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WO1993015155A1 - Composition de revetement a auto-depot - Google Patents

Composition de revetement a auto-depot Download PDF

Info

Publication number
WO1993015155A1
WO1993015155A1 PCT/US1993/000138 US9300138W WO9315155A1 WO 1993015155 A1 WO1993015155 A1 WO 1993015155A1 US 9300138 W US9300138 W US 9300138W WO 9315155 A1 WO9315155 A1 WO 9315155A1
Authority
WO
WIPO (PCT)
Prior art keywords
ion
grams
liter
fluoride ion
coating composition
Prior art date
Application number
PCT/US1993/000138
Other languages
English (en)
Inventor
Takumi Honda
Kazuhisa Naito
Mitsuyuki Koga
Original Assignee
Henkel Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel Corporation filed Critical Henkel Corporation
Priority to US08/256,913 priority Critical patent/US5510410A/en
Publication of WO1993015155A1 publication Critical patent/WO1993015155A1/fr

Links

Classifications

    • 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
    • C09D5/088—Autophoretic paints
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
    • C23C22/44—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides

Definitions

  • the present invention relates to an aqueous auto ⁇ deposition coating composition in the form of an acidic coating composition (pH approximately 1.6 to 5) that con- tains water-dispersible or water-soluble organic film- forming resin, fluoride ion and/or complex fluoride ion, chromium ion (hexavalent chromium ion or hexavalent chro ⁇ mium ion + trivalent chromium ion) , and tungstate ion and/or olybdate ion.
  • an acidic coating composition pH approximately 1.6 to 5
  • fluoride ion and/or complex fluoride ion chromium ion (hexavalent chromium ion or hexavalent chro ⁇ mium ion + trivalent chromium ion)
  • chromium ion hexavalent chromium ion or hexavalent chro ⁇ mium ion + trivalent chro
  • This aqueous autodeposition coating composition is capable of forming a highly corrosion- resistant, strongly adherent resin film on metal surfaces when brought into contact with the surface of a metal, for example, a ferriferous metal, zinciferous metal, alumini- ferous metal, magnesium-based metal, and so forth.
  • a metal for example, a ferriferous metal, zinciferous metal, alumini- ferous metal, magnesium-based metal, and so forth.
  • Autodeposition coating compositions are acidic coating compositions that contain organic film-forming resin and that can form a resin film on a metal surface when brought into contact with the metal surface. Autodepositing coat- ing compositions are disclosed in, for example,
  • a characteristic feature of the known coating com ⁇ positions is their ability to lay down a resin film upon the immersion of a clean metal surface in the particular coating composition. Moreover, the coating film's thick ⁇ ness and weight increase with immersion time. In the case of these compositions, the chemical activity of the coating composition overlying the metal surface (metal ion eluted from the metal surface by etching induces association of the resin particles with resulting deposition on the metal surface) results in the efficient deposition of a resin film on the metal surface without the application, as in electrodeposition, of an external electrical source.
  • the present invention takes as its object the introduction of a film which has a much better adherence and corrosion resistance than the films formed by prior-art coating compositions, but which is produced without a rinse treatment (for example, with a chromium-containing solu ⁇ tion) prior to film curing.
  • the present invention is an aqueous autodeposition coating composition that has a pH of about 1.6 to about 5.0 and contains
  • a water-dispersible or water-soluble organic film-forming resin at least one of fluoride ions or fluoride ions and complex fluoride ions, (iii) hexavalent chromium ion or hexavalent chromium ion and trivalent chromium ion, and (iv) at least one of tungstate ions and molybdate ions.
  • a highly adherent, strongly corrosion-resistant resin film is formed on the metal surface when the aqueous auto ⁇ deposition coating composition of the present invention is brought into contact with a metal surface, for example, the surface of ferriferous, zinciferous, aluminiferous, or magnesium-based metal.
  • the present invention can provide films with a better adherence and corrosion resistance than the films afforded by prior autodeposition coating compositions precisely since it comprises an acidic coating composition (pH approximately 1.6 to 5) that contains an organic film- forming resin, fluoride ion or fluoride ion and complex fluoride ion, chromium ion with its excellent rust-inhibiting activity for metals, and also tungstate ion and/or molybdate ion.
  • the present invention provides a highly adherent, highly corrosion-resistant film without having to carry out the post-treatments (pre-film-cure rinse treat ⁇ ment, for example, with a chromium-containing solution) that have been required to improve the adherence and cor- rosion resistance of films produced by autodeposition coating compositions.
  • a resin of the type disclosed in Japanese Patent Appli ⁇ cation Laid Open Number Sho 61-168673 is an example of a resin useful as the organic film-forming resin in the present invention.
  • the organic film-forming resin which can be useful in the practice of the present invention can comprise: urethane resins, epoxy resins, polyester resins, and polymer resins composed of one or more monomers selected from methyl acrylate, ethyl acrylate, n-butyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-ethyl- hexyl acrylate, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, 2-hydroxyethyl methacrylate, 2-hy- droxypropyl methacrylate, glycidyl acrylate, glycidyl methacrylate, acrylamide, methacryla ide, acrylonitrile, ethylene, styrene, vinyl chloride, vinylidene chloride, vinyl acetate, acrylic acid, methacrylic acid, and the like.
  • the organic film-forming resin useful in the present invention can be anionic, cationic, nonionic, or amphoteric and is not restricted in this regard.
  • the content of resin solids in the coating composition preferably falls within the range of 5 to 550 g/L and more preferably falls within the range of 50 to 100 g/L.
  • Sources for the fluoride ion and complex fluoride ion used in the invention are, for example, zirconium hydrogen fluoride, titanium hydrogen fluoride, silicon hydrogen fluoride, boron hydrogen fluoride, hydrofluoric acid, and the ammonium, lithium, sodium, and potassium salts of the preceding acids.
  • the content of fluoride and complex fluoride ion in the coating composition preferably falls within the range of 0.1 to 5 g/L as fluorine and more pre ⁇ ferably falls within the range of 0.5 to 3 g/L as fluorine.
  • the pH of the coating composition of the present invention should be maintained within the range of app- roximately 1.6 to 5. Formation of the resin film becomes problematic when the pH is substantially outside this range.
  • the pH of the coating composition may be regulated using one or more acids selected from the following: inorganic acids selected from the acids listed above as sources of fluoride and complex fluoride ion and their salts, as well as nitric acid, phosphoric acid, and boric acid; and organic acids selected from phytic acid and tannic acid.
  • inorganic acids selected from the acids listed above as sources of fluoride and complex fluoride ion and their salts, as well as nitric acid, phosphoric acid, and boric acid
  • organic acids selected from phytic acid and tannic acid.
  • the addition of nitric acid, phosphoric acid, boric acid, phytic acid, or tannic acid has the effect of improving film adherence to the substrate.
  • the hexavalent chromium ion used in the present invention can be supplied to the coating composition as chromic acid or a chromate salt compound.
  • the chromic acid can be supplied as an aqueous solution of chromic anhydride or chromic acid.
  • the chromate salt can be supplied in the form of the ammonium, sodium, barium, potassium, strontium, zinc, etc., salt of chromic acid or dichromic acid.
  • the hexavalent chromium ion passivates metal surfaces and thereby produces an excellent rust-inhibiting activity for metals.
  • a portion of the hexavalent chromium ion is converted to trivalent chromium ion by reduction on the metal surface during the course of film formation (de ⁇ position) or by reduction by the functional groups in the resin when the film is dried by heating.
  • This trivalent chromium ion acts to make the hexavalent chromium ion less soluble in water and also functions as a crosslinker for the resin.
  • the trivalent chromium ion used in the present invention can be supplied by reduction of part of the hexa- valent chromium ion or by the dissolution of a trivalent chromium compound, e.g., chromium hydroxide, chromium car ⁇ bonate, chromium hydroxide, etc. , in an aqueous chromic acid solution. While the hexavalent chromium ion acts to inhibit metal corrosion, it is readily soluble in water and is easily eluted from the film when the film is brought into contact with moisture. This results in a substantial deterioration in the film's rust-inhibiting activity.
  • a trivalent chromium compound e.g., chromium hydroxide, chromium car ⁇ bonate, chromium hydroxide, etc.
  • the trivalent chromium bonds with hexavalent chromium to form a sparingly water-soluble chromium chromate, and this inhibits elution of the hexavalent chromium from the film and thus supports retention of the rust-inhibiting activity.
  • the trivalent chromium also bonds with the functional groups in the resin and thereby functions to substantially raise the molecular weight of the resin and improve the corrosion resistance of the film formed on the metal.
  • the total chromium ion content in the coating composi ⁇ tion should be 0.1 to 20 g/L and preferably is 0.5 to 2 g/L.
  • the hexavalent chromium ion/trivalent chromium ion ratio preferably falls within the range of 0.6 to 5. When the ratio falls substantially outside this range, the hexavalent chromium will again become readily elutable from the film and the stability of the coating composition itself will be impaired.
  • the hexa ⁇ valent chromium and/or trivalent chromium are taken into the resin film simultaneously with formation of the resin film.
  • a critical feature of the present invention is the additional presence of tungstate ion and/or molybdate ion in the coating composition that contains organic film- forming resin, fluoride or fluoride ion and complex fluoride ion, and chromium ion (hexavalent chromium ion or hexavalent chromium ion plus trivalent chromium ion) .
  • the tungstate ion and/or molybdate ion present in the aqueous coating composition of the pre ⁇ sent invention forms a complex with a portion of the chromium ion.
  • the chromium in this complex appears to substitute for metal ion eluted from the surface of the metal workpiece, which results in an efficient deposition of the chromium onto the surface of the metal workpiece and ultimately coverage of the metal surface by chromium and organic film-forming resin.
  • the chromium (ion) taken into the resin film is largely present relatively near the surface of the resin film.
  • the chromium (ion) taken into the resin film is largely present both near the metal surface and relatively near the surface of the resin film. This results in the production of a film having an excellent adherence and corrosion resistance that cannot be achieved by the prior-art rinse treatments (chromium-con ⁇ taining solution, etc.).
  • the tungstate ion used in the present invention can be supplied in the form of tungstic acid, sodium tungstate, calcium tungstate, potassium tungstate, etc.
  • the molybdate ion used in the present invention can be supplied in the form of molybdic acid, sodium molybdate, calcium molybdate, potassium molybdate, etc.
  • the content of tungstate ion and molybdate ion in the coating composition should be 0.1 to 5 g/L and is preferably 0.3 to 2 g/L.
  • the coating composition of the present invention may also contain pigment(s) on an optional basis.
  • Aqueous coating compositions were prepared using an acrylic emulsion (41.5% solids, Rhoplex WL-91 from the Rohm
  • the aqueous coating compositions prepared in Composition Production Examples A through O were used in these examples.
  • the aqueous coating composition baths were held at approximately 20 to 22 ⁇ C
  • the aqueous coating composition prepared in Composition Production Example P was used in this compari ⁇ son example.
  • the aqueous coating composition bath was held at approximately 20 to 22 ⁇ C.
  • the aqueous coating composition prepared in Composition Production Example P was used in this comparison example.
  • the aqueous coating composition bath was held at approxi- mately 20 to 22"C.
  • the sample was immersed in an aqueous chromium-containing solution (Palene 60, trademark of Nihon Parkerizing Company, Limited) for 60 seconds at room temperature and then dried in an oven for 20 minutes at 180"C.
  • the sample was subsequently submitted to the various tests, and the results of the performance testing of the test sheet are reported in Table 2.
  • the aqueous coating composition prepared in Composition Production Example Q was used in these comparison examples.
  • the aqueous coating composition baths were held at approx ⁇ imately 20 to 22 ⁇ C.
  • the sample was immersed in an aqueous chromium-containing solution (Palene 60, trademark of Nihon Parkerizing Company, Limited) for 60 seconds at room temperature and then dried in an oven for 20 minutes at 180 ⁇ C.
  • the sample was subsequently submitted to the various tests, and the results of the performance testing of the test sheets are reported in Table 2.
  • Test Methods and Evaluation Standards l. Film adherence (checkerboard adhesive tape peeling test)
  • test sheet was prepared by cutting a cross in the coating to reach the base metal, and the test sheet was then subjected to salt-spray testing in accordance with JIS Z-2371 (500 hours for the cold-rolled steel sheet, galvannealed hot-dipped zinc-plated steel sheet, and electrogalvanized steel sheet and 1,000 hours for the aluminum sheet) .
  • the test sheet was subsequently subjected to tape peeling, and the peel width from the cross cut (one side, mm) was measured.
  • Coatings with a much better adherence and corrosion resistance than heretofore available from the prior art are formed by contacting metal surfaces with the aqueous auto- deposition coating composition of the present invention. Furthermore, this is achieved without having to carry out a rinse treatment, for example, with a chromium-containing solution, prior to film curing.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

Composition aqueuse de revêtement à auto-dépôt. Elle forme un film présentant une adhérence et une résistance à la corrosion supérieures à celles des films formés par les compositions de revêtement connues de l'état de la technique, mais n'exige aucun traitement avant le durcissement, par exemple par rinçage avec une solution contenant du chrome. Ladite composition aqueuse de revêtement à auto-dépôt présente un pH compris entre 1,6 et 5 environ, et renferme (i) une résine filmogène organique et hydrosoluble ou dispersible dans l'eau; (ii) des ions fluorure et/ou des ions fluorure associés à des ions fluorure complexes; (iii) un ion chrome hexavalent ou un ion chrome hexavalent et un ion chrome trivalent; et (iv) des ions tungstate et/ou molybdate.
PCT/US1993/000138 1992-01-31 1993-01-15 Composition de revetement a auto-depot WO1993015155A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US08/256,913 US5510410A (en) 1992-01-31 1993-01-15 Autodeposition coating composition

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP4057092A JPH05214265A (ja) 1992-01-31 1992-01-31 自己析出型水性被覆組成物
JP4/40570 1992-01-31

Publications (1)

Publication Number Publication Date
WO1993015155A1 true WO1993015155A1 (fr) 1993-08-05

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PCT/US1993/000138 WO1993015155A1 (fr) 1992-01-31 1993-01-15 Composition de revetement a auto-depot

Country Status (4)

Country Link
JP (1) JPH05214265A (fr)
CA (1) CA2128087A1 (fr)
MX (1) MX9300331A (fr)
WO (1) WO1993015155A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037554A1 (fr) * 1995-05-24 1996-11-28 Henkel Corporation Composition pour autodepot et procede faisant appel a une resine de revetement terpolymere acrylique
EP0787831A1 (fr) * 1995-08-11 1997-08-06 Nippon Steel Corporation Composition de resine-chromate et tole traitee en surface
EP0937757A1 (fr) * 1998-02-19 1999-08-25 Nihon Parkerizing Co., Ltd. Composition, procédé pour le traitement hydrophilique de l'aluminium ou d'un alliage d'aluminium et utilisation de cette composition
US7294211B2 (en) 2002-01-04 2007-11-13 University Of Dayton Non-toxic corrosion-protection conversion coats based on cobalt
CN100422234C (zh) * 2001-11-14 2008-10-01 亨克尔两合股份公司 自沉积阴离子环氧树脂水分散体
US10125424B2 (en) 2012-08-29 2018-11-13 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates
US10400337B2 (en) 2012-08-29 2019-09-03 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing lithium, associated methods for treating metal substrates, and related coated metal substrates
US11518960B2 (en) 2016-08-24 2022-12-06 Ppg Industries Ohio, Inc. Alkaline molybdenum cation and phosphonate-containing cleaning composition

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102142779B1 (ko) * 2018-11-28 2020-08-07 주식회사 포스코 Mg함유 아연도금강판의 Cr(III) 표면처리용 조성물 및 이를 이용하여 표면처리된 Mg 함유 아연도금강판
WO2021008860A1 (fr) 2019-07-12 2021-01-21 Henkel Ag & Co. Kgaa Formulation de revêtement à dépôt autocatalytique monocouche

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5712860A (en) * 1980-06-27 1982-01-22 Dainippon Toryo Co Ltd Treatment of surface of plated zinc film
EP0046268A2 (fr) * 1980-08-14 1982-02-24 Union Carbide Corporation Composition de revêtement anti-corrosion autodéposable
EP0261238A1 (fr) * 1986-04-04 1988-03-30 HAYDU, Robert Revetement protecteur pour metaux

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5712860A (en) * 1980-06-27 1982-01-22 Dainippon Toryo Co Ltd Treatment of surface of plated zinc film
EP0046268A2 (fr) * 1980-08-14 1982-02-24 Union Carbide Corporation Composition de revêtement anti-corrosion autodéposable
EP0261238A1 (fr) * 1986-04-04 1988-03-30 HAYDU, Robert Revetement protecteur pour metaux

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPIL Week 8209, Derwent Publications Ltd., London, GB; AN 82-16683E & JP,A,57 012 860 (DAINIPPON TORYO KK) 22 January 1982 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037554A1 (fr) * 1995-05-24 1996-11-28 Henkel Corporation Composition pour autodepot et procede faisant appel a une resine de revetement terpolymere acrylique
EP0787831A1 (fr) * 1995-08-11 1997-08-06 Nippon Steel Corporation Composition de resine-chromate et tole traitee en surface
EP0787831A4 (fr) * 1995-08-11 1998-11-11 Nippon Steel Corp Composition de resine-chromate et tole traitee en surface
EP0937757A1 (fr) * 1998-02-19 1999-08-25 Nihon Parkerizing Co., Ltd. Composition, procédé pour le traitement hydrophilique de l'aluminium ou d'un alliage d'aluminium et utilisation de cette composition
US6248181B1 (en) 1998-02-19 2001-06-19 Nihon Parkerizing Co., Ltd. Composition and method for hydrophilic treatment of aluminum or aluminum alloy
CN100422234C (zh) * 2001-11-14 2008-10-01 亨克尔两合股份公司 自沉积阴离子环氧树脂水分散体
US7294211B2 (en) 2002-01-04 2007-11-13 University Of Dayton Non-toxic corrosion-protection conversion coats based on cobalt
US10125424B2 (en) 2012-08-29 2018-11-13 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates
US10400337B2 (en) 2012-08-29 2019-09-03 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing lithium, associated methods for treating metal substrates, and related coated metal substrates
US10920324B2 (en) 2012-08-29 2021-02-16 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates
US11518960B2 (en) 2016-08-24 2022-12-06 Ppg Industries Ohio, Inc. Alkaline molybdenum cation and phosphonate-containing cleaning composition

Also Published As

Publication number Publication date
MX9300331A (es) 1994-03-31
CA2128087A1 (fr) 1993-08-05
JPH05214265A (ja) 1993-08-24

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