WO2014027825A1 - Composition de solution de revêtement extrêmement hydrofuge et procédé pour la préparation d'une composition de revêtement - Google Patents

Composition de solution de revêtement extrêmement hydrofuge et procédé pour la préparation d'une composition de revêtement Download PDF

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Publication number
WO2014027825A1
WO2014027825A1 PCT/KR2013/007289 KR2013007289W WO2014027825A1 WO 2014027825 A1 WO2014027825 A1 WO 2014027825A1 KR 2013007289 W KR2013007289 W KR 2013007289W WO 2014027825 A1 WO2014027825 A1 WO 2014027825A1
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Prior art keywords
silane
coating
coating solution
composition
weight
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PCT/KR2013/007289
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English (en)
Korean (ko)
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박상권
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동국대학교 산학협력단
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Publication of WO2014027825A1 publication Critical patent/WO2014027825A1/fr

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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
    • C09D183/02—Polysilicates
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662—Synthetic film-forming substance
    • C09D5/1675—Polyorganosiloxane-containing compositions
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1681—Antifouling coatings characterised by surface structure, e.g. for roughness effect giving superhydrophobic coatings or Lotus effect
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials 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

Definitions

  • the present invention relates to a coating solution composition and a method for preparing the coating composition that can be applied to the window.
  • the lotus leaf effect is an effect that keeps the insect wings such as leaves and butterflies of plants, such as lotus leaf and rice, at all times by self-cleaning ability.
  • the secret of the lotus leaf effect is that in 1975, Professor Wilhelm Barthlot, a botanist at the University of Bonn, Germany, observed the lotus leaf under a high-magnification microscope, indicating that micrometer-sized protrusions were formed on the surface. They then found cilia of nanometer size (nm: 1 billionth of a meter) on the surface of the projections. Because of this surface structure, the lotus leaf rolls down without attaching water droplets, and thus has a self-cleaning ability to automatically wash down pollutants.
  • Products applying the above-mentioned lotus leaf effect in real life also appear one after another, which is also called super water repellent surface technology, which is a field of wet and surface modification technology, by physically chemically modifying the surface of the solid surface
  • the contact angle is 150 ° or more, the physical phenomenon of the super water-repellent surface for the identification of the phenomena already occurring in the natural world for easy industrial use, analysis of the wet phenomenon and Applied technology.
  • This super water repellency is known to be realized by the microstructure existing on the surface and the low-energy material (wax in the case of lotus leaf) covering the surface, and the smooth surface without the microstructure is a low energy organic material or polymer (fluorine-based or silicone-based resin). Even with coating, the maximum contact angle is limited to about 120 °. Water droplets with high surface tension show very high contact angles by contacting only very limited areas with the projections of superhydrophobic surfaces with low surface energy, resulting in self-cleaning functions as they drop with contaminants attached to water droplets.
  • the present inventors have developed a highly transparent self-cleaning functional coating material which can be used in windows of construction and automobiles, and further applicable to solar cell protective glass or outdoor display outermost glass.
  • the present invention is to provide a coating solution composition and a method for preparing the coating composition to maximize transparency and super water repellency.
  • the present invention relates to a coating solution composition
  • a coating solution composition comprising a silica precursor, a neutral catalyst, an alcohol, and a non-fluorine silane-based organic material.
  • the present invention comprises the steps of (a) forming a silica nanostructure on a substrate using a silica precursor, a neutral catalyst, alcohol and water; And (b) after the step (a), using a non-fluorine silane-based organic coating the silane-based organic; relates to a method for producing a coating composition comprising a.
  • the coating composition of the present invention is excellent in transparency and can implement the self-cleaning functionality, it can be applied to architectural and automotive windows. When applied to architectural exterior and interior materials of glass and ceramic as well as building windows, it can contribute to the creation of a green environment by realizing self-cleaning functionality, and ultimately contribute to the reduction of carbon dioxide emissions.
  • 1 is a cross-sectional view of the coating structure produced in the present invention.
  • Example 3 is a light transmission diagram for Example 8 and Comparative Example 2.
  • Example 5 is a contact angle results (25 °C) according to the coating solution composition for Example 9 It is a graph.
  • FIG. 6 is a graph of contact angle results according to temperature for Example 10.
  • the present invention relates to a coating solution composition
  • a coating solution composition comprising a silica precursor, a neutral catalyst, an alcohol, and a non-fluorine silane-based organic material.
  • the total amount of the coating solution composition may include 10 to 40 parts by weight of silica precursor, 0.0001 to 0.02 parts by weight of neutral catalyst, 35 to 88 parts by weight of alcohol, and 0.13 to 2.6 parts by weight of non-fluorine silane-based organic material.
  • silica precursor 0.0001 to 0.02 parts by weight of neutral catalyst
  • 35 to 88 parts by weight of alcohol 35 to 88 parts by weight of alcohol
  • 0.13 to 2.6 parts by weight of non-fluorine silane-based organic material When it is included in the weight ratio by the sol-gel reaction of the substrate with the coating solution composition of the present invention, by treating with a non-fluorine silane-based organic material it can be obtained a coating composition having high transparency and super water-repellent properties.
  • the silica precursor may be, but not limited to, silicon alkoxide-based, and more specifically, tetramethyl orthosilicate, tetraethyl orthosilicate (TEOS), tetrapropoxy silane, tetraisooxy It may be tetraisopropoxy silane.
  • TEOS tetramethyl orthosilicate
  • TEOS tetraethyl orthosilicate
  • tetrapropoxy silane tetraisooxy It may be tetraisopropoxy silane.
  • the neutral catalyst may be, but is not limited to, ammonium fluoride (NH 4 F).
  • the non-fluorine silane-based organic material is not limited thereto, but may be a chlorotrialkyl silane-based organic material such as chlorotrimethyl silane, or an alkyltrichloro silane such as octadecyltrichlorosilane. ) May be an organic material.
  • the alcohol may be, but is not limited to, methanol, ethanol or isopropanol.
  • the invention also relates to a process for the preparation of the coating composition. More specifically (a) forming a silica nanostructure on the substrate using a silica precursor, a neutral catalyst, alcohol and water; And (b) after the step (a), using a non-fluorine silane-based organic coating the silane-based organic; relates to a method for producing a coating composition comprising a.
  • the substrate is not limited thereto, but may be a glass substrate, the impurities may be removed so that the nanostructure is uniformly generated on the glass surface.
  • the impurities may be removed so that the nanostructure is uniformly generated on the glass surface.
  • to remove impurities on the glass surface by treating the hydrogen peroxide and sulfuric acid solution to remove the organic material adsorbed / adhered to the glass surface.
  • step (a) is to form a silica nanostructure on the glass substrate by a sol-gel (sol-gel) method in order to implement super water-repellent properties while maintaining high transparency, more specifically, silica precursor, water
  • a sol-gel (sol-gel) method in order to implement super water-repellent properties while maintaining high transparency
  • silica precursor, water A transparent and uniform coating film can be obtained by preparing an alcohol solution in which a catalyst is dissolved and immersing the glass substrate in the solution to cause a sol-gel reaction (hydrolysis reaction and condensation reaction).
  • the reaction temperature may be 20 to 50 ° C and 25 ° C.
  • the contact angle according to the reaction time is changed.
  • the reaction time can be reacted for 1 to 50 hours, 25 hours.
  • the silica precursor may be, but not limited to, silicon alkoxide-based, and more specifically, tetramethyl orthosilicate, tetraethyl orthosilicate (TEOS), tetrapropoxy silane, tetraisooxy It may be tetraisopropoxy silane.
  • TEOS tetramethyl orthosilicate
  • TEOS tetraethyl orthosilicate
  • tetrapropoxy silane tetraisooxy It may be tetraisopropoxy silane.
  • the neutral catalyst may be, but is not limited to, ammonium fluoride (NH 4 F).
  • the alcohol may be, but is not limited to, methanol, ethanol or isopropanol.
  • the glass substrate on which the silica nanostructure coating film is formed may be taken out at a speed of 3 to 10 mm / min with a dip coater, and then dried.
  • the surface may be modified by using a non-fluorine silane-based organic material on the surface of the glass substrate on which the silica nanostructure is formed.
  • a non-fluorine silane-based organic material on the surface of the glass substrate on which the silica nanostructure is formed.
  • the non-fluorine silane-based organic material is not limited thereto, but may be a chlorotrialkyl silane-based organic material such as chlorotrimethyl silane, or an alkyltrichloro silane such as octadecyltrichlorosilane. ) May be an organic material.
  • the glass substrate coated with silica nanostructures may be dipped in a solvent in which a non-fluorine silane-based organic material is dissolved, and then coated for 20 to 100 ° C., 50 ° C., 0.5 to 5 hours, and 1 hour.
  • a glass slide of 1 mm thickness (Paul Marienfeld GmbH, Germany) was used.
  • the glass was immersed in a solution of hydrogen peroxide and sulfuric acid in a volume ratio of 1: 3 for 12 hours or more to remove impurities on the surface.
  • the solution was washed with distilled water and then dried at 105 ° C. for 1 hour.
  • methanol anhydrous grade in which tetraethyl orthosilicate (TEOS, reagent grade, Aldrich), water and ammonium fluoride (NH 4 F, reagent grade, Aldrich) catalyst are dissolved Aldrich) solution was used.
  • TEOS tetraethyl orthosilicate
  • NH 4 F ammonium fluoride
  • the mixed coating solution was stirred at room temperature for about 30 minutes.
  • the glass substrate coated with the silica nanostructures was immersed in a hexane solution in which trimethylchlorosilane ((CH 3 ) 3 SiCl) was dissolved in 0.01 parts by weight, reacted at 50 ° C for 1 hour, and then cured at 125 ° C for 1 hour.
  • the system organic coating was completed.
  • the coating solution composition of step 2) was prepared by using a concentration of 19 parts by weight of TEOS, 10 parts by weight of water, and 0.003 parts by weight of ammonium fluoride.
  • step 3 the coating time of step 3 was 10 hours.
  • step 2 the coating solution of step 2 was used in various compositions as follows (see Fig. 5).
  • A 26 parts by weight of TEOS, 14 parts by weight of water, 0.005 parts by weight of ammonium fluoride
  • step 2 Proceed in the same manner as in Example 1, but the temperature of step 2) was maintained at 40 °C, 45 °C or 50 °C (see Figure 6).
  • Example 1 a glass slide glass substrate with only coarse step 1) was used.
  • Example 8 a low iron glass substrate was used which passed only step 1).
  • the light transmittance of the coating formed on the glass substrate was measured using a UV-Vis spectrometer (Lambda 35, Perkin Elmer), and the light transmittances of Example 8 and Comparative Example 2 are shown in FIG.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Example 6
  • Example 7 Example 8
  • Example 9 Example 10
  • Wet dildo143 115 135 142 53 93 154 130 See Figure 5 See Figure 6 Excellent a Excellent a Very bad b Bad c Excellent a Excellent a Very bad b Excellent d Good or excellent a Good or excellent a
  • glass substrate / 2 silica nanostructure / 3: silane-based organic material

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Combustion & Propulsion (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention porte sur une composition de solution de revêtement hautement transparent et extrêmement hydrofuge qui peut être appliquée sur une fenêtre et sur un procédé pour la préparation de la composition de revêtement. Puisque la composition de revêtement de la présente invention a une excellente transparence et peut assurer une fonction d'autonettoyage, la présente invention peut être appliquée à des fenêtres à des fins de construction et pour des automobiles. Dans le cas où la présente invention est appliquée à des matériaux de construction d'extérieur et d'intérieur en verre et en céramique, ainsi qu'à des fenêtres à des fins de construction, la présente invention peut contribuer à un environnement vert en assurant une fonction autonettoyante et elle peut en fin de compte aussi jouer un rôle important dans la réduction des émissions de dioxyde de carbone.
PCT/KR2013/007289 2012-08-13 2013-08-13 Composition de solution de revêtement extrêmement hydrofuge et procédé pour la préparation d'une composition de revêtement WO2014027825A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020120088146A KR101401754B1 (ko) 2012-08-13 2012-08-13 초발수성 코팅용액 조성물 및 코팅 조성물의 제조방법
KR10-2012-0088146 2012-08-13

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WO2014027825A1 true WO2014027825A1 (fr) 2014-02-20

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021067042A1 (fr) * 2019-09-30 2021-04-08 Saudi Arabian Oil Company Procédés de réduction de condensation

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KR102089504B1 (ko) * 2018-07-03 2020-03-16 주식회사 쓰리에스테크 밀폐성이 향상된 포장용 박스
KR102097481B1 (ko) * 2018-07-18 2020-04-06 주식회사 쓰리에스테크 포장용 박스
KR102019315B1 (ko) * 2018-12-14 2019-09-06 고려대학교 산학협력단 초발수 특성을 가지는 표면 형성방법
KR102633015B1 (ko) * 2021-05-13 2024-02-01 경상국립대학교산학협력단 초발수성 코팅의 제조 방법
KR20230056437A (ko) * 2021-10-20 2023-04-27 한국기계연구원 발수제 조성물
KR102658521B1 (ko) 2021-11-12 2024-04-18 삼화페인트공업주식회사 태양광 패널 자가세정 실릴화 폴리우레탄, 이의 제조방법 및 이를 포함하는 태양광 패널 자가세정 제품
KR20230092082A (ko) 2021-12-16 2023-06-26 주식회사 지디원 자동차용 초발수 코팅제

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KR20060011218A (ko) * 2004-07-29 2006-02-03 엘지전자 주식회사 초발수성 코팅층 형성을 위한 코팅용 조성물, 이의 제조방법 및 이를 이용한 코팅 방법
KR20110118475A (ko) * 2010-04-23 2011-10-31 삼성전자주식회사 초발수 코팅 조성물, 상기 조성물의 경화물을 포함하는 초발수 코팅층, 및 상기 초발수 코팅층을 포함하는 열교환기
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KR20060011218A (ko) * 2004-07-29 2006-02-03 엘지전자 주식회사 초발수성 코팅층 형성을 위한 코팅용 조성물, 이의 제조방법 및 이를 이용한 코팅 방법
KR20110118475A (ko) * 2010-04-23 2011-10-31 삼성전자주식회사 초발수 코팅 조성물, 상기 조성물의 경화물을 포함하는 초발수 코팅층, 및 상기 초발수 코팅층을 포함하는 열교환기
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WO2021067042A1 (fr) * 2019-09-30 2021-04-08 Saudi Arabian Oil Company Procédés de réduction de condensation

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