EP1292719A1 - Agent adhesif dans des solutions pour conversion - Google Patents

Agent adhesif dans des solutions pour conversion

Info

Publication number
EP1292719A1
EP1292719A1 EP01957837A EP01957837A EP1292719A1 EP 1292719 A1 EP1292719 A1 EP 1292719A1 EP 01957837 A EP01957837 A EP 01957837A EP 01957837 A EP01957837 A EP 01957837A EP 1292719 A1 EP1292719 A1 EP 1292719A1
Authority
EP
European Patent Office
Prior art keywords
aqueous solution
group
radicals
organic
solution according
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.)
Withdrawn
Application number
EP01957837A
Other languages
German (de)
English (en)
Inventor
Bernd Schenzle
Heike Quellhorst
Alina Monica Koch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP1292719A1 publication Critical patent/EP1292719A1/fr
Withdrawn legal-status Critical Current

Links

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

Definitions

  • the invention is in the field of anti-corrosion treatment of metal surfaces on which a corrosion-protective conversion layer is produced.
  • This conversion layer serves as a primer for subsequent painting.
  • chromium-free conversion treatment of aluminum surfaces with fluorides of boron, silicon, titanium or zirconium in combination with organic polymers is known in principle to achieve permanent corrosion protection and to create a basis for subsequent painting:
  • US-A-5 129 967 discloses treatment baths for a no-rinse treatment (referred to there as “dried in place conversion coating") containing aluminum
  • EP-B-8 942 discloses treatment solutions, preferably containing aluminum cans
  • DE-C-24 33 704 describes treatment baths to increase paint adhesion and permanent corrosion protection to, among other things.
  • Aluminum which can contain 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 Zr ⁇ 2. The pH values of this
  • US-A-4 992 116 describes treatment baths for the conversion treatment of aluminum with pH values between about 2.5 and 5, which contain at least three components:
  • a molar ratio between the fluoric acid and phosphate of about 2.5: 1 to about 1:10 must be observed.
  • WO 92/07973 teaches a chromium-free treatment process for aluminum, which as essential components in acidic aqueous solution 0.01 to about 18 wt .-% H 2 ZrF 6 and 0.01 to about 10 wt .-% of a 3- (N- C ⁇ ⁇ alkyl-N-2-hydroxyethylaminomethyl) -4hydroxystyrene polymer used.
  • Optional components are 0.05 to 10% by weight of dispersed SiO 2 , 0.06 to 0.6% by weight of a solubilizer for the polymer and surfactant.
  • Lacquers differ from solutions for conversion treatment in that the lacquer layer adheres to the base due to sorption forces and no chemical reaction with the base occurs. In contrast, a conversion solution reacts chemically with the base, so that atoms from the base are built into the conversion layer.
  • the object of the invention is to improve the adhesion between a conversion layer and a lacquer layer applied thereon.
  • the invention relates to an aqueous solution for producing a conversion layer on metal surfaces, which has a pH in the range from 1.5 to 6 and the complex fluorides of Ti, Zr, Hf, Si and / or B in such an amount that the The content of Ti, Zr, Hf, Si and / or B is 20 to 500 mg / l, and contains 0.1 to 2 g / l of adhesion-promoting lacquer additives and the composition of the aqueous solution is chosen so that none on the metallic surface crystalline zinc-containing phosphate layer is formed.
  • the aqueous solution preferably has a pH in the range from 2.5 to 4.5.
  • the complex fluorides of the elements mentioned can be introduced into the aqueous solution in the form of the corresponding fluoric acids or their alkali metal and / or ammonium salts. However, it is also possible to form the complex fluorides only in the aqueous solution itself by reacting hydrofluoric acid or fluorides with the ions of the metals mentioned. For example, complex fluorides of titanium or zircon are formed by the reaction of oxides or salts of these elements with hydrofluoric acid.
  • the aqueous solution can contain free fluoride, for example in the form of hydrofluoric acid or alkali metal or ammonium fluorides.
  • the free fluoride content can range from 0.001 to 1 g / l. This addition of free fluoride increases the pickling action of the aqueous solution and thus the rate of conversion layer formation, particularly in the case of hot-dip galvanized steel or aluminum.
  • the aqueous solution preferably contains the complex fluorides of Ti, Zr, Hf, Si and / or B in an amount such that the content of Ti, Zr, Hf, Si and / or B is 50 to 400 mg / l.
  • the adhesion-promoting paint additives are preferably selected from water-soluble compounds which contain at least one element M selected from the group B, Al, Si, Ti and Zr.
  • the connections can be single or multi-core, in particular dual-core. In the case of bi- or polynuclear compounds, it is preferred that they contain different elements M in the molecule. Examples include compounds which contain both Al and Ti or both Al and Zr.
  • Compounds preferred as adhesion-promoting lacquer additives are those in which the element M has at least one hydroxyl group and one or more organic radicals R are bonded, the organic radical or the organic radicals R being selected independently of one another from hydrocarbon radicals having 3 to 16 carbon atoms or from radicals - (CH2) X -Y, where x is an integer in the range from 1 to 10 and Y represents a hydroxyl group, a mercapto group, a primary or secondary amino group, a carboxyl group, an acrylic or methacrylic acid residue or an oxirane group or in each case a molecular fragment which contains one or more of the groups or acid residues mentioned.
  • the at least one hydroxyl group can already be bound to the element M when the compound is introduced into the aqueous solution to produce a conversion layer.
  • the hydroxyl group bonded to the element M only forms by reaction of a precursor compound with water in the aqueous solution to produce a conversion layer.
  • one or more alcoholate groups can be bound to the element M and are replaced by OH groups by reaction with water.
  • Suitable organic radicals R are, in particular, those radicals which are known in silane chemistry as reactive groups for linking the silanes to components of paints and varnishes. Examples of such residues have been listed above. Several different organic radicals R can also be bound to the element M.
  • the secondary amino group mentioned can be part of a diamine or polyamine unit, for example. For example, it can be part of an ethylenediamine or an ethylenediamine which is methyl-substituted at the terminal nitrogen atom. If, for example, Y is an ethylenediamine residue, this means that both a secondary and a primary amino group are present in the organic residue R.
  • Y is a carboxyl group
  • this is in general connected to the (CH 2 ) ⁇ chain via a C atom of the carboxyl group.
  • an acrylic or methacrylic acid residue it is bound to the (CH 2 ) X chain via the carboxyl function itself, that is to say in an ester-like manner.
  • An oxirane group can form part of a glycidoxypropyl residue, for example.
  • Y can represent not only one of the above-mentioned groups as such, but also a molecular fragment containing several atoms, which contains one or more of the groups or acid residues listed above.
  • Y can mean a molecular fragment in which both a hydroxyl group and a carboxyl group are present.
  • the glycidoxypropyl group already mentioned by way of example is a molecular fragment in which both a hydroxyl group and an oxirane unit occur.
  • hydroxyl groups or their precursor fragments and the organic radicals R enumerated above further groups or ligands which do not react chemically under the reaction conditions such as occur in the use according to the invention can be bound to the element M.
  • these can be alkyl radicals or carboxyl radicals.
  • the molecules of the adhesion-promoting coating additive are multinuclear, that is to say contain at least 2, possibly different, elements M, these are generally linked via ligands.
  • These can be carboxyl groups, for example.
  • hydroxyl groups or alcoholate groups can also perform such a bridging function.
  • adhesion-promoting coating additives which contain Al as element M or a combination of Al with one of the other elements M mentioned, in particular with Zr.
  • the aqueous solution preferably additionally contains 50 to 2000 mg / l, in particular 100 to 1000 mg / l, organic polymers.
  • the organic polymers can be selected from epoxy resins, aminoplast resins, tannins, phenol-formaldehyde resins, polycarboxylic acids, polymeric alcohols and / or their esterification products with polycarboxylic acids, poly-4-vinylphenol compounds, amino or copolymer compounds containing amino groups and polymers or copolymers of vinylpyrrolidone , The Use of such polymers in the field of
  • Metal surface treatment is known. For example, they are characterized in more detail in DE-A-100 10 758, whereupon more preferred for closer selection
  • the aqueous solution can additionally contain 0.001 to 2, preferably 0.005 to 0.5 g / l ions of one or more of the metals Mn, Ce, Li, V, W, Mo, Mg, Zn, Co and Ni.
  • these additional metal ions can further improve the corrosion protection effect and paint adhesion. For environmental reasons, however, attempts will be made to avoid using Co and Ni.
  • the aqueous solution may additionally contain 0.001 to 1.5, preferably 0.1 to 1 g / l phosphoric acid, phosphorous acid, phosphonic acid and / or their anions and / or their esters. Esters are to be chosen so that they are water-soluble or water-dispersible. These additives also improve corrosion protection and paint adhesion. However, according to the basic idea of the present invention, care should be taken not to choose such a combination of additives which leads to the formation of a crystalline zinc-containing phosphate layer. For example, this is achieved in that the treatment solution does not simultaneously contain zinc and / or manganese in concentrations of above 0.3 g / l and phosphoric acid or phosphate ions in concentrations of above 3 g / l.
  • the aqueous solution further contains one or more components which are known in the technical field of phosphating as so-called phosphating accelerators.
  • phosphating accelerators have the main task of preventing the formation of bubbles of elemental hydrogen on the metal surface. This effect is also known as the depolarization effect.
  • this also has the consequence in the solution according to the invention that the conversion layer is formed more quickly and that it is formed more uniformly.
  • the aqueous solution select one or more phosphating accelerators 0.05 to 2 g / l m-nitrobenzenesulfonate ions, 0.1 to 10 g / l hydroxylamine in free or bound form, 0.05 to 2 g / l m-nitrobenzoate ions, 0.05 to 2 g / l p-nitrophenol .
  • the aqueous solution be free of chromium. Additions of chromium compounds to the aqueous solution could have a positive effect on the corrosion protection in individual cases, but corrosion protection and paint adhesion that can be achieved with the method according to the invention are sufficient even without the use of chromium compounds in the area of application concerned.
  • the aqueous solution which contains the individual components in the application concentration for producing the conversion layer, can be prepared by dissolving the individual components in water in the desired application concentration at the place of use.
  • a concentrate consisting of one or more containers is transported to the user, who prepares the ready-to-use solution from the concentrate or concentrates by dilution with water at the place of use.
  • the invention comprises an aqueous concentrate present in one or more, in particular in two, containers, which after dilution with water by a factor between 50 and 500, in particular between 100 and 300, and if necessary adjusting the pH, an aqueous solution of the above described composition results.
  • the concentrate in one or two containers depends in particular on whether it contains an organic polymer and whether this polymer is stable in the presence of the other components of the concentrate. If no organic polymer is present or if it is stable in the aqueous concentrate in the presence of the other constituents, the concentrate is preferably provided in a container.
  • polymers such as polyacrylates are generally not stable in the presence of the inorganic components of the concentrate, but flocculate or lead to gel formation. In this case, it is preferable that
  • one container preferably containing the complex fluorides and the other container preferably containing the organic polymers.
  • the adhesion-promoting lacquer additives can either be added to the container with the complex fluorides or to the container with the organic polymers, the latter being preferred.
  • the adhesion-promoting coating additives can, however, also be provided in a third container and only in the ready-to-use diluted solution of the other
  • Another aspect of the invention lies in a method for the corrosion protection treatment of metal surfaces, wherein the metal surfaces are brought into contact with an aqueous solution of the type described above for a period of between 0.5 and 5 minutes to produce a conversion layer.
  • the metal surfaces are preferably selected from those which are used in architecture, in mechanical engineering, in the furniture and household appliance industry and in shipbuilding, aircraft and vehicle construction. These are in particular surfaces of steel, of electrolytically or hot-dip galvanized or alloy-galvanized steel, as well as of zinc, aluminum and magnesium as well as alloys that consist of at least 50 atomic percent of iron, zinc, aluminum or magnesium.
  • the aqueous solution used in the process according to the invention preferably has a temperature between ambient temperature (about 15 to 20 ° C.) to about 70 ° C. The temperature range from 25 to 40 ° C. is preferred.
  • the metal surfaces can be sprayed with the aqueous solution aqueous solution or by immersion in the aqueous solution and in the no-rinse process. In general, the aqueous solution is allowed to act on the metal surfaces for a period in the range from about 0.5 to about 5 minutes by spraying or dipping. A period in the range of 1 to 3 minutes is preferred for spray processes, and a period of 2 to 5 minutes is preferred for immersion processes.
  • the solutions are dried without intermediate rinsing about 3 to about 30 seconds after application to the metal surfaces.
  • automobile bodies or household appliances are often made from different materials.
  • steel and / or steels galvanized in different ways can be combined with one another or with components made of aluminum and / or magnesium or their alloys in each case.
  • a particular strength of the method according to the invention is that an effective corrosion protection layer is also produced on the different materials in such cases.
  • a special embodiment of the invention is characterized in that vehicle bodies or household appliances are treated which have surfaces made of at least 2 materials selected from zinc, aluminum, magnesium, alloys of these metals with one another or with other alloy components.
  • the step of forming the conversion layer is followed by painting the metal surfaces with an electrodeposable dip or with a powder coating.
  • Electrolytic dip coating in particular cathodic dip coating, is preferred for vehicle bodies.
  • Modern lead-free or low-lead cathodic electrodeposition lacquers are also suitable for this purpose, that is to say those immersion lacquers which contain less than 500 mg of lead per kg of dry substance in the lacquer suspension.
  • Household appliances can also be dip-coated electrolytically.
  • powder coating is preferred.
  • powder coating is often preferred in the architectural sector and in the furniture industry. So that's it
  • the method according to the invention is preferably characterized in that the coating is carried out after the anti-corrosion treatment with an electrocoat or a powder coating.
  • the method according to the invention is usually embedded in the sequence cleaning, conversion protection treatment and painting. Between these process steps, one or more rinsing stages with process water, city water or fully demineralized water can be provided. Spraying or dipping processes can be used for the rinsing steps.
  • the exemplary embodiments show a typical sequence of processes.
  • test panels were subjected to the following procedure, with all the steps being carried out in the immersion process:

Landscapes

  • 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)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

L'invention concerne une solution aqueuse pour la réalisation d'une couche de conversion sur des surfaces métalliques. Cette solution, dont le pH varie dans la plage de 1,5 à 6, contient des fluorures complexes de Ti, Zr, Hf, Si et/ou B en une quantité telle que la teneur en Ti, Zr, Hf, Si et/ou B est de 20 à 500 mg/l, ainsi que 0,1 à 2 g/l d'additif de peinture adhésif. La composition de la solution aqueuse est sélectionnée de sorte qu'aucun dépôt de phosphate zincifère cristallin ne se forme sur la surface métallique. L'additif de peinture comporte de préférence un élément M sélectionné dans le groupe comprenant B, Al, Si, Ti et Zr, au moins un groupe hydroxyle et un ou plusieurs restes organiques R étant liés à l'élément M. Le ou les reste(s) organique(s) R sont sélectionnés indépendamment l'un de l'autre à partir de restes d'hydrocarbures comptant 3 à 16 atomes C ou à partir de restes (CH2)x-Y, x étant un nombre entier entre 1 et 10 et Y signifiant un groupe hydroxyle, un groupe mercapto, un groupe amino primaire ou secondaire, un groupe carboxyle, un reste d'acide méthacrylique ou acrylique, un groupe oxirane, ou bien un fragment molécule de ceux-ci contenant un ou plusieurs des groupes ou des restes d'acides mentionnés.
EP01957837A 2000-06-21 2001-06-09 Agent adhesif dans des solutions pour conversion Withdrawn EP1292719A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10030462 2000-06-21
DE10030462A DE10030462A1 (de) 2000-06-21 2000-06-21 Haftvermittler in Konversionslösungen
PCT/EP2001/006546 WO2001098557A1 (fr) 2000-06-21 2001-06-09 Agent adhesif dans des solutions pour conversion

Publications (1)

Publication Number Publication Date
EP1292719A1 true EP1292719A1 (fr) 2003-03-19

Family

ID=7646440

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01957837A Withdrawn EP1292719A1 (fr) 2000-06-21 2001-06-09 Agent adhesif dans des solutions pour conversion

Country Status (6)

Country Link
US (1) US20040020564A1 (fr)
EP (1) EP1292719A1 (fr)
JP (1) JP2004501280A (fr)
AU (1) AU2001279651A1 (fr)
DE (1) DE10030462A1 (fr)
WO (1) WO2001098557A1 (fr)

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US7815751B2 (en) * 2005-09-28 2010-10-19 Coral Chemical Company Zirconium-vanadium conversion coating compositions for ferrous metals and a method for providing conversion coatings
JP4975378B2 (ja) * 2006-06-07 2012-07-11 日本パーカライジング株式会社 金属の表面処理液、表面処理方法、表面処理材料
US8673091B2 (en) * 2007-08-03 2014-03-18 Ppg Industries Ohio, Inc Pretreatment compositions and methods for coating a metal substrate
US9347134B2 (en) 2010-06-04 2016-05-24 Prc-Desoto International, Inc. Corrosion resistant metallate compositions
CN111621774A (zh) 2012-08-29 2020-09-04 Ppg工业俄亥俄公司 含锂的锆预处理组合物，处理金属基材的相关方法，和相关的经涂覆的金属基材
CA2883180C (fr) 2012-08-29 2017-12-05 Ppg Industries Ohio, Inc. Compositions de pretraitement du zirconium qui contiennent du molybdene, procedes associes permettant de traiter des substrats metalliques et substrats metalliques recouverts associes
US9273399B2 (en) 2013-03-15 2016-03-01 Ppg Industries Ohio, Inc. Pretreatment compositions and methods for coating a battery electrode
US20150309973A1 (en) * 2014-04-28 2015-10-29 Elwha LLC, Methods, systems, and devices for machines and machine states that facilitate modification of documents based on various corpora and/or modification data
CN109642325A (zh) * 2016-08-12 2019-04-16 Prc-迪索托国际公司 通过薄膜预处理和密封组合物来处理金属基材的***和方法
KR20190043155A (ko) 2016-08-24 2019-04-25 피피지 인더스트리즈 오하이오 인코포레이티드 금속 기판을 처리하기 위한 알칼리성 조성물
JP6899641B2 (ja) * 2016-10-06 2021-07-07 株式会社日本触媒 樹脂組成物
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Also Published As

Publication number Publication date
AU2001279651A1 (en) 2002-01-02
US20040020564A1 (en) 2004-02-05
WO2001098557A1 (fr) 2001-12-27
DE10030462A1 (de) 2002-01-03
JP2004501280A (ja) 2004-01-15

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