KR101903033B1 - a water repellent coating composition - Google Patents

a water repellent coating composition Download PDF

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KR101903033B1
KR101903033B1 KR1020170071924A KR20170071924A KR101903033B1 KR 101903033 B1 KR101903033 B1 KR 101903033B1 KR 1020170071924 A KR1020170071924 A KR 1020170071924A KR 20170071924 A KR20170071924 A KR 20170071924A KR 101903033 B1 KR101903033 B1 KR 101903033B1
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water
weight
mixture
coating composition
parts
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KR1020170071924A
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Korean (ko)
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하성호
최진녕
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한남대학교 산학협력단
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/18Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to a water-repellent coating composition and a method for manufacturing the same. More particularly, the present invention relates to a water-repellent coating composition comprising nanoparticles having a diameter of 10-200 nm, a silane coupling agent, a solvent, an acid compound and a catalyst, and a method for manufacturing the same. The present invention can provide a method for manufacturing a water-repellent coating composition which is excellent in water repellency, water resistance, weather resistance, durability and dimensional stability and can be used stably for a long period of time by minimizing moisture penetration even when woods, fibers, and construction materials are stored outdoor or penetrated by water. Further, the present invention can provide a water-repellent coating composition which forms a uniform hydrophobic coating layer on surfaces of woods, fibers, construction materials, etc. and exhibits excellent heat resistance, durability, weather resistance, water repellency, and moisture barrier properties and high contact angle.

Description

발수용 코팅 조성물{a water repellent coating composition}A water repellent coating composition,

본 발명은 발수용 코팅 조성물 및 그 제조방법에 관한 것으로, 더욱 상세하게는 직경이 10~200nm인 나노입자, 실란 커플링제, 용매, 산 화합물 및 촉매를 포함하는 발수용 코팅 조성물 및 그 제조방법에 관한 것이다. More particularly, the present invention relates to a foot-receiving coating composition comprising nanoparticles having a diameter of 10 to 200 nm, a silane coupling agent, a solvent, an acid compound and a catalyst, and a process for producing the same .

섬유, 목재, 건자재 등은 표면에 다공성 및 흡수성 구조를 가지기 때문에 물에 대한 흡수력이 높고 수분의 침투가 용이하며, 함수량이 급격히 증가하게 된다. Textiles, timber, and building materials have a porous and absorptive structure on the surface, so they have a high absorption capacity for water, easy penetration of water, and a sudden increase in water content.

목재 및 건자재를 옥외 보관하거나 침수 시에 수분이 침투하게 되면 치수안정성, 내구성, 강도 등이 저하되고 부패와 부식이 급속히 진행되어 건축물, 구조물 등의 재료로 사용할 수 없게 된다. When wood and building materials are kept outdoors or when water is immersed in water, dimensional stability, durability, strength and the like are deteriorated and corruption and corrosion progress rapidly, making it impossible to use them as materials for buildings and structures.

따라서 목재를 옥외에 보관하거나 목재가 침수되더라도 수분의 침투를 최소화하여 장기간 안정적으로 사용될 수 있는 목재용 코팅 조성물의 개발이 절실히 요구된다. Accordingly, there is a desperate need to develop a coating composition for wood that can be used stably for a long period of time by minimizing the penetration of water even when the wood is stored outside or when the wood is submerged.

이와 관련하여 한국공개특허 제10-1993-0006134호는 석재 및 목재 표면에 발수성을 제공하는, 알칼리 금속 아미노 유기 작용성 실리코네이트와 적어도 하나의 알칼리금속 유기 실리코네이트를 함유하는 수성 혼합물을 포함하는 수성 조성물을 개시하고 있다. In this regard, Korean Patent Laid-Open No. 10-1993-0006134 discloses a water-based composition comprising an aqueous mixture containing an alkali metal amino organic functional silicate and at least one alkali metal organosiliconate to provide water repellency to the stone and wood surface ≪ / RTI >

한국공개특허 제10-2016-0004503호는 알킬기로 소수화 표면 처리된 금속산화물 입자 3 내지 10중량% 및 알코올 90 내지 97중량%를 포함하는 상도용 초발수 코팅제와, 합성고무를 포함하는 석유계 수지 10 내지 40중량% 및 케톤계와 아세테이트계 혼합용제 60 내지 90중량%를 포함하는 하도용 베이스 코팅제를 개시하고 있다.Korean Patent Laid-Open No. 10-2016-0004503 discloses a water-repellent coating material for phase superposition comprising 3 to 10% by weight of metal oxide particles subjected to hydrophobic surface treatment with an alkyl group and 90 to 97% by weight of alcohol, 10 to 40% by weight of a mixed solvent of a ketone type and an acetate type, and 60 to 90% by weight of an acetate type mixed solvent.

또한 한국공개특허 제10-1994-7001899호는 0.3 내지 30 중량%의 플루오로지방족 라디칼 함유 폴리(옥시알킬렌)화합물, 0.3 내지 30 중량%의 방오제 및 0 내지 60 중량%의 환경적으로 허용될 수 있는 수-혼화성 유기용매Korean Patent Laid-Open No. 10-1994-7001899 also discloses a fluoroaliphatic radical-containing poly (oxyalkylene) compound in an amount of 0.3 to 30% by weight, 0.3 to 30% by weight of an antifouling agent and 0 to 60% Water - miscible organic solvent

와 물을 함유하는 처리용 조성물을 개시하고 있다. And water are disclosed.

그러나 상기 문헌에 개시된 기술은 코팅제의 수분 차단성, 발수성, 내오염성 등이 불량하여 목재, 건자재 등의 표면을 통한 수분 침투를 효과적으로 방지할 수 없다.However, the technique disclosed in the above document can not effectively prevent moisture penetration through the surface of wood, building materials, etc. due to poor water barrier properties, water repellency, and stain resistance of the coating agent.

또한 목재, 건자재 등의 표면에 내구성, 내후성, 발수성 등이 우수한 균일한 코팅층을 형성할 수 없어 건축물, 구조물 등의 재료로 장기간 안정적으로 사용될 수 없다. In addition, it is impossible to form a uniform coating layer having excellent durability, weather resistance, water repellency, etc. on the surface of wood and building materials, and thus it can not be stably used for a long time with materials such as buildings and structures.

한국공개특허 제10-1993-0006134호Korean Patent Publication No. 10-1993-0006134 한국공개특허 제10-2016-0004503Korean Patent Publication No. 10-2016-0004503 한국공개특허 제10-1994-7001899호Korean Patent Publication No. 10-1994-7001899

본 발명은 상기 종래 기술의 문제점을 해결하기 위한 것으로서, 발수성, 내수성, 내오염성, 내후성, 내구성, 치수안정성 등이 우수하여 목재, 섬유, 건자재 등을 옥외에 보관하거나 침수되더라도 수분의 침투를 최소화하여 장기간 안정적으로 사용될 수 있는 발수용 코팅 조성물의 제조방법을 제공하는 데 그 목적이 있다. Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above problems of the prior art, and it is an object of the present invention to provide a water- And which can be used stably for a long period of time.

또한 본 발명은 목재, 섬유, 건자재 등의 표면에 균일한 소수성 코팅층을 형성하고, 내열성, 내구성, 내후성, 발수성, 수분차단성 등이 우수하고 높은 접촉각을 나타내는 발수용 코팅 조성물을 제공하는 것을 목적으로 한다. It is another object of the present invention to provide a foot-receiving coating composition which forms a uniform hydrophobic coating layer on the surfaces of wood, fibers, building materials, etc. and exhibits excellent heat resistance, durability, weatherability, water repellency, do.

상기와 같은 목적을 달성하기 위하여 본 발명은 (a) 직경이 10~200nm인 나노입자 및 용매를 혼합하여 제1혼합물을 제조하는 단계; (b) 실란 커플링제, 용매 및 산 화합물을 혼합하여 제2혼합물을 제조하는 단계; (c) 상기 제1혼합물 및 제2혼합물을 혼합하여 혼합액을 제조하는 단계; 및 (d) 상기 혼합액에 용매, 산 화합물 및 촉매를 첨가하여 코팅 조성물을 제조하는 단계를 포함하는 발수용 코팅 조성물의 제조방법을 제공한다. According to an aspect of the present invention, there is provided a method for preparing a nanoparticle nanoparticle, (b) mixing a silane coupling agent, a solvent and an acid compound to prepare a second mixture; (c) mixing the first mixture and the second mixture to prepare a mixed solution; And (d) adding a solvent, an acid compound, and a catalyst to the mixed solution to prepare a coating composition.

본 발명의 일실시예에 있어서, 상기 (b) 단계는 실란 커플링제, 용매 및 산 화합물을 100:20~200:10~50의 중량비로 30~100℃에서 1~20시간 혼합하여 제2혼합물을 제조하는 것을 특징으로 한다.In step (b), the silane coupling agent, the solvent, and the acid compound are mixed at a weight ratio of 100: 20 to 200: 10 to 50 at 30 to 100 ° C for 1 to 20 hours to form a second mixture Is produced.

본 발명의 일실시예에 있어서, 상기 (c) 단계는 제1혼합물 및 제2혼합물을 100:10~50의 중량비로 30~100℃에서 1~10시간 혼합하여 혼합액을 제조하는 것을 특징으로 한다.In one embodiment of the present invention, the step (c) is characterized in that the mixture is prepared by mixing the first mixture and the second mixture at a weight ratio of 100: 10 to 50 at 30 to 100 ° C for 1 to 10 hours .

본 발명의 일실시예에 있어서, 상기 (d) 단계는 상기 혼합액 100중량부에 대하여 용매 100~500중량부, 산 화합물 1~10중량부 및 촉매 0.05~2중량부를 사용하는 것을 특징으로 한다.In one embodiment of the present invention, in the step (d), 100 to 500 parts by weight of a solvent, 1 to 10 parts by weight of an acid compound and 0.05 to 2 parts by weight of a catalyst are used for 100 parts by weight of the mixed solution.

본 발명의 일실시예에 있어서, 상기 실란 커플링제는 메틸트리메톡시실란, 3-글리시독시프로필트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란을 포함하는 것을 특징으로 한다.In one embodiment of the present invention, the silane coupling agent is characterized by containing methyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, dimethyldimethoxysilane, and octyltriethoxysilane.

또한 본 발명은 직경이 10~200nm인 나노입자, 실란 커플링제, 용매, 산 화합물 및 촉매를 포함하는 발수용 코팅 조성물을 제공한다.The present invention also provides a foot-receiving coating composition comprising nanoparticles having a diameter of 10 to 200 nm, a silane coupling agent, a solvent, an acid compound and a catalyst.

본 발명의 일실시예에 있어서, 상기 실란 커플링제는 상기 나노입자의 표면에 결합되는 것을 특징으로 한다. In one embodiment of the present invention, the silane coupling agent is bonded to the surface of the nanoparticles.

본 발명의 일실시예에 있어서, 상기 실란 커플링제는 메틸트리메톡시실란, 3-글리시독시프로필트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란을 포함하는 것을 특징으로 한다. In one embodiment of the present invention, the silane coupling agent is characterized by containing methyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, dimethyldimethoxysilane, and octyltriethoxysilane.

본 발명은 발수성, 내수성, 내오염성, 내후성, 내구성, 치수안정성 등이 우수하여 목재, 섬유, 건자재 등을 옥외에 보관하거나 침수되더라도 수분의 침투를 최소화하여 장기간 안정적으로 사용될 수 있는 발수용 코팅 조성물의 제조방법을 제공할 수 있다. The present invention relates to a water-absorbing coating composition which is excellent in water repellency, water resistance, stain resistance, weather resistance, durability and dimensional stability and can be stably used for a long period of time by minimizing moisture penetration even when stored in wood or fiber, A manufacturing method can be provided.

또한 본 발명은 목재, 섬유, 건자재 등의 표면에 균일한 소수성 코팅층을 형성하고, 내열성, 내구성, 내후성, 발수성, 수분차단성 등이 우수하고 높은 접촉각을 나타내는 발수용 코팅 조성물을 제공할 수 있다. Also, the present invention can provide a foot-receiving coating composition which forms a uniform hydrophobic coating layer on the surfaces of wood, fibers, building materials and the like and exhibits excellent heat resistance, durability, weather resistance, water repellency, moisture barrier property and high contact angle.

도 1은 실시예 1의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
도 2는 실시예 2의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
도 3은 실시예 3의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
도 4는 실시예 4의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
도 5는 실시예 5의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
도 6은 실시예 6의 코팅 조성물(a) 및 상기 코팅 조성물을 목재 표면에 코팅한 후 물을 적하한 상태(b)를 나타낸다.
Fig. 1 shows a coating composition (a) of Example 1 and a state (b) in which water is dropped after coating the coating composition on a wood surface.
Fig. 2 shows a coating composition (a) of Example 2 and a state (b) in which water is dropped after the coating composition is coated on a wood surface.
Fig. 3 shows a coating composition (a) of Example 3 and a state (b) in which water is dropped after coating the coating composition on a wood surface.
Fig. 4 shows a coating composition (a) of Example 4 and a state (b) in which water is dropped after coating the coating composition on a wood surface.
5 shows a coating composition (a) of Example 5 and a state (b) in which water is dropped after coating the coating composition on a wood surface.
Fig. 6 shows a coating composition (a) of Example 6 and a state (b) in which water is dropped after coating the coating composition on a wood surface.

이하 실시예를 바탕으로 본 발명을 상세히 설명한다. 본 발명에 사용된 용어, 실시예 등은 본 발명을 보다 구체적으로 설명하고 통상의 기술자의 이해를 돕기 위하여 예시된 것에 불과할 뿐이며, 본 발명의 권리범위 등이 이에 한정되어 해석되어서는 안 된다.Hereinafter, the present invention will be described in detail based on examples. It is to be understood that the terminology, examples and the like used in the present invention are merely illustrative of the present invention in order to more clearly explain the present invention and to facilitate understanding of the ordinary artisan, and should not be construed as being limited thereto.

본 발명에 사용되는 기술 용어 및 과학 용어는 다른 정의가 없다면 이 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 통상적으로 이해하고 있는 의미를 나타낸다.Technical terms and scientific terms used in the present invention mean what the person skilled in the art would normally understand unless otherwise defined.

본 발명은 (a) 직경이 10~200nm인 나노입자 및 용매를 혼합하여 제1혼합물을 제조하는 단계; (b) 실란 커플링제, 용매 및 산 화합물을 혼합하여 제2혼합물을 제조하는 단계; (c) 상기 제1혼합물 및 제2혼합물을 혼합하여 혼합액을 제조하는 단계; 및 (d) 상기 혼합액에 용매, 산 화합물 및 촉매를 첨가하여 코팅 조성물을 제조하는 단계를 포함하는 발수용 코팅 조성물의 제조방법을 제공한다. (A) mixing a nanoparticle having a diameter of 10 to 200 nm and a solvent to prepare a first mixture; (b) mixing a silane coupling agent, a solvent and an acid compound to prepare a second mixture; (c) mixing the first mixture and the second mixture to prepare a mixed solution; And (d) adding a solvent, an acid compound, and a catalyst to the mixed solution to prepare a coating composition.

상기 (a) 단계는 나노입자와 용매를 혼합하여 나노입자를 분산시키는 단계로서, 직경이 10~200nm인 나노입자 및 용매를 혼합하여 제1혼합물을 제조한다.In the step (a), the nanoparticles are dispersed by mixing the nanoparticles with a solvent. The nanoparticles having a diameter of 10 to 200 nm and the solvent are mixed to prepare a first mixture.

용매로는 메탄올, 에탄올, 프로판올, 이소프로판올, 부탄올 등의 알코올이 제한 없이 사용될 수 있으며, 에탄올이 사용되는 것이 바람직하다.As the solvent, alcohols such as methanol, ethanol, propanol, isopropanol, and butanol can be used without limitation, and ethanol is preferably used.

나노입자로는 실리카, 알루미나, 제올라이트, 지르코니아, 산화철, 산화마그네슘, 탄산칼슘, 마이카 등이 제한 없이 사용될 수 있으며, 알루미나가 사용되는 것이 바람직하다. As the nanoparticles, silica, alumina, zeolite, zirconia, iron oxide, magnesium oxide, calcium carbonate, mica and the like can be used without limitation, and alumina is preferably used.

나노입자의 직경은 10~200nm이고, 10~60nm인 것이 바람직하다. 직경이 10nm 미만인 경우 수분 차단 특성이 저하되고, 200nm를 초과하는 경우 균일한 코팅층을 형성할 수 없어 내구성 및 내후성이 저하된다. The diameter of the nanoparticles is preferably 10 to 200 nm, more preferably 10 to 60 nm. When the diameter is less than 10 nm, the moisture barrier properties are deteriorated. When the diameter exceeds 200 nm, a uniform coating layer can not be formed, and durability and weather resistance are lowered.

상기 용매 100중량부에 대하여 나노입자 1~15중량부를 혼합하여 제1혼합물을 제조하는 것이 발수성, 내구성, 내후성 등의 측면에서 바람직하다. It is preferable that 1 to 15 parts by weight of the nanoparticles are mixed with 100 parts by weight of the solvent to prepare the first mixture in view of water repellency, durability and weatherability.

상기 (a) 단계를 통해 제조된 제1혼합물은 나노입자의 분산성이 우수하여 제2혼합물과의 혼합을 통해 나노입자 표면에 실란 커플링제를 효과적으로 결합시켜 발수성이 우수한 코팅 조성물을 제조할 수 있다. The first mixture prepared through the step (a) is excellent in the dispersibility of the nanoparticles and can effectively bind the silane coupling agent to the surface of the nanoparticles through mixing with the second mixture to produce a coating composition having excellent water repellency .

상기 (b) 단계는 실란 커플링제, 용매 및 산 화합물을 혼합하여 실란 커플링제를 가수분해하는 단계로서, 실란 커플링제, 용매 및 산 화합물을 100:20~200:10~50의 중량비로 30~100℃에서 1~20시간 혼합하여 제2혼합물을 제조한다.The step (b) is a step of hydrolyzing a silane coupling agent by mixing a silane coupling agent, a solvent and an acid compound, wherein the silane coupling agent, the solvent, and the acid compound are mixed at a weight ratio of 100:20 to 200: And the mixture is mixed at 100 DEG C for 1 to 20 hours to prepare a second mixture.

실란 커플링제는 유기 화합물과 결합할 수 있는 유기 관능기 및 무기물과 반응할 수 있는 가수분해기를 가지며, 상기 실란 커플링제는 나노입자의 표면에 결합하여 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등의 특성을 나타낸다. The silane coupling agent has an organic functional group capable of binding with an organic compound and a hydrolyzable group capable of reacting with an inorganic substance, and the silane coupling agent binds to the surface of the nanoparticles and is excellent in water repellency, water resistance, moisture barrier properties, durability, Lt; / RTI >

실란 커플링제로는 알킬기 함유 실란, 아미노기 함유 실란, 에폭시기 함유 실란, 아크릴레이트기 함유 실란, 이소시아네이트기 함유 실란, 불소기 함유 실란, 비닐기 함유 실란 등이 제한 없이 사용될 수 있다. As the silane coupling agent, an alkyl group-containing silane, an amino group-containing silane, an epoxy group-containing silane, an acrylate group-containing silane, an isocyanate group-containing silane, a fluorine group-containing silane and a vinyl group-containing silane can be used without limitation.

알킬기 함유 실란으로는 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란 등이 있다. Examples of the alkyl group-containing silane include methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane.

에폭시기 함유 실란으로는 2-글리시독시에틸메틸디메톡시실란, 2-글리시독시에틸메틸디에톡시실란, 3-글리시독시프로필메틸디메톡시실란, 3-글리시독시프로필메틸디에톡시실란, 2-글리시독시에틸트리메톡시실란, 2-글리시독시에틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란, 3-글리시독시프로필트리에톡시실란, 2-(3,4-에폭시시클로헥실)에틸메틸디메톡시실란, 2-(3,4-에폭시시클로헥실)에틸메틸디에톡시실란, 3-(3,4-에폭시시클로헥실)프로필메틸디메톡시실란, 3-(3,4-에폭시시클로헥실)프로필메틸디에톡시실란, 2-(3,4-에폭시시클로헥실)에틸트리메톡시실란, 2-(3,4-에폭시시클로헥실)에틸트리에톡시실란, 3-(3,4-에폭시시클로헥실)프로필트리메톡시실란, 3-(3,4-에폭시시클로헥실)프로필트리에톡시실란 등이 있다. Examples of the epoxy group-containing silane include 2-glycidoxyethylmethyldimethoxysilane, 2-glycidoxyethylmethyldiethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2 Glycidoxyethyltrimethoxysilane, 2-glycidoxyethyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4- Epoxycyclohexyl) ethylmethyldimethoxysilane, 2- (3,4-epoxycyclohexyl) ethylmethyldiethoxysilane, 3- (3,4-epoxycyclohexyl) propylmethyldimethoxysilane, 3- 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3- 4-epoxycyclohexyl) propyltrimethoxysilane, and 3- (3,4-epoxycyclohexyl) propyltriethoxysilane.

아크릴레이트기 함유 실란으로는 3-메타크릴록시프로필메틸디메톡시실란, 3-메타크릴록시프로필트리메톡시실란, 3-메타크릴록시프로필메틸디에톡시실란, 3-메타크릴록시프로필트리에톡시실란, 3-아크릴록시프로필트리메톡시실란, 메타크릴록시메틸트리에톡시실란, 메타크릴록시메틸트리메톡시실란 등이 있다. Examples of the acrylate group-containing silane include 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropylmethyldiethoxysilane, 3-methacryloxypropyltriethoxysilane , 3-acryloxypropyltrimethoxysilane, methacryloxymethyltriethoxysilane, methacryloxymethyltrimethoxysilane, and the like.

불소기 함유 실란으로는 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란, 트리플루오로프로필트리메톡시실란, 트리데카플루오로옥틸트리메톡시실란, 헵타데카플루오로데실트리메톡시실란, 헵타데카플루오로데실트리이소프로폭시실란 등이 있다. Examples of the fluorine group-containing silane include heptadecafluoro-1,1,2,2-tetradecyltrimethoxysilane, trifluoropropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, heptadecafluorodecyl Trimethoxysilane, heptadecafluorodecyltriisopropoxysilane, and the like.

코팅 조성물의 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등을 향상시키기 위해서는 알킬기 함유 실란 및 에폭시기 함유 실란의 혼합 실란 커플링제가 사용되는 것이 바람직하며, 알킬기 함유 실란 및 에폭시기 함유 실란의 중량비는 100:1~15인 것이 바람직하다. In order to improve the water repellency, water resistance, moisture barrier property, durability, weather resistance and the like of the coating composition, a mixed silane coupling agent of an alkyl group-containing silane and an epoxy group-containing silane is preferably used and the weight ratio of the alkyl group- 1 to 15 is preferable.

예를 들면 실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란 및 3-글리시독시프로필트리메톡시실란을 사용할 수 있으며, 메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 중량비는 100:10~200:10~200인 것이 바람직하다. For example, methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane and 3-glycidoxypropyltrimethoxysilane may be used as the silane coupling agent, and methyltrimethoxysilane, dimethyldimethoxysilane, The weight ratio of octyltriethoxysilane is preferably 100: 10-200: 10-200.

또한 코팅 조성물의 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등을 향상시키기 위해서는 알킬기 함유 실란, 에폭시기 함유 실란 및 불소기 함유 실란의 혼합 실란 커플링제가 사용되는 것이 바람직하며, 알킬기 함유 실란, 에폭시기 함유 실란 및 불소기 함유 실란의 중량비는 100:1~15:5~200인 것이 바람직하다. In order to improve the water repellency, water resistance, moisture barrier property, durability and weather resistance of the coating composition, it is preferable to use an alkyl group-containing silane, an epoxy group-containing silane and a mixed silane coupling agent containing a fluorine group- The weight ratio of the silane and the fluorine group-containing silane is preferably 100: 1 to 15: 5 to 200.

예를 들면 실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란을 사용할 수 있으며, 메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 중량비는 100:1~20:1~20인 것이 바람직하다. For example, silane coupling agents such as methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and heptadecafluoro-1,1,2,2-tetradecyl Trimethoxysilane, and the weight ratio of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane is preferably 100: 1 to 20: 1 to 20.

용매로는 메탄올, 에탄올, 프로판올, 이소프로판올, 부탄올 등의 알코올이 제한 없이 사용될 수 있으며, 에탄올이 사용되는 것이 바람직하다.As the solvent, alcohols such as methanol, ethanol, propanol, isopropanol, and butanol can be used without limitation, and ethanol is preferably used.

산 화합물로는 염산, 아세트산, 황산, 질산 등이 사용될 수 있으며, 수용액의 형태로 사용되는 것이 바람직하다. 예를 들면 0.01N 염산 수용액이 사용될 수 있다. As the acid compound, hydrochloric acid, acetic acid, sulfuric acid, nitric acid and the like can be used, and it is preferable to use them in the form of an aqueous solution. For example, 0.01N hydrochloric acid aqueous solution may be used.

실란 커플링제, 용매 및 산 화합물은 100:20~200:10~50의 중량비로 사용되는 것이 발수성, 내구성, 내후성 등의 측면에서 바람직하다. The silane coupling agent, the solvent and the acid compound are preferably used in a weight ratio of 100: 20 to 200: 10 to 50 in terms of water repellency, durability and weather resistance.

상기 실란 커플링제, 용매 및 산 화합물을 혼합한 후 30~100℃에서 1~20시간 반응시켜 제2혼합물을 제조하며, 이러한 단계를 통하여 실란 커플링제의 알콕시기는 가수 분해되어 수산화기가 형성된다. 상기 수산화기는 제1혼합물에 포함된 나노입자의 표면에 결합하여 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등의 특성을 나타낸다. The silane coupling agent, the solvent and the acid compound are mixed and reacted at 30 to 100 ° C for 1 to 20 hours to prepare a second mixture. Through this step, the alkoxy group of the silane coupling agent is hydrolyzed to form a hydroxyl group. The hydroxyl group binds to the surface of the nanoparticles contained in the first mixture to exhibit properties such as water repellency, water resistance, moisture barrier properties, durability and weatherability.

상기 (c) 단계는 상기 제1혼합물 및 제2혼합물을 혼합하여 혼합액을 제조하는 단계로서, 제1혼합물 및 제2혼합물을 100:10~50의 중량비로 30~100℃에서 1~10시간 혼합하여 혼합액을 제조한다.(C) mixing the first mixture and the second mixture to prepare a mixture, mixing the first mixture and the second mixture in a weight ratio of 100: 10 to 50 at 30 to 100 ° C for 1 to 10 hours To prepare a mixed solution.

제1혼합물 및 제2혼합물의 중량비는 100:10~50이며, 중량비가 100:10을 초과하는 경우 나노입자 표면에 실란 커플링제가 충분히 결합되지 않아 수분 차단 특성이 저하되고, 100:50 미만인 경우 균일한 코팅층을 형성할 수 없어 내구성 및 내후성이 저하된다. The weight ratio of the first mixture and the second mixture is 100: 10 to 50, and when the weight ratio is more than 100: 10, the moisture barrier property is deteriorated because the silane coupling agent is not sufficiently bonded to the surface of the nanoparticles, A uniform coating layer can not be formed and durability and weather resistance are lowered.

상기 제1혼합물 및 제2혼합물을 혼합한 후 30~100℃에서 1~10시간 반응시켜 혼합액을 제조하며, 이러한 단계를 통하여 실란 커플링제의 수산화기는 제1혼합물에 포함된 나노입자의 표면에 결합하여 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등의 특성을 나타낸다. The first mixture and the second mixture are mixed and reacted at 30 to 100 ° C for 1 to 10 hours to prepare a mixed solution. Through this step, the hydroxyl group of the silane coupling agent is bonded to the surface of the nanoparticles contained in the first mixture Thereby exhibiting properties such as water repellency, water resistance, moisture barrier properties, durability, and weather resistance.

상기 (d) 단계는 상기 혼합액에 용매, 산 화합물 및 촉매를 첨가하여 코팅 조성물을 제조하는 단계로서, 상기 혼합액 100중량부에 대하여 용매 100~500중량부, 산 화합물 1~10중량부 및 촉매 0.05~2중량부를 사용하는 것을 특징으로 한다.(D) is a step of preparing a coating composition by adding a solvent, an acid compound, and a catalyst to the mixed solution, wherein 100 to 500 parts by weight of a solvent, 1 to 10 parts by weight of an acid compound, and 0.05 To 2 parts by weight.

용매로는 메탄올, 에탄올, 프로판올, 이소프로판올, 부탄올 등의 알코올이 제한 없이 사용될 수 있으며, 에탄올이 사용되는 것이 바람직하다.As the solvent, alcohols such as methanol, ethanol, propanol, isopropanol, and butanol can be used without limitation, and ethanol is preferably used.

산 화합물로는 염산, 아세트산, 황산, 질산 등이 사용될 수 있으며, 수용액의 형태로 사용되는 것이 바람직하다. 예를 들면 0.01N 염산 수용액이 사용될 수 있다. As the acid compound, hydrochloric acid, acetic acid, sulfuric acid, nitric acid and the like can be used, and it is preferable to use them in the form of an aqueous solution. For example, 0.01N hydrochloric acid aqueous solution may be used.

촉매로는 옥틸산, 스테아르산, 나프텐산, 아세틸아세토네이트 등의 Cu, Fe, Co, Mn, Al, Ti, Zr, Ni 등의 유기 금속염; Ti, Sn, Bi, Zr, Al 등의 금속 알콕사이드; 옥틸페놀, 노닐페놀 등의 페놀 화합물; 1-부탄올, 2-에틸헥산올 등의 알코올류; 2-메틸이미다졸, 2-에틸-4-메틸이미다졸, 2-페닐이미다졸, 1-시아노에틸-2-페닐이미다졸, 1-시아노에틸-2-에틸-4-메틸-이미다졸, 2-페닐-4,5-디하이드록시메틸이미다졸, 2-페닐-4-메틸-5-하이드록시메틸이미다졸 등의 이미다졸 유도체 등을 사용할 수 있다. 예를 들면 알루미늄 아세틸아세토네이트를 사용하는 것이 바람직하다. Examples of the catalyst include organic metal salts such as Cu, Fe, Co, Mn, Al, Ti, Zr and Ni such as octylic acid, stearic acid, naphthenic acid and acetylacetonate; Metal alkoxides such as Ti, Sn, Bi, Zr and Al; Phenol compounds such as octyl phenol and nonyl phenol; Alcohols such as 1-butanol and 2-ethylhexanol; Methylimidazole, 2-phenylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-cyanoethyl-2-ethyl- Imidazole derivatives such as methyl-imidazole, 2-phenyl-4,5-dihydroxymethylimidazole and 2-phenyl-4-methyl-5-hydroxymethylimidazole can be used. For example, it is preferable to use aluminum acetylacetonate.

촉매를 사용함으로써 코팅 조성물을 기재에 코팅할 때 더 낮은 온도에서 코팅층이 쉽게 형성되며, 코팅층의 내열성, 열안정성 등이 우수하게 된다. When a coating composition is coated on a substrate by using a catalyst, the coating layer is easily formed at a lower temperature, and the heat resistance and thermal stability of the coating layer are excellent.

상기 혼합액 100중량부에 대하여 용매 100~500중량부, 산 화합물 1~10중량부 및 촉매 0.05~2중량부를 사용하는 것이 발수성, 내구성, 내후성 등의 측면에서 바람직하다. It is preferable to use 100 to 500 parts by weight of the solvent, 1 to 10 parts by weight of the acid compound and 0.05 to 2 parts by weight of the catalyst with respect to 100 parts by weight of the mixed solution in terms of water repellency, durability and weather resistance.

또한 본 발명은 직경이 10~200nm인 나노입자, 실란 커플링제, 용매, 산 화합물 및 촉매를 포함하는 발수용 코팅 조성물에 관한 것이다. The present invention also relates to a foot-receiving coating composition comprising nanoparticles having a diameter of 10 to 200 nm, a silane coupling agent, a solvent, an acid compound and a catalyst.

상기 실란 커플링제는 나노입자의 표면에 화학적으로 또는 물리적으로 결합되어 발수성, 내수성, 수분 차단 특성, 내구성, 내후성 등의 특성을 나타낸다. The silane coupling agent is chemically or physically bonded to the surface of the nanoparticles to exhibit properties such as water repellency, water resistance, moisture barrier properties, durability, and weather resistance.

상기 실란 커플링제로 메틸트리메톡시실란, 3-글리시독시프로필트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 혼합 실란 커플링제를 사용하는 것이 바람직하다.It is preferable to use a mixed silane coupling agent of methyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane as the silane coupling agent.

또한 실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란의 혼합 실란 커플링제를 사용하는 것이 바람직하다. Further, as the silane coupling agent, there may be mentioned methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and heptadecafluoro-1,1,2,2-tetradecyltrimethoxysilane It is preferable to use a mixed silane coupling agent.

상기 코팅 조성물은 발수성, 내수성, 내오염성, 내후성, 내구성, 치수안정성 등이 우수하여 목재, 섬유, 건자재 등을 옥외에 보관하거나 침수되더라도 수분의 침투를 최소화함으로써 장기간 안정적으로 사용될 수 있다. The coating composition is excellent in water repellency, water resistance, stain resistance, weather resistance, durability, dimensional stability, and can be used stably for a long period of time by minimizing the penetration of moisture even when it is stored outside or immersed in wood, fibers and building materials.

또한 상기 코팅 조성물은 목재, 섬유, 건자재 등의 표면에 균일한 소수성 코팅층을 형성하고, 내열성, 내구성, 내후성, 발수성, 수분차단성 등이 우수하고 높은 접촉각을 나타낼 수 있다. Further, the coating composition forms a uniform hydrophobic coating layer on the surface of wood, fibers, building materials, etc., and can exhibit a high contact angle with excellent heat resistance, durability, weather resistance, water repellency, moisture barrier property and the like.

이하 실시예 및 비교예를 통해 본 발명을 상세히 설명한다. 하기 실시예는 본 발명의 실시를 위하여 예시된 것일 뿐, 본 발명의 내용이 하기 실시예에 의하여 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples. The following examples are intended to illustrate the practice of the present invention and are not intended to limit the scope of the present invention.

(실시예 1)(Example 1)

직경이 50nm인 알루미나 5중량부 및 에탄올 100중량부를 혼합하여 제1혼합물을 제조하였다. 5 parts by weight of alumina having a diameter of 50 nm and 100 parts by weight of ethanol were mixed to prepare a first mixture.

3-글리시독시프로필트리메톡시실란, 에탄올 및 0.01N 염산 수용액을 60℃에서 12시간 혼합하여 제2혼합물을 제조하였다. 3-glycidoxypropyltrimethoxysilane, ethanol and 0.01N hydrochloric acid aqueous solution were mixed at 60 DEG C for 12 hours to prepare a second mixture.

상기 제1혼합물 및 제2혼합물을 60℃에서 4시간 혼합하여 혼합액을 제조하였다. The first mixture and the second mixture were mixed at 60 DEG C for 4 hours to prepare a mixed solution.

상기 혼합액에 에탄올, 0.01N 염산 수용액 및 알루미늄 아세틸아세토네이트를 첨가하여 코팅 조성물을 제조하였다. Ethanol, 0.01N hydrochloric acid aqueous solution and aluminum acetylacetonate were added to the mixed solution to prepare a coating composition.

(실시예 2)(Example 2)

실란 커플링제로 메틸트리메톡시실란 및 3-글리시독시프로필트리메톡시실란을 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 코팅 조성물을 제조하였다. A coating composition was prepared in the same manner as in Example 1 except that methyltrimethoxysilane and 3-glycidoxypropyltrimethoxysilane were used as a silane coupling agent.

(실시예 3)(Example 3)

실란 커플링제로 메틸트리메톡시실란 및 디메틸디메톡시실란을 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 코팅 조성물을 제조하였다. A coating composition was prepared in the same manner as in Example 1 except that methyltrimethoxysilane and dimethyldimethoxysilane were used as a silane coupling agent.

(실시예 4)(Example 4)

실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 3-글리시독시프로필트리메톡시실란 및 옥틸트리에톡시실란을 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 코팅 조성물을 제조하였다. A coating composition was prepared in the same manner as in Example 1, except that methyltrimethoxysilane, dimethyldimethoxysilane, 3-glycidoxypropyltrimethoxysilane and octyltriethoxysilane were used as silane coupling agents.

(실시예 5)(Example 5)

실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 3-글리시독시프로필트리메톡시실란 및 옥틸트리에톡시실란을 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 코팅 조성물을 제조하였다. A coating composition was prepared in the same manner as in Example 1, except that methyltrimethoxysilane, dimethyldimethoxysilane, 3-glycidoxypropyltrimethoxysilane and octyltriethoxysilane were used as silane coupling agents.

(실시예 6)(Example 6)

실란 커플링제로 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란을 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 코팅 조성물을 제조하였다. Silane coupling agents such as methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and heptadecafluoro-1,1,2,2-tetradecyltrimethoxy The coating composition was prepared in the same manner as in Example 1 except that silane was used.

상기 실시예로부터 제조된 코팅 조성물의 함수율 및 접촉각을 측정하여 그 결과를 아래의 표에 나타내었다. The water content and the contact angle of the coating composition prepared from the above examples were measured, and the results are shown in the following table.

(함수율)(Water content)

실시예에 의하여 제조된 코팅 조성물을 목재의 표면에 코팅하고 건조시킨 후, 코팅층이 형성된 목재의 표면에 2.5g의 물을 적하한 다음 함수율을 측정하였다. The coating composition prepared according to the examples was coated on the surface of wood and dried. Then, 2.5 g of water was dropped on the surface of the wood on which the coating layer was formed, and water content was measured.

함수율은 고체 내에 포함된 수분의 양을 나타내는 것으로 KS F 2199에 의거하여 측정하였다. Moisture content is measured according to KS F 2199, which represents the amount of moisture contained in the solid.

함수율은 다음의 식에 의하여 계산된다. The water content is calculated by the following formula.

함수율(%) = (m1-m2)/m2×100Moisture content (%) = (m1-m2) / m2 x 100

(m1은 시험편의 건조 전 질량, m2는 시험편의 건조 후 질량)(m1 is the mass of the test piece before drying, and m2 is the mass after drying of the test piece)

(접촉각)(Contact angle)

실시예에 의하여 제조된 코팅 조성물을 목재의 표면에 코팅하고 건조시킨 후, 코팅층이 형성된 목재의 표면에 물을 적하한 다음 접촉각을 측정하였다. The coating composition prepared according to the example was coated on the surface of wood and dried. Then, water was dropped on the surface of the wood on which the coating layer was formed, and then the contact angle was measured.

접촉각은 KS L 2110에 의거하여 측정하였다. The contact angle was measured according to KS L 2110.

실시예 1Example 1 1-11-1 1-21-2 1-31-3 1-41-4 제1혼합물The first mixture 100100 100100 100100 100100 제2혼합물The second mixture 3-글리시독시프로필트리메톡시실란3-glycidoxypropyltrimethoxysilane 12.7412.74 12.7412.74 42.4642.46 42.4642.46 에탄올ethanol 15.0015.00 15.0015.00 50.0050.00 50.0050.00 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 2.902.90 2.902.90 9.709.70 9.709.70 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 1.001.00 에탄올ethanol 250250 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 0.100.10 1.001.00 0.100.10 1.001.00 함수율(%)Moisture content (%) 14.3214.32 14.2714.27 13.9913.99 13.0913.09 접촉각(°)Contact angle (°) 15.0015.00 17.0017.00 27.0027.00 25.0025.00

실시예 2Example 2 2-12-1 2-22-2 2-32-3 제1혼합물The first mixture 100100 100100 100100 제2혼합물The second mixture 메틸트리메톡시실란Methyltrimethoxysilane 3.053.05 9.159.15 15.2515.25 3-글리시독시프로필트리메톡시실란3-glycidoxypropyltrimethoxysilane 10.6110.61 6.376.37 2.122.12 에탄올ethanol 16.3416.34 14.4814.48 12.6312.63 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 3.643.64 5.095.09 6.546.54 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 에탄올ethanol 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 1.001.00 1.001.00 1.001.00 함수율(%)Moisture content (%) 13.9913.99 13.6513.65 14.2014.20 접촉각(°)Contact angle (°) 34.0034.00 32.0032.00 36.0036.00

실시예 3Example 3 3-13-1 3-23-2 3-33-3 제1혼합물The first mixture 100100 100100 100100 제2혼합물The second mixture 메틸트리메톡시실란Methyltrimethoxysilane 15.2515.25 9.159.15 3.053.05 디메틸디메톡시실란Dimethyldimethoxysilane 2.882.88 8.658.65 14.4214.42 에탄올ethanol 5.005.00 5.005.00 5.005.00 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 7.307.30 7.507.50 7.707.70 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 에탄올ethanol 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 1.001.00 1.001.00 1.001.00 함수율(%)Moisture content (%) 12.5312.53 12.9512.95 12.9012.90 접촉각(°)Contact angle (°) 62.0062.00 69.0069.00 79.0079.00

실시예 4Example 4 4-14-1 4-24-2 4-34-3 제1혼합물The first mixture 100100 100100 100100 제2혼합물The second mixture 메틸트리메톡시실란Methyltrimethoxysilane 12.2012.20 9.159.15 3.053.05 3-글리시독시프로필트리메톡시실란3-glycidoxypropyltrimethoxysilane 1.701.70 1.701.70 1.701.70 디메틸디메톡시실란Dimethyldimethoxysilane 1.731.73 3.173.17 6.066.06 옥틸트리에톡시실란Octyltriethoxysilane 1.451.45 2.662.66 5.085.08 에탄올ethanol 8.008.00 9.009.00 10.0010.00 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 4.504.50 4.404.40 4.304.30 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 에탄올ethanol 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 1.001.00 1.001.00 1.001.00 함수율(%)Moisture content (%) 12.5512.55 12.3212.32 12.2512.25 접촉각(°)Contact angle (°) 82.0082.00 92.0092.00 94.0094.00

실시예 5Example 5 5-15-1 5-25-2 5-35-3 제1혼합물The first mixture 100100 100100 100100 제2혼합물The second mixture 메틸트리메톡시실란Methyltrimethoxysilane 12.2012.20 9.159.15 0.610.61 3-글리시독시프로필트리메톡시실란3-glycidoxypropyltrimethoxysilane 0.420.42 0.420.42 0.420.42 디메틸디메톡시실란Dimethyldimethoxysilane 2.602.60 4.044.04 8.088.08 옥틸트리에톡시실란Octyltriethoxysilane 2.182.18 3.393.39 6.776.77 에탄올ethanol 8.008.00 9.009.00 10.0010.00 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 4.504.50 4.404.40 4.304.30 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 에탄올ethanol 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 1.001.00 1.001.00 1.001.00 함수율(%)Moisture content (%) 12.1312.13 12.0312.03 11.3211.32 접촉각(°)Contact angle (°) 83.0083.00 85.0085.00 100.30100.30

실시예 6Example 6 6-16-1 6-26-2 6-36-3 제1혼합물The first mixture 100100 100100 100100 제2혼합물The second mixture 메틸트리메톡시실란Methyltrimethoxysilane 12.2012.20 9.159.15 3.053.05 3-글리시독시프로필트리메톡시실란3-glycidoxypropyltrimethoxysilane 0.420.42 0.420.42 0.420.42 디메틸디메톡시실란Dimethyldimethoxysilane 0.580.58 0.580.58 0.580.58 옥틸트리에톡시실란Octyltriethoxysilane 0.480.48 0.480.48 0.480.48 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란Heptadecafluoro-1,1,2,2-tetradecyltrimethoxysilane 1.001.00 2.672.67 7.337.33 에탄올ethanol 8.008.00 9.009.00 10.0010.00 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 4.504.50 4.404.40 4.304.30 0.01N 염산 수용액0.01 N hydrochloric acid aqueous solution 1.501.50 1.501.50 1.501.50 에탄올ethanol 250250 250250 250250 알루미늄 아세틸아세토네이트Aluminum acetylacetonate 1.001.00 1.001.00 1.001.00 함수율(%)Moisture content (%) 11.1411.14 11.1311.13 10.7910.79 접촉각(°)Contact angle (°) 112.00112.00 115.00115.00 118.10118.10

상기 표 1 내지 6의 결과로부터, 실시예 4 내지 6의 코팅 조성물을 목재의 표면에 코팅하는 경우, 함수율이 낮고 접촉각이 증가함을 확인할 수 있으며, 특히 실시예 6의 경우 수분 차단 특성이 가장 우수함을 알 수 있다(도 4 내지 6).From the results shown in Tables 1 to 6, it can be seen that when the coating compositions of Examples 4 to 6 are coated on the surface of wood, the water content is low and the contact angle is increased. In particular, in Example 6, (Figs. 4 to 6).

따라서 실시예 4 내지 6의 코팅 조성물은 발수성, 내수성, 내오염성, 내후성, 내구성, 치수안정성 등이 우수하여 목재, 섬유, 건자재 등을 옥외에 보관하거나 침수되더라도 수분의 침투를 최소화함으로써 장기간 안정적으로 사용될 수 있다. Therefore, the coating compositions of Examples 4 to 6 are excellent in water repellency, water resistance, stain resistance, weather resistance, durability, and dimensional stability, so that the penetration of moisture is minimized even when wood, fiber, and building materials are stored outdoors or flooded, .

반면 실시예 1 내지 3은 실시예 4 내지 6에 비해 수분 차단 특성이 다소 열등함을 알 수 있다(도 1 내지 3). On the other hand, Examples 1 to 3 show that the moisture barrier properties are somewhat inferior to those of Examples 4 to 6 (Figs. 1 to 3).

Claims (8)

(a) 직경이 10~200nm인 나노입자 및 용매를 혼합하여 제1혼합물을 제조하는 단계;
(b) 실란 커플링제, 용매 및 산 화합물을 혼합하여 제2혼합물을 제조하는 단계;
(c) 상기 제1혼합물 및 제2혼합물을 혼합하여 혼합액을 제조하는 단계; 및
(d) 상기 혼합액에 용매, 산 화합물 및 촉매를 첨가하여 코팅 조성물을 제조하는 단계를 포함하는 발수용 코팅 조성물의 제조방법에 있어서,
상기 (b) 단계는 실란 커플링제, 용매 및 산 화합물을 100:20~200:10~50의 중량비로 30~100℃에서 1~20시간 혼합하여 제2혼합물을 제조하고,
상기 (c) 단계는 제1혼합물 및 제2혼합물을 100:10~50의 중량비로 30~100℃에서 1~10시간 혼합하여 혼합액을 제조하며,
상기 (d) 단계는 상기 혼합액 100중량부에 대하여 용매 100~500중량부, 산 화합물 1~10중량부 및 촉매 0.05~2중량부를 사용하며,
상기 실란 커플링제는 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란의 혼합 실란 커플링제를 사용하고,
메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 중량비는 100:1~20:1~20 이며,
메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 총 함량 100중량부에 대하여 3-글리시독시프로필트리메톡시실란 1~15중량부 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란 5~200중량부가 사용되는 것을 특징으로 하는 발수용 코팅 조성물의 제조방법.
(a) mixing a nanoparticle having a diameter of 10 to 200 nm and a solvent to prepare a first mixture;
(b) mixing a silane coupling agent, a solvent and an acid compound to prepare a second mixture;
(c) mixing the first mixture and the second mixture to prepare a mixed solution; And
(d) adding a solvent, an acid compound and a catalyst to the mixed solution to prepare a coating composition,
In the step (b), the silane coupling agent, the solvent and the acid compound are mixed at a weight ratio of 100:20 to 200:10 to 50 at 30 to 100 ° C for 1 to 20 hours to prepare a second mixture,
In the step (c), the mixture is prepared by mixing the first mixture and the second mixture at a weight ratio of 100: 10 to 50 at 30 to 100 ° C for 1 to 10 hours,
(D) is performed by using 100 to 500 parts by weight of a solvent, 1 to 10 parts by weight of an acid compound, and 0.05 to 2 parts by weight of a catalyst with respect to 100 parts by weight of the mixed solution,
The silane coupling agent is selected from the group consisting of methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and heptadecafluoro-1,1,2,2-tetradecyltrimethane Lt; RTI ID = 0.0 > siloxane < / RTI > coupling agent,
The weight ratio of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane is 100: 1 to 20: 1 to 20,
1 to 15 parts by weight of 3-glycidoxypropyltrimethoxysilane and 1 to 15 parts by weight of heptadecafluoro-1,1, 2, 3, 4, 5, 6 and 10 parts by weight based on 100 parts by weight of the total amount of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane. , And 5 to 200 parts by weight of 2-tetradecyltrimethoxysilane are used.
삭제delete 삭제delete 삭제delete 삭제delete 제1항의 제조방법에 의하여 제조되는 발수용 코팅 조성물에 있어서,
직경이 10~200nm인 나노입자, 실란 커플링제, 용매, 산 화합물 및 촉매를 포함하고,
상기 실란 커플링제는 상기 나노입자의 표면에 결합되고,
상기 실란 커플링제는 메틸트리메톡시실란, 디메틸디메톡시실란, 옥틸트리에톡시실란, 3-글리시독시프로필트리메톡시실란 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란의 혼합 실란 커플링제를 사용하고,
메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 중량비는 100:1~20:1~20 이며,
메틸트리메톡시실란, 디메틸디메톡시실란 및 옥틸트리에톡시실란의 총 함량 100중량부에 대하여 3-글리시독시프로필트리메톡시실란 1~15중량부 및 헵타데카플루오로-1,1,2,2-테트라데실트리메톡시실란 5~200중량부가 사용되는 것을 특징으로 하는 발수용 코팅 조성물.
11. A foot-releasing coating composition produced by the method of claim 1,
A nanoparticle having a diameter of 10 to 200 nm, a silane coupling agent, a solvent, an acid compound and a catalyst,
The silane coupling agent binds to the surface of the nanoparticles,
The silane coupling agent is selected from the group consisting of methyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and heptadecafluoro-1,1,2,2-tetradecyltrimethane Lt; RTI ID = 0.0 > siloxane < / RTI > coupling agent,
The weight ratio of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane is 100: 1 to 20: 1 to 20,
1 to 15 parts by weight of 3-glycidoxypropyltrimethoxysilane and 1 to 15 parts by weight of heptadecafluoro-1,1, 2, 3, 4, 5, 6 and 10 parts by weight based on 100 parts by weight of the total amount of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane. And 5 to 200 parts by weight of 2-tetradecyltrimethoxysilane are used.
삭제delete 삭제delete
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021086144A1 (en) * 2019-10-31 2021-05-06 김명호 Nanocomposite composition having excellent barrier properties

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010143806A (en) * 2008-12-19 2010-07-01 Tokuyama Corp Surface-treated silica-based particle and process of manufacturing same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010143806A (en) * 2008-12-19 2010-07-01 Tokuyama Corp Surface-treated silica-based particle and process of manufacturing same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021086144A1 (en) * 2019-10-31 2021-05-06 김명호 Nanocomposite composition having excellent barrier properties

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