EP4063535A2 - Procédé de traitement antérieur de l'acier et du fer dans un bain de traitement - Google Patents

Procédé de traitement antérieur de l'acier et du fer dans un bain de traitement Download PDF

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Publication number
EP4063535A2
EP4063535A2 EP22164138.4A EP22164138A EP4063535A2 EP 4063535 A2 EP4063535 A2 EP 4063535A2 EP 22164138 A EP22164138 A EP 22164138A EP 4063535 A2 EP4063535 A2 EP 4063535A2
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EP
European Patent Office
Prior art keywords
bath
treatment
iron
acid
solution
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.)
Pending
Application number
EP22164138.4A
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German (de)
English (en)
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EP4063535A3 (fr
Inventor
Robert Ecker
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Individual
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Individual
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Filing date
Publication date
Priority claimed from DE102021004167.4A external-priority patent/DE102021004167A1/de
Application filed by Individual filed Critical Individual
Publication of EP4063535A2 publication Critical patent/EP4063535A2/fr
Publication of EP4063535A3 publication Critical patent/EP4063535A3/fr
Pending legal-status Critical Current

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    • 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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/22—Orthophosphates containing alkaline earth metal cations
    • 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
    • C23C22/73—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 characterised by the process
    • C23C22/77—Controlling or regulating of the coating process
    • 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
    • C23C22/82—After-treatment

Definitions

  • the invention relates to a method for the pretreatment of steel and iron in a treatment bath.
  • the aim is therefore to achieve a significant improvement in the result by using a new chemical composition of the materials used. This is particularly useful with regard to the tightness of the layers to be formed. Without dense and thinner layers, previously known pre-treatment methods are only limited to a few applications.
  • the applied passivation layer should be absolutely tight. In the past this was achieved by blowing off the surface. In addition, the layer thickness was usually well over 20 ⁇ m.
  • the aim of the new process is to use improved chemical materials to meet the requirements for effective pre-treatment.
  • the requirements for the pre-treatment can only be met if the reaction of the chemical reagents in a bath works optimally.
  • the aim is also that the reaction leads to a thinner and denser layer of 20 to 30 ⁇ m, 10 to 25 ⁇ m or even just 7 to 15 ⁇ m or 10 to 15 ⁇ m leading to an improvement in the quality of the surface.
  • a primer will then no longer be absolutely necessary.
  • the regeneration of the chemical components of the bath in compliance with the specified parameters is to be observed through constant analysis of the bath and is mandatory.
  • the chemical reaction especially the lack of oxygen (reaction), avoids contamination by sludge formation.
  • An imbalance e.g. B. with oxygen must not occur in any phase of the treatment.
  • the optimal layer thickness which is generated by a good reaction in the bath, is the result of the required high quality of the bath.
  • a good constant flow and compliance with the specified temperature and time of treatment contribute to the fact that a subsequent layer of paint can be applied.
  • the parameters should be constantly monitored by a controller and preferably regulated automatically at predetermined intervals being held. Sensors are used to ensure compliance with the limit values, especially for pH values, Fe II, free acid, temperature and level. A special calculation of the values can keep the bath in a defined condition via an automatic control.
  • the set temperature must not fall below 52 °C and the temperature level must not exceed 60 °C.
  • the passivation also represents a temporary protection against corrosion. However, this can only be guaranteed if the quality of the surface is consistently good.
  • Complicated components cannot always be optimally flowed through. It is therefore necessary for these components to be moved. This is preferably done with a lifting/lowering station that moves the parts up and down.
  • the components are guided over an adhesive water dryer.
  • the rate of maturation (drying) of the components depends on temperature factors.
  • the parts should be dried in a holding water dryer immediately after passivation in the tank.
  • the time interval between the end of treatment and drying should not be longer than 5 - 10 minutes.
  • the temperature in the adhesive water dryer should be between 150 and 210 °C.
  • the drying time is between 3 and 15 minutes.
  • the selection of the paint layers is important with regard to adhesion. While the layer (pre-treatment) adheres to the surface during passivation, the paint can peel off. Taking this problem into account, suitable powder coatings should be selected for this purpose.
  • composition of the bath 85% ortho-phosphoric acid, 5% calcium hydroxide (98% in solution) and 10% ammonium nitrate (98% in solution) are first mixed as basic chemicals.
  • This basic chemistry is used in the treatment tank with between 8 and 13 parts by volume of basic chemistry and 92 to 87% deionized water (demineralized water).
  • the parameters for the treatment are only set after the chemistry in the treatment tank has been measured using titration.
  • the result of the titration must always show the following parameters in the bath: 9.5 - 11.5% free acid and 9 - 13.0 g/l iron II.
  • This titration of the bath solution constantly monitors the content in the bath. For the end product to be successful, these parameters must be adhered to.
  • the figure 2 shows how the results of the titration are determined using a two-point titration.
  • the measurement method is in figure 3 shown. Only the control of the bath with the specified parameters ensures the success of the result.
  • the ion exchanger is also relevant.
  • the ion exchange resin to be used is new here.
  • the proportion of Fe II ions should be kept constant as described above for the composition of the bath.
  • the increase of FE II during the treatment of the iron parts is inevitable. This increase in FE II can be reduced with a strongly acidic, macroporous cation exchange resin, such as Lanxes Levatit Mono + SP 112 H.
  • Lewatit ® MonoPlus SP 112 H belongs to the group of strongly acidic, macroporous cation exchangers. It is characterized by beads with the same diameter (monodisperse particle size distribution) based on a styrene-divinylbenzene copolymer. Its monodisperse beads are chemically and mechanically extremely stable and osmotically highly resilient, it is suitable for all full desalination applications. The very high monodispersity (uniformity coefficient: max. 1.1) and the low proportion of fines of max. 0.1% ( ⁇ 0.315 mm) leads to lower pressure losses compared to standard ion exchangers.
  • the design of the ion exchanger shows the figure 5 .
  • the bath concentration is switched on in the by-pass.
  • Checking the residual concentration of iron (II) gives the measurement and the permeate.
  • the figure 6 shows the structure as an RI scheme.
  • Another aspect of the invention is the maintenance of the ion exchanger. This care is to be carried out according to the following process steps: removal from the treatment bath, filtration, feeding into the ion exchanger, outlet filter, 75% loading with iron (II), switching to regeneration (by-pass), checking the eluate using TitroLine, iron (II) ok . switching, treatment.
  • a powder layer can be applied.
  • the powder coating forms a chemical bond with the passivated surface.
  • bracketing as after the sandblasting, but a durable crosslinking.
  • the layer thickness is approx. 60 ⁇ m with the passivation and the powder coating.
  • Phosphating is a chemical process in which thin, finely crystalline and water-insoluble phosphates are produced from phosphoric acid solutions on metal surfaces in an immersion process.
  • the metal phosphate layers which range in color from light to anthracite, are firmly anchored in the metal surface as they result from a chemical reaction with the base metal.
  • this phosphate layer is an extremely effective protection against corrosion.
  • Phosphating is a chemical process in which thin, finely crystalline and water-insoluble phosphates are produced from phosphoric acid solutions on metal surfaces in an immersion process.
  • the metal phosphate layers which range in color from light to anthracite, are firmly anchored in the metal surface as they result from a chemical reaction with the base metal.
  • this phosphate layer is an extremely effective protection against corrosion.
  • the process presented is more economical and environmentally friendly than conventional pre-treatment processes. With the new process, layer thicknesses of 10 - 20 ⁇ m or even 20 to 30 ⁇ m can be formed.
  • the adhesive tensile strength is up to 16 MPa.
  • the treatment process is also significantly simplified. While the zinc and manganese phosphating requires 6 - 7 process baths, the process described manages with one bath. However, the parts must be well degreased. Depending on the oil or grease load on the components, spray degreasing is used for this purpose.
  • the acid-wetted surface is treated strictly according to the specified parameters. This has the advantage that no additional sink is required and no complex disposal is required.
  • the resulting layers are better developed than the usual layers.
  • the layer thickness reaches a thickness of 10 - 20 ⁇ m depending on the treatment time and chemistry (additives).
  • a layer thickness of the phosphate layer of 15 to 35 and particularly preferably between 20 and 30 ⁇ m is preferred.
  • the adhesive tensile strength is between 10 and 16 MPa.
  • the tightness of the layer is better than a hot-dip galvanized layer or a cathodic dip painting of the same thickness.
  • the substances contained in the systems are properly processed with rinsing water before they are fed into a public sewage treatment plant, for example.
  • the treatment is limited only to the treatment of exhausted phosphating. These solutions are diluted to a concentration of 2%. In relation to the total volume of wastewater discharged.

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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)
EP22164138.4A 2021-03-25 2022-03-24 Procédé de traitement antérieur de l'acier et du fer dans un bain de traitement Pending EP4063535A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102021001551 2021-03-25
DE102021004167.4A DE102021004167A1 (de) 2021-03-25 2021-08-13 Verfahren für Vorbehandlung von Stahl und Eisen in einem Behandlungsbad

Publications (2)

Publication Number Publication Date
EP4063535A2 true EP4063535A2 (fr) 2022-09-28
EP4063535A3 EP4063535A3 (fr) 2022-11-30

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP22164138.4A Pending EP4063535A3 (fr) 2021-03-25 2022-03-24 Procédé de traitement antérieur de l'acier et du fer dans un bain de traitement

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EP (1) EP4063535A3 (fr)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017176696A1 (fr) 2016-04-04 2017-10-12 Rhodia Operations Systèmes de solvant de triamide alkylthiophosphorique et d'huile de neem destinés à être utilisés dans des applications agricoles

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005023023B4 (de) * 2005-05-19 2017-02-09 Chemetall Gmbh Verfahren zur Vorbereitung von metallischen Werkstücken zum Kaltumformen, mit dem Verfahren beschichtete Werkstücke und ihre Verwendung
DE112015002448A5 (de) * 2014-05-23 2017-03-16 Robert Ecker Verfahren zum Phosphatieren und Vorrichtung zum Beizen und Phosphatieren von Eisenmetallen
DE102019002417A1 (de) * 2018-12-20 2020-06-25 IAP Industrial Acid Proofing Europe GmbH Verfahren und Vorrichtung zum Phosphatieren von Bauteilen aus Eisenmetall

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017176696A1 (fr) 2016-04-04 2017-10-12 Rhodia Operations Systèmes de solvant de triamide alkylthiophosphorique et d'huile de neem destinés à être utilisés dans des applications agricoles

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Publication number Publication date
EP4063535A3 (fr) 2022-11-30

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