KR101296803B1 - Manufacturing method of pressure sensitive adhesive with electrical conductivity and the material - Google Patents
Manufacturing method of pressure sensitive adhesive with electrical conductivity and the material Download PDFInfo
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- KR101296803B1 KR101296803B1 KR1020110096823A KR20110096823A KR101296803B1 KR 101296803 B1 KR101296803 B1 KR 101296803B1 KR 1020110096823 A KR1020110096823 A KR 1020110096823A KR 20110096823 A KR20110096823 A KR 20110096823A KR 101296803 B1 KR101296803 B1 KR 101296803B1
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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
- 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
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- 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
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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
- C09J9/02—Electrically-conducting adhesives
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Abstract
본 발명은, 도전성 아크릴 점착제 및 그 제조 방법에 관한 것으로, 보헤마이트 졸을 합성하는 제1단계와; 상기 제1단계에서 합성된 보헤마이트 졸을 유기실란을 사용하여 표면 개질하는 제2단계와; 탄소나노튜브를 산을 통하여 전처리하는 제3단계와; 상기 3단계에서 산처리 된 탄소나노튜브를 아크릴 단량체를 통하여 표면 개질하는 제 4단계와; 표면 개질된 탄소나노튜브와 표면개질된 보헤마이트 졸 및 아크릴 단량체와 유화제를 사용하여 무기물과 아크릴이 혼합된 유화물을 제조하는 제5단계; 그리고, 상기 제5단계의 유화물과 반응개시제를 혼합하여 수계 유화중합 아크릴 점착제를 제조하는 제6단계;를 포함하여 구성되는 도전성 아크릴 점착제 및 그 제조 방법을 기술적 요지로 한다.
이에 따라, 수분산 된 보헤마이트 졸 및 탄소나노튜브를 표면 개질 후 전유탁액으로 제조하여 아크릴 점착제를 합성함으로서, 분산성이 양호하고 아크릴 점착제에 전기전도성 등이 부여되는 이점이 있다. The present invention relates to a conductive acrylic pressure-sensitive adhesive and a manufacturing method thereof, comprising: a first step of synthesizing a boehmite sol; A second step of surface modifying the boehmite sol synthesized in the first step using an organosilane; A third step of pretreating the carbon nanotubes through an acid; A fourth step of surface-modifying the carbon nanotubes acid-treated in the third step through an acrylic monomer; A fifth step of preparing an emulsion of inorganic and acryl using surface-modified carbon nanotubes, surface-modified boehmite sol, and acrylic monomer and emulsifier; In addition, the sixth step of preparing the aqueous emulsion polymerization acrylic pressure-sensitive adhesive by mixing the emulsion of the fifth step and the reaction initiator; and a conductive acrylic pressure-sensitive adhesive comprising a method and a manufacturing method thereof.
Accordingly, by dispersing the boehmite sol and the carbon nanotubes with water after the surface modification to synthesize the acrylic adhesive, there is an advantage that the dispersibility is good and the electrical conductivity is imparted to the acrylic adhesive.
Description
본 발명은 수계 유화중합 아크릴 점착제에 탄소나노튜브와 보헤마이트를 함유하여 전기전도성을 향상시킨 하이브리드 점착제를 제조하되, 탄소나노튜브와 보헤마이트를 표면 처리하여 아크릴 점착제와의 상용성을 높이고 기능성을 부여한 도전성 아크릴 점착제 및 그 제조 방법에 관한 것이다. The present invention is to prepare a hybrid pressure-sensitive adhesive to improve the electrical conductivity by containing carbon nanotubes and boehmite in the water-based emulsion polymer adhesive, surface treatment of carbon nanotubes and boehmite to increase the compatibility with the acrylic pressure-sensitive adhesive and give functionality A conductive acrylic adhesive and its manufacturing method are related.
일반적으로, 전자 부품 혹은 전자 기기들은 수송, 보관, 조립 중 표면의 손상을 최소화하기 위하여 보호 필름을 부착하여 관리한다. 이 보호 필름은 정전기 발생에 의한 기기의 손상이 없도록 도전성을 부여하여야 하며, 이를 위해서는 점착제에 도전성을 부여할 필요가 있다.In general, electronic components or electronic devices are managed by attaching a protective film to minimize surface damage during transportation, storage and assembly. The protective film should be provided with conductivity so as not to damage the device due to the generation of static electricity. To this end, it is necessary to give conductivity to the pressure-sensitive adhesive.
점착제에 도전성을 부여하기 위하여 첨가하는 물질로는 카본블랙과 같은 전도성 고분자 등이 있다. 그러나 전도성 고분자는 점착제와의 혼화성이 좋지 못하여 효과적으로 전도성을 향상시키기가 쉽지 않은 문제가 있다. 이밖에 금속 섬유, 금속 박편, 카본블랙, 흑연 등과 같은 도전성 충진제를 첨가할 수도 있으나 이들 대부분 다량 첨가 시 점착력 약화나 점착제와의 혼화성 문제가 발생할 수 있을 뿐만 아니라 도전성 충진제의 첨가에 의해 불투명하여지고 계면결합으로 인하여 기계적 강도가 저하되는 등의 문제점이 있다. Examples of the material added to impart conductivity to the pressure-sensitive adhesive include conductive polymers such as carbon black. However, the conductive polymer has a problem in that it is not easy to effectively improve conductivity because of poor compatibility with the pressure-sensitive adhesive. In addition, conductive fillers such as metal fibers, metal flakes, carbon black, graphite, and the like may be added, but most of them may cause a weakening of adhesion and miscibility with the adhesive, and become opaque due to the addition of the conductive filler. There is a problem that the mechanical strength is lowered due to interfacial bonding.
상기한 종래기술의 문제점을 해결하기 위해 대한민국 특허청 등록특허공보 등록번호 제10-964561호에 도전성 점착제 조성물이 소개되어 있다. In order to solve the above problems of the prior art, a conductive adhesive composition is introduced in Korean Patent Registration No. 10-964561.
상기 종래기술은 아크릴계 점착제 100중량부; 그라펜 분말 0.1 내지 15중량부; 및 가교제 0.1 내지 10 중량부를 포함하는 도전성 점착제 조성물로서, 상기 아크릴계 점착제는 아크릴계 단량체를 주성분으로 용매 속에서 라디칼 중합하여 제조한다. 아크릴계 단량체는 유리전이온도가 상온 이하로 점착성을 부여하는 2-에틸헥실 아크릴레이트 (2-ethylhexyl acrlate), 부틸아크릴레이트 (butyl acrylate) 등과 같은 지방족 알코올과 아크릴산 혹은 메타크릴산의 축합물을 주성분으로 하며, 접착력에 상승효과를 부여하고 내열성 증대를 위한 가교점을 제공하는 카르복실산기를 갖는 비닐화합물, 예를 들면 아크릴산, 메타크릴산, 이타콘산 (itaconic acid) 등을 함께 공중합 한다. 그리고 상기 가교제는 분자 내에 2개 이상의 에폭시기, 이소시아네이트기, 아민기 또는 아지리딘기을 가진 화합물을 사용하여 점착제 조성물을 형성시킨다. The prior art 100 parts by weight of the acrylic pressure-sensitive adhesive; 0.1 to 15 parts by weight of graphene powder; And 0.1 to 10 parts by weight of a crosslinking agent, wherein the acrylic pressure sensitive adhesive is prepared by radical polymerization in a solvent based on an acrylic monomer. Acrylic monomers are mainly composed of condensates of aliphatic alcohols such as 2-ethylhexyl acrylate, butyl acrylate, and acrylic acid or methacrylic acid, which have a glass transition temperature of less than room temperature. And a vinyl compound having a carboxylic acid group, for example, acrylic acid, methacrylic acid, itaconic acid, etc., which together give a synergistic effect to adhesion and provide a crosslinking point for increasing heat resistance. And the crosslinking agent forms a pressure-sensitive adhesive composition using a compound having two or more epoxy groups, isocyanate groups, amine groups or aziridine groups in the molecule.
그러나 상기 종래기술은 점착제가 일부 도전성을 가지나 도전성 물질의 분산안정성은 양호하지 못한다는 문제점이 있다. However, the prior art has a problem that the pressure-sensitive adhesive has some conductivity, but the dispersion stability of the conductive material is not good.
따라서 본 발명은 상기한 종래기술들의 문제점을 해결하기 위해 창작된 것으로, 수분산 된 보헤마이트 졸 및 탄소나노튜브를 표면 개질 후 전유탁액으로 제조 하여 아크릴 점착제를 합성함으로서, 분산성이 양호하고, 아크릴 점착제에 전기전도성을 부여하는 도전성 아크릴 점착제 및 그 제조 방법을 제공하는 것을 목적으로 한다.Therefore, the present invention was created to solve the problems of the above-described prior art, by dispersing the boehmite sol and carbon nanotubes dispersed in the surface of the emulsion prepared by synthesizing the acrylic adhesive, good dispersibility, It is an object to provide a conductive acrylic pressure-sensitive adhesive that provides electrical conductivity to an acrylic pressure-sensitive adhesive and a method for producing the same.
상기한 목적을 달성하기 위한 본 발명은, 보헤마이트 졸을 합성하는 제1단계와; 상기 제1단계에서 합성된 보헤마이트 졸을 유기실란을 사용하여 표면 개질하는 제2단계와; 탄소나노튜브를 산을 통하여 전처리하는 제3단계와; 상기 3단계에서 산처리 된 탄소나노튜브를 아크릴 단량체를 통하여 표면 개질하는 제 4단계와; 표면 개질된 탄소나노튜브와 표면개질된 보헤마이트 졸 및 아크릴 단량체와 유화제를 사용하여 무기물과 아크릴이 혼합된 유화물을 제조하는 제5단계; 그리고, 상기 제5단계의 유화물과 반응개시제를 혼합하여 수계 유화중합 아크릴 점착제를 제조하는 제6단계;를 포함하여 구성되는 도전성 아크릴 점착제 및 그 제조 방법을 기술적 요지로 한다. The present invention for achieving the above object, the first step of synthesizing the boehmite sol; A second step of surface modifying the boehmite sol synthesized in the first step using an organosilane; A third step of pretreating the carbon nanotubes through an acid; A fourth step of surface-modifying the carbon nanotubes acid-treated in the third step through an acrylic monomer; A fifth step of preparing an emulsion of inorganic and acryl using surface-modified carbon nanotubes, surface-modified boehmite sol, and acrylic monomer and emulsifier; In addition, the sixth step of preparing the aqueous emulsion polymerization acrylic pressure-sensitive adhesive by mixing the emulsion of the fifth step and the reaction initiator; and a conductive acrylic pressure-sensitive adhesive comprising a method and a manufacturing method thereof.
상기 제1단계는, 탈이온수 100중량부에 보헤마이트 전구체인 알루미늄이소프로폭사이드를 10~30중량부 첨가하여 형성되는 것이 바람직하다. The first step is preferably formed by adding 10 to 30 parts by weight of aluminum isopropoxide, which is a boehmite precursor, to 100 parts by weight of deionized water.
상기 제2단계는, 상기 1단계에서 형성된 보헤마이트 졸 100중량부에 유기실란 2~20중량부가 첨가되고 교반되어 형성되는 것이 바람직하다. The second step, 2 to 20 parts by weight of the organosilane is preferably added to 100 parts by weight of the boehmite sol formed in the first step is formed by stirring.
상기 제4단계는, 제3단계에서 산처리된 탄소나노튜브 100중량부에 아크릴 단량체 10~40 중량부와 반응개시제를 섞어 용매에 분산하여 형성되는 것이 바람직하다The fourth step is preferably formed by mixing 10-40 parts by weight of the acrylic monomer with 100 parts by weight of the acid-treated carbon nanotubes and a reaction initiator and dispersing it in a solvent.
상기 제6단계는, 상기 제5단계의 유화물과 반응개시제를 탈이온수에 혼합시켜 형성되는 것이 바람직하다. The sixth step is preferably formed by mixing the emulsion of the fifth step and the reaction initiator in deionized water.
상기 유기실란은 메틸트리메톡시실란, 메타크릴릭트리메톡시실란, 비닐트리메톡시실란, 글리시독시프로필트리메톡시실란 중에 어느 하나가 되는 것이 바람직하다. It is preferable that the said organosilane becomes any of methyl trimethoxysilane, methacrylic trimethoxysilane, vinyl trimethoxysilane, and glycidoxy propyl trimethoxysilane.
상기 아크릴 단량체는, 2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 라우릴아크릴레이트, 라우릴메타크릴레이트, 메틸아크릴레이트, 이소옥틸아크릴레이트, 이소데실아크릴레이트, 아크릴산, 메타크릴릭산, 에틸메타크릴레이트, n-부틸메타크릴레이트,이소부틸메타크릴레이트,t-부틸메타크릴레이트,아크릴로니트릴,에틸아크릴레이트,이소부틸아크릴레이트,2-에틸헥실메타크릴레이트,에틸렌,옥타데실메타크릴레이트,2-하이드록시에틸메타크릴레이트,2-하이드록시프로필메타크릴레이트,디메틸아미노에틸메타크릴레이트,t-부틸아미노에틸메타크릴레이트,디에틸아미노에틸메타크릴레이트,글리시딜메타크릴레이트,2-하이드록시에틸아크릴레이트,2-하이드록시프로필아크릴레이트,아크릴아마이드 및 N-메틸올아크릴아마이드 중에 어느 하나 또는 이들을 둘 이상 혼합한 혼합물을 사용하는 것이 바람직하다.The acryl monomer is 2-ethylhexyl acrylate, n-butyl acrylate, lauryl acrylate, lauryl methacrylate, methyl acrylate, isooctyl acrylate, isodecyl acrylate, acrylic acid, methacrylic acid, ethyl Methacrylate, n-butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, acrylonitrile, ethyl acrylate, isobutyl acrylate, 2-ethylhexyl methacrylate, ethylene, octadecyl methacrylate Acrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, dimethylaminoethyl methacrylate, t-butylaminoethyl methacrylate, diethylaminoethyl methacrylate, glycidyl methacrylate Any one of acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, acrylamide and N-methylol acrylamide Preference is given to using mixtures of two or more of them.
상기 반응개시제는, 하이드로젠퍼록사이드, 포타슘퍼설페이트, 아조비스이소부틸로니트릴, 벤조일퍼록사이드, 아세틸퍼록사이드, 디아우릴퍼록사이드, 디 tert-부틸퍼록사이드 및 큐밀하이드로퍼록사이드 중에 어느 하나가 되는 것이 바람직하다. The reaction initiator is any one of hydrogen peroxide, potassium persulfate, azobisisobutylonitrile, benzoyl peroxide, acetyl peroxide, diauryl peroxide, di tert-butyl peroxide and cumyl hydroperoxide. It is preferable to be.
상기 용매는, 에틸아세테이트, 부틸아세테이트, 메틸에틸케톤, 사이클로헥산, 디클로로에탄, 디클로로벤젠, 헵탄, 톨루엔, n-부탄올, 자일렌, 디메틸포름아마이드, N-메틸피롤리돈 중에 어느 하나가 되는 것이 바람직하다. The solvent may be any one of ethyl acetate, butyl acetate, methyl ethyl ketone, cyclohexane, dichloroethane, dichlorobenzene, heptane, toluene, n-butanol, xylene, dimethylformamide, and N-methylpyrrolidone. desirable.
이에 따라, 수분산 된 보헤마이트 졸 및 탄소나노튜브를 표면 개질 후 전유탁액으로 제조하여 아크릴 점착제를 합성함으로서, 분산성이 양호하고 아크릴 점착제에 전기전도성 등이 부여되는 이점이 있다. Accordingly, by dispersing the boehmite sol and the carbon nanotubes with water after the surface modification to synthesize the acrylic adhesive, there is an advantage that the dispersibility is good and the electrical conductivity is imparted to the acrylic adhesive.
상기의 구성에 의한 본 발명은, 수계 유화중합 아크릴 점착제에 탄소나노튜브와 보헤마이트를 함유하여 분산성이 양호하고 전기전도성을 향상시킨 하이브리드 점착제를 제조하되, 탄소나노튜브와 보헤마이트를 표면 처리하여 아크릴 점착제와의 상용성이 높아지고, 분산성이 양호하고 전기전도성 등의 기능성이 부여되는 효과가 있다.According to the present invention, a hybrid pressure-sensitive adhesive having good dispersibility and improved electrical conductivity by containing carbon nanotubes and boehmite in an aqueous emulsion-polymerized acrylic pressure-sensitive adhesive is prepared, and the carbon nanotubes and boehmite are surface treated. The compatibility with an acrylic adhesive becomes high, there exists an effect which dispersibility is favorable and the functionality, such as electrical conductivity, is provided.
도 1은 본발명의 도전성 아크릴 점착제 및 점착 쉬트 제조 방법의 모식도 이고,
도 2는 본 발명의 보헤마이트와 탄소나노튜브가 분산된 형상의 TEM 결과를 나타낸 사진이다. 1 is a schematic view of the conductive acrylic pressure-sensitive adhesive and the adhesive sheet production method of the present invention,
Figure 2 is a photograph showing the TEM results of the shape in which the boehmite and carbon nanotubes of the present invention are dispersed.
이하 첨부된 도면을 참조로 본 발명의 바람직한 실시예를 설명하기로 한다.Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings.
도시된 바와 같이, 본 발명에 따른 도전성 아크릴 점착제 제조 방법은 먼저, 탈이온수에 알루미늄이소프로폭사이드를 10~30중량부 첨가하여 나노 사이즈의 수분산 보헤마이트 졸을 졸-겔 공정을 통하여 제조 한다.As shown, the conductive acrylic pressure-sensitive adhesive manufacturing method according to the present invention first, by adding 10 to 30 parts by weight of aluminum isopropoxide to deionized water to prepare a nano-size water dispersion boehmite sol through the sol-gel process .
그 다음, 제조 된 수분산 보헤마이트 졸에 유기실란을 2~20중량부 첨가하여 교반을 통하여 표면 개질 한다. Then, 2 to 20 parts by weight of the organosilane is added to the prepared aqueous dispersion of boehmite sol, and the surface is modified by stirring.
그 다음, 황 또는 질산 용액에 탄소나노튜브 0.5~10중량부를 분산시켜 초음파를 가하여 탄소나노튜브의 표면에 하이드록실 및 카르복실 반응기를 부여하고 세척 및 건조를 하여 산처리 된 탄소나노튜브를 제조 한다.Next, 0.5-10 parts by weight of carbon nanotubes are dispersed in sulfur or nitric acid solution, and ultrasonic waves are applied to the surface of the carbon nanotubes to give hydroxyl and carboxyl reactors, followed by washing and drying to prepare acid-treated carbon nanotubes. .
그 다음, 산처리 된 탄소나노튜브에 아크릴 단량체 10~40중량부와 개시제를 섞어 용매에 분산 후 70~80℃에서 초음파와 교반을 통하여 아크릴 단량체로 탄소나노튜브를 표면 개질 시키고 세척 및 건조를 한다.Next, 10-40 parts by weight of an acrylic monomer and an initiator are mixed with the acid-treated carbon nanotubes, dispersed in a solvent, and the surface of the carbon nanotubes is surface-modified with acrylic monomers by ultrasonic and stirring at 70-80 ° C, followed by washing and drying. .
그 다음, 유화제를 첨가한 수분산 보헤마이트 졸에 탄소나노튜브를 0.1~5중량부 첨가하고 초음파 및 강력한 교반을 통하여 분산 시킨 뒤 아크릴 단량체를 첨가하고 다시 강력한 교반을 통하여 전유탁액을 제조한다.Next, 0.1 to 5 parts by weight of carbon nanotubes are added to the water-dispersed boehmite sol to which the emulsifier is added, dispersed through ultrasonic waves and vigorous stirring, and then acrylic monomer is added to prepare the total emulsion through vigorous stirring.
그 다음, 보헤마이트 및 탄소나노튜브가 분산된 전유탁액과 개시제를 75~85℃의 탈이온수에 2~4시간동안 천천히 떨어뜨리며 반응시킨 후, 추가적으로 1~2시간 반응을 시켜 하이브리드 아크릴 점착제를 제조한다.Next, the preemulsion of the boehmite and carbon nanotubes dispersed therein and the initiator were slowly reacted with deionized water at 75 to 85 ° C. for 2 to 4 hours, and then reacted for 1 to 2 hours to obtain a hybrid acrylic pressure sensitive adhesive. Manufacture.
그리고 필요 시, 제조된 아크릴 점착제를 이형 필름 위에 코팅 후 탈포 및 건조를 통하여 점착 쉬트를 제조한다.And, if necessary, the adhesive sheet is prepared by degassing and drying the coated acrylic adhesive on a release film.
이하, 본 발명의 이해를 돕기 위하여 바람직한 실시예를 제시하나, 하기 실시예는 본 발명을 예시하는 것일뿐 본 발명의 범위가 하기 실시예에 한정되는 것은 아니다.
Hereinafter, preferred examples are provided to help understanding of the present invention, but the following examples are merely to illustrate the present invention, and the scope of the present invention is not limited to the following examples.
반응조에 탈이온수 11g에 보헤마이트의 전구체로서 알루미늄이소프로폭사이드 1.5g을 첨가한 후 90℃로 승온하여 2시간 동안 가수분해를 시킨 뒤 질산 1.3g을 첨가하여 90℃에서 24시간 반응시켜 졸-겔 반응을 통한 수분산 보헤마이트 졸을 제조한다.After adding 1.5 g of aluminum isopropoxide as a precursor of boehmite to 11 g of deionized water in the reactor, the temperature was raised to 90 ° C. for hydrolysis for 2 hours, and 1.3 g of nitric acid was added to react at 90 ° C. for 24 hours. A waterborne boehmite sol is prepared via a gel reaction.
그 다음 제조 된 보헤마이트 졸에 메틸트리메톡시실란을 0.25g 투입 후 2시간 교반 하고, 4시간 숙성을 하여 보헤마이트 졸의 표면 개질을 한다.Then, 0.25 g of methyltrimethoxysilane was added to the prepared boehmite sol, stirred for 2 hours, and aged for 4 hours to modify the surface of the boehmite sol.
그 다음 탄소나노튜브 0.05g을 황/질산 10㎖에 중탕하에 6시간 동안 초음파를 가하고 필터링 및 건조를 한다.Then, 0.05 g of carbon nanotubes were sonicated in 10 ml of sulfur / nitric acid for 6 hours in a bath, filtered, and dried.
그 다음 산처리 된 탄소나노튜브와 메틸아크릴레이트 0.01g 및 아조비스이소부티로니트릴 0.01g을 섞고 N-메틸피롤리돈에 분산시킨 후, 70℃에서 2시간 초음파를 가한 뒤 24시간 교반을 하고, 세척 및 건조를 하여 아크릴 단량체로 표면 개질 된 탄소나노튜브를 제조한다.Then, acid-treated carbon nanotubes were mixed with 0.01 g of methyl acrylate and 0.01 g of azobisisobutyronitrile, dispersed in N-methylpyrrolidone, and ultrasonically stirred at 70 ° C. for 2 hours, followed by stirring for 24 hours. To prepare a carbon nanotube surface-modified with acrylic monomer by washing, drying.
그 다음 표면 개질 된 보헤마이트 졸에 유화제 2g을 첨가하여 준비한 후, 부틸아크릴레이트 10g, 2-에틸헥실아크릴레이트 33g, 메틸메타아크릴레이트 11g, 메타아크릴릭산 0.5g을 및 표면 개질 된 탄소나노튜브를 호모게나이저를 통하여 골고루 분산한 뒤, 상기 유화제가 섞인 보헤마이트 졸과 탄소나노튜브가 섞인 단량체를 50℃에서 호모게나이저를 사용하여 전유탁액을 제조한다.Then, prepared by adding 2 g of an emulsifier to the surface-modified boehmite sol, 10 g of butyl acrylate, 33 g of 2-ethylhexyl acrylate, 11 g of methyl methacrylate, 0.5 g of methacrylic acid, and the surface-modified carbon nanotube After uniformly dispersing through a homogenizer, the whole emulsion is prepared by using a homogenizer at 50 ° C. for a monomer in which the boehmite sol and carbon nanotubes mixed with the emulsifier are mixed.
상기에서 제조된 전유탁액에 대하여 TEM 이미지를 측정한 결과 도 2와 같이 보헤마이트 졸 및 탄소나노튜브가 양호하게 분산되어 있음을 알 수 있다. As a result of measuring the TEM image of the prepared emulsion, it can be seen that the boehmite sol and the carbon nanotubes are well dispersed as shown in FIG. 2.
그 다음 반응조에 탈이온수 25g을 85℃로 승온 시킨 후 전유탁액 2g을 넣고 초기 반응개시제로 포타슘퍼설페이트 0.1g과 정제수 1.5g의 혼합물을 투입하고 나머지 전유탁액과 후 반응개시제 포타슘설페이트 0.1g과 탈이온수 5g을 동시에 3시간 동안 투입한 후, 85℃에서 1시간 반응시키고, 40℃ 냉각 후 중화제로 암모니아수 0.3g과 탈이온수 0.4g의 혼합물을 투입하고 10분 교반하여 점착제를 제조한다.Then, 25 g of deionized water was heated to 85 ° C. in a reactor, and then 2 g of total emulsion was added. A mixture of 0.1 g of potassium persulfate and 1.5 g of purified water was added as an initial reaction initiator, and 0.1 g of potassium sulfate after the remaining total emulsion was added. After 5 g of deionized water and 3 hours at the same time, the reaction was carried out at 85 ℃ for 1 hour, after cooling 40 ℃ into a mixture of 0.3g ammonia water and 0.4g deionized water as a neutralizing agent and stirred for 10 minutes to prepare a pressure-sensitive adhesive.
필요 시, 상기 점착제를 이형지 위에 코팅을 한 후 탈포 및 건조 작업을 통하여 점착 쉬트를 제조한다. If necessary, the adhesive sheet is coated on a release paper, and then a pressure-sensitive adhesive sheet is prepared by defoaming and drying.
Claims (17)
상기 제1단계에서 합성된 보헤마이트 졸을 유기실란을 사용하여 표면 개질하는 제2단계와;
탄소나노튜브를 산을 통하여 전처리하는 제3단계와;
상기 3단계에서 산처리 된 탄소나노튜브를 아크릴 단량체를 통하여 표면 개질하는 제 4단계와;
표면 개질된 탄소나노튜브와 표면개질된 보헤마이트 졸 및 아크릴 단량체와 유화제를 사용하여 무기물과 아크릴이 혼합된 유화물을 제조하는 제5단계; 그리고,
상기 제5단계의 유화물과 반응개시제를 혼합하여 수계 유화중합 아크릴 점착제를 제조하는 제6단계;를 포함하여 구성됨을 특징으로 하는 도전성 아크릴 점착제 제조 방법.A first step of synthesizing the boehmite sol;
A second step of surface modifying the boehmite sol synthesized in the first step using an organosilane;
A third step of pretreating the carbon nanotubes through an acid;
A fourth step of surface-modifying the carbon nanotubes acid-treated in the third step through an acrylic monomer;
A fifth step of preparing an emulsion of inorganic and acryl using surface-modified carbon nanotubes, surface-modified boehmite sol, and acrylic monomer and emulsifier; And,
And a sixth step of preparing the aqueous emulsion polymerization acrylic pressure-sensitive adhesive by mixing the emulsion of the fifth step and the reaction initiator.
상기 1단계에서 형성된 보헤마이트 졸 100중량부에 유기실란 2~20중량부가 첨가되고 교반되어 형성됨을 특징으로 하는 도전성 아크릴 점착제 제조 방법.3. The method according to claim 2,
2 to 20 parts by weight of the organosilane is added to 100 parts by weight of the boehmite sol formed in the step 1 and is formed by stirring.
제3단계에서 산처리된 탄소나노튜브 100중량부에 아크릴 단량체 10~40 중량부와 반응개시제를 섞어 용매에 분산하여 형성됨을 특징으로 하는 도전성 아크릴 점착제 제조 방법.The method of claim 3, wherein the fourth step,
10 to 40 parts by weight of the acrylic monomer and the reaction initiator are mixed with 100 parts by weight of the acid-treated carbon nanotubes in the third step, and the dispersion is formed in a solvent.
상기 제5단계의 유화물과 반응개시제를 탈이온수에 혼합시켜 형성됨을 특징으로 하는 도전성 아크릴 점착제 제조 방법.The method of claim 4, wherein the sixth step is
Conductive acrylic pressure-sensitive adhesive manufacturing method characterized in that formed by mixing the emulsion and the reaction initiator of the fifth step in deionized water.
2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 라우릴아크릴레이트, 라우릴메타크릴레이트, 메틸아크릴레이트, 이소옥틸아크릴레이트, 이소데실아크릴레이트, 아크릴산, 메타크릴릭산, 에틸메타크릴레이트, n-부틸메타크릴레이트,이소부틸메타크릴레이트,t-부틸메타크릴레이트,아크릴로니트릴,에틸아크릴레이트,이소부틸아크릴레이트,2-에틸헥실메타크릴레이트,에틸렌,옥타데실메타크릴레이트,2-하이드록시에틸메타크릴레이트,2-하이드록시프로필메타크릴레이트,디메틸아미노에틸메타크릴레이트,t-부틸아미노에틸메타크릴레이트,디에틸아미노에틸메타크릴레이트,글리시딜메타크릴레이트,2-하이드록시에틸아크릴레이트,2-하이드록시프로필아크릴레이트,아크릴아마이드 및 N-메틸올아크릴아마이드 중에 어느 하나 또는 이들을 둘 이상 혼합한 혼합물을 사용함을 특징으로 하는 도전성 아크릴 점착제 제조 방법.The method of claim 6, wherein the acrylic monomer,
2-ethylhexyl acrylate, n-butyl acrylate, lauryl acrylate, lauryl methacrylate, methyl acrylate, isooctyl acrylate, isodecyl acrylate, acrylic acid, methacrylic acid, ethyl methacrylate, n -Butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, acrylonitrile, ethyl acrylate, isobutyl acrylate, 2-ethylhexyl methacrylate, ethylene, octadecyl methacrylate, 2- Hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, dimethylaminoethyl methacrylate, t-butylaminoethyl methacrylate, diethylaminoethyl methacrylate, glycidyl methacrylate, 2-hydroxy Hydroxyethyl acrylate, 2-hydroxypropyl acrylate, acrylamide and N-methylol acrylamide, any one or a mixture of two or more thereof A method for producing a conductive acrylic adhesive, characterized in that the mixture is used.
산처리된 탄소나노튜브에 아크릴 단량체와 반응개시제를 섞어 용매에 분산하여 형성됨을 특징으로 하는 도전성 아크릴 점착제.The method of claim 10, wherein the surface-modified carbon nanotubes,
A conductive acrylic pressure-sensitive adhesive, characterized in that the acid-treated carbon nanotubes are formed by mixing an acrylic monomer and a reaction initiator and dispersed in a solvent.
2-에틸헥실아크릴레이트, n-부틸아크릴레이트, 라우릴아크릴레이트, 라우릴메타크릴레이트, 메틸아크릴레이트, 이소옥틸아크릴레이트, 이소데실아크릴레이트, 아크릴산, 메타크릴릭산, 에틸메타크릴레이트, n-부틸메타크릴레이트,이소부틸메타크릴레이트,t-부틸메타크릴레이트,아크릴로니트릴,에틸아크릴레이트,이소부틸아크릴레이트,2-에틸헥실메타크릴레이트,에틸렌,옥타데실메타크릴레이트,2-하이드록시에틸메타크릴레이트,2-하이드록시프로필메타크릴레이트,디메틸아미노에틸메타크릴레이트,t-부틸아미노에틸메타크릴레이트,디에틸아미노에틸메타크릴레이트,글리시딜메타크릴레이트,2-하이드록시에틸아크릴레이트,2-하이드록시프로필아크릴레이트,아크릴아마이드 및 N-메틸올아크릴아마이드 중에 어느 하나 또는 이들을 둘 이상 혼합한 혼합물을 사용함을 특징으로 하는 도전성 아크릴 점착제.The method of claim 10, wherein the acrylic monomer,
2-ethylhexyl acrylate, n-butyl acrylate, lauryl acrylate, lauryl methacrylate, methyl acrylate, isooctyl acrylate, isodecyl acrylate, acrylic acid, methacrylic acid, ethyl methacrylate, n -Butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, acrylonitrile, ethyl acrylate, isobutyl acrylate, 2-ethylhexyl methacrylate, ethylene, octadecyl methacrylate, 2- Hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, dimethylaminoethyl methacrylate, t-butylaminoethyl methacrylate, diethylaminoethyl methacrylate, glycidyl methacrylate, 2-hydroxy Hydroxyethyl acrylate, 2-hydroxypropyl acrylate, acrylamide and N-methylol acrylamide, any one or a mixture of two or more thereof A conductive acrylic adhesive, characterized in that the mixture is used.
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| CN104371574A (en) * | 2014-11-18 | 2015-02-25 | 苏州东辰林达检测技术有限公司 | Heat-resistant and anti-aging conductive viscose and preparation method thereof |
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| KR101644710B1 (en) * | 2014-12-04 | 2016-08-11 | 계명대학교 산학협력단 | Preparing method of adhesive having conductive materials |
| KR101955873B1 (en) * | 2017-06-30 | 2019-05-27 | 이주엽 | Adhesive having excellent conductivity and chemical resistance |
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