EP0754251B1 - Procede sans chrome de traitement sans rincage de l'aluminium et de ses alliages et solutions aqueuses appropriees - Google Patents

Procede sans chrome de traitement sans rincage de l'aluminium et de ses alliages et solutions aqueuses appropriees Download PDF

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Publication number
EP0754251B1
EP0754251B1 EP95915174A EP95915174A EP0754251B1 EP 0754251 B1 EP0754251 B1 EP 0754251B1 EP 95915174 A EP95915174 A EP 95915174A EP 95915174 A EP95915174 A EP 95915174A EP 0754251 B1 EP0754251 B1 EP 0754251B1
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EP
European Patent Office
Prior art keywords
water
treatment
organic film
treatment solution
bis
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
EP95915174A
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German (de)
English (en)
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EP0754251A1 (fr
Inventor
Uwe Karmaschek
Raschad Mady
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Publication of EP0754251A1 publication Critical patent/EP0754251A1/fr
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Classifications

    • 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
    • C23C22/34—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 fluorides or complex fluorides
    • C23C22/36—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 fluorides or complex fluorides containing also phosphates
    • C23C22/361—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 fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds

Definitions

  • the invention relates to the preparation of cleaned metal surfaces, especially of strips of aluminum or aluminum alloys for one subsequent coating with organic coatings, in particular on the manufacture of metal goods for architectural applications and for the food packaging sector is thought.
  • no-rinse processes are generally known today.
  • the metal surface is cleaned of oil, dirt and other residues. Any residues of chemicals from this first stage are removed by rinsing with water.
  • the clean metal surface is wetted with an aqueous bath solution, which is no longer rinsed off but dried in situ on the metal surface and converted there into a solid film of the bath components.
  • Such coatings can substantially improve the surface quality, particularly with regard to corrosion protection and adhesion of subsequently applied cover layers.
  • chrome-free conversion treatment of aluminum surfaces with fluorides boron, silicon, titanium or zirconium alone or in combination with organic polymers is to achieve permanent corrosion protection and to create a basis for subsequent painting known in principle:
  • DE-C-24 33 704 describes treatment baths for increasing paint adhesion and permanent corrosion protection on, inter alia, aluminum, the 0.1 to 5 g / l polyacrylic acid or its salts or esters and 0.1 to 3.5 g / l ammonium fluorozirconate, calculated as ZrO 2 .
  • the pH values of these baths can fluctuate over a wide range. The best results are generally obtained when the pH is 6-8.
  • WO 92/07973 teaches a chromium- free treatment process for aluminum, the essential components in acidic aqueous solution being 0.01 to about 18% by weight of H 2 ZrF 6 and 0.01 to about 10% by weight of a 3- (NC 1 -4 alkyl-N-2-hydroxyethylaminomethyl) -4-hydroxystyrene polymer used.
  • German patent application DE-A-43 17 217 describes a process for the pretreatment of surfaces made of aluminum or its alloys before a second, permanently corrosion-protective conversion treatment, in which the surfaces are brought into contact with acidic aqueous treatment solutions, the complex fluorides of the elements boron, Contain silicon, titanium, zircon or hafnium individually or in a mixture with one another in concentrations of the fluoro anions of between 100 and 4000, preferably 200 to 2000, mg / l and a pH between 0.3 and 3.5, preferably between 1 and 3.
  • the treatment solutions can additionally contain polymers of the type of the polyacrylates and / or the reaction products of poly (vinylphenol) with aldehydes and organic hydroxyl-containing amines in concentrations below 500 mg / l, preferably below 200 mg / l.
  • Phosphoric acid is another optional component of these baths.
  • US-A-4 136 073 claims a chromium-free treatment process for aluminum surfaces, in which the surfaces are brought into contact with acidic (pH 1.2 to 5.5) aqueous solutions containing an organic film former and a soluble titanium compound in the weight ratio polymer: titanium contained between 100: 1 and 1:10.
  • the preferred titanium concentration is between 0.01 and 5% by weight.
  • the present invention is based on the object of a chrome-free “no-rinse” method of the type described at the beginning or suitable for this
  • a chrome-free “no-rinse” method of the type described at the beginning or suitable for this
  • To create treatment agents for architectural applications and in particular suitable for use in the food packaging sector are.
  • those for food applications typical requirements such as sterilizability from the treated material manufactured packaging and avoiding peeling the coating when opening cans ("feathering").
  • a uniform, visually appealing finish layer can be created on the metal surface, which, for example, in the subsequent overcoats with clear coats meets the aesthetic requirements, particularly in the field of food packaging.
  • Such treatment solutions best meet the different requirements for the behavior of the coating which contain both Ti (IV) and Zr (IV), a weight ratio Ti: Zr in the range 3: 1 to 1: 3 being particularly preferred.
  • the pH of the solutions should preferably be between 1.5 and 2.5.
  • the fluoride is preferably used as a complex-bound fluoride, for example as TiF 6 2- or ZrF 6 2- .
  • the organic film former is advantageously a synthetic polymer with a sufficient content of free carboxyl groups, its Water solubility or homogeneous dispersibility in water in the process Ensure pH range.
  • Polymers are particularly suitable of acrylic acid and / or methacrylic acid, which may also be restricted Amounts of copolymers and the corresponding esters, nitriles and / or may contain amides.
  • Preferred organic film formers are clear soluble polyacrylic acids, especially in the pH range of aqueous treatment baths retain their clear solubility. In general it is about are polyacrylic acids of a not too high molecular weight, for example those with molecular weights from 20,000 to about 150,000, preferably from 40,000 to about 100,000.
  • aqueous treatment solutions according to the invention can be pre-cleaned
  • Metal tapes can be applied in any type of application is suitable, a uniformly defined liquid film in the specified Generate quantity ranges on the metal surface.
  • Roller application process with two or three rollers ("Chemcoater"), but also wetting the tape by spraying or dipping with subsequent squeezing of the excess liquid film through, for example, plastic-coated leveling rollers or adjustable ones Air knife is applicable.
  • the temperature of the treatment solution can vary between 15 and 50 ° C are. The temperature is preferably chosen between 20 and 35 ° C.
  • the applied liquid film is allowed to act on the metal surface for a reaction time of about 1 to 40 seconds, whereupon the film is dried and thermally treated at an elevated temperature.
  • a deformable water-insoluble solid film with a mass per unit area of about 50 to 350 mg / m 2 , preferably of about 100 to 250 mg / m 2 remains on the metal surface.
  • the drying and / or the thermal treatment of the applied liquid film or the chemicals applied with it can take place in the temperature range from approximately 50 to 125 ° C., the range between 50 and 80 ° C. being preferred.
  • Both acidic and alkaline cleaners are suitable.
  • the layers obtained with the aqueous treatment solution according to the invention deliver an even finish without discoloration of the base material. she meet in combination with suitable organic applied below Coatings meet the requirements for the food packaging sector.
  • the invention further relates to the aqueous suitable for this process Treatment solution concentrates.
  • the concentrates so that they are for use in the invention Process with 2 to 50 parts by weight of water per part by weight of concentrate be diluted.
  • Table 1 contains bath compositions according to the invention, Table 3 comparative examples in which either the phosphate or the polymer component was omitted. Test results for this are summarized in Table 4.
  • Bath compositions Ex. 1 Ex. 2 Ex. 3 Ex. 4 Ex. 5 Ti 4+ - 7.1 g / l 3.6 g / l 7.1 g / l 3.6 g / l Zr 4+ 10.8 g / l - 5.4 g / l 5.4 g / l 10.8 g / l PO 4 -3 12.0 g / l 12.0 g / l 12.0 g / l 12.0 g / l 12.0 g / l 12.0 g / l 12.0 g / l F - 13.5 g / l 16.9 g / l 15.2 g / l 23.7 g / l 22.0 g / l OP 0.7 g / l 0.7

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Claims (9)

  1. Procédé de production de couches de conversion sans chrome sur des surfaces d'aluminium et de ses alliages dans un procédé sans rinçage par traitement avec des solutions aqueuses d'un pH compris entre 1 et 3,5, qui contiennent du titane et/ou du zirconium ainsi que des agents filmogènes organiques,
    caractérisé en ce qu'
    on met en contact la surface avec des solutions qui se composent pour l'essentiel de
    a) 2,2 à 22,0 g/litre de Zr(IV) et/ou 1,4 à 14,0 g/litre de Ti(IV),
    b) 2,4 à 24,0 g/litre d'orthophosphate,
    c) 3,0 à 30,0 g/litre de fluorure,
    d) 0,15 à 1,5 g/litre d'un agent filmogène organique soluble dans l'eau ou dispersable de manière homogène dans l'eau et
    e) de l'eau
    on sèche les solutions après un temps d'action compris entre 1 et 40 secondes sans rinçage à des températures comprises entre 50 et 125°C sur la surface.
  2. Procédé selon la revendications 1,
    caractérisé en ce que
    les solutions de traitement contiennent :
    a) 4,3 à 13,0 g/litre de Zr(IV) et/ou 2,8 à 8,5 g/litre de Ti(IV),
    b) b 4,8 à 14,3 g/litre d'orthophosphate,
    c) 6,0 à 18,2 g/litre de fluorure,
    d) 0,28 à 0,82 g/litre d'un agent filmogène organique soluble dans l'eau ou dispersable de manière homogène dans l'eau.
  3. Procédé selon l'une des revendications 1 ou 2, ou les deux,
    caractérisé en ce que
    la solution de traitement contient aussi bien du titane que du zirconium, le rapport pondéral Ti:Zr se situant de préférence dans un intervalle de 3:1 à 1:3.
  4. Procédé selon l'une ou plusieurs des revendications 1 à 3,
    caractérisé en ce que
    l'agent filmogène organique est un polymère contenant un groupe carboxyle, en particulier un homo- et/ou copolymère d'acide acrylique et/ou méthacrylique et
    il présente une masse molaire moyenne comprise entre 20 000 et 150 000, de préférence entre 40 000 et 100 000.
  5. Procédé selon une ou plusieurs des revendications 1 à 4,
    caractérisé en ce que
    la solution de traitement présente une température comprise entre 15 et 50°C, de préférence entre 20 et 35°C.
  6. Procédé selon une ou plusieurs des revendications 1 à 5,
    caractérisé en ce que
    la solution de traitement présente un pH compris entre 1,5 et 2,5.
  7. Procédé selon une ou plusieurs des revendications 1 à 6,
    caractérisé en ce que
    la solution de traitement est déposée en une pellicule liquide avec mise en place comprise entre 3 et 10 ml/m2, en particulier entre 4 et 8 ml/m2 sur la surface du métal.
  8. Procédé selon une ou plusieurs des revendications 1 à 7,
    caractérisé en ce qu'
    on sèche la pellicule de liquide à une température comprise entre 50 et 80°C.
  9. Concentré aqueux qui par dilution avec de 2 à 50 parties en poids d'eau par partie en poids de concentré donne une solution de traitement prête à l'emploi qui se compose pour l'essentiel de
    a) 2,2 à 22,0 g/litre de Zr(IV) et/ou 1,4 à 14,0 g/litre de Ti(IV),
    b) 2,4 à 24,0 g/litre d'orthophosphate,
    c) 3,0 à 30,0 g/litre de fluorure,
    d) 0,15 à 1,5 g/litre d'un agent filmogène organique soluble dans l'eau ou dispersable de manière homogène dans l'eau et
    e) de l'eau
    et qui sert aux fins d'application dans le procédé selon une ou plusieurs des revendications 1 à 8.
EP95915174A 1994-04-08 1995-03-31 Procede sans chrome de traitement sans rincage de l'aluminium et de ses alliages et solutions aqueuses appropriees Expired - Lifetime EP0754251B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4412138A DE4412138A1 (de) 1994-04-08 1994-04-08 Chromfreies Verfahren zur No-Rinse Behandlung von Aluminium und seinen Legierungen sowie hierfür geeignete wäßrige Badlösungen
DE4412138 1994-04-08
PCT/EP1995/001197 WO1995027807A1 (fr) 1994-04-08 1995-03-31 Procede sans chrome de traitement sans rinçage de l'aluminium et de ses alliages et solutions aqueuses appropriees

Publications (2)

Publication Number Publication Date
EP0754251A1 EP0754251A1 (fr) 1997-01-22
EP0754251B1 true EP0754251B1 (fr) 1998-05-20

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EP95915174A Expired - Lifetime EP0754251B1 (fr) 1994-04-08 1995-03-31 Procede sans chrome de traitement sans rincage de l'aluminium et de ses alliages et solutions aqueuses appropriees

Country Status (7)

Country Link
US (1) US5868872A (fr)
EP (1) EP0754251B1 (fr)
JP (1) JP3662586B2 (fr)
CA (1) CA2187463A1 (fr)
DE (2) DE4412138A1 (fr)
ES (1) ES2117863T3 (fr)
WO (1) WO1995027807A1 (fr)

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Also Published As

Publication number Publication date
US5868872A (en) 1999-02-09
DE4412138A1 (de) 1995-10-12
JPH09511548A (ja) 1997-11-18
DE59502263D1 (de) 1998-06-25
EP0754251A1 (fr) 1997-01-22
JP3662586B2 (ja) 2005-06-22
WO1995027807A1 (fr) 1995-10-19
CA2187463A1 (fr) 1995-10-19
ES2117863T3 (es) 1998-08-16

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