KR100463926B1 - Multi Functional Silicon-polymer Composite for Coating - Google Patents
Multi Functional Silicon-polymer Composite for Coating Download PDFInfo
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- KR100463926B1 KR100463926B1 KR10-2001-0074784A KR20010074784A KR100463926B1 KR 100463926 B1 KR100463926 B1 KR 100463926B1 KR 20010074784 A KR20010074784 A KR 20010074784A KR 100463926 B1 KR100463926 B1 KR 100463926B1
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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
- C09D—COATING 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/02—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
본 발명은 코팅시 기재의 표면에 내화학성, 내마모성, 부식방지, 발수 및 발유 특성을 제공하여 기재에 다기능성이 부여되도록 하는 조성물에 관한 것으로, 본 발명에서는 알킬 폴리 실록산에 금속 산화물-졸 및 불소수지를 함유하는 투명한 다기능성 코팅제 조성물이 제공된다. 본 발명에 따른 불화 폴리 실록산 다기능성 코팅제 조성물은 내화학성, 내마모성, 분산성, 내수성, 내유성 및 내후성이 우수한 투명한 조성물로 광학소재, 자동차 유리, 페인트 소광제, 각종 전기 및 건축 재료 등의 기능을 향상시키기 위한 코팅제로 폭넓게 응용될 수 있다.The present invention relates to a composition which provides chemical resistance, abrasion resistance, corrosion protection, water repellent and oil repellent properties to the surface of the substrate upon coating so that the substrate is provided with multifunctionality. A transparent multifunctional coating composition containing a resin is provided. The fluorinated polysiloxane multifunctional coating composition according to the present invention is a transparent composition having excellent chemical resistance, abrasion resistance, dispersibility, water resistance, oil resistance and weather resistance, and improves the functions of optical materials, automotive glass, paint matting agents, various electrical and building materials, and the like. It can be widely applied as a coating for making.
Description
본 발명은 다기능성 실리콘 폴리머 코팅제 조성물에 관한 것으로, 특히 코팅시 기재의 표면에 내화학성, 내마모성, 부식방지, 발수 및 발유 특성을 제공하여 기재에 다기능성을 부여할 수 있도록 한 코팅제 조성물에 관한 것이다.The present invention relates to a multifunctional silicone polymer coating composition, and more particularly, to a coating composition which provides chemical resistance, abrasion resistance, corrosion protection, water repellency and oil repellent properties to the surface of a substrate during coating to impart versatility to the substrate. .
코팅하고자 하는 표면은 금속, 합금, 유리, 지류, 세라믹, 플라스틱 및 기타물질이 포함될 수 있다. 현재 시판되고 있는 투명한 폴리카보네이트로 구성된 자동차 헤드램프, 안경 및 카메라 등의 광학재료에는 내마모성 및 내스크래치성이 요구된다. 또한 빌딩 및 기타 건축물과 같은 지상에 고정된 시설에는 그리핑방지(antigriping)소수성이 필요하며, 표면에 결빙을 방지하고, 방오 및 부식방지 기능이 요구된다.Surfaces to be coated may include metals, alloys, glass, feeders, ceramics, plastics and other materials. Optical materials such as automobile headlamps, glasses, and cameras made of transparent polycarbonate currently on the market require abrasion resistance and scratch resistance. In addition, ground-fixed installations such as buildings and other buildings require anti-gripping hydrophobicity, prevent freezing on surfaces, and antifouling and corrosion protection.
기존 기능성 코팅제는 가수분해 매체인 알콜 및 물 등의 용매에 콜로이드 실리카 분산액 또는 실리카겔 등의 실리카를 첨가한 다음, 가수분해를 할 수 있는 실리콘 알콕사이드와 혼합하여 내마모성 코팅제를 제조하는 방법이 미합중국 특허 제 3,708,225 호, 제 3,976,497 호, 제 3,986,997 호, 제 4,027,073 호, 제 4,159,206 호 및 제 4,117,315 호에 기술되어 있다.Existing functional coating agent is a method of preparing a wear-resistant coating agent by adding a colloidal silica dispersion or silica, such as silica gel to a solvent such as alcohol and water as a hydrolysis medium, and then mixed with a hydrolyzable silicon alkoxide. 3,976,497, 3,986,997, 4,027,073, 4,159,206 and 4,117,315.
한편, 우천시에 유리에 닿은 빗방울이 창유리 표면에 달라붙는 것을 방지하기 위한 소수성 처리제는 알킬 폴리 실록산, 무기산 및 수계 용매로 제조하는 방법이 미합중국 특허 제 3,579,540 호, 일본국 특허 공개 공보 제 1975-15473 호 등에 기술되어 있다.On the other hand, the hydrophobic treatment agent for preventing the raindrops on the glass from sticking to the surface of the window during rainy weather is prepared by alkyl polysiloxanes, inorganic acids and aqueous solvents, the United States Patent No. And the like.
그러나, 종래의 기능성 코팅제는 한두가지의 제한된 성능 밖에 제공하지 못하므로 여러 종류의 특성을 향상시키기 위해서는 기재에 각각의 기능성 코팅제를 이중, 삼중으로 코팅해야 하므로 비용 증가는 물론이고 작업이 불편하고 적용이 제한적인 문제점이 있다.However, conventional functional coatings provide only one or two limited performances, so in order to improve various kinds of properties, each functional coating agent must be coated on the substrate in double or triple, so that the operation is inconvenient and the application is inconvenient. There is a limited problem.
본 발명의 목적은 코팅하고자하는 기재의 표면에 내화학성, 내마모성, 부식방지, 발수 및 발유 특성을 제공하여 기재의 특성을 획기적으로 향상시킬 수 있는 다기능성 실리콘 폴리머 코팅제를 제공하는 것이다.It is an object of the present invention to provide a multifunctional silicone polymer coating that can significantly improve the properties of a substrate by providing chemical resistance, abrasion resistance, corrosion protection, water repellent and oil repellent properties on the surface of the substrate to be coated.
본 발명은 코팅시 기재의 표면에 내화학성, 내마모성, 부식방지, 발수 및 발유 특성을 제공하여 기재에 다기능성이 부여되도록 하는 조성물에 관한 것으로, 본 발명에서는 알킬 폴리 실록산에 금속 산화물-졸 및 불소수지를 함유하는 투명한 다기능성 코팅제 조성물이 제공된다.본 발명의 다기능성 코팅제 조성물은 전체 조성물 중 알킬 트리알콕시 실란 20 내지 40 중량 %, 실란 커플링제(오르가노실란) 5∼15 중량 %, 알콜 용매 20∼62 중량 %, 산촉매 1∼3 중량 %, 금속 산화물졸 10∼30 중량 %, 불소 함유 수지 또는 화합물 1∼5 중량 % 그리고 경화 촉매 1∼3 중량 %를 포함한다.상기 알킬 트리알콕시 실란은 메틸 트리메톡시실란, 메틸 트리에톡시 실란, 디메틸 디메톡시 실란, 메틸 트리부톡시 실란 등이나 이들의 2 이상 혼합물이 될 수 있다.상기 실란 커플링제는, 바람직하게는 비닐실란, 아미노 실란, 에톡시 실란 중에서 선택된 한 종류 이상의 실란을 포함한다.상기 알콜 용매는, C1내지 C4함유 수혼화성 알콜류나 MEK(메틸에틸케톤); 1-헥사놀; 톨루엔 등의 수불화성 알콜류를 한 종류 이상 포함한다.상기 금속 산화물 졸은 실리카졸, 티타늄졸, 알루미나졸 중 하나 이상을 포함하며, 바람직하게는 평균 입자 크기가 10∼30 nm 이고, 고체함량이 5∼30 wt% 이다.상기 불소함유 수지 또는 화합물은 바람직하게는 RCH2CH2OH 또는 RCH2CH2OOCCH=CH2를 포함한다. 여기서 R은 CF3(CF2)8를 나타낸다.상기 경화촉매는 트리메틸아민, 칼륨아세테이트, 4차 암모늄 카르복실레이트 및 디시안 디아마이드 중 하나 이상을 포함할 수 있다.일반적으로 소수성 코팅제는 디메틸 폴리 실록산 등의 규소 화합물이 가격이 저렴하고 유연성과 내구성을 갖추고 있어 가장 널리 쓰이고 있으나 최근에는 발유성 및 방오성을 요구하는 기재가 많아 가격은 다소 고가이지만 불소를 함유한 초소수성 코팅제가 많이 연구되고 있다.The present invention relates to a composition which provides chemical resistance, abrasion resistance, corrosion protection, water repellent and oil repellent properties to the surface of the substrate upon coating so that the substrate is provided with multifunctionality. A transparent multifunctional coating composition containing a resin is provided. The multifunctional coating composition of the present invention comprises 20 to 40% by weight of alkyl trialkoxy silane, 5 to 15% by weight of silane coupling agent (organosilane), alcohol solvent in the total composition. 20 to 62% by weight, 1 to 3% by weight acid catalyst, 10 to 30% by weight metal oxide sol, 1 to 5% by weight fluorine-containing resin or compound and 1 to 3% by weight curing catalyst. Methyl trimethoxysilane, methyl triethoxy silane, dimethyl dimethoxy silane, methyl tributoxy silane, or the like, or a mixture of two or more thereof may be used. At least one type of silane selected from vinyl silane, amino silane, and ethoxy silane. The alcohol solvent may include C 1 to C 4 containing water miscible alcohols and MEK (methyl ethyl ketone); 1-hexanol; And one or more kinds of water-fluorinated alcohols such as toluene. The metal oxide sol includes one or more of silica sol, titanium sol, and alumina sol, preferably having an average particle size of 10 to 30 nm and a solid content of 5 The fluorine-containing resin or compound preferably comprises RCH 2 CH 2 OH or RCH 2 CH 2 OOCCH = CH 2 . Wherein R represents CF 3 (CF 2 ) 8. The curing catalyst may comprise one or more of trimethylamine, potassium acetate, quaternary ammonium carboxylate and dicyan diamide. Generally, the hydrophobic coating agent is dimethyl poly Silicon compounds such as siloxane are the most widely used because they are inexpensive, have flexibility and durability, but recently, many substrates requiring oil repellency and antifouling properties are expensive, but superhydrophobic coatings containing fluorine have been studied.
불소화합물은 모든 화합물 중 가장 분자간 인력이 작고 표면 에너지가 낮다. 일례로 -CF3는 임계 표면 장력이 6 dyne/cm로 메틸기(-CH3)의 표면장력 22∼24 dyne/cm의 1/4의 수준으로 표면 코팅시 우수한 발수, 발유 효과를 나타낸다. 그러나 실제 적용 시에는 경제성 문제도 고려해야 하므로 폴리 실록산에 불소 화합물을 소량 첨가하여 사용하는 것이 좋은 것으로 알려져 있다. 그러나 기재 보호 코팅은 소수성뿐만 아니라 내열성, 내마모성, 항균, 내화학성 및 대전 방지 기능도 필요로 한다. 이에 본 발명에서는 평균 입자 크기가 10∼30 nm 정도인 금속 산화물-졸을 첨가하면 우수한 특성을 얻을 수 있음이 확인된다.Fluorine compounds have the lowest intermolecular attraction and the lowest surface energy of all compounds. For example, -CF 3 has an excellent water / oil repelling effect upon surface coating with a critical surface tension of 6 dyne / cm and a quarter of 22 to 24 dyne / cm of surface tension of methyl group (-CH 3 ). However, it is known to use a small amount of fluorine compound in the polysiloxane because economical considerations must be taken into account in practical applications. Substrate protective coatings, however, require not only hydrophobicity but also heat resistance, abrasion resistance, antibacterial, chemical resistance and antistatic function. In the present invention, it is confirmed that excellent properties can be obtained by adding a metal oxide-sol having an average particle size of about 10 to 30 nm.
내열 및 내마모성 충진 재료는 알루미나졸이나 실리카 졸 등이 좋고 항균 및 방오 특성은 티타늄 졸, 도전막은 주석화합물, 자외선 흡수 용도로 세륨 산화물을 함유하는 충진제를 사용한다. 또한 축합 반응을 촉진시키고 코팅액의 저장 안전성을 위해서 촉매의 도입이 요구되는데 촉매로서는 산, 염기 및 금속 유기화합물 등이 있으며, 저장수명(shelf life)과 경화 속도의 균형이 양호한 특성을 갖는 것으로 완충 잠재성 축합 촉매인 나트륨 아세테이트, 칼륨 아세테이트 및 4차 암모늄 카르복실레이트, 트리메틸아민 및 피리딘과 같은 아민류 염기성 pH를 갖는 콜로이드 실리카 등이 대표적이다. 본 발명에서 구현된 다기능성 코팅제 조성물은 바람직하게는, 실란 화합물 200 내지 250 중량부, 평균 입자 크기가 10∼30 nm인 금속 산화물-졸 50 내지 60 중량부, 불소 화합물을 전체 조성물의 2 내지 5 중량%, 알콜 용매 150 내지 200 중량부, 기타 첨가제 10내지 50 중량부를 포함한다.The heat and abrasion resistant filling materials are preferably alumina sol or silica sol. Antibacterial and antifouling properties include titanium sol, tin film as a conductive film, and a filler containing cerium oxide for UV absorption. In addition, the introduction of a catalyst is required to promote the condensation reaction and the storage stability of the coating liquid. The catalysts include acids, bases, and organic metal compounds, and have a good balance of shelf life and curing rate. Typical condensation catalysts are sodium acetate, potassium acetate and colloidal silica having amine basic pHs such as quaternary ammonium carboxylate, trimethylamine and pyridine. The multifunctional coating composition embodied in the present invention is preferably from 200 to 250 parts by weight of the silane compound, from 50 to 60 parts by weight of the metal oxide-sol having an average particle size of 10 to 30 nm, from 2 to 5 of the total composition. % By weight, 150-200 parts by weight of alcohol solvent, and 10-50 parts by weight of other additives.
상기와 같은 본 발명의 코팅제 조성물은 내후, 내마모, 발수 및 발유, 항균, 대전 방지 기능이 부가된 투명한 조성물로 금속, 합금, 유리, 지류, 세라믹, 플라스틱 및 기타 다양한 기재에 사용되어 코팅된 기재의 특성을 획기적으로 향상시킬 수 있으므로, 광학소재, 자동차 유리, 페인트 소광제, 각종 전기 및 건축 재료 등의 기능을 향상시키기 위한 코팅제로 폭넓게 응용될 수 있다.As described above, the coating composition of the present invention is a transparent composition having added weather resistance, abrasion resistance, water repellency and oil repellency, antibacterial, and antistatic function, and is used for coating on metals, alloys, glass, paper, ceramics, plastics, and various other substrates. Since it can significantly improve the properties of, it can be widely applied as a coating agent for improving the functions of optical materials, automotive glass, paint matting agent, various electrical and building materials.
아래에 본 발명의 실시예 및 시험예를 보여준다. 그러나 이들 실시예는 본 발명의 이해를 용이하게 하기 위하여 제시되는 것일 뿐, 본 발명이 이들 실시예에 의해 한정되는 것은 아니다.Examples and test examples of the present invention are shown below. However, these examples are only presented to facilitate understanding of the present invention, the present invention is not limited by these examples.
(실시예 1)(Example 1)
냉각기 및 교반기가 부착된 5 리터 반응기에 메틸트리에톡시실란 200 g, γ-아미노프로필에톡시실란 40 g을 혼합한 다음 이소프로판을 150 g을 넣고 50∼60℃에서 1 시간 동안 가열 교반 시키면서 평균 입자 크기가 12 nm인 실리카졸(Ludox LS-30, 30 wt% SiO2, Dupont) 50g을 서서히 적하시켰다. 모두 적하시킨 후 초산을 적당량 투입하여 pH를 4 정도로 조정하고 12시간 동안 계속 반응시켜 메틸폴리실록산을 얻었다. 여기에 불소수지(FC-C-1022, 한국정밀화학)를 천체 조성물의 3 wt% 첨가시키고 경화촉매로 트리메틸아인 10g을 가한 후 상온에서 5일간 숙성시켜 소수성 코팅액을 제조하였으며 아래 실험예에 의한 방법으로 테스트한 결과를 표 1에 나타내었다.200 g of methyltriethoxysilane and 40 g of γ-aminopropylethoxysilane were mixed in a 5-liter reactor equipped with a cooler and a stirrer. Then, 150 g of isopropane was added thereto and heated and stirred at 50 to 60 ° C. for 1 hour. 50 g of silica sol (Ludox LS-30, 30 wt% SiO 2 , Dupont) having a particle size of 12 nm was slowly added dropwise. After all were added dropwise, an appropriate amount of acetic acid was added to adjust the pH to about 4, and the reaction was continued for 12 hours to obtain methylpolysiloxane. A hydrophobic coating solution was prepared by adding 3 wt% of fluorocarbon resin (FC-C-1022, Korea Fine Chemical) to the celestial composition, adding 10 g of trimethyl ayne as a curing catalyst, and then aging at room temperature for 5 days. The test results are shown in Table 1.
(실시예 2)(Example 2)
상기의 실시예 1에서 실리카졸 대신 입자 크기가 20∼30 nm인 티타늄졸 50 g를 첨가시킨 것을 제외하고는 실시예 1과 동일하게 제조하였으며, 아래 실험예에 의한 방법으로 테스트한 결과를 표 1에 나타내었다.In Example 1, except that 50 g of titanium sol having a particle size of 20 to 30 nm was added instead of silica sol, it was prepared in the same manner as in Example 1, and the results thereof were tested by the method according to the following experimental example. Shown in
(실시예 3)(Example 3)
상기의 실시예 1에서 불소수지를 제외한 것 외에는 실시예 1과 동일하게 제조하였으며, 아래 실험예에 의한 방법으로 테스트한 결과를 표 1에 나타내었다.Except for the fluorine resin in Example 1 above was prepared in the same manner as in Example 1, the results of the test by the method according to the experimental example shown in Table 1 below.
(비교예 1)(Comparative Example 1)
상업제품인 카샤인(유한T.N.C)을 아래 실험예에 의한 방법으로 테스트한 결과를 표 1에 나타내었다.Table 1 shows the results of testing the commercial product carshine (Limit T.N.C) by the method according to the experimental example below.
(비교예 2)(Comparative Example 2)
상업제품인 레인오케이(옥시)을 아래 실험예에 의한 방법으로 테스트한 결과를 표 1에 나타내었다.Table 1 shows the results of testing a commercial product, Lane-O (oxy), by the method according to the following experimental example.
(실험예)Experimental Example
1. 경도 측정 방법1. How to measure hardness
두께 2 mm (9 cm × 9 cm)의 유리판위에 상기 실시예 및 비교예에서 제조된 조성물을 코팅한 시편을 충분히 만든 다음 각각 1개씩을 건조기에서 150℃, 20분간 건조시켜 측정기로 1 kgf힘으로 10 mm 그어 5회 반복(KS D6711 기준)하여 연필경도를 측정하였다.After making enough specimens coated with the composition prepared in Examples and Comparative Examples on a glass plate of 2 mm (9 cm × 9 cm) thickness, each one was dried at 150 ℃ for 20 minutes in a dryer, 1 kg f force Pencil hardness was measured by repeating 10 mm and 5 times (based on KS D6711).
2. 내식성 측정2. Corrosion resistance measurement
상기 1항의 시편을 5% NaCl 용액에 720 시간 침적시켜(JIS-K-5400 8.23) 내식성 테스트를 진행하였다.The specimen of claim 1 was immersed in 5% NaCl solution for 720 hours (JIS-K-5400 8.23) for corrosion resistance test.
3. 발수성 테스트3. Water repellency test
약 20 cm × 20 cm 유리 시험편 위에 실시예 및 비교예에서 얻어진 조성물을 코팅시켜 건조기에서 150℃, 20분간 건조 후 JIS-S-1092 스프레이법으로 발수도를 측정하였다.The composition obtained in Examples and Comparative Examples was coated on a about 20 cm × 20 cm glass test piece, dried at 150 ° C. for 20 minutes in a drier, and water repellency was measured by the JIS-S-1092 spray method.
주) 발수도Note) water repellency
- 100 : 표면에 부착된 습기가 없는 것.-100: no moisture attached to the surface.
- 90 : 표면에 부착된 습기가 약간 있는 것.-90: Some moisture on the surface.
- 80 : 표면에 물방울 떨어지는 부분이 젖은 것-80: The part of water drop falling on the surface is wet
- 70 : 표면에 상당한 부분이 젖은 것-70: a considerable portion of the surface is wet
본 발명에 따른 불화 폴리 실록산 다기능성 코팅제 조성물은 내화학성, 내마모성, 분산성, 내수성, 내유성 및 내후성이 우수한 투명한 조성물로 금속, 합금, 유리, 지류, 세라믹, 플라스틱 및 기타 다양한 기재에 사용되어 코팅된 기재의 특성을 획기적으로 향상시킬 수 있다. 본 발명의 코팅제 조성물은 다양한 분야에서 다양한 용도로 사용될 수 있으며, 특히 광학소재, 자동차 유리, 페인트 소광제, 각종 전기 및 건축 재료 등의 기능을 향상시키기 위한 코팅제로 폭넓게 응용될 수 있고, 투명하고 경화속도가 빠르므로 미관을 필요로 하는 기재와 실내 건축자재 등에 응용될 수 있다.The fluorinated polysiloxane multifunctional coating composition according to the present invention is a transparent composition having excellent chemical resistance, abrasion resistance, dispersibility, water resistance, oil resistance and weather resistance, and is used for coating on metals, alloys, glass, paper, ceramics, plastics and various other substrates. The properties of the substrate can be improved significantly. The coating composition of the present invention can be used for various purposes in various fields, and in particular, it can be widely applied as a coating agent for improving the functions of optical materials, automotive glass, paint matting agents, various electrical and building materials, and the like. Because of its high speed, it can be applied to materials that require aesthetics and interior building materials.
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KR101054843B1 (en) | 2009-04-08 | 2011-08-05 | 부산대학교 산학협력단 | Ultra small coating material and ultra small coating film formation method |
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KR101003266B1 (en) | 2008-09-30 | 2010-12-21 | 재단법인대구경북디자인센터 | Process Of Water-Repellent Treatment for Polyester Fabrics Using TiO2-Sol |
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