KR101355097B1 - Aqueous emulsion pressure sensitive adhesive composition and adhesive film using the same - Google Patents

Aqueous emulsion pressure sensitive adhesive composition and adhesive film using the same Download PDF

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KR101355097B1
KR101355097B1 KR1020120003580A KR20120003580A KR101355097B1 KR 101355097 B1 KR101355097 B1 KR 101355097B1 KR 1020120003580 A KR1020120003580 A KR 1020120003580A KR 20120003580 A KR20120003580 A KR 20120003580A KR 101355097 B1 KR101355097 B1 KR 101355097B1
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nanoparticles
adhesive material
aqueous emulsion
sensitive adhesive
water
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KR20130082389A (en
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류연정
서창호
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도레이첨단소재 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • 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
    • 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]
    • C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385—Acrylic polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • 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
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer

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

Abstract

본 발명은 수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름에 관한 것으로서, 보다 상세하게는 친환경 규제에 적극적으로 대응할 수 있고 사용 환경을 친환경적으로 개선할 수 있으며, 또한 우수한 내열성과 전단력을 갖는 수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름에 관한 것이다. 이를 위해 본 발명에 따른 수계형 에멀젼 점착소재 조성물은 2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 메틸메타크릴레이트 및 아크릴산 모노머 중 적어도 하나의 모노머를 포함하는 모노머 혼합물, 탈이온수, 계면활성제, 나노입자, 탄산수소나트륨 및 암모늄 퍼설페이트를 포함하는 것을 특징으로 한다.The present invention relates to an aqueous emulsion adhesive material composition and an adhesive film using the same, and more particularly, an aqueous emulsion having active heat resistance and environmentally friendly environment improvement, and excellent heat resistance and shear strength. It relates to an adhesive material composition and an adhesive film using the same. To this end, the aqueous emulsion pressure-sensitive adhesive composition according to the present invention is a monomer mixture, deionized water, surfactants, containing at least one monomer of 2-ethylhexyl acrylate, n-butyl acrylate, methyl methacrylate and acrylic acid monomer And nanoparticles, sodium bicarbonate and ammonium persulfate.

Description

수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름{AQUEOUS EMULSION PRESSURE SENSITIVE ADHESIVE COMPOSITION AND ADHESIVE FILM USING THE SAME}Aqueous emulsion adhesive material composition and adhesive film using same {AQUEOUS EMULSION PRESSURE SENSITIVE ADHESIVE COMPOSITION AND ADHESIVE FILM USING THE SAME}

본 발명은 수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름에 관한 것으로서, 보다 상세하게는 친환경 규제에 적극적으로 대응할 수 있고 사용 환경을 친환경적으로 개선할 수 있으며, 또한 우수한 내열성과 전단력을 갖는 수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름에 관한 것이다.The present invention relates to an aqueous emulsion adhesive material composition and an adhesive film using the same, and more particularly, an aqueous emulsion having active heat resistance and environmentally friendly environment improvement, and excellent heat resistance and shear strength. It relates to an adhesive material composition and an adhesive film using the same.

종래에 범용적으로 사용되는 점착제는 휘발성 유기 용제를 용매로 하여 제조하는 용제형 점착제가 대부분이다. 하지만, 산업이 고도화되면서 환경규제들이 점차 강화되고 있는데 반하여 휘발성 유기용제를 사용하는 경우 많은 환경문제들이 야기된다. 따라서 점착제 분야에서도 환경 유해 성분이 적은 점착제에 대한 요구가 증가되고 있다.Conventionally, adhesives generally used in general are solvent type adhesives prepared by using a volatile organic solvent as a solvent. However, environmental regulations are gradually being strengthened as the industry is advanced, and many environmental problems are caused when volatile organic solvents are used. Therefore, in the pressure-sensitive adhesive field, there is an increasing demand for pressure-sensitive adhesives with less environmentally harmful components.

이러한 요구에 따라 최근에는 용제형 점착제를 대체할 수 있는 물을 용매로 사용하는 수성형의 점착제가 개발되고 있다. 이러한 종래기술로 한국 공개특허공보 제1996-41303호는 수성 아크릴 에멀션에 다가 알코올의 단랑체 또는 중합체를 첨가하여 제조되는 수성 점착제 조성물을 개시하고, 한국 공개특허공보 제1997-42907호는 저분자량 폴리아크릴산 등과 고분자량 폴리아크릴산 등을 특정 중량비로 배합한 수성 점착제 조성물을 개시하고 있으며, 또한 일본 공개특허공보 제2005-146271호는 (메타)아크릴산 알킬 에스테르, 중합성 불포화 카복실산 및 상기와 공중합 가능한 단량체의 유화 중합물인 수성 분산체 및 점착 부여 수지의 수성 에멀션을 포함하고, 점도, 응집물 발생율 및 불휘발 성분의 양이 한정된 수성 에멀션형 점착제를 개시하고 있다.Recently, an aqueous pressure sensitive adhesive using water as a solvent, which can replace a solvent pressure sensitive adhesive, has been developed. In this prior art, Korean Laid-Open Patent Publication No. 1996-41303 discloses an aqueous pressure-sensitive adhesive composition prepared by adding monomeric or polymer of polyhydric alcohol to an aqueous acrylic emulsion, and Korean Laid-Open Patent Publication No. 1997-42907 discloses a low molecular weight poly An aqueous pressure-sensitive adhesive composition is disclosed in which acrylic acid and the like and high molecular weight polyacrylic acid are blended in a specific weight ratio. Japanese Unexamined Patent Publication No. 2005-146271 discloses an alkyl ester of (meth) acrylic acid, a polymerizable unsaturated carboxylic acid and a monomer copolymerizable with the above. An aqueous emulsion pressure sensitive adhesive comprising an aqueous dispersion of an emulsion polymer and an aqueous emulsion of a tackifying resin and having a limited amount of viscosity, aggregate generation rate and nonvolatile components is disclosed.

그러나, 이러한 수성형 점착제는 용제형 점착제에 비해 점착 물성이나 내열성이 낮다는 문제점이 있다. 이러한 문제점을 해결하기 위하여 나노입자 등 다양한 필러가 활용되는 점착소재가 개발되고 있다. 일반적으로 가로, 세로, 높이로 입자의 크기를 나타내는데 나노입자란 가로, 세로, 높이 중 한 가지 이상이 나노미터의 범위에 드는 것을 나노입자라고 칭한다. However, such an aqueous adhesive has a problem in that adhesive physical properties and heat resistance are lower than those of a solvent adhesive. In order to solve this problem, adhesive materials that utilize various fillers such as nanoparticles have been developed. Generally, the size of a particle is expressed by width, length, and height. Nanoparticles are referred to as nanoparticles when one or more of width, length, and height fall within a range of nanometers.

최근 나노복합재료에 대한 연구 및 적용이 한창이며, 본 특허 또한 그 연장선에 있다고 할 수 있겠다. 필러로서 적용되는 나노입자의 종류 또한 유기, 무기, 금속 등으로 그 종류가 매우 다양하다. 이러한 나노입자는 단독으로 사용되기 보다는 고분자 등에 첨가제(필러)로 첨가하여 해당 고분자의 특성을 향상과 부족한 물성을 보완하는 역할을 하게 된다. 일반적으로 고분자에 이런 나노입자를 첨가함으로써 기계적 강도 증가, 내용매성, 열적안정성, 전단력 증가, 내구성증가 등 여러 유용한 특성이 향상되며 그로 인해 적용범위 또한 확장되고 있다.Recently, research and application of nanocomposite materials are in full swing, and this patent can be said to be an extension of them. Kinds of nanoparticles applied as fillers also vary widely in organic, inorganic, metal, and the like. These nanoparticles are added to the polymer as an additive (filler) rather than used alone to improve the properties of the polymer and to compensate for the lack of physical properties. In general, the addition of such nanoparticles to polymers improves various useful properties such as increased mechanical strength, solvent resistance, thermal stability, increased shear force, and increased durability, thereby expanding the scope of application.

한국 공개특허공보 제1996-41303호Korean Unexamined Patent Publication No. 1996-41303 한국 공개특허공보 제1997-42907호Korean Unexamined Patent Publication No. 1997-42907 일본 특허공개공보 제2005-146271호Japanese Patent Publication No. 2005-146271

본 발명은 상기와 같은 문제점을 해결하기 위해 안출한 것으로서, 본 발명의 목적은 친환경 규제에 적극적으로 대응할 수 있고 사용 환경을 친환경적으로 개선할 수 있으며, 또한 우수한 내열성과 전단력을 갖는 수계형 에멀젼 점착소재 조성물 및 이를 이용한 점착필름을 제공하고자 하는 것이다.The present invention has been made to solve the above problems, the object of the present invention can actively respond to environmental regulations, improve the environment for use environmentally, and also has a water-based emulsion adhesive material having excellent heat resistance and shear force It is to provide a composition and an adhesive film using the same.

본 발명의 상기 및 다른 목적과 이점은 바람직한 실시예를 설명한 하기의 설명으로부터 보다 분명해 질 것이다.These and other objects and advantages of the present invention will become more apparent from the following description of a preferred embodiment thereof.

상기 목적은, 2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 메틸메타크릴레이트 및 아크릴산 모노머 중 적어도 하나의 모노머를 포함하는 모노머 혼합물, 탈이온수, 계면활성제, 나노입자, 탄산수소나트륨 및 암모늄 퍼설페이트를 포함하는 것을 특징으로 하는 수계형 에멀젼 점착소재 조성물에 의해 달성된다.The object is a monomer mixture comprising at least one monomer of 2-ethylhexyl acrylate, n-butyl acrylate, methyl methacrylate and acrylic acid monomer, deionized water, surfactants, nanoparticles, sodium bicarbonate and ammonium per It is achieved by the aqueous emulsion adhesive material composition, characterized in that it comprises a sulfate.

여기서, 상기 나노입자의 함량은 상기 수계형 에멀젼 점착소재 조성물 총 중량 대비 2 내지 10중량%인 것을 특징으로 한다.Here, the content of the nanoparticles is characterized in that 2 to 10% by weight relative to the total weight of the aqueous emulsion adhesive material composition.

바람직하게는, 상기 나노입자는 무기계 나노입자로서, 몬모릴로나이트계 나노입자인 것을 특징으로 한다.Preferably, the nanoparticles are inorganic nanoparticles, characterized in that montmorillonite-based nanoparticles.

바람직하게는, 상기 나노입자는 그 표면이 유기화제로 표면처리된 것을 특징으로 한다.Preferably, the nanoparticles are characterized in that the surface is surface-treated with an organic agent.

또한 상기 목적은 기재필름과 상기 기재필름의 적어도 일 면에 상술한 수계형 에멀젼 점착소재 조성물로 코팅된 수계형 에멀젼 점착소재를 포함하는 것을 특징으로 하는 점착필름에 의해 달성된다.In addition, the above object is achieved by a pressure-sensitive adhesive film comprising a water-based emulsion pressure-sensitive adhesive material coated on the at least one surface of the base film and the water-based emulsion pressure-sensitive adhesive composition.

본 발명에 따르면, 용제를 물로 대체할 수 있기 때문에 친환경 규제에 적극적으로 대응할 수 있고 사용 환경을 친환경적으로 개선할 수 있으며, 또한 나노입자를 포함함으로써 수계형 아크릴점착제가 가지고 있는 가장 큰 문제점인 내열성을 향상시킬 수 있고 전단력이 우수한 등의 효과를 가진다.According to the present invention, since the solvent can be replaced with water, it can actively respond to environmental regulations, improve the environment for use, and also include nanoparticles, so that heat resistance, which is the biggest problem of the water-based acrylic adhesive agent, is included. It can improve and have an excellent shearing force.

도 1은 종래의 필러가 첨가되지 않은 점착필름의 단면도
도 2는 본 발명에 따른 점착필름의 단면도. 1 is a cross-sectional view of an adhesive film without a conventional filler
2 is a cross-sectional view of the adhesive film according to the present invention.

이하, 본 발명의 실시예와 도면을 참조하여 본 발명을 상세히 설명한다. 이들 실시예는 오로지 본 발명을 보다 구체적으로 설명하기 위해 예시적으로 제시한 것일 뿐, 본 발명의 범위가 이들 실시예에 의해 제한되지 않는다는 것은 당업계에서 통상의 지식을 가지는 자에 있어서 자명할 것이다.Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. It will be apparent to those skilled in the art that these embodiments are provided by way of illustration only for the purpose of more particularly illustrating the present invention and that the scope of the present invention is not limited by these embodiments .

본 발명에 따른 수계형 에멀젼 점착소재 조성물은 수계형 에멀젼 점착소재의 구성과 필러의 활용을 통한 전단력 및 내열성 향상을 주된 목적으로 하는 나노물질을 포함하는 내열성 및 전단력이 우수한 수계형 에멀젼 점착소재 조성물에 관한 것으로서, 2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 메틸메타크릴레이트 및 아크릴산 모노머 중 적어도 하나의 모노머를 포함하는 모노머 혼합물, 탈이온수, 계면활성제, 나노입자, 탄산수소나트륨 및 암모늄 퍼설페이트를 포함하는 것을 특징으로 한다.The water-based emulsion pressure-sensitive adhesive composition according to the present invention is excellent in heat resistance and shear force-containing water-based emulsion pressure-sensitive adhesive composition comprising a nano-material for the main purpose to improve the shear force and heat resistance through the composition of the water-based emulsion adhesive material and the use of the filler A monomer mixture comprising at least one monomer of 2-ethylhexyl acrylate, n-butyl acrylate, methyl methacrylate and acrylic acid monomer, deionized water, surfactants, nanoparticles, sodium bicarbonate and ammonium persulfate Characterized in that it comprises a.

즉 본 발명에 따른 수계형 에멀젼 점착소재 조성물은 나노입자가 포함된 내열성 및 전단력이 우수한 수계형 에멀젼 점착소재 조성물에 관한 것으로, 상세하게는 아크릴계 수계 점착제의 제조와 그 물성 향상에 관련된 것으로서, 이를 위해 수계형 아크릴점착제를 제조하기 위해 반 회분식(Semibatch) 중합방식을 고안하고 이에 주요 중합소재인 2-EHA(2-Ethylhexyl acrylate)와 BA(Butyl acrylate)를 배합하여 가장 우수한 물성의 수계형 점착소재를 합성하는 것에 관한 것이다. 특히 합성된 수계형 아크릴 점착제의 내열성을 높여주기 위해 나노입자를 첨가하는 것이 본 발명의 핵심이다.That is, the water-based emulsion pressure-sensitive adhesive composition according to the present invention relates to a water-based emulsion pressure-sensitive adhesive composition having excellent heat resistance and shearing force, including nanoparticles, and more particularly, to the production of acrylic water-based pressure-sensitive adhesive and its physical properties. In order to manufacture a water-based acrylic adhesive, a semi-batch polymerization method was devised, and the main polymerization material, 2-EHA (2-Ethylhexyl acrylate) and BA (Butyl acrylate), were mixed to produce the water-based adhesive material having the most excellent physical properties. It is about synthesizing. In particular, the addition of nanoparticles to enhance the heat resistance of the synthetic water-based acrylic pressure-sensitive adhesive is the core of the present invention.

또한 상기 나노입자의 함량은 상기 수계형 에멀젼 점착소재 조성물 총 중량 대비 2 내지 10중량%인 것을 특징으로 한다. 상기 나노입자의 함량이 2중량% 미만일 경우 입자첨가에 따른 효과가 나타나지 않으며 10중량%를 초과하여도 입자첨가에 따른 효과가 비슷하혀 필요 이상으로 첨가할 필요가 없기 때문에 상기 범위로 하는 것이 바람직하다. 즉 무기입자를 적게 사용하면서도 원하는 성능 향상 내지 효과를 볼 수 있는 범위가 상술한 범위이다.In addition, the content of the nanoparticles is characterized in that 2 to 10% by weight relative to the total weight of the aqueous emulsion adhesive material composition. When the content of the nanoparticles is less than 2% by weight, the effect of particle addition does not appear, and even if it exceeds 10% by weight, the effect of particle addition is similar, so it is preferable to set the above range because it is not necessary to add more than necessary. . That is, the range of the desired performance improvement or effect while using less inorganic particles is the above-mentioned range.

상기 나노입자는 유기계, 무기계, 금속계 중 무기계이며 무기계중에서도 클레이이며, 더욱 바람직하게 클레이중 그 성분이 몬모릴로나이트인 것을 특징으로 한다.The nanoparticles are inorganic among organic, inorganic, and metallic, and are clay in inorganic. More preferably, the nanoparticles are montmorillonite.

또한 본 발명에 따른 수계형 에멀젼 점착소재 조성물은 상기 나노입자를 수계형 점착소재 조성물에 분산시 분산효율을 높이고 나노입자 사이의 뭉침을 방지하기 위하여 나노입자의 표면이 유기화제로 표면처리된 것을 특징으로 한다. 즉, 이러한 표면처리를 통해 첨가제로서 매트릭스와의 상용성을 높여 부작용을 줄이고, 기계적 강도 증가, 내용매성, 열적안정성, 전단력 증가, 내구성증가 등과 같은 물성을 향상시킬 수 있는 역할을 하는 것이다. 본 발명에서 사용되는 몬모릴로나이트로 구성된 나노입자(CLAYTONE®, Southern Clay)는 현재 판매사인 Rockwood에서 표면처리된 것과 그렇지 않은 것으로 구분되어 판매중인데, 본 발명에서는 상술한 이유로 몬모릴로나이트의 표면에 유기성분인 4급암모늄이온(Quaternary ammonium ions)을 결합하여 표면처리된 몬모릴로나이트로 구성된 나노입자를 사용하는 것이 바람직하다. In addition, the aqueous emulsion adhesive material composition according to the present invention is characterized in that the surface of the nanoparticles surface-treated with an organic agent to increase the dispersion efficiency when the nanoparticles are dispersed in the aqueous adhesive material composition and to prevent agglomeration between the nanoparticles. It is done. In other words, through such a surface treatment to increase the compatibility with the matrix as an additive to reduce the side effects, and to improve the physical properties such as increased mechanical strength, solvent resistance, thermal stability, increased shear strength, durability. Nanoparticles (CLAYTONE®, Southern Clay) composed of montmorillonite used in the present invention are currently marketed and sold as those that are not surface-treated by Rockwood, the company in the present invention, in the present invention for the above-described reasons of the organic component on the surface of montmorillonite It is preferable to use nanoparticles composed of montmorillonite surface-treated by combining quaternary ammonium ions.

또한 본 발명에 따른 점착필름은 기재필름과 상기 기재필름의 적어도 일 면에 상술한 수계형 에멀젼 점착소재 조성물로 도포된 수계형 에멀젼 점착소재를 포함하는 것을 특징으로 한다.In addition, the pressure-sensitive adhesive film according to the present invention is characterized in that it comprises a water-based emulsion pressure-sensitive adhesive material coated with the above-described water-based emulsion pressure-sensitive adhesive composition on at least one surface of the base film.

상기 기재필름은 특별히 한정되지 않으나 폴리에틸렌테레프탈레이트 필름 등의 폴리에스테르계 필름, 폴리에틸렌 필름, 폴리프로필렌 필름 등이 사용될 수 있다.The base film is not particularly limited, but polyester-based films such as polyethylene terephthalate films, polyethylene films, polypropylene films, and the like may be used.

또한 상기 수계형 에멀젼 점착소재는 20㎛이상의 두께로 코팅된 것이 바람직하다.In addition, the aqueous emulsion adhesive material is preferably coated with a thickness of 20㎛ or more.

이하, 실시예와 비교예를 통하여 본 발명의 구성 및 그에 따른 효과를 보다 상세히 설명하고자 한다. 그러나, 본 실시예는 본 발명을 보다 구체적으로 설명하기 위한 것이며, 본 발명의 범위가 이들 실시예에 한정되는 것은 아니다.Hereinafter, the structure and effect of the present invention will be described in more detail with reference to examples and comparative examples. However, this embodiment is intended to explain the present invention more specifically, and the scope of the present invention is not limited to these embodiments.

[실시예 1]Example 1

본 실시예는 에멀젼 중합의 방법으로 합성된다. 먼저, 아크릴점착제를 조성하기 위해 2-에틸헥실아크릴레이트(2-EHA, 99.5%) 75g, n-부틸아크릴레이트(BA, 99.0%) 150g, 메틸메타크릴레이트(MMA, 99.0%) 17,5g과 아크릴산(AA, 99.5%) 7.5g이 사용되고, 용제로 탈이온수(Deionized water) 172.5g을 사용하며, 개시제로 암모늄 퍼설페이트(APS, 99.0%) 1.25g이 사용되고 마이셀을 형성시키기 위한 계면활성제로 소듐도데실설페이트(SDS, activity in water; 34.5~38.5%) 2g과 폴리옥시에틸렌알킬에테르황산염(anionic surfactant with nonionic segment) 3g이 사용되며, pH를 제어하기 위해 탄산수소나트륨(NaHCO3,99.0%) 1.25g을 사용하여 수계형 에멀젼 점착소재를 만들고, 코로나 처리한 50㎛ PET 기재필름에 코팅두께 30㎛±2㎛로 코팅한 후 100℃ 건조오븐에서 5분 동안 건조시켜 실시예 1로 하였다. This example is synthesized by the method of emulsion polymerization. First, 75 g of 2-ethylhexyl acrylate (2-EHA, 99.5%), 150 g of n-butyl acrylate (BA, 99.0%), 17,5 g of methyl methacrylate (MMA, 99.0%) to form an acrylic adhesive And 7.5 g of acrylic acid (AA, 99.5%) are used, 172.5 g of deionized water is used as a solvent, 1.25 g of ammonium persulfate (APS, 99.0%) is used as an initiator, and as a surfactant to form micelles. sodium dodecyl sulfate (SDS, activity in water; 34.5 ~ 38.5%) 2g and polyoxyethylene alkyl ether sulfate (anionic surfactant with nonionic segment) 3g is used, NaHCO (sodium hydrogen carbonate in order to control the pH 3, 99.0% ) 1.25g to prepare a water-based emulsion pressure-sensitive adhesive material, coated on a corona treated 50㎛ PET base film with a coating thickness of 30㎛ ± 2㎛ and dried in 100 ℃ drying oven for 5 minutes to give Example 1.

[실시예 2 내지 4][Examples 2 to 4]

다음으로 실시예 1에 하기 표 1과 같이 몬모릴로나이트로 구성된 나노입자(CLAYTONE?, Southern Clay)의 성분비를 포함한 수계형 에멀젼 점착소재 조성물을 제조하여 코로나 처리한 50㎛ PET 기재필름에 코팅두께 30㎛±2㎛로 코팅한 후 100℃ 건조오븐에서 5분 동안 건조시켜 각각 실시예 2 내지 5로 하였다. 하기 표 1에서 "수계형 에멀젼 점착소재"는 "수계형 에멀젼 점착소재 조성물"에서 "나노입자"를 제외한 구성을 의미하고 "%"는 "중량%"를 나타낸다.Next, in Example 1, a water-based emulsion adhesive material composition including a component ratio of montmorillonite-containing nanoparticles (CLAYTONE®, Southern Clay) as shown in Table 1 was prepared, and the coating thickness was 30 μm ± on a 50 μm PET base film treated with corona treatment. After coating at 2㎛ dried in an oven for 5 minutes at 100 ℃ dry to obtain Examples 2 to 5, respectively. In the following Table 1, "water-based emulsion pressure-sensitive adhesive material" means a configuration except "nanoparticles" in "water-based emulsion pressure-sensitive adhesive composition" and "%" represents "weight%".

실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 수계형 에멀젼 점착소재(%)Water-based emulsion adhesive material (%) 9898 9696 9494 9292 몬모릴로나이트(%)Montmorillonite (%) 22 44 66 88

상기 실시예 1 내지 5에 따른 조성물 수계형 에멀젼 점착소재를 사용하여 다음과 같은 실험예를 통해 물성을 측정하고 그 결과를 다음 표 2, 3에 나타내었다.Physical properties of the composition-based emulsion pressure-sensitive adhesive material according to Examples 1 to 5 were measured through the following experimental examples, and the results are shown in Tables 2 and 3 below.

[실험예][Experimental Example]

1. 초기점착력(probe tack)1. Probe tack

초기점착력은 Texture Analyzer(Stable Micro Systems, TA-XT2i)를 이용하여 상온에서 측정하였다. 사용된 프로브(probe)는 polished stainless steel cylinder probe이며 프로브의 지름은 5 mm이다. 초기점착력은 프로브가 0.5 mm/sec의 속도로 점착제의 표면에 접근하여 1초 동안 100 gf/cm2의 힘으로 머무른 후, 10 mm/s의 속도로 떨어질 때의 힘을 측정하는 것으로 최대값을 사용하였다.Initial adhesion was measured at room temperature using a Texture Analyzer (Stable Micro Systems, TA-XT2i). The probe used was a polished stainless steel cylinder probe with a probe diameter of 5 mm. The initial adhesive force is measured by measuring the force when the probe approaches the surface of the adhesive at a rate of 0.5 mm / sec, stays at a force of 100 gf / cm 2 for 1 second, and then falls at a rate of 10 mm / s. Used.

2. 박리강도(180°2. Peel strength (180 °) peelpeel strengthstrength ))

박리강도 측정에 사용되는 점착필름은 2.5 cm의 너비로 제조하였다. 점착제 필름은 스테인리스 스틸(stainless steel) 표면에 붙여진 후, 2kg의 고무롤러로 두 번 왕복하여 접착하였다. 박리강도는 Texture Analyzer(Stable Micro Systems, TA-XT2i)를 이용하여 상온에서 300 mm/min의 속도록 측정하였다. 박리강도는 측정된 값의 평균값을 이용하였다.The pressure-sensitive adhesive film used to measure the peel strength was prepared in a width of 2.5 cm. The pressure-sensitive adhesive film was pasted on a stainless steel surface, and then bonded back and forth twice with a rubber roller of 2 kg. Peel strength was measured at a rate of 300 mm / min at room temperature using a Texture Analyzer (Stable Micro Systems, TA-XT2i). Peel strength was used as the average of the measured values.

3. 유지력(Shear adhesion failure temperature, SAFT)3. Shear adhesion failure temperature (SAFT)

유지력 측정에 사용되는 점착필름은 2.5 cm의 너비로 제조하여 스테인리스 스틸에 2.5 cm2의 넓이로 붙이고 2 kg의 고무롤러로 일회 왕복하여 접착하였다. 접착된 점착 필름의 한 쪽 끝에 l kg의 추를 매달아 25℃부터 200℃까지 0.4℃/min의 승온 속도로 온도가 증가하는 오븐에 넣어 파괴가 일어날 때의 온도를 측정하였다.A pressure-sensitive adhesive film used for measuring the holding force was manufactured in a width of 2.5 cm, attached to a stainless steel in a width of 2.5 cm 2 and bonded by reciprocating once with a rubber roller of 2 kg. One kg of the adhered adhesive film was suspended at one end of a weight and placed in an oven where the temperature increased from 25 ° C. to 200 ° C. at a temperature increase rate of 0.4 ° C./min.

4. TGA4. TGA

TGA(Thermo gravimetric analysis)는 열중량 분석으로 8~10mg의 샘플을 상온에서 고온(400℃)으로 일정속도로 온도를 증가시키며, 그에 따른 시료의 중량감소를 확인하는 것이다. 장비는 TA Instrument사의 TGA-Q5000을 사용하였다.Thermo gravimetric analysis (TGA) is a thermogravimetric analysis that increases the temperature of a sample of 8-10 mg from room temperature to high temperature (400 ° C.) at a constant rate and confirms the weight loss. The instrument used TA Instrument's TGA-Q5000.

아래 표 2는 수계형 에멀젼 점착소재에 몬모릴로나이트로 구성된 나노입자의 첨가량에 따른 초기점착력, 박리강도 및 유지력의 결과를 나타낸 것이다.Table 2 below shows the results of the initial adhesion strength, peel strength and retention strength according to the addition amount of the montmorillonite nanoparticles to the aqueous emulsion adhesive material.

실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 Probe Tack(gf)Probe Tack (gf) 220220 231231 226226 240240 220220 Peel Strength(gf)Peel Strength (gf) 435435 420420 449449 432432 451451 SAFT(℃)SAFT (℃) 121121 189189 200200 200200 200200

상기 표 2에서 확인할 수 있듯이, 본 발명에 따른 수계형 에멀젼 점착소재를 구성하는 몬모릴로나이트로 구성된 나노입자의 첨가량 범위 내에서는 몬모릴로나이트로 구성된 나노입자를 사용하더라도 수계형 에멀젼 점착소재의 초기점착력에는 큰 영향을 주지 않음을 알 수 있으며, 또한 본 발명을 구성하는 몬모릴로나이트로 구성된 나노입자의 첨가량 범위 내에서는 몬모릴로나이트로 구성된 나노입자를 사용하더라도 수계형 에멀젼 점착소재의 박리강도엔 큰 영향을 주지 않음을 알 수 있다. 그러나, 유지력의 경우에는 몬모릴로나이트로 구성된 나노입자의 첨가에 따라 유지력이 증가하는 것을 확인할 수 있으며, 첨가량이 낮더라도 첨가하지 않았을 때보다 월등한 물성향상을 확인할 수 있다.As can be seen in Table 2, within the range of the addition amount of the montmorillonite nanoparticles constituting the water-based emulsion pressure-sensitive adhesive material according to the invention even if the nanoparticles consisting of montmorillonite has a great effect on the initial adhesion of the water-based emulsion pressure-sensitive adhesive material In addition, it can be seen that even if the nanoparticles composed of montmorillonite are used within the range of addition of the montmorillonite-containing nanoparticles constituting the present invention, the peel strength of the water-based emulsion adhesive material is not significantly affected. However, in the case of holding power, it can be seen that the holding power increases with the addition of the nanoparticles composed of montmorillonite, and even if the addition amount is low, it can be confirmed that the physical properties are superior to those without addition.

다음으로 아래 표 3은 수계형 에멀젼 점착소재에 몬모릴로나이트로 구성된 나노입자의 첨가량에 따른 5% 열중량 감소 온도를 나타낸다.Next, Table 3 below shows the 5% thermogravimetric reduction temperature according to the amount of the nanoparticles composed of montmorillonite in the aqueous emulsion adhesive material.

실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 5%열중량 감소 온도(℃)5% thermogravimetric reduction temperature (℃) 161161 170170 178178 185185 188188

상기 표 3에서 확인할 수 있는 바와 같이, 몬모릴로나이트로 구성된 나노입자가 첨가된 점착소재 조성물의 열안정성이 첨가되지 않은 경우에 비해 10℃ 정도 올라간 것을 확인할 수 있다.As can be seen in Table 3, it can be confirmed that the nanoparticles composed of montmorillonite have risen by about 10 ° C. compared with the case where the thermal stability of the pressure-sensitive adhesive material composition is not added.

본 명세서에서는 본 발명자들이 수행한 다양한 실시예 가운데 몇 개의 예만을 들어 설명하는 것이나 본 발명의 기술적 사상은 이에 한정하거나 제한되지 않고, 당업자에 의해 변형되어 다양하게 실시될 수 있음은 물론이다. It is to be understood that the present invention is not limited to the above embodiments and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention.

1 : 기재필름 2 : 수계형 에멀젼 점착소재
3 : 나노입자 1: Base film 2: Water-based emulsion adhesive material
3: Nanoparticles

Claims (5)

수계형 에멀젼 점착소재 조성물에 있어서,
2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 메틸메타크릴레이트 및 아크릴산 모노머 중 적어도 하나의 모노머를 포함하는 모노머 혼합물, 탈이온수, 계면활성제인 소듐도데실설페이트와 폴리옥시에틸렌알킬에테르황산염, 나노입자, 탄산수소나트륨 및 암모늄 퍼설페이트를 포함하고,
상기 나노입자는 몬모릴로나이트계 나노입자로서 수계형 에멀젼 점착소재 조성물 총 중량 대비 6 내지 8중량%를 포함하는 것을 특징으로 하는, 수계형 에멀젼 점착소재 조성물. In the water-based emulsion adhesive material composition,
Monomer mixture comprising at least one monomer of 2-ethylhexyl acrylate, n-butyl acrylate, methyl methacrylate and acrylic acid monomer, deionized water, surfactant sodium dodecyl sulfate and polyoxyethylene alkyl ether sulfate, nano Particles, sodium bicarbonate and ammonium persulfate,
The nanoparticles are montmorillonite-based nanoparticles, characterized in that it comprises 6 to 8% by weight relative to the total weight of the aqueous emulsion adhesive material composition, the aqueous emulsion adhesive material composition. 삭제delete 삭제delete 제1항에 있어서,
상기 나노입자는 그 표면이 유기화제로 표면처리된 것을 특징으로 하는, 수계형 에멀젼 점착소재 조성물. The method of claim 1,
The nanoparticles are characterized in that the surface is surface-treated with an organic agent, water-based emulsion adhesive material composition. 점착필름으로서,
기재필름과,
상기 기재필름의 적어도 일 면에 제1항 또는 제4항에 따른 수계형 에멀젼 점착소재 조성물로 코팅된 수계형 에멀젼 점착소재를 포함하는 것을 특징으로 하는, 점착필름. As an adhesive film,
Base film,
The adhesive film, characterized in that it comprises at least one surface of the aqueous emulsion pressure-sensitive adhesive material coated with a water-based emulsion pressure-sensitive adhesive composition according to claim 1 on at least one side of the base film.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100823783B1 (en) * 2004-05-07 2008-04-21 아사히 가세이 케미칼즈 가부시키가이샤 Aqueous Resin Dispersion for Adhesive and Composition Thereof
KR100867391B1 (en) * 2000-09-21 2008-11-06 롬 앤드 하스 캄파니 Aqueous nanocomposite dispersions: processes, compositions, and uses thereof
KR20110119864A (en) * 2010-04-28 2011-11-03 서울대학교산학협력단 Method for preparing the aqueous acrylic adhesive using the clay

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100867391B1 (en) * 2000-09-21 2008-11-06 롬 앤드 하스 캄파니 Aqueous nanocomposite dispersions: processes, compositions, and uses thereof
KR100823783B1 (en) * 2004-05-07 2008-04-21 아사히 가세이 케미칼즈 가부시키가이샤 Aqueous Resin Dispersion for Adhesive and Composition Thereof
KR20110119864A (en) * 2010-04-28 2011-11-03 서울대학교산학협력단 Method for preparing the aqueous acrylic adhesive using the clay

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