KR101151921B1 - Soluble acrylic adhesive using physical adsorption and manufacturing method thereof - Google Patents
Soluble acrylic adhesive using physical adsorption and manufacturing method thereof Download PDFInfo
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- KR101151921B1 KR101151921B1 KR1020090110219A KR20090110219A KR101151921B1 KR 101151921 B1 KR101151921 B1 KR 101151921B1 KR 1020090110219 A KR1020090110219 A KR 1020090110219A KR 20090110219 A KR20090110219 A KR 20090110219A KR 101151921 B1 KR101151921 B1 KR 101151921B1
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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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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Abstract
본 발명은 물리적 흡착력을 이용한 수용성 아크릴계 점착제 및 그 제조방법에 관한 것이다.The present invention relates to a water-soluble acrylic pressure-sensitive adhesive using a physical adsorption force and a method for producing the same.
본 발명의 수용성 아크릴계 점착제는 아크릴 수지로서 유리전이온도 값이 높은 아크릴계 단량체를 이용하여 높은 열풍에도 물성의 변화를 일으키지 않으며, 이를 함유하는 에멀젼형의 점착제 조성물에 기포를 주입함으로써, 이를 점착제로 사용시 상기 주입된 기포에 의한 물리적인 흡착력에 의하여 점착제 성능을 구현할 수 있다. 이에, 종래의 점착제에 비하여 박리강도, 내수성, 열 노화성, 내한성, 내습성 등의 물성이 우수한 성능을 보인다.The water-soluble acrylic pressure-sensitive adhesive of the present invention does not cause a change in physical properties even with high hot air by using an acrylic monomer having a high glass transition temperature value as an acrylic resin, and by injecting bubbles into the pressure-sensitive adhesive composition containing the same, when used as an adhesive Pressure-sensitive adhesive performance can be realized by the physical adsorption force by the injected bubble. Thus, it exhibits superior performance in physical properties such as peel strength, water resistance, heat aging resistance, cold resistance, moisture resistance, and the like as compared with the conventional adhesives.
수용성, 흡착력, 아크릴계 점착제Water Soluble, Adsorption, Acrylic Adhesive
Description
본 발명은 물리적 흡착력을 이용한 수용성 아크릴계 점착제 및 그 제조방법에 관한 것으로서, 더욱 상세하게는 아크릴 수지로서 유리전이온도 값이 높은 아크릴계 단량체를 이용하여 높은 열풍에도 물성의 변화를 일으키지 않으며, 이를 함유하는 에멀젼형의 점착제 조성물에 기포를 주입함으로써, 물리적인 흡착력을 생성시킨 수용성 아크릴계 점착제 및 그 제조방법에 관한 것이다. The present invention relates to a water-soluble acrylic pressure-sensitive adhesive using a physical adsorption force and a method for manufacturing the same, and more particularly, to an acrylic resin containing an acrylic monomer having a high glass transition temperature value does not cause a change in physical properties even in high hot air, an emulsion containing the same. It relates to a water-soluble acrylic pressure-sensitive adhesive and a method for producing the same, by injecting bubbles into the pressure-sensitive adhesive composition.
종래에 사용되어 온 점착제들은 유리전이온도 값이 낮은 수지를 이용하여 면의 점착력을 이용한 유기용제형 점착제, 혹은 일반적인 수용성 아크릴계 에멀젼형 점착제로서 클로로프렌 고무나 천연고무, SBR(Styrene Butadiene Rubber)등 고무계통의 폴리머를 기재로 사용하고 이러한 재료를 용해하기 위한 용제로서 벤젠이나 톨루엔, 자일렌 초산에틸 등과 같은 휘발성 유기용제를 사용하였다. 그런데 이러한 유기용제들은 인체에 유해한 성분으로서 점착제 도포작없이 유해한 가스를 발생시켜 작업자에게 환각 작용을 일으키게 하는 등 환경을 오염시킬 뿐만 아니라, 불쾌한 냄새가 오랫동안 남아 있는 등의 문제점이 있었다. The conventionally used adhesives are organic solvent type adhesives using cotton adhesive force using resin having low glass transition temperature, or general water-soluble acrylic emulsion type adhesives such as chloroprene rubber, natural rubber, SBR (Styrene Butadiene Rubber), etc. The polymer of was used as a substrate and a volatile organic solvent such as benzene, toluene, ethyl xylene, and the like was used as a solvent for dissolving such materials. By the way, such organic solvents are harmful to the human body to generate harmful gases without the pressure-sensitive adhesive coating to cause a hallucination action to workers, such as polluting the environment, there was a problem such that an unpleasant smell remains for a long time.
최근 각종 환경 관련 규제가 점차 강화됨에 따라 유기 용제형 점착제 대신에 수용성 에멀젼형 점착제에 대한 개발이 시도되고 있다. 그러나 수용성 에멀젼 형 점착제 조성물은 유기용제를 사용하여 제조한 점착제에 비해 점착물성이 떨어지고 내수성이 약하며, 점착물성이 약하다. 특히, 내수성이 약한 기존의 아크릴 에멀젼 점착제 조성물은 사용중 주위의 수분이나 습기를 흡수하여 시간이 지날수록 점착물성이 저하하게 되어 반복 사용에 문제가 있다.Recently, as various environmental regulations are gradually strengthened, development of water-soluble emulsion-type adhesives has been attempted instead of organic solvent-type adhesives. However, the water-soluble emulsion type pressure-sensitive adhesive composition is inferior in adhesiveness, weak in water resistance, and weak in adhesiveness compared to the pressure-sensitive adhesive prepared using an organic solvent. In particular, the conventional acrylic emulsion pressure-sensitive adhesive composition having a weak water resistance absorbs moisture or moisture in the surroundings during use, and as a result, the adhesive property decreases with time, thereby causing problems in repeated use.
상기와 같은 문제점을 해결하기 위하여, 본 발명의 목적은 유리전이온도 값이 높은 아크릴계 단량체를 함유하고, 에멀젼형의 아크릴계 점착제 조성물에 기포가 주입된 수용성 아크릴계 점착제를 제공하는 것이다.
본 발명의 다른 목적은 상기 수용성 아크릴계 점착제의 제조방법을 제공하는 것이다. In order to solve the above problems, it is an object of the present invention to provide a water-soluble acrylic pressure-sensitive adhesive containing an acrylic monomer having a high glass transition temperature value, the bubble is injected into the emulsion-type acrylic pressure-sensitive adhesive composition.
Another object of the present invention is to provide a method for producing the water-soluble acrylic pressure-sensitive adhesive.
본 발명은 점착제 제조시 아크릴 수지로서 유리전이온도 값이 높은 단량체를 이용하여 높은 열풍에도 물성의 변화를 일으키지 않으며, 이를 함유하는 에멀젼형의 점착제 조성물에 기포를 주입함으로써 물리적인 흡착력을 생성시킨 점착제를 제조하여 반복사용성이 높은 점착제를 제조한다.
더욱 구체적으로, 본 발명은 유리전이온도 60 내지 120℃의 범위를 가지는 아크릴계 수지 60 내지 70중량%, 에톡시 알킬페놀 계면활성제 1 내지 5중량%, 수산화칼륨 중화제 0.5 내지 2.5중량%, 에틸렌글리콜 디글리시딜 에테르 가교제 1 내지 3중량%, t-부틸퍼옥시-2-에틸헥사노에이트 개시제 0.05 내지 0.2중량% 및 전체 중량비율에서 상기 성분 함량을 제외한 용매 잔량으로 이루어진 에멀젼형의 아크릴계 점착제 조성물에 기포가 주입되어 형성된 수용성 아크릴계 점착제를 제공한다.
본 발명의 아크릴계 점착제 조성물에서, 아크릴계 수지는 스티렌, 메틸메타크릴레이트, i-부틸 메타크릴레이트 및 t-부틸 메타크릴레이트로 이루어진 군에서 선택되는 아크릴계 단량체 단독 또는 이들의 혼합형태로 이루어진 공중합체를 사용한다. 더욱 바람직하게는, 상기 아크릴계 수지가 메틸메타크릴레이트 30 내지 70 중량% 및 i-부틸 메타크릴레이트 30 내지 70중량%로 이루어진 공중합체인 것이다.
또한, 본 발명은 상기 에멀젼형의 아크릴 점착제 조성물을 회분식 반응기 내에서 100 내지 1000rpm 속도로 교반하면서 공기를 주입하여 아크릴 점착제 조성물 내 기포를 형성하고, 상기 기포가 형성된 아크릴 점착제 조성물을 기재 표면에 도포하고, 열풍 건조 후 상온에서 냉각하여 점착제층을 형성하는 것으로 이루어진 수용성 아크릴계 점착제의 제조방법을 제공한다.
상기에서 기포가 형성된 아크릴 점착제 조성물은 500 내지 1000㎛ 두께로 도포되며, 상기 열풍 건조는 70～140℃의 열풍을 10～20m/min의 속도로 1 내지 10분 동안 분사하여 건조하는 것이다. The present invention does not cause a change in physical properties even in high hot air by using a monomer having a high glass transition temperature as an acrylic resin when preparing the pressure-sensitive adhesive, the pressure-sensitive adhesive that generates physical adsorption by injecting bubbles into the pressure-sensitive adhesive composition containing the same To prepare a high pressure repeatability adhesive.
More specifically, the present invention is 60 to 70% by weight acrylic resin having a glass transition temperature range of 60 to 120 ℃, 1 to 5% by weight ethoxy alkylphenol surfactant, 0.5 to 2.5% by weight potassium hydroxide neutralizer, ethylene glycol di Emulsion type acrylic pressure-sensitive adhesive composition consisting of 1 to 3% by weight of glycidyl ether crosslinking agent, 0.05 to 0.2% by weight of t -butylperoxy-2-ethylhexanoate initiator and the remaining amount of solvent excluding the above component content in the total weight ratio. It provides a water-soluble acrylic pressure-sensitive adhesive formed by injecting bubbles.
In the acrylic pressure-sensitive adhesive composition of the present invention, the acrylic resin is a copolymer composed of an acrylic monomer alone or a mixture thereof selected from the group consisting of styrene, methyl methacrylate, i -butyl methacrylate and t- butyl methacrylate. use. More preferably, the acrylic resin is a copolymer consisting of 30 to 70% by weight of methyl methacrylate and 30 to 70% by weight of i -butyl methacrylate.
In addition, the present invention injects air while stirring the emulsion-type acrylic pressure-sensitive adhesive composition in a batch reactor at a speed of 100 to 1000rpm to form bubbles in the acrylic pressure-sensitive adhesive composition, and apply the bubble-formed acrylic pressure-sensitive adhesive composition to the substrate surface It provides a method for producing a water-soluble acrylic pressure-sensitive adhesive consisting of forming a pressure-sensitive adhesive layer by cooling at room temperature after hot air drying.
Bubble-formed acrylic pressure-sensitive adhesive composition is applied to a thickness of 500 to 1000㎛, the hot air drying is to dry by spraying hot air of 70 ~ 140 ℃ at a rate of 10 to 20m / min for 1 to 10 minutes.
상기한 바와 같이, 본 발명의 수용성 아크릴계 조성물은 유리전이온도 값이 높은 아크릴계 단량체를 함유하므로, 높은 열풍에도 물성의 변화를 일으키지 않으며, 에멀젼형의 수용성 아크릴계 조성물에 기포를 주입함으로써, 이를 점착제로 사용시 점착제면의 점착력이 아닌 상기 주입된 기포에 의한 물리적인 흡착력에 의하여 점착제 성능을 구현할 수 있다. 이에, 종래의 점착제에 비하여 박리강도, 내수성, 열 노화성, 내한성, 내습성 등의 물성이 우수한 성능을 보인다.
또한, 본 발명의 수용성 아크릴계 점착제는 물리적인 흡착력을 생성시킨 점착제로서, 반복사용율이 높다. As described above, since the water-soluble acrylic composition of the present invention contains an acrylic monomer having a high glass transition temperature value, it does not cause a change in physical properties even in high hot air, and when used as an adhesive by injecting bubbles into an emulsion-type water-soluble acrylic composition. Pressure-sensitive adhesive performance can be realized by the physical adsorption force by the injected bubbles rather than the adhesive force of the pressure-sensitive adhesive surface. Thus, it exhibits excellent performance in physical properties such as peel strength, water resistance, heat aging resistance, cold resistance, and moisture resistance, as compared with the conventional adhesives.
In addition, the water-soluble acrylic pressure-sensitive adhesive of the present invention is a pressure-sensitive adhesive that generates a physical adsorption force, high repeat use rate.
본 발명은 유리전이온도 60 내지 120℃의 범위를 가지는 아크릴계 수지 60 내지 70중량%, 에톡시 알킬페놀 계면활성제 1 내지 5중량%, 수산화칼륨 중화제 0.5 내지 2.5중량%, 에틸렌글리콜 디글리시딜 에테르 가교제 1 내지 3중량%, t-부틸퍼옥시-2-에틸헥사노에이트 개시제 0.05 내지 0.2중량% 및 상기 전체 중량비율에서 상기 성분 함량을 제외한 용매 잔량으로 이루어진 에멀젼에 기포층이 형성된 수용성 아크릴계 점착제를 제공한다. The present invention is 60 to 70% by weight acrylic resin having a glass transition temperature range of 60 to 120 ℃, 1 to 5% by weight ethoxy alkylphenol surfactant, 0.5 to 2.5% by weight potassium hydroxide neutralizer, ethylene glycol diglycidyl ether A water-soluble acrylic pressure-sensitive adhesive having a bubble layer formed in an emulsion composed of 1 to 3% by weight of a crosslinking agent, 0.05 to 0.2% by weight of t -butylperoxy-2-ethylhexanoate initiator, and the remaining amount of solvent except the component content in the total weight ratio. to provide.
본 발명의 아크릴계 수지는 본 발명에 따른 수용성 아크릴계 점착제의 주성분으로서, 유리전이온도 60 내지 120℃의 범위를 가지는 아크릴계 단량체에서 선택되는 단독 또는 이들의 혼합형태로 이루어진 공중합체로 구성될 수 있다. 상기 아크릴계 단량체로는 유리전이온도 값이 높은 스티렌(Styrene, St), 메틸메타크릴레이트(methyl methacrylate, MMA), i-부틸 메타크릴레이트, t-부틸 메타크릴레이트 등이 있고, 바람직하게는 메틸메타크릴레이트 30 내지 70 중량% 및 i-부틸 메타크릴레이트 30 내지 70중량%로 이루어진 공중합체가 사용되는 것이다.Acrylic resin of the present invention as a main component of the water-soluble acrylic pressure-sensitive adhesive according to the present invention, may be composed of a copolymer consisting of a single or a mixture thereof selected from the acrylic monomer having a glass transition temperature of 60 to 120 ℃ range. Examples of the acryl-based monomers include styrene (Styrene, St), methyl methacrylate (MMA), i -butyl methacrylate and t- butyl methacrylate having a high glass transition temperature, and preferably methyl. Copolymers consisting of 30 to 70% by weight of methacrylate and 30 to 70% by weight of i -butyl methacrylate are used.
삭제delete
본 발명에 따른 수용성 아크릴계 점착제에 있어서, 계면활성제는 유화중합에 있어서 필요 불가결한 성분이지만 성능측면에서 보면, 내수성, 내열성 등을 저하시키는 요인이 된다. 그 이유는 폴리머 입자 계면에 존재하는 계면활성제가 피막 생성시, 융착 계면에 편재하기 때문이다.In the water-soluble acrylic pressure-sensitive adhesive according to the present invention, the surfactant is an indispensable component in the emulsion polymerization, but in view of performance, it is a factor that lowers water resistance, heat resistance and the like. This is because the surfactant present at the polymer particle interface is localized at the fusion interface when the film is formed.
본 발명에서는 이러한 문제점을 해결하기 위하여, 비이온성 계면활성제인 에톡시 알킬페놀(Ethoxylated alkyl phenol)을 사용한다. 비이온성 계면활성제는 1 분자 중에 라디칼 중합이 가능한 이중결합이 있고, 모노머와 공중합하기 때문에, 폴리머 입자에 유리되어 있지 않으며, 피막 생성 후, 점착제 층에 편재되지 않기 때문에 점착제 수지 조성물의 내수성 및 내한성을 향상시켜 준다.
이때, 본 발명은 에톡시 알킬페놀 계면활성제 1 내지 5중량%를 함유하여, 흡착력을 이용한 유리전이온도 값이 높은 수용성 아크릴계 점착제를 제공한다.In the present invention, in order to solve this problem, ethoxylated alkyl phenol, which is a nonionic surfactant, is used. Since the nonionic surfactant has a double bond capable of radical polymerization in one molecule and copolymerizes with the monomer, the nonionic surfactant is not liberated in the polymer particles and is not localized in the pressure-sensitive adhesive layer after film formation, so that the water resistance and cold resistance of the pressure-sensitive adhesive resin composition Improves.
At this time, the present invention contains 1 to 5% by weight of an ethoxy alkylphenol surfactant, to provide a water-soluble acrylic pressure-sensitive adhesive having a high glass transition temperature value using the adsorption force.
본 발명의 수용성 아크릴계 점착제는 상기 아크릴계 기초수지의 유동성을 유지하면서 응집력을 향상시킬 수 있도록 가교도를 조절하기 위하여 가교제 에틸렌글리콜 디글리시딜 에테르 1 내지 3중량%를 포함한다. 이때, 상기 에틸렌글리콜 디글리시딜 에테르 가교제 사용량이 1중량% 미만이면, 충분한 가교가 이루어지지 않아 기포층이 형성 유지되기 힘들고, 3중량%를 초과하면, 지나친 가교가 이루어져 다른 첨가제와 혼화성이 저하된다. 일반적으로 아크릴 에멀젼형 점착제는 중합이 에멀젼 입자 내에서 이루어지며, 가교 시스템으로는 2개 이상의 중합성 이중결합을 가지는 모노머를 공중합하는 방법, 또는 상호 반응성이 있는 관능기 함유 모노머를 공중합 하는 방법 등이 이용될 수 있으나, 본 발명에서는 기재밀착성 및 내열성 등을 극대화하기 위하여 가교제를 사용하여 아크릴 입자 내 또는 입자간 가교를 형성시키는 2차 가교 시스템을 이용한다.The water-soluble acrylic pressure-sensitive adhesive of the present invention contains 1 to 3% by weight of the crosslinking agent ethylene glycol diglycidyl ether in order to adjust the degree of crosslinking so as to improve the cohesive force while maintaining the fluidity of the acrylic base resin. In this case, when the amount of the ethylene glycol diglycidyl ether crosslinking agent is less than 1% by weight, sufficient crosslinking is not achieved, and thus, the bubble layer is hardly formed and maintained. When the amount of the ethylene glycol diglycidyl ether crosslinking agent is less than 1% by weight, excessive crosslinking occurs due to miscibility with other additives. Degrades. In general, the acrylic emulsion pressure sensitive adhesive is polymerized in the emulsion particles, and as a crosslinking system, a method of copolymerizing monomers having two or more polymerizable double bonds or a method of copolymerizing mutually reactive functional group-containing monomers is used. However, in the present invention, a secondary crosslinking system using crosslinking agents to form crosslinks in the acrylic particles or interparticles is used to maximize substrate adhesion and heat resistance.
본 발명의 가교제인 에틸렌글리콜 디글리시딜 에테르의 관능기인 글리시딜기는 중합 반응 이후, -CO-O-CH2-COH- 결합으로 바뀌면서 2차 가교 시스템을 형성한다.The glycidyl group, which is a functional group of ethylene glycol diglycidyl ether, a crosslinking agent of the present invention, is converted to -CO-O-CH 2 -COH- bond after the polymerization reaction to form a secondary crosslinking system.
본 발명은 전술한 수용성 아크릴계 점착제의 제조방법을 제공하며, 구체적으로 설명하면 다음과 같다.The present invention provides a method for producing the above-mentioned water-soluble acrylic pressure-sensitive adhesive, specifically described as follows.
먼저, 회분 반응기 안에, 초기 회분 반응기 내에 투입되는 혼합물의 전체 중량 대비 50 내지 80중량%의 용매, 15 내지 30중량%의 혼합물 단량체, 0.3 내지 1중량%의 수산화칼륨 중화제, 0.05 내지 0.2중량%의 수용성 개시제를 넣어 혼합한 후, 질소 분위기에서 반응기 온도가 약 90℃가 될 때까지 교반하면서 혼합한다.First, in a batch reactor, 50 to 80% by weight solvent, 15 to 30% by weight mixture monomer, 0.3 to 1% by weight potassium hydroxide neutralizer, 0.05 to 0.2% by weight relative to the total weight of the mixture The water-soluble initiator is added and mixed, followed by stirring with stirring until the reactor temperature is about 90 ° C in a nitrogen atmosphere.
그 다음, 전체 프리에멀젼 중량 당 25중량%의 용매, 1 내지 5중량%의 계면활성제, 0.5 내지 2.5중량%의 수산화칼륨 중화제, 1 내지 3중량%의 가교제, 0.05 내지 0.2중량%의 수용성 개시제를 완전히 혼합한 후, 상기 혼합물에 60 내지 70중량%의 혼합물 단량체를 혼합하여 프리에멀젼을 제조한다.Then, 25 wt% solvent, 1-5 wt% surfactant, 0.5-2.5 wt% potassium hydroxide neutralizer, 1-3 wt% crosslinking agent, 0.05-0.2 wt% water-soluble initiator per weight of the total preemulsion After complete mixing, 60 to 70% by weight of the mixture monomer is mixed with the mixture to prepare a preemulsion.
이후, 상기 프리에멀젼을 일정한 속도로 약 3시간 동안 반응기에 투입하여 반응시켜 아크릴계 점착제 조성물을 수득한다. Thereafter, the pre-emulsion was added to the reactor at a constant rate for about 3 hours to react to obtain an acrylic pressure-sensitive adhesive composition.
그 다음, 수득한 아크릴계 점착제 조성물을 회분식 반응기 내에 미량펌프[FMI LAB PUMP, Fluid Metering Inc., 미국]를 이용하여, 100 내지 1000rpm의 일정한 속도로 교반되도록 하여 반응기내에 일정한 공기를 주입하는 것으로, 구체적으로는 500rpm의 속도로 교반되는 반응기 내에 0.1㎖/s의 일정한 공기를 주입하며 20분간 교반시켜 아크릴계 점착제 조성물 내 기포를 형성한다.Then, using the obtained acrylic pressure-sensitive adhesive composition in a batch reactor by using a small pump [FMI LAB PUMP, Fluid Metering Inc., USA], to be stirred at a constant speed of 100 to 1000rpm to inject a constant air into the reactor, For example, 0.1 ml / s of constant air is injected into the reactor, which is stirred at a speed of 500 rpm, and stirred for 20 minutes to form bubbles in the acrylic pressure-sensitive adhesive composition.
그 다음, 상기 기포가 형성된 아크릴 에멀젼 점착제 조성물을 기재 표면에 500 내지 1000㎛ 두께로, 더욱 바람직하게는 약 700㎛ 두께로 도포하여 평탄작업을 실시하고, 이어서 70～140℃의 열풍을 10～20m/min의 속도로 1 내지 10분 동안 분사하여 건조시킨 후, 상온에서 냉각한다. 더욱 바람직하게는 70～140℃의 열풍을 20m/min의 속도로 5분간 분사한다. Next, the bubble-formed acrylic emulsion pressure-sensitive adhesive composition is applied to the surface of the substrate with a thickness of 500 to 1000 μm, more preferably about 700 μm, to perform flat work, and then hot air at 70 to 140 ° C. for 10 to 20 m. After drying by spraying for 1 to 10 minutes at a rate of / min, it is cooled at room temperature. More preferably, hot air of 70 to 140 ° C. is sprayed for 5 minutes at a speed of 20 m / min.
상기 건조된 점착제층에는 약 1㎛의 균일한 기포층이 형성된다. 이에, 본 발명의 제조방법으로부터 제조된 수용성 아크릴계 점착제를 사용시 점착제면의 점착력이 아닌 주입된 기포에 의한 물리적인 흡착력에 의하여 점착제 성능을 구현할 수 있다. The dried pressure-sensitive adhesive layer is formed with a uniform bubble layer of about 1㎛. Thus, when using the water-soluble acrylic pressure-sensitive adhesive prepared from the manufacturing method of the present invention, it is possible to implement the pressure-sensitive adhesive performance by the physical adsorption force by the injected bubbles rather than the adhesive force of the pressure-sensitive adhesive surface.
이하에서 실시예에 의거하여 본 발명을 더욱 구체적으로 설명하겠는바, 본 발명이 다음 실시예에 의하여 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples.
실시예Example
다음 표1의 구성 성분 및 함량으로 이루어지는 점착제 조성물을 제조한다.Next, the pressure-sensitive adhesive composition consisting of the components and contents of Table 1 is prepared.
비교예Comparative example
다음 표2의 구성 성분 및 함량으로 이루어지는 점착제 조성물을 제조한다.Next, the pressure-sensitive adhesive composition consisting of the components and contents of Table 2 is prepared.
상기 실시예 및 비교예에서 제조한 점착제 조성물을 다음표에 나타낸 조건으로 물성을 측정하였고, 그 결과를 다음 표 3에 나타내었다.Physical properties of the pressure-sensitive adhesive compositions prepared in Examples and Comparative Examples were measured under the conditions shown in the following table, and the results are shown in Table 3 below.
에멀젼 점착제의 유리 전이 온도값을 측정 하였고, 그 결과를 다음 표 4에 나타내었다.The glass transition temperature of the emulsion pressure-sensitive adhesive was measured, and the results are shown in Table 4 below.
상기한 바와 같이, 본 발명의 수용성 아크릴계 점착제를 이용하면, 종래의 점착제에 비하여 박리강도, 내수성, 열 노화성, 내한성, 내습성 등의 물성이 우수하며, 특히 내수성이 뛰어나 반복사용성이 우수한 점착제 활용이 가능하다.As described above, when the water-soluble acrylic pressure-sensitive adhesive of the present invention is used, it is excellent in physical properties such as peel strength, water resistance, heat aging resistance, cold resistance, moisture resistance, etc., in comparison with the conventional pressure-sensitive adhesive, and in particular, the pressure-sensitive adhesive has excellent water resistance and excellent repeatability. This is possible.
Claims (9)
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| JP2003003037A (en) | 2001-06-25 | 2003-01-08 | Mitsubishi Chemicals Corp | Aqueous resin emulsion, production method thereof, and coating agent |
| KR100804547B1 (en) | 2006-10-26 | 2008-02-20 | 엘지엠엠에이 주식회사 | Composition of pmma with glossy, anti-static, abrasion resistant, impact resistant |
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| JP2003003037A (en) | 2001-06-25 | 2003-01-08 | Mitsubishi Chemicals Corp | Aqueous resin emulsion, production method thereof, and coating agent |
| KR100804547B1 (en) | 2006-10-26 | 2008-02-20 | 엘지엠엠에이 주식회사 | Composition of pmma with glossy, anti-static, abrasion resistant, impact resistant |
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