WO2017039118A1 - Solution de revêtement pour traitement de surface présentant une stabilité de coefficient de friction, de résistance à la corrosion, et de propriété écologique, et procédé de préparation de couche de revêtement à l'aide de ladite solution de revêtement - Google Patents

Solution de revêtement pour traitement de surface présentant une stabilité de coefficient de friction, de résistance à la corrosion, et de propriété écologique, et procédé de préparation de couche de revêtement à l'aide de ladite solution de revêtement Download PDF

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WO2017039118A1
WO2017039118A1 PCT/KR2016/005372 KR2016005372W WO2017039118A1 WO 2017039118 A1 WO2017039118 A1 WO 2017039118A1 KR 2016005372 W KR2016005372 W KR 2016005372W WO 2017039118 A1 WO2017039118 A1 WO 2017039118A1
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coating solution
weight
surface treatment
corrosion resistance
friction coefficient
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PCT/KR2016/005372
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English (en)
Korean (ko)
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이주형
이주영
황준
이용규
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주식회사 제이엘서피스
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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
    • 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
    • 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

Definitions

  • the present invention relates to a friction coefficient stability, corrosion resistance and environmentally friendly surface treatment coating solution, a method for producing a coating layer using the coating solution.
  • the most commonly used metals in the current industrial field are steel structures containing iron (Fe), and most of them are exposed to natural environment (snow, rain, salt, temperature, humidity, oxygen, etc.), and thus prevent rust surface to enhance corrosion resistance and durability. It is common to do the treatment.
  • Corrosion of structures containing iron meets oxygen and moisture in the air to form Fe (OH) 3 and Fe 2 O 3 , which are most often accelerated by other chemicals in the air, soot, salt in seawater, and acid rain. .
  • FIG. 1 shows a photo schematically showing a car and a cancer cell in which corrosion has occurred.
  • Figure 2 shows a photograph of a hot-dip galvanized bolt is a conventional rust generated.
  • corrosion has similarities with cancer cells in that it can destroy everything at the moment of occurrence.
  • Zinc plating As a representative surface plating method to block the external environment causing such corrosion, zinc plating is used to protect metals from corrosion in a wide range of fields. Zinc plating also has sacrificial anode protection because it has a greater tendency to ionize than iron in a cathodic manner.
  • the methods mainly used for post-treatment include chromate and phosphate treatment.
  • the chromate process uses hexavalent chromium (Cr 6 + ), which requires an alternative to the hexavalent chromium due to deadly toxicity and environmental pollution.
  • the European Union launched the End of Life Vehicle Directive (ELV), which proposed limiting toxic heavy metals (such as Pb, Cd, Hg and hexavalent Cr) in the coating of automotive components.
  • EUV End of Life Vehicle Directive
  • the European Union also issued a directive to prohibit the use of certain hazardous substances in all electronic equipment imported into the country on 1 July 2006.
  • FIG. 3 is a photograph of a finger addicted to heavy metal hexavalent chromium
  • FIG. 4 is a photograph of a patient in which cancer is generated by a carcinogen.
  • Korean Patent Laid-Open Publication No. 10-2015-0075001 (Surface treatment solution having excellent corrosion resistance and blackening resistance and a method of manufacturing a surface-treated Zn-Al-Mg alloy plated steel sheet using the same) ) Is a method for producing a surface treatment solution for providing excellent corrosion resistance to a zinc-aluminum-magnesium alloy steel sheet, and it has excellent corrosion resistance and has improved blackening resistance in which the surface of the film does not turn black even under high temperature and high humidity. Since chromium is used, it is not preferable because it is in a direction that is not in line with global environmental regulations.
  • the Republic of Korea Patent No. 1209079 (eco-friendly water-soluble anti-corrosive coating composition and environmentally friendly anti-corrosion coating method of steel structures using the same) relates to an eco-friendly water-soluble anti-corrosive coating composition and coating method to the steel structure environmentally friendly corrosion resistance, chemical resistance, durability It relates to a water-soluble paint that can give.
  • the use of a mixture of water-soluble epoxy resins provided excellent corrosion resistance, but the coating film is very thick (50-75 ⁇ m), so its use is limited and the field of application is limited.
  • the productivity is very low because curing takes longer than 8 hours after coating.
  • the Republic of Korea Patent No. 0579989 (torque stabilizer) relates to a stabilizer that provides a stable fastening force when assembling bolts, nuts, screws by mixing a modified alkyd resin, a water dispersible surfactant and an aqueous pigment in a certain component ratio.
  • the variation of the friction coefficient due to the stabilizer was 14%. Since this is a very high deviation, it is unsuitable for process application, and thus, in the present invention, it was intended to develop a stabilizer at a level satisfying the 1-2%.
  • Patent Document 1 Republic of Korea Patent Publication No. 2015-0075001
  • Patent Document 2 Republic of Korea Registered Patent No. 1209079
  • Patent Document 3 Republic of Korea Registered Patent No. 0579989
  • the present invention has been made to solve the conventional problems as described above, according to an embodiment of the present invention, the object of the present invention is to provide a high stability and high corrosion resistance environmentally friendly surface treatment solution of the friction coefficient.
  • a first object of the present invention is a friction coefficient stability, corrosion resistance and environmentally-friendly, characterized in that in the surface treatment coating solution, (3-aminopropyl) preethoxysilane, dipropylene glycol, stearic acid and tetraethoxysilane It can be achieved as a surface treatment coating solution.
  • the first object 5 to 17% by weight of (3-aminopropyl) preethoxysilane, 50 to 75% by weight of dipropylene glycol, 1 to 6% by weight of stearic acid and 8 to 15% by weight of tetraethoxysilane It may be characterized by including.
  • 13 to 17% by weight of (3-aminopropyl) preethoxysilane preferably, 65 to 75% by weight of dipropylene glycol, 4 to 6% by weight of stearic acid and 13 to 13% of tetraethoxysilane It may be characterized by including 15% by weight.
  • a second object of the present invention in the surface treatment coating solution, comprises (3-aminopropyl) preethoxysilane, dipropylene glycol, stearic acid, tetraethoxysilane, tetrabutyl titanate and tetraisopropyl titanate It can be achieved as a friction coefficient stability, corrosion resistance and environmentally friendly surface treatment coating solution characterized in that.
  • the second object 5 to 17% by weight of (3-aminopropyl) preethoxysilane, 50 to 75% by weight of dipropylene glycol, 1 to 6% by weight of stearic acid, 8 to 15% by weight of tetraethoxysilane, It may be characterized in that it comprises 0.5 to 1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • a third object of the present invention in the method for producing a coating layer, the step of washing the surface of the metal base material to be subjected to the surface treatment to produce a coating layer; Immersing the base material in a container in which the coating solution according to claim 4 is stored; Removing the base material from the container and dehydrating the coating solution to uniformly apply the coating solution; And dry-curing the base material to form a coating layer. It can be achieved as a method of manufacturing a coating layer using a frictional coefficient stability, corrosion resistance, and environmentally friendly surface treatment coating solution, which comprises a.
  • the washing may include removing foreign substances on the surface of the base material by acetone ultrasonic cleaning.
  • the immersing step may be characterized in that the base material is immersed in the coating solution for 3 to 5 seconds by dipping (Dipping) method.
  • the applying step it may be characterized in that the dewatering means for 10 to 20 seconds by rotating to 200 ⁇ 1000rpm.
  • the step of forming the coating layer it may be characterized in that the dry curing at 100 ⁇ 130 °C for 15 to 35 minutes.
  • the step of forming the coating layer after the step of forming the coating layer, it may be characterized in that it further comprises the step of cooling to a temperature of less than 60 °C.
  • the coating solution is (3-aminopropyl) preethoxysilane 5 to 17% by weight, dipropylene glycol 50 to 75% by weight, stearic acid 1 to 6% by weight, tetraethoxysilane 8 15 wt%, tetrabutyl titanate 0.5-1 wt% and tetraisopropyl titanate greater than 0 wt% to 0.5 wt%.
  • the coating solution is 13 to 17% by weight of (3-aminopropyl) preethoxysilane, 65 to 75% by weight of dipropylene glycol, 4 to 6% by weight of stearic acid and tetra 13 to 15% by weight of oxysilane, 0.5 to 1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • a fourth object of the present invention in the coating layer using the surface treatment coating solution, the coating layer using the friction coefficient stability, corrosion resistance and environmentally friendly surface treatment coating solution, characterized in that formed by the manufacturing method according to the above-mentioned third object Can be achieved as
  • the method for producing a coating layer using the coating solution has the effect of high stability and high corrosion resistance and environmentally friendly friction coefficient.
  • FIG. 1 is a photo schematically showing a car and a cancer cell in which corrosion has occurred
  • Figure 2 is a photograph of a hot dip galvanized bolt is conventional rust generated
  • Figure 6 is a block diagram of a coating layer manufacturing method using an environmentally friendly coating solution according to an embodiment of the present invention
  • Example 10 is an E-SEM analysis photograph of a zinc-based surface treatment bolt surface treated with a coating solution according to Example 5 of the present invention.
  • Example 11 is an EDX elemental analysis result table of a zinc-based surface treated bolt surface treated with a conventional hot dip galvanized bolt and a coating solution according to Example 5 of the present invention
  • Figure 13 is a photograph after 1900 hours of salt spray test of zinc-based surface treatment bolt surface treatment with a coating solution according to Example 5 of the present invention
  • Figure 14 shows a friction coefficient analysis result table of the zinc-based surface treatment bolt surface-treated with the coating solution according to an embodiment of the present invention.
  • Embodiments described herein will be described with reference to cross-sectional and / or plan views, which are ideal exemplary views of the present invention.
  • the thicknesses of films and regions are exaggerated for effective explanation of technical content. Therefore, the shape of the exemplary diagram may be modified by manufacturing techniques and / or tolerances. Accordingly, the embodiments of the present invention are not limited to the specific forms shown, but also include changes in forms generated according to manufacturing processes.
  • the etched regions shown at right angles may be rounded or have a predetermined curvature.
  • the regions illustrated in the figures have properties, and the shape of the regions illustrated in the figures is intended to illustrate a particular form of region of the device and is not intended to limit the scope of the invention.
  • terms such as first and second are used to describe various components in various embodiments of the present specification, these components should not be limited by such terms. These terms are only used to distinguish one component from another.
  • the embodiments described and illustrated herein also include complementary embodiments thereof.
  • Surface treatment coating solution including (3-aminopropyl) preethoxysilane, dipropylene glycol, stearic acid, tetraethoxysilane, tetrabutyl titanate and tetraisopropyl titanate, friction Coefficient stability, corrosion resistance and environmental friendliness are all satisfied.
  • the coefficient of friction stability, corrosion resistance and environmentally friendly surface treatment coating solution is (3-aminopropyl) preethoxysilane 5 to 17% by weight, dipropylene glycol 50 to 75% by weight, stearic acid 1 to 6% by weight, tetraethoxy 8-15 weight percent silane, 0.5-1 weight percent tetrabutyl titanate and 0-0.5 weight percent tetraisopropyl titanate.
  • Figure 5 shows the ratio table of the environmentally friendly coating solution according to an embodiment of the present invention.
  • Example 1 of the present invention 5 to 7% by weight of (3-aminopropyl) preethoxysilane, 50 to 55% by weight of dipropylene glycol, 1-2% by weight of stearic acid and tetra It can be seen that it is composed by mixing 8 to 9% by weight of oxysilane, 0.5 to 1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • Example 2 of the present invention 7 to 10% by weight of (3-aminopropyl) preethoxysilane, 55 to 60% by weight of dipropylene glycol, 2-3% by weight of stearic acid and It can be seen that 9 to 10 wt% of tetraethoxysilane, 0.5 to 1 wt% of tetrabutyl titanate, and 0 to 0.5 wt% of tetraisopropyl titanate are mixed.
  • Example 3 of the present invention 10 to 13% by weight (3-aminopropyl) preethoxysilane, 60 to 65% by weight dipropylene glycol, 3 to 4% by weight stearic acid and tetra It can be seen that it is composed by mixing 9 to 10% by weight of oxysilane, 0.5 to 1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • Example 4 of the present invention 13 to 15% by weight of (3-aminopropyl) preethoxysilane, 65 to 70% by weight of dipropylene glycol, 4 to 5% by weight of stearic acid and It can be seen that 11 to 13% by weight of tetraethoxysilane, 0.5 to 1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • Example 5 of the present invention 15 to 17% by weight of (3-aminopropyl) preethoxysilane, 70 to 75% by weight of dipropylene glycol, 5 to 6% by weight of stearic acid and It can be seen that 13-15% by weight of tetraethoxysilane, 0.5-1% by weight of tetrabutyl titanate and 0 to 0.5% by weight of tetraisopropyl titanate.
  • Eco-friendly metal surface coating solution according to an embodiment of the present invention to propose a direction to improve the environmental and economic problems as a technology to replace the chromate, etc. to prepare for the environmental problems of the recent RoHS (hazardous substance use regulation) do.
  • the eco-friendly metal surface coating solution of the present invention mainly consists of silane-based compounds having a structure of R'Si (OR) 3 and has excellent corrosion resistance by forming a film on various metals such as magnesium alloy, steel, and metal surface-treated with zinc. Among them, metals surfaced with zinc are most suitable.
  • the performance of the eco-friendly metal surface coating solution according to an embodiment of the present invention is to form a self-assembled film by forming a Si-OM bond and Si-O-Si as a film forming mechanism of the silane compound on the metal surface of the external environment Provides excellent corrosion resistance by protecting the base material from corrosion factors.
  • (3-aminopropyl) triethoxysilane plays the most preferred role to provide a strong adhesion between the coating solution and the metal base material. And tetraethoxysilane is most preferable in order to form a stable film.
  • tetrabutyl titanate, tetraisopropyl titanate, and stearic acid were mixed as the corrosion resistance increasing additive, and as a solvent, a combination of dipropylene glycol showed the best corrosion resistance performance.
  • This coating layer is to use the above-mentioned friction coefficient stability, corrosion resistance and environmentally friendly surface treatment coating solution.
  • Figure 6 shows a block diagram of a coating layer manufacturing method using an environmentally friendly metal surface coating solution according to an embodiment of the present invention.
  • Figure 7 shows a flow chart of a coating layer manufacturing method using an environmentally friendly metal surface coating solution according to an embodiment of the present invention.
  • the coating layer manufacturing method according to an embodiment of the present invention, as shown in Figure 6 and 7, washing the surface of the metal base material to be subjected to the surface treatment to generate the coating layer (S1) and the washed base material
  • the step (S2) and the step of immersing the eco-friendly metal surface coating solution according to the embodiment of the present invention stored in the container and the dehydration by removing the base material from the container (S3) and the base material uniformly It can be seen that it comprises the step (S4) to form a coating layer by dry curing.
  • the coating solution according to an embodiment of the present invention for producing a coating layer is 5 to 17% by weight of (3-aminopropyl) preethoxysilane, 50 to 75% by weight of dipropylene glycol, 1 to 1 part of stearic acid. 6% by weight, 8-15% by weight of tetraethoxysilane, 0.5-1% by weight of tetrabutyl titanate and 0-0.5% by weight of tetraisopropyl titanate.
  • the coating solution according to an embodiment of the present invention (3-aminopropyl) preethoxysilane 13-17 wt%, dipropylene glycol 65-75 wt%, stearic acid 4-6 wt% and tetraethoxy 13-15 weight percent silane, 0.5-1 weight percent tetrabutyl titanate and 0-0.5 weight percent tetraisopropyl titanate.
  • the washing step as a pretreatment process, to perform acetone ultrasonic cleaning for about 1 minute to remove foreign substances on the surface of the galvanized base material.
  • the base material in order to coat the coating solution on the washed base material, the base material is immersed in the coating solution for 3 to 5 seconds by a dipping method.
  • the dehydration means is rotated at an rpm suitable for each base material between 200 and 1000 rpm to dehydrate for about 15 seconds to be evenly applied.
  • the coating layer after coating the coating solution, it is dried and cured at about 100 ⁇ 130 °C for about 15 to 35 minutes to form a coating layer.
  • the coating process according to the embodiment of the present invention has an advantage of entering the factory site and worker efficiency because it can be easily and easily carried out for mass production application.
  • the dry cured finished product is cooled to a temperature below 60 ° C.
  • Stearic acid and ethanol were purchased from Samjeon Pure Chemical Co., Ltd., (3-aminopropyl) triethoxysilane and tetraethoxysilane were obtained from isomeric materials.
  • Propylene glycol was purchased from SKC, tetrabutyl titanate was purchased from Sigma Aldrich, and tetraisopropyl titanate was purchased from UCP Corporation.
  • salt spray test analysis was carried out in accordance with KS D 9502 in a standardized manner, this specification is sprayed 5% NaCl solution at 35 °C, the temperature in the chamber is maintained at 35 °C corrosion resistance experiments. After 1,000 hours of salt spray test, the corrosion resistance performance was evaluated by the ratio of hematite generation area.
  • Figure 8 shows the adhesion and corrosion resistance test results of the coating layer prepared by the coating solution prepared according to an embodiment of the present invention.
  • the adhesion performance of the coating solution _1 to the coating solution _5 according to Example 1 according to the coating solution composition range condition according to the embodiment of the present invention was applied to the coating solution _1 coating. Except for showing excellent adhesion performance. Among them, it was confirmed that the adhesion performance of the coating solution _4 and the coating solution _5 had the most excellent quality.
  • coating solutions 1 to 3 according to Examples 1 to 3 showed a red blue redness of less than 5% of the total area after the salt spray test 1,000 hours
  • Coating solution _4 and coating solution _5 according to Examples 4 to 5 showed a red blue red color development rate of less than 0% of the total area it was confirmed that it has excellent corrosion resistance.
  • the experimental data of the present invention observed the morphological changes of the coating surface.
  • the morphological change of the surface after the surface treatment with an environmentally friendly coating solution according to Examples 1 to 5 of the present invention was precisely analyzed by E-SEM.
  • FIG. 9 shows an E-SEM analysis photograph of a conventional hot dip galvanized bolt.
  • 10 shows E-SEM analysis photographs of zinc-based surface treatment bolts surface-treated with a coating solution (coating solution_5) according to Example 5 of the present invention.
  • the surface image was confirmed at a magnification of 1,000 times, and it was confirmed that a dense and uniform coating surface was formed in the product treated with the coating solution_5 compared with before coating.
  • the experimental data of the present invention analyzed the components of the coating surface. After the surface treatment with an environmentally friendly coating solution according to an embodiment of the present invention, the components were analyzed through EDX to confirm the components of the surface of the coating layer.
  • 11 is a table showing EDX elemental analysis results of zinc-based surface treatment bolts surface-treated with a conventional hot dip galvanized bolt and a coating solution_5 according to Example 5 of the present invention.
  • FIG. 12 shows a photograph after 1900 hours of a salt spray test of a conventional hot dip galvanized bolt.
  • Figure 13 shows a photograph after a salt spray test 1900 hours of zinc-based surface treatment bolts surface-treated with a coating solution according to Example 5 of the present invention.
  • Figure 14 shows a friction coefficient analysis result table of the zinc-based surface treatment bolt surface-treated with the coating solution according to an embodiment of the present invention.
  • the above-described apparatus and method may not be limitedly applied to the configuration and method of the above-described embodiments, but the embodiments may be selectively combined in whole or in part in each of the embodiments so that various modifications may be made. It may be configured.

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Abstract

La présente invention concerne une solution de revêtement pour traitement de surface présentant une stabilité de coefficient de friction, de résistance à la corrosion, et de propriété écologique, et un procédé de préparation de couche de revêtement à l'aide de ladite solution de revêtement. Plus particulièrement, une solution de revêtement selon un mode de réalisation de la présente invention contient de 13 à 17 % en poids de (3-aminopropyl)triéthoxysilane, de 65 à 75 % en poids de dipropylène glycol, de 4 à 6 % en poids d'acide stéarique, de 13 à 15 % en poids de tétraéthoxysilane, de 0,5 à 1 % en poids de titanate de tétrabutyle, et une proportion supérieure à 0 % en poids et jusqu'à 0,5 % en poids de titanate de tétraisopropyle, et a pour effet de satisfaire simultanément à la stabilité du coefficient de frottement, de la résistance à la corrosion, et d'une propriété écologique.
PCT/KR2016/005372 2015-08-28 2016-05-20 Solution de revêtement pour traitement de surface présentant une stabilité de coefficient de friction, de résistance à la corrosion, et de propriété écologique, et procédé de préparation de couche de revêtement à l'aide de ladite solution de revêtement WO2017039118A1 (fr)

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KR1020150121803A KR101708794B1 (ko) 2015-08-28 2015-08-28 마찰계수 안정성, 내식성 및 친환경 표면처리 코팅용액, 그 코팅용액을 이용한 코팅층의 제조방법
KR10-2015-0121803 2015-08-28

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KR20100076529A (ko) * 2008-12-26 2010-07-06 주식회사 포스코 금속표면처리용 조성물 및 이의 제조방법

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CN110804396A (zh) * 2019-12-09 2020-02-18 万华化学集团股份有限公司 一种防腐蚀涂料及其制备方法与应用

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