得られることから、共押し出しされた粘着剤層形成材料が溶融した状態でセパレータと貼り合わせる方法が検討されている。しかしながら、このようにして得られる粘着シートは、セパレータの剥離が困難となり、粘着シートのハンドリング性が低下する場合が多い。また、このような問題に対し、軽剥離のセパレータを用いると、ハンドリング性は向上するものの、粘着シートの保管時に粘着剤層の粘着力が低下する場合が多い。このように、粘着シートの良好なハンドリング性と適度な粘着力とを両立することは困難である。   As a method for producing a pressure-sensitive adhesive sheet having a pressure-sensitive adhesive layer and a base material layer, a molding method is known in which the material constituting the base material layer and the material constituting the pressure-sensitive adhesive layer are co-extruded because of excellent production efficiency and cost. (For example, Patent Document 1). Moreover, the separator is arrange | positioned so that the adhesive sheet may contact | connect an adhesive layer normally as a protective material until it is used. In such a pressure-sensitive adhesive sheet, when the pressure-sensitive adhesive sheet is formed by co-extrusion, it is possible to suppress the mixing of foreign matter between the pressure-sensitive adhesive layer and the separator, and the surface where the pressure-sensitive adhesive layer and the separator are in contact with each other is smooth. Since a sheet is obtained, a method in which the coextruded pressure-sensitive adhesive layer forming material is bonded to a separator in a molten state has been studied. However, the pressure-sensitive adhesive sheet thus obtained often makes it difficult to separate the separator, and the handling property of the pressure-sensitive adhesive sheet is often lowered. In addition, when a lightly peeled separator is used for such a problem, the handling property is improved, but the adhesive strength of the adhesive layer is often reduced during storage of the adhesive sheet. Thus, it is difficult to achieve both good handling properties of the pressure-sensitive adhesive sheet and appropriate pressure-sensitive adhesive strength.

粘着シートに用いるセパレータは、剥離剤の種類やその剥離力等により所望のセパレータが適宜選定される。しかしながら、上記の通り、溶融した粘着剤層形成材料と貼り合せられる場合、得られた粘着シートにおいてセパレータ本来の能力が発揮されない場合がある。そのため、溶融共押し出し成形で製造される粘着シートに用いるセパレータは、まず候補となるセパレータを選択し、実際に粘着シートを製造したうえで、セパレータの適性を検討する必要がある。そのため、粘着シートの構成を変更するごとに、粘着シートを作製し、セパレータの適性を検討する必要があり、適切なセパレータの選定は容易ではない。   As the separator used for the pressure-sensitive adhesive sheet, a desired separator is appropriately selected depending on the type of the release agent, its release force, and the like. However, as above-mentioned, when pasted with the molten adhesive layer forming material, the original capability of a separator may not be exhibited in the obtained adhesive sheet. Therefore, the separator used for the pressure-sensitive adhesive sheet manufactured by melt coextrusion molding must first select a candidate separator, actually manufacture the pressure-sensitive adhesive sheet, and then examine the suitability of the separator. Therefore, every time the configuration of the pressure-sensitive adhesive sheet is changed, it is necessary to prepare a pressure-sensitive adhesive sheet and examine the suitability of the separator, and it is not easy to select an appropriate separator.

特開2009−275209号公報JP 2009-275209 A

本発明は上記従来の課題を解決するためになされたものであり、その目的とするところは、少なくとも粘着剤層を有する粘着シートに適したセパレータを簡便に選定することができる方法を提供することにある。   The present invention has been made to solve the above-described conventional problems, and an object of the present invention is to provide a method capable of easily selecting a separator suitable for a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer. It is in.

本発明のセパレータの選定方法は、少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せ、少なくとも粘着剤層とセパレータとを有する粘着シートを得る工程、得られた粘着シートから該セパレータを剥離し、該粘着シートの粘着剤層と評価用セパレータとを貼り合せて評価用粘着シートを作製する工程、および、該評価用粘着シートを、一対のクッション材と一対のプレス板で狭持し、プレス板面温度140℃、圧力5MPaで1分間保持した後、剥離速度300mm/分での180°剥離試験により評価用セパレータの剥離力を評価する工程を含む。
好ましい実施形態においては、上記評価工程において測定された剥離力が2.0N/50mm以下であるセパレータを選定する。
好ましい実施形態においては、上記粘着シートの粘着剤層はポリオレフィン系樹脂を含む。
好ましい実施形態においては、上記ポリオレフィン系樹脂はメタロセン触媒を用いて重合された非晶質プロピレン−(1−ブテン)共重合体を含む。
本発明の別の実施形態においては、粘着シートが提供される。該粘着シートは、基材層、粘着剤層、および、上記選定方法により選定されたセパレータを含む。
The method for selecting a separator according to the present invention includes the steps of obtaining a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer and a separator by pasting the separator with at least a material forming the pressure-sensitive adhesive layer, and separating the separator from the obtained pressure-sensitive adhesive sheet. The adhesive sheet of the pressure-sensitive adhesive sheet and the separator for evaluation are bonded to each other, and the pressure-sensitive adhesive sheet for evaluation is sandwiched between a pair of cushion materials and a pair of press plates. And holding the press plate surface temperature at 140 ° C. and a pressure of 5 MPa for 1 minute, and then evaluating the peeling force of the separator for evaluation by a 180 ° peeling test at a peeling speed of 300 mm / min.
In preferable embodiment, the separator whose peeling force measured in the said evaluation process is 2.0 N / 50mm or less is selected.
In preferable embodiment, the adhesive layer of the said adhesive sheet contains polyolefin resin.
In a preferred embodiment, the polyolefin-based resin includes an amorphous propylene- (1-butene) copolymer polymerized using a metallocene catalyst.
In another embodiment of the present invention, an adhesive sheet is provided. The pressure-sensitive adhesive sheet includes a base material layer, a pressure-sensitive adhesive layer, and a separator selected by the above selection method.

本発明によれば、粘着シートに好適なセパレータを簡便に選定することができる。   According to the present invention, a separator suitable for an adhesive sheet can be easily selected.

本発明のセパレータの選定方法は、粘着シートに好適なセパレータを選定する方法である。本発明の方法によれば、少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せることにより得られる粘着シートに好適なセパレータを簡便に選択することができる。本発明のセパレータの選定方法は、少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せ、少なくとも粘着剤層とセパレータとを有する粘着シートを得る工程、得られた粘着シートから該セパレータを剥離し、該粘着シートの粘着剤層と評価用セパレータとを貼り合せて評価用粘着シートを作製する工程、および、該評価用粘着シートを一対のクッション材および一対のプレス板で狭持し、プレス板面温度140℃、圧力5MPaで1分間保持した後、剥離速度300mm/分での180°剥離試験により評価用セパレータの剥離力を評価する工程を含む。本発明の選定方法により、セパレータの剥離力を評価することにより、粘着シートに好適なセパレータを簡便に選定することができる。   The separator selection method of the present invention is a method for selecting a separator suitable for an adhesive sheet. According to the method of the present invention, it is possible to easily select a separator suitable for a pressure-sensitive adhesive sheet obtained by laminating with a separator in a state where at least the material forming the pressure-sensitive adhesive layer is melted. The method for selecting a separator according to the present invention includes a step of obtaining a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer and a separator, at least in a state where a material forming the pressure-sensitive adhesive layer is melted, and the separator from the obtained pressure-sensitive adhesive sheet. The adhesive sheet of the pressure-sensitive adhesive sheet and the separator for evaluation are bonded together to produce a pressure-sensitive adhesive sheet for evaluation, and the pressure-sensitive adhesive sheet for evaluation is sandwiched between a pair of cushion materials and a pair of press plates And a press plate surface temperature of 140 ° C. and a pressure of 5 MPa for 1 minute, and then a step of evaluating the peeling force of the separator for evaluation by a 180 ° peeling test at a peeling speed of 300 mm / min. The separator suitable for the pressure-sensitive adhesive sheet can be easily selected by evaluating the peeling force of the separator by the selection method of the present invention.

A.少なくとも粘着剤層とセパレータとを有する粘着シートを得る工程
本発明の選定方法は少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せ、少なくとも粘着剤層とセパレータとを有する粘着シートを得る工程を含む。該粘着シートは、代表的には、基材層、粘着剤層およびセパレータをこの順に有する。
A. Step of obtaining a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer and a separator The selection method of the present invention is a method in which a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer and a separator is bonded together with at least a material forming the pressure-sensitive adhesive layer in a molten state. A obtaining step. The pressure-sensitive adhesive sheet typically has a base material layer, a pressure-sensitive adhesive layer, and a separator in this order.

上記粘着シートを成形する方法としては、特に制限はなく、少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せられる工程を含んでいればよい。上記成形方法は、例えば、粘着剤層を形成する材料および基材層を形成する材料を溶融後、押し出し、粘着剤層と基材層との積層体を得る工程、少なくとも粘着剤層を形成する材料が溶融した状態で、該積層体の粘着剤層とセパレータとを貼り合せ、粘着シートを得る工程を含む。   There is no restriction | limiting in particular as a method of shape | molding the said adhesive sheet, What is necessary is just to include the process bonded together with a separator in the state which the material which forms an adhesive layer at least was fuse | melted. In the molding method, for example, a material for forming the pressure-sensitive adhesive layer and a material for forming the base material layer are melted and then extruded to obtain a laminate of the pressure-sensitive adhesive layer and the base material layer, and at least the pressure-sensitive adhesive layer is formed. The process includes a step of bonding the pressure-sensitive adhesive layer of the laminate and the separator to obtain a pressure-sensitive adhesive sheet in a state where the material is melted.

上記粘着剤層と基材層の積層体を得る工程において、該積層体は、例えば、ダイスに連結した少なくとも2台の押出し機のうち、1台に粘着剤層を形成する材料を、別の1台に基材層を形成する材料を、それぞれ供給し、溶融後、押出しすることにより、得られ得る。上記粘着シートを成形する際の条件(例えば、ダイス温度)は、該粘着シートの各層を構成する材料に応じて、適宜設定することができる。例えば、ダイス温度は、粘着シートの各層の形成材料が溶融状態となる温度に設定され得る。一つの実施形態においては、ダイス温度は160℃〜220℃に設定され得る。   In the step of obtaining the laminate of the pressure-sensitive adhesive layer and the base material layer, for example, the laminate is made of another material that forms the pressure-sensitive adhesive layer in one of at least two extruders connected to a die. It can be obtained by supplying the materials for forming the base material layer on one unit, extruding after melting. The conditions (for example, die temperature) at the time of forming the pressure-sensitive adhesive sheet can be appropriately set according to the material constituting each layer of the pressure-sensitive adhesive sheet. For example, the die temperature can be set to a temperature at which the forming material of each layer of the pressure-sensitive adhesive sheet is in a molten state. In one embodiment, the die temperature may be set between 160 ° C and 220 ° C.

上記積層体とセパレータとを貼り合せる工程は、具体的には、上記積層体を得る工程において、押し出された積層体の少なくとも該粘着剤層を形成する材料が溶融した状態で該積層体の粘着剤層とセパレータとを接触させ、タッチロール成形法により引き取ることにより、行われ得る。上記粘着剤層を形成する材料とセパレータとを接触させる際の条件(例えば、粘着剤層を構成する材料とセパレータとを接触させる温度および接触圧力)は、粘着シートの各層を構成する材料に応じて、適宜設定することができる。例えば、粘着剤層を構成する材料とセパレータとを接触させる温度は、少なくとも粘着剤層を形成する材料が溶融した状態が維持される温度に設定され得る。一つの実施形態においては、粘着剤層を構成する材料とセパレータとを接触させる温度は、120℃〜200℃に設定され得る。   More specifically, the step of bonding the laminate and the separator is, in the step of obtaining the laminate, in the state in which at least the material forming the pressure-sensitive adhesive layer of the extruded laminate is melted. It can be carried out by bringing the agent layer and the separator into contact with each other and taking it out by a touch roll molding method. The conditions for contacting the material forming the pressure-sensitive adhesive layer and the separator (for example, the temperature and contact pressure at which the material forming the pressure-sensitive adhesive layer is brought into contact with the separator) depend on the material forming each layer of the pressure-sensitive adhesive sheet. And can be set as appropriate. For example, the temperature at which the material constituting the pressure-sensitive adhesive layer is brought into contact with the separator can be set to a temperature at which at least the material forming the pressure-sensitive adhesive layer is maintained in a molten state. In one embodiment, the temperature which makes the material which comprises an adhesive layer and a separator contact may be set to 120 to 200 degreeC.

この工程で用いるセパレータ(以下、製造用セパレータともいう)としては、任意の適切なセパレータを用いることができる。例えば、当該技術分野において、粘着シートのセパレータとして、汎用されているセパレータを用いることができ、具体的には、三菱樹脂製の商品名MRF−38、東山フイルム社製の商品名HY−S06等が挙げられる。   Any appropriate separator can be used as a separator used in this step (hereinafter also referred to as a production separator). For example, a separator that is widely used in the technical field can be used as the separator for the pressure-sensitive adhesive sheet. Specifically, trade name MRF-38 manufactured by Mitsubishi Plastics, trade name HY-S06 manufactured by Higashiyama Film Co., Ltd. Is mentioned.

B.評価用粘着シートの作製工程
本発明の選定方法における評価工程で用いる評価用粘着シートは、以下のようにして得られる。まず、上記A項の方法により得られた粘着シートからセパレータを剥離する。該セパレータの剥離は、任意の適切な手段により行うことができ、任意の剥離機を用いて剥離してもよく、手で剥離してもよい。
B. Step for producing evaluation pressure-sensitive adhesive sheet The pressure-sensitive adhesive sheet for evaluation used in the evaluation step in the selection method of the present invention is obtained as follows. First, the separator is peeled from the pressure-sensitive adhesive sheet obtained by the method of item A above. The separator can be peeled off by any appropriate means, and may be peeled off using any peeling machine or may be peeled off manually.

次いで、セパレータを剥離した粘着シートの粘着剤層と選定の対象となる評価用セパレータを貼り合せる。後述する剥離力の評価工程において、プレスを行うため、評価用粘着シートの作製工程においては、該粘着シートと該評価用セパレータとを強固に貼り合せる必要はなく、該粘着シートと該評価用セパレータとの積層状態が維持される程度に貼り合せられていればよい。   Next, the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet from which the separator has been peeled off is attached to the evaluation separator to be selected. Since the pressing is performed in the peeling force evaluation process described later, it is not necessary to firmly bond the pressure-sensitive adhesive sheet and the evaluation separator in the production process of the pressure-sensitive adhesive sheet for evaluation, and the pressure-sensitive adhesive sheet and the evaluation separator. It is only necessary to be bonded to such an extent that the laminated state is maintained.

C.評価用セパレータの剥離力評価工程
上記評価用セパレータの剥離力評価工程は以下のようにして行う。上記B工程で得られた評価用粘着シートを一対のクッション材で狭持した後、さらに一対のプレス板で狭持し、プレス板面温度140℃、圧力5MPaで1分間保持し、プレスを行う。粘着シートに用いられるセパレータは、プレス板面温度が140℃を超えると、セパレータと粘着剤層との剥離が急激に困難になる傾向がある。したがって、プレス板面温度を140℃として評価用粘着シートのプレスを行い、プレス後の粘着シートにおける評価用セパレータの剥離力を評価することにより、粘着シートのセパレータとして適したセパレータを選定することができる。なお、本発明の剥離力評価試験におけるプレス板面温度は、プレス板表面の温度をいう。
C. Peeling power evaluation process of evaluation separator The peeling power evaluation process of the evaluation separator is performed as follows. After sandwiching the evaluation pressure-sensitive adhesive sheet obtained in the step B with a pair of cushion materials, the sheet is further sandwiched with a pair of press plates and held at a press plate surface temperature of 140 ° C. and a pressure of 5 MPa for 1 minute to perform pressing. . When the separator used for the pressure-sensitive adhesive sheet has a press plate surface temperature exceeding 140 ° C., the separator and the pressure-sensitive adhesive layer tend to be peeled off rapidly. Therefore, it is possible to select a separator suitable as a separator for the pressure-sensitive adhesive sheet by pressing the pressure-sensitive adhesive sheet for evaluation at a press plate surface temperature of 140 ° C. and evaluating the peeling force of the separator for evaluation in the pressure-sensitive adhesive sheet after pressing. it can. In addition, the press plate surface temperature in the peeling force evaluation test of the present invention refers to the temperature of the press plate surface.

上記プレスにおいて、評価用粘着シートとプレス板との間には、粘着シートに過度の圧力がかかることを防止するため、クッション材が配置される。このクッション材としては、熱プレスに適用可能な任意の適切なクッション材を用いることができ、例えば、ゴム、耐熱性エラストマー、有機または無機繊維をバインダーで結合したもの、不織布、ゴムと不織布との積層体等が挙げられる。プレスに用いるクッション材は、評価用粘着シートにかかる圧力が適当な圧力となるよう適切なクッション材を選択して用いればよい。例えば、クッション材の構成材料、サイズ(面積)を調整することにより、評価用粘着シートにかかる圧力を調整することができる。より具体的には、サイズが150mm×200mmのセパレータに対しては、面積が130mm×160mmのゴム板が用いられ得る。   In the said press, in order to prevent that an excessive pressure is applied to an adhesive sheet between the evaluation adhesive sheet and a press board, a cushioning material is arrange | positioned. As this cushion material, any appropriate cushion material applicable to hot press can be used. For example, rubber, heat-resistant elastomer, organic or inorganic fibers bonded with a binder, nonwoven fabric, rubber and nonwoven fabric A laminated body etc. are mentioned. As the cushion material used for the press, an appropriate cushion material may be selected and used so that the pressure applied to the evaluation pressure-sensitive adhesive sheet becomes an appropriate pressure. For example, the pressure applied to the evaluation pressure-sensitive adhesive sheet can be adjusted by adjusting the constituent material and size (area) of the cushion material. More specifically, a rubber plate having an area of 130 mm × 160 mm can be used for a separator having a size of 150 mm × 200 mm.

また、プレス時にクッション材および評価用粘着シートのブロッキングを防止するため、クッション材と評価用粘着シートとの間にそれぞれ樹脂シートを配置し、プレスを行ってもよい。該樹脂シートは、セパレータとして適用可能な樹脂シートであればよく、任意の適切なシートを用いることができ、例えば、ポリエチレンテレフタレート系樹脂シート、ポリイミド系樹脂フィルム等を用いることができる。該樹脂シートの厚みは、通常、38μm〜75μmである。   Further, in order to prevent blocking of the cushion material and the evaluation pressure-sensitive adhesive sheet during pressing, a resin sheet may be disposed between the cushion material and the evaluation pressure-sensitive adhesive sheet, and pressing may be performed. The resin sheet may be a resin sheet applicable as a separator, and any appropriate sheet can be used. For example, a polyethylene terephthalate resin sheet, a polyimide resin film, or the like can be used. The thickness of the resin sheet is usually 38 μm to 75 μm.

評価用粘着シートのプレスは、上記のプレス板面温度および圧力を設定可能な任意の適切な手段を用いて行うことができる。例えば、市販のプレス機を用いて行うことができ、具体的には、東洋精機社製、MINI TEST PRESS−10等が挙げられる。   The evaluation pressure-sensitive adhesive sheet can be pressed using any appropriate means capable of setting the press plate surface temperature and pressure. For example, it can carry out using a commercially available press machine, and specifically, Toyo Seiki Co., Ltd. make, MINI TEST PRESS-10 etc. are mentioned.

プレス後の評価用粘着シートは、室温になるまで放置し、評価用セパレータの剥離試験を行う。該剥離試験は、剥離速度300mm/分、剥離角度180°にて評価用セパレータを剥離することにより行う。   The evaluation pressure-sensitive adhesive sheet after pressing is allowed to stand until it reaches room temperature, and a peel test of the evaluation separator is performed. The peeling test is performed by peeling off the evaluation separator at a peeling speed of 300 mm / min and a peeling angle of 180 °.

上記剥離試験により測定された剥離力から、セパレータに要求する特性に応じて、所望のセパレータを選択することができる。例えば、ハンドリング性に優れ、かつ、適度な粘着力が保持されたセパレータを所望する場合には、上記剥離試験で測定された剥離力が2.0N/50mm以下であるセパレータが好適に用いられ得る。また、より粘着剤層とセパレータとの密着性の高いセパレータを所望する場合には、上記剥離試験で測定された剥離力が2.0N/50mmを超えるセパレータを用いればよい。市販のテープ貼り付け装置(例えば、日東精機社製のバックグラインド用保護テープ貼り付け装置、商品名DR3000III等)での取り扱いの点から、上記剥離試験で測定された剥離力2.0N/50mmを基準として、所望のセパレータを選択し得る。なお、よりハンドリング性の高いセパレータを所望する場合には、上記剥離試験で測定された剥離力がより小さいセパレータを用いればよい。   A desired separator can be selected from the peel force measured by the peel test according to the characteristics required of the separator. For example, when a separator excellent in handling properties and having an appropriate adhesive strength is desired, a separator having a peel strength measured by the peel test of 2.0 N / 50 mm or less can be suitably used. . In addition, when a separator having higher adhesion between the pressure-sensitive adhesive layer and the separator is desired, a separator having a peel force measured by the peel test exceeding 2.0 N / 50 mm may be used. From the point of handling with a commercially available tape applicator (for example, protective tape applicator for back grind manufactured by Nitto Seiki Co., Ltd., trade name DR3000III, etc.), the peel force of 2.0 N / 50 mm measured in the above peel test is As a reference, a desired separator can be selected. In addition, when a separator with higher handling property is desired, a separator having a smaller peeling force measured by the above peeling test may be used.

D.粘着シート
本発明が適用される粘着シートは、代表的には、基材層、粘着剤層、およびセパレータを含む。また、該粘着シートは必要に応じて、任意の適切な他の層を含んでいてもよい。該他の層としては、例えば、耐熱性を付与する表面層が挙げられる。
D. Adhesive Sheet The adhesive sheet to which the present invention is applied typically includes a base material layer, an adhesive layer, and a separator. Moreover, this adhesive sheet may contain arbitrary appropriate other layers as needed. As this other layer, the surface layer which provides heat resistance is mentioned, for example.

粘着シートの厚み(セパレータの厚みを除く)は、好ましくは90μm〜285μmであり、より好ましくは105μm〜225μmであり、さらに好ましくは130μm〜210μmである。   The thickness of the pressure-sensitive adhesive sheet (excluding the thickness of the separator) is preferably 90 μm to 285 μm, more preferably 105 μm to 225 μm, and further preferably 130 μm to 210 μm.

D−1.セパレータ
上記セパレータは、本発明のセパレータの選定方法により選定されたものである。セパレータは、通常、基材層および剥離剤層を有する。該基材層および剥離剤層は、任意の適切な材料で構成され得る。好ましくは、該セパレータは、本発明の選定方法において評価したセパレータの剥離力が2.0N/50mm以下であり、より好ましくは0.05N/50mm〜2.0N/50mmであり、さらに好ましくは0.05N/50mm〜1.8N/50mmである。このようなセパレータを用いることにより、優れたハンドリング性を有し、かつ、適度な粘着力が保持された粘着シートが得られる。また、セパレータが粘着剤層からより剥がれにくい粘着シートとする場合には、本発明の選定方法において評価した剥離力が2.0N/50mmを超えるセパレータを用いればよい。
D-1. Separator The separator is selected by the separator selection method of the present invention. The separator usually has a base material layer and a release agent layer. The base material layer and the release agent layer can be composed of any appropriate material. Preferably, the separator has a peel strength of 2.0 N / 50 mm or less, more preferably 0.05 N / 50 mm to 2.0 N / 50 mm, and still more preferably 0, as evaluated by the selection method of the present invention. 0.05 N / 50 mm to 1.8 N / 50 mm. By using such a separator, it is possible to obtain a pressure-sensitive adhesive sheet having excellent handling properties and maintaining an appropriate pressure-sensitive adhesive force. Moreover, when the separator is a pressure-sensitive adhesive sheet that is more difficult to peel off from the pressure-sensitive adhesive layer, a separator having a peel strength evaluated by the selection method of the present invention exceeding 2.0 N / 50 mm may be used.

セパレータの厚みは、特に制限はなく、任意の適切な厚みに設定し得る。セパレータの厚みは、例えば、25μm〜250μmに設定し得る。   The thickness of the separator is not particularly limited and can be set to any appropriate thickness. The thickness of a separator can be set to 25 micrometers-250 micrometers, for example.

D−2.粘着剤層
上記粘着剤層は、任意の適切な粘着剤により構成され、例えば、ポリオレフィン系樹脂、アクリル系樹脂、スチレン系樹脂等の熱可塑性樹脂を含む粘着剤等が挙げられる。該粘着剤層は、好ましくはポリオレフィン系樹脂を含み、具体的には、低密度ポリエチレン、超低密度ポリエチレン、低結晶ポリプロピレン、非晶質プロピレン−(1−ブテン)共重合体、アイオノマー樹脂、エチレン−酢酸ビニル共重合体、エチレン−(メタ)アクリ酸共重合体、エチレン−(メタ)アクリル酸エステル−無水マレイン酸共重合体、エチレン−メタクリル酸グリシジル共重合体などのエチレン共重合体やポリオレフィン変性ポリマー等が挙げられる。該粘着剤層は、より好ましくは非晶質プロピレン−(1−ブテン)共重合体を含む。このような粘着剤層を用いることにより、被着体への汚染が少なく、粘着力と剥離性とが両立され、かつ、共押し出し成形により製造し得る粘着シートが得られる。さらに、このような粘着剤層であれば、基材層との共押し出し成形により粘着シートを製造することが可能であり、少ない工程数で、かつ、有機溶剤を使用することなく粘着シートを得ることができる。なお、本明細書において、「非晶質」とは、結晶質のように明確な融点を有さない性質をいう。
D-2. Pressure-sensitive adhesive layer The pressure-sensitive adhesive layer is composed of any appropriate pressure-sensitive adhesive, and examples thereof include pressure-sensitive adhesives including thermoplastic resins such as polyolefin resins, acrylic resins, and styrene resins. The pressure-sensitive adhesive layer preferably contains a polyolefin-based resin, specifically, low-density polyethylene, ultra-low-density polyethylene, low-crystalline polypropylene, amorphous propylene- (1-butene) copolymer, ionomer resin, ethylene -Ethylene copolymers and polyolefins such as vinyl acetate copolymer, ethylene- (meth) acrylic acid copolymer, ethylene- (meth) acrylic acid ester-maleic anhydride copolymer, ethylene-glycidyl methacrylate copolymer Examples thereof include modified polymers. The pressure-sensitive adhesive layer more preferably contains an amorphous propylene- (1-butene) copolymer. By using such a pressure-sensitive adhesive layer, there can be obtained a pressure-sensitive adhesive sheet that is less contaminated on the adherend, has both adhesive strength and peelability, and can be manufactured by coextrusion molding. Furthermore, with such a pressure-sensitive adhesive layer, it is possible to produce a pressure-sensitive adhesive sheet by coextrusion molding with a base material layer, and a pressure-sensitive adhesive sheet is obtained with a small number of steps and without using an organic solvent. be able to. In this specification, “amorphous” means a property that does not have a clear melting point such as crystalline.

上記非晶質プロピレン−(1−ブテン)共重合体は、好ましくは、メタロセン触媒を用いて、プロピレンと1−ブテンとを重合することにより得ることができる。より詳細には、非晶質プロピレン−(1−ブテン)共重合体は、例えば、メタロセン触媒を用いてプロピレンと1−ブテンとを重合させる重合工程を行い、当該重合工程の後、触媒残さ除去工程、異物除去工程等の後処理工程を行うことにより、得ることができる。非晶質プロピレン−(1−ブテン)共重合体は、このような工程を経て、例えば、パウダー状、ペレット状等の形状で得られる。メタロセン触媒としては、例えば、メタロセン化合物とアルミノキサンとを含むメタロセン均一混合触媒、微粒子状の担体上にメタロセン化合物が担持されたメタロセン担持型触媒等が挙げられる。メタロセン触媒を用いて重合された非晶質プロピレン−(1−ブテン)共重合体は、狭い分子量分布を示す。   The amorphous propylene- (1-butene) copolymer is preferably obtained by polymerizing propylene and 1-butene using a metallocene catalyst. More specifically, the amorphous propylene- (1-butene) copolymer performs, for example, a polymerization step in which propylene and 1-butene are polymerized using a metallocene catalyst, and the catalyst residue is removed after the polymerization step. It can be obtained by performing post-processing steps such as a step and a foreign matter removing step. The amorphous propylene- (1-butene) copolymer is obtained in such a form as a powder or a pellet through such steps. Examples of the metallocene catalyst include a metallocene homogeneous mixed catalyst containing a metallocene compound and an aluminoxane, a metallocene supported catalyst in which a metallocene compound is supported on a particulate carrier, and the like. Amorphous propylene- (1-butene) copolymer polymerized using a metallocene catalyst exhibits a narrow molecular weight distribution.

上記非晶質プロピレン−(1−ブテン)共重合体における、プロピレン由来の構成単位の含有割合は、好ましくは80モル%〜99モル%であり、より好ましくは85モル%〜99モル%であり、さらに好ましくは90モル%〜99モル%である。   The content ratio of the structural unit derived from propylene in the amorphous propylene- (1-butene) copolymer is preferably 80 mol% to 99 mol%, more preferably 85 mol% to 99 mol%. More preferably, it is 90 mol% to 99 mol%.

上記非晶質プロピレン−(1−ブテン)共重合体における、1−ブテン由来の構成単位の含有割合は、好ましくは1モル%〜15モル%であり、より好ましくは1モル%〜10モル%である。このような範囲であれば、靭性と柔軟性とのバランスに優れた粘着シートを得ることができる。   The content ratio of the structural unit derived from 1-butene in the above-mentioned amorphous propylene- (1-butene) copolymer is preferably 1 mol% to 15 mol%, more preferably 1 mol% to 10 mol%. It is. If it is such a range, the adhesive sheet excellent in the balance of toughness and a softness | flexibility can be obtained.

上記非晶質プロピレン−(1−ブテン)共重合体は、ブロック共重合体であってもよく、ランダム共重合体であってもよい。   The amorphous propylene- (1-butene) copolymer may be a block copolymer or a random copolymer.

上記非晶質プロピレン−(1−ブテン)共重合体は、本発明の効果を損なわない範囲で、さらにその他のモノマー由来の構成単位を含んでいてもよい。その他のモノマーとしては、例えば、エチレン、1−ペンテン、1−ヘキセン、1−オクテン、1−デセン、4−メチル−1−ペンテン、3−メチル−1−ペンテン等のα−オレフィン等が挙げられる。   The amorphous propylene- (1-butene) copolymer may further contain other monomer-derived structural units as long as the effects of the present invention are not impaired. Examples of other monomers include α-olefins such as ethylene, 1-pentene, 1-hexene, 1-octene, 1-decene, 4-methyl-1-pentene, and 3-methyl-1-pentene. .

上記粘着剤層は、本発明の効果を損なわない範囲で、さらにその他の成分を含んでいてもよい。当該その他の成分としては、例えば、酸化防止剤、紫外線吸収剤、光安定剤、耐熱安定剤、帯電防止剤等が挙げられる。その他の成分の種類および使用量は、目的に応じて適切に選択され得る。   The pressure-sensitive adhesive layer may further contain other components as long as the effects of the present invention are not impaired. Examples of the other components include an antioxidant, an ultraviolet absorber, a light stabilizer, a heat resistance stabilizer, and an antistatic agent. The kind and usage-amount of another component can be suitably selected according to the objective.

粘着剤層の厚みは、好ましくは20μm〜100μmであり、より好ましくは30μm〜65μmである。   The thickness of the pressure-sensitive adhesive layer is preferably 20 μm to 100 μm, more preferably 30 μm to 65 μm.

D−3.基材層
上記基材層は、任意の適切な材料を用いて構成することができ、例えば、ポリエステル(ポリエチレンテレフタレート、ポリエチレンナフタレート、ポリブチレンテレフタレート、ポリブチレンナフタレートなど)、ポリオレフィン(ポリエチレン、ポリプロピレン、エチレン−プロピレン共重合体など)、ポリビニルアルコール、ポリ塩化ビニリデン、ポリ塩化ビニル、塩化ビニル−酢酸ビニル共重合体、エチレン−酢酸ビニル共重合体、ポリ酢酸ビニル、ポリアミド、ポリイミド、セルロース類、フッ素系樹脂、ポリエーテル、ポリスチレン系樹脂(ポリスチレンなど)、ポリカーボネート、ポリエーテルスルホン等が挙げられる。好ましくは、上記基材層は、エチレン−酢酸ビニル共重合体を含む。
D-3. Base material layer The base material layer can be constituted by using any appropriate material. For example, polyester (polyethylene terephthalate, polyethylene naphthalate, polybutylene terephthalate, polybutylene naphthalate, etc.), polyolefin (polyethylene, polypropylene) , Ethylene-propylene copolymer, etc.), polyvinyl alcohol, polyvinylidene chloride, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyamide, polyimide, celluloses, fluorine Resin, polyether, polystyrene resin (polystyrene, etc.), polycarbonate, polyethersulfone and the like. Preferably, the base material layer includes an ethylene-vinyl acetate copolymer.

上記基材層は、本発明の効果を損なわない範囲で、さらにその他の成分を含んでいてもよい。当該その他の成分としては、例えば、上記で説明した粘着剤層に含まれ得るその他の成分と同様の成分が用いられ得る。   The base material layer may further contain other components as long as the effects of the present invention are not impaired. As said other component, the component similar to the other component which may be contained in the adhesive layer demonstrated above can be used, for example.

基材層の厚みは、好ましくは30μm〜185μmであり、より好ましくは65μm〜175μmである。   The thickness of a base material layer becomes like this. Preferably they are 30 micrometers-185 micrometers, More preferably, they are 65 micrometers-175 micrometers.

D−4.その他の層
本発明の粘着シートに含まれる他の層としては、例えば、粘着シートに耐熱性を付与し得る表面層が挙げられる。該表面層は耐熱性を有する任意の適切な樹脂を用いることができ、好ましくはポリプロピレン系樹脂を含む。上記ポリプロピレン系樹脂は、好ましくはメタロセン触媒を用いた重合により得られる。より詳細には、ポリプロピレン系樹脂は、例えば、メタロセン触媒を用いてプロピレンを含むモノマー組成物を重合させる重合工程を行い、当該重合工程の後、触媒残さ除去工程、異物除去工程等の後処理工程を行うことにより、得ることができる。ポリプロピレン系樹脂は、このような工程を経て、例えば、パウダー状、ペレット状等の形状で得られる。メタロセン触媒としては、例えば、上記で例示したものが挙げられる。
D-4. Other layers Examples of other layers contained in the pressure-sensitive adhesive sheet of the present invention include a surface layer that can impart heat resistance to the pressure-sensitive adhesive sheet. The surface layer can be made of any suitable resin having heat resistance, and preferably contains a polypropylene resin. The polypropylene resin is preferably obtained by polymerization using a metallocene catalyst. More specifically, for example, the polypropylene-based resin performs a polymerization step of polymerizing a monomer composition containing propylene using a metallocene catalyst, and after the polymerization step, a post-treatment step such as a catalyst residue removal step and a foreign matter removal step. Can be obtained. The polypropylene resin is obtained through such a process, for example, in a powder form, a pellet form, or the like. Examples of the metallocene catalyst include those exemplified above.

上記ポリプロピレン系樹脂は市販品を用いてもよい。市販品のポリプロピレン系樹脂の具体例としては、日本ポリプロ(株)製の商品名「WINTEC(ウィンテック)」、「WELNEX(ウェルネックス)」シリーズ等が挙げられる。   A commercially available product may be used as the polypropylene resin. Specific examples of commercially available polypropylene resins include trade names “WINTEC” and “WELNEX” series manufactured by Nippon Polypro Co., Ltd.

上記表面層は、本発明の効果を損なわない範囲で、さらにその他の成分を含んでいてもよい。当該その他の成分としては、上記で説明した粘着剤層に含まれ得るその他成分と同じものが挙げられる。その他の成分の種類および使用量は、目的に応じて適切に選択され得る。   The surface layer may further contain other components as long as the effects of the present invention are not impaired. Examples of the other components include the same components as the other components that can be included in the pressure-sensitive adhesive layer described above. The kind and usage-amount of another component can be suitably selected according to the objective.

以下、実施例により本発明を具体的に説明するが、本発明はこれら実施例になんら限定されるものではない。なお、実施例等における、試験および評価方法は以下のとおりである。また、部は重量部を意味する。   EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited to these Examples at all. In addition, the test and evaluation method in an Example etc. are as follows. Moreover, a part means a weight part.

(参考例1)試験用粘着シートの作製
耐熱性を付与し得る表面層を形成する材料として、メタロセン触媒により重合したポリプロピレン系樹脂(日本ポリプロ社製、商品名「WELNEX:RFGV4A」;融点130℃、軟化点120℃、Mw/Mn=2.9)を用いた。
基材層を形成する材料として、エチレン−酢酸ビニル共重合体(三井デュポン社製、商品名「エバフレックスP−1007」)を用いた。
粘着剤層を形成する材料として、メタロセン触媒により重合した非晶質プロピレン−(1−ブテン)共重合体(住友化学社製、商品名「タフセレンH5002」:プロピレン由来の構成単位90モル%/1−ブテン由来の構成単位10モル%、Mw=230,000、Mw/Mn=1.8)を用いた。
上記表面層を形成する材料100部、上記基材層を形成する材料100部および上記粘着剤層を形成する材料100部をそれぞれの押し出し機に投入し、Tダイ溶融共押し出しした(ダイス温度:180℃)。ダイスから共押し出しされた表面層/基材層/粘着剤層の積層体の粘着剤層に製造用セパレータ(三菱樹脂社製、MRF38、厚み38μm)をタッチロールにより貼り合せ(エアギャップ:150mm、接触温度:165℃)、表面層(厚み30μm)/基材層(厚み130μm)/粘着剤層(厚み45μm)/セパレータの試験用粘着シートを得た。なお、表面層、基材層および粘着剤層の厚みは、Tダイ出口の形状により制御した。
Reference Example 1 Preparation of Test Adhesive Sheet Polypropylene resin polymerized with a metallocene catalyst (trade name “WELNEX: RFGV4A” manufactured by Nippon Polypro Co., Ltd.) as a material for forming a surface layer capable of imparting heat resistance; melting point 130 ° C. , Softening point 120 ° C., Mw / Mn = 2.9).
As a material for forming the base material layer, an ethylene-vinyl acetate copolymer (manufactured by Mitsui DuPont, trade name “Evaflex P-1007”) was used.
As a material for forming the pressure-sensitive adhesive layer, an amorphous propylene- (1-butene) copolymer polymerized by a metallocene catalyst (manufactured by Sumitomo Chemical Co., Ltd., trade name “Tufselen H5002”: propylene-derived structural unit 90 mol% / 1 -Butene-derived structural unit 10 mol%, Mw = 230,000, Mw / Mn = 1.8).
100 parts of the material for forming the surface layer, 100 parts of the material for forming the base material layer, and 100 parts of the material for forming the pressure-sensitive adhesive layer were put into each extruder and co-extruded with a T die (die temperature: 180 ° C). A production separator (Mitsubishi Resin, MRF38, thickness 38 μm) is bonded to the pressure-sensitive adhesive layer of the surface layer / base material layer / pressure-sensitive adhesive layer layer co-extruded from the die using a touch roll (air gap: 150 mm, A pressure-sensitive adhesive sheet for test of contact temperature: 165 ° C., surface layer (thickness 30 μm) / base material layer (thickness 130 μm) / adhesive layer (thickness 45 μm) / separator was obtained. In addition, the thickness of the surface layer, the base material layer, and the pressure-sensitive adhesive layer was controlled by the shape of the T-die outlet.

[実施例1]粘着シートに適したセパレータの選定
(評価用セパレータ1)
参考例1で得られた粘着シートから粘着剤層側のセパレータを剥離した。次いで、粘着剤層に、評価用セパレータ1(東山フイルム社製、HY−S30、厚み38μm)を貼り合せ、評価用粘着シートを得た。
得られた評価用粘着シートをプレス機(東洋精機社製、MINI TEST PRESS−10、板面面積:250mm×250mm)を用いてプレスした。樹脂シート(セパレータ)として三菱樹脂製、MRN38を、クッション材としてゴム板(厚み:1mm、130mm×160mm)を用いた。評価用粘着シートは、ステンレス板(SUS板)/樹脂シート/クッション材/樹脂シート/評価用粘着シート/樹脂シート/クッション材/樹脂シート/ステンレス板の順に積層した後、プレス板で狭持し、プレス板面温度140℃、プレス圧力5MPaで1分間保持した。次いで、粘着シートを室温まで放置し、粘着シートの評価用セパレータの剥離力(剥離速度:300mm/分、剥離角度:180°)を測定した。測定した剥離力を表1に示す。
[Example 1] Selection of a separator suitable for an adhesive sheet (Evaluation Separator 1)
The pressure-sensitive adhesive layer separator was peeled from the pressure-sensitive adhesive sheet obtained in Reference Example 1. Next, an evaluation separator 1 (Higashiyama Film Co., Ltd., HY-S30, thickness 38 μm) was bonded to the adhesive layer to obtain an evaluation adhesive sheet.
The obtained pressure-sensitive adhesive sheet for evaluation was pressed using a press machine (manufactured by Toyo Seiki Co., Ltd., MINI TEST PRESS-10, plate surface area: 250 mm × 250 mm). MRN38 made by Mitsubishi Plastics was used as the resin sheet (separator), and a rubber plate (thickness: 1 mm, 130 mm × 160 mm) was used as the cushioning material. The adhesive sheet for evaluation is laminated in the order of stainless steel plate (SUS plate) / resin sheet / cushion material / resin sheet / adhesive sheet for evaluation / resin sheet / cushion material / resin sheet / stainless steel plate, and then sandwiched by a press plate. The pressing plate surface temperature was held at 140 ° C. and the pressing pressure of 5 MPa for 1 minute. Next, the pressure-sensitive adhesive sheet was allowed to stand to room temperature, and the peeling force (peeling speed: 300 mm / min, peeling angle: 180 °) of the separator for evaluation of the pressure-sensitive adhesive sheet was measured. The measured peel force is shown in Table 1.

(評価用セパレータ2)
評価用セパレータ1に代えて、評価用セパレータ2(東山フイルム社製、HY−TS11、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 2)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 2 (Higashiyama Film Co., Ltd., HY-TS11, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ3)
評価用セパレータ1に代えて、評価用セパレータ3(東山フイルム社製、HY−TS15、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 3)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 3 (Higashiyama Film Co., Ltd., HY-TS15, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ4)
評価用セパレータ1に代えて、評価用セパレータ4(三菱樹脂社製、MRE38、厚み38μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 4)
The peel strength of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 4 (MRE38, thickness 38 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ5)
評価用セパレータ1に代えて、評価用セパレータ5(三菱樹脂社製、MRN38、厚み38μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 5)
The peeling force of the evaluation separator was measured in the same manner as in the evaluation separator 1 except that the evaluation separator 5 (manufactured by Mitsubishi Plastics, MRN38, thickness 38 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ6)
評価用セパレータ1に代えて、評価用セパレータ6(三菱樹脂社製、MRF38、厚み38μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 6)
The peel strength of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 6 (MRF38, thickness 38 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ7)
評価用セパレータ1に代えて、評価用セパレータ7(東山フイルム社製、HY−S10、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 7)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 7 (Higashiyama Film, HY-S10, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ8)
評価用セパレータ1に代えて、評価用セパレータ8(東山フイルム社製、HY−S06、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 8)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 8 (Higashiyama Film Co., Ltd., HY-S06, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ9)
評価用セパレータ1に代えて、評価用セパレータ9(東山フイルム社製、HY−TS05G、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 9)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 9 (Higashiyama Film Co., Ltd., HY-TS05G, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

(評価用セパレータ10)
評価用セパレータ1に代えて、評価用セパレータ10(東山フイルム社製、HY−US20、厚み75μm)を用いた以外は評価用セパレータ1と同様にして、評価用セパレータの剥離力を測定した。測定した剥離力を表1に示す。
(Evaluation separator 10)
The peeling force of the evaluation separator was measured in the same manner as the evaluation separator 1 except that the evaluation separator 10 (Higashiyama Film Co., Ltd., HY-US20, thickness 75 μm) was used instead of the evaluation separator 1. The measured peel force is shown in Table 1.

Figure 0005801615
Figure 0005801615

[実施例2]選定したセパレータを用いた粘着シートの評価
評価用セパレータ1〜10を用いた以外は参考例1と同様にして、粘着シート1〜10を得た。得られた粘着シート1〜10を以下の評価に供した。結果を表2に示す。
[評価]
(1)セパレータの剥離力
得られた粘着シートにおけるセパレータの剥離力(剥離速度:300mm/min、剥離角度:180°)を測定した。
(2)粘着剤層の粘着力
得られた粘着シートを50℃にて2日間エージングした後、粘着剤層に貼り合せられたセパレータを剥離し、該粘着剤層の4インチ半導体ウエハのミラー面(シリコン製)に対する粘着力を、JIS Z 0237(2000)に準じた方法(貼り合わせ条件:2kgローラー1往復、剥離速度:300mm/min、剥離角度180°)により測定した。測定した値が0.005N/20mm以上であれば、粘着シートとして十分な粘着力を有している。
[Example 2] Evaluation of adhesive sheet using selected separator Adhesive sheets 1 to 10 were obtained in the same manner as in Reference Example 1 except that evaluation separators 1 to 10 were used. The obtained adhesive sheets 1 to 10 were subjected to the following evaluation. The results are shown in Table 2.
[Evaluation]
(1) Separation force of separator The separation force (peeling speed: 300 mm / min, peeling angle: 180 °) of the separator in the obtained pressure-sensitive adhesive sheet was measured.
(2) Adhesive strength of the pressure-sensitive adhesive layer After the obtained pressure-sensitive adhesive sheet was aged at 50 ° C. for 2 days, the separator bonded to the pressure-sensitive adhesive layer was peeled off, and the mirror surface of the 4-inch semiconductor wafer of the pressure-sensitive adhesive layer The adhesive strength to (made of silicon) was measured by a method according to JIS Z 0237 (2000) (bonding condition: 2 kg roller 1 reciprocation, peeling speed: 300 mm / min, peeling angle 180 °). If the measured value is 0.005 N / 20 mm or more, it has sufficient adhesive strength as an adhesive sheet.

Figure 0005801615
Figure 0005801615

実施例1で測定したセパレータの剥離力が2.0N/50mm以下であるセパレータ1〜5を用いた粘着シート1〜5は、セパレータの剥離が容易であり、かつ、粘着剤層の粘着力が適度に維持されていた。また、実施例1で測定したセパレータの剥離力が2.0N/50mmを超えるセパレータ6〜10を用いた粘着シート6〜10は、セパレータ1〜5に比べてセパレータを剥離するために必要な力が大きかった。   The pressure-sensitive adhesive sheets 1 to 5 using the separators 1 to 5 whose separator peeling force measured in Example 1 is 2.0 N / 50 mm or less are easy to peel off the separator, and the pressure-sensitive adhesive layer has a pressure-sensitive adhesive strength. It was maintained moderately. Moreover, the pressure-sensitive adhesive sheets 6 to 10 using the separators 6 to 10 whose separator peeling force measured in Example 1 exceeds 2.0 N / 50 mm are required to peel the separator as compared with the separators 1 to 5. Was big.

本発明のセパレータの選定方法は、例えば、粘着シートに用いるセパレータの選定に好適に用いることができる。   The method for selecting a separator of the present invention can be suitably used for selecting a separator used for an adhesive sheet, for example.

Claims (4)

少なくとも粘着剤層を形成する材料が溶融した状態でセパレータと貼り合せ、少なくとも粘着剤層とセパレータとを有する粘着シートを得る工程、
得られた粘着シートから該セパレータを剥離し、該粘着シートの粘着剤層と評価用セパレータとを貼り合せて評価用粘着シートを作製する工程
評価用粘着シートを一対のクッション材および一対のプレス板で狭持し、プレス板面温度140℃、圧力5MPaで1分間保持した後、剥離速度300mm/分での180°剥離試験により評価用セパレータの剥離力を評価する工程、および、
該評価工程で測定された剥離力2.0N/50mmを基準とし、セパレータに要求する特性に応じて、所望のセパレータを選択する工程を含む、セパレータの選定方法。
A step of obtaining a pressure-sensitive adhesive sheet having at least a pressure-sensitive adhesive layer and a separator, pasted with a separator in a state where a material forming at least a pressure-sensitive adhesive layer is melted
The step of peeling the separator from the obtained pressure-sensitive adhesive sheet, and bonding the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet and the separator for evaluation to produce a pressure-sensitive adhesive sheet for evaluation ,
The evaluation pressure-sensitive adhesive sheet is sandwiched between a pair of cushion materials and a pair of press plates, held at a press plate surface temperature of 140 ° C. and a pressure of 5 MPa for 1 minute, and then evaluated by a 180 ° peel test at a peel rate of 300 mm / min. A step of evaluating the peeling force of the separator , and
A method for selecting a separator, comprising a step of selecting a desired separator according to the characteristics required of the separator based on the peel force of 2.0 N / 50 mm measured in the evaluation step .
前記評価工程において測定された剥離力が2.0N/50mm以下であるセパレータを選定する、請求項1に記載のセパレータの選択方法。   The method for selecting a separator according to claim 1, wherein a separator having a peel force measured in the evaluation step of 2.0 N / 50 mm or less is selected. 前記粘着シートの粘着剤層がポリオレフィン系樹脂を含む、請求項1または2に記載のセパレータの選定方法。   The selection method of the separator of Claim 1 or 2 with which the adhesive layer of the said adhesive sheet contains polyolefin resin. 前記ポリオレフィン系樹脂がメタロセン触媒を用いて重合された非晶質プロピレン−(1−ブテン)共重合体を含む、請求項3に記載のセパレータの選定方法。
The method for selecting a separator according to claim 3, wherein the polyolefin-based resin includes an amorphous propylene- (1-butene) copolymer polymerized using a metallocene catalyst.
JP2011131911A 2011-06-14 2011-06-14 Separator selection method and pressure-sensitive adhesive sheet using the separator selected by the selection method Expired - Fee Related JP5801615B2 (en)

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KR1020127027326A KR101427504B1 (en) 2011-06-14 2012-05-30 Method for selecting separator, and pressure-sensitive adhesive sheet using separator selected by the method
CN201280002198.6A CN103038300B (en) 2011-06-14 2012-05-30 Selection method for separator and adhesive sheet using separator selected by selection method
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