EP1100982B1 - Decapant pour aciers speciaux - Google Patents

Decapant pour aciers speciaux Download PDF

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Publication number
EP1100982B1
EP1100982B1 EP99942796A EP99942796A EP1100982B1 EP 1100982 B1 EP1100982 B1 EP 1100982B1 EP 99942796 A EP99942796 A EP 99942796A EP 99942796 A EP99942796 A EP 99942796A EP 1100982 B1 EP1100982 B1 EP 1100982B1
Authority
EP
European Patent Office
Prior art keywords
weight
acid
pickling
compound
hydrogen fluoride
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
EP99942796A
Other languages
German (de)
English (en)
Other versions
EP1100982A1 (fr
Inventor
Eckart SCHÖNFELDER
Günther Schwane
Harald Werner
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.)
Chemetall GmbH
Original Assignee
Chemetall GmbH
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 Chemetall GmbH filed Critical Chemetall GmbH
Publication of EP1100982A1 publication Critical patent/EP1100982A1/fr
Application granted granted Critical
Publication of EP1100982B1 publication Critical patent/EP1100982B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/025—Cleaning or pickling metallic material with solutions or molten salts with acid solutions acidic pickling pastes

Definitions

  • the invention relates to a wetting and emulsifying agent-free aqueous pickling agent for stainless steels based on sulfuric acid or phosphoric acid and hydrogen fluoride.
  • the most important acids for pickling stainless steels or Acid mixtures are hydrofluoric acid, hydrofluoric acid / nitric acid, Hydrofluoric acid / sulfuric acid with some considerable additives of iron III compounds already in the starting phase of Mordant.
  • Another method is a so-called single bath degreasing and pickling of iron containing or objects made of it. It works with solutions the acids, wetting agents and / or emulsifiers as well Oxidizing agents aromatic, water soluble Nitro compounds, e.g. Nitrobenzenesulfonate included (DE-A-25 07 059).
  • Single-bath degreasing and pickling leads to the entry of oils or fats in the Pickling bath, which makes the pickling process unpredictable Way is affected. In particular, training prevents a uniform pickling pattern.
  • the content of Wetting agents and / or emulsifiers also make it more difficult Preparation of the rinse and Wastewater.
  • the object of the invention is an aqueous mordant for To provide stainless steels that are known, in particular aforementioned disadvantages, does not have, and is procedurally simple and inexpensive to carry out.
  • the task is solved by the mordant of the beginning formulated according to the invention in such a way is that it (each as 100 wt .-% substance) 1.5 to 16% by weight sulfuric acid or 2.0 to 30% by weight Phosphoric acid and 0.5 to 14 wt .-% hydrogen fluoride and 0.5 to 15.5% by weight of acid-soluble aromatic Nitro compound contains no iron III compound is supplied and only in the start phase iron II Oxidizing agent oxidizing to iron III are supplied can.
  • mordants according to the invention can also be used in the Starting phase without iron II oxidizing to iron III Oxidizing agents are used.
  • iron II oxidizing to iron III Oxidizing agents are used.
  • small amounts of oxidizing agents admit based on peroxide compounds for example 0.05% by weight.
  • the mordant according to the invention can be used as a bath stain Spray or tweezers are used.
  • a pickling agent which, when used as a bath pickle, contains 5.0 to 11% by weight of sulfuric acid or 8.0 to 20% by weight of phosphoric acid and 4.0 to 10% by weight. Contains hydrogen fluoride and 4.5 to 11 wt .-% acid-soluble aromatic nitro compound.
  • the pickling agent with the aforementioned concentration ranges is characterized by a sufficiently high pickling rate without the base material being attacked. In addition, it is particularly inexpensive.
  • magnesium in the amounts mentioned will Mordant transferred to a thixotropic gel. This will the order of a sufficient amount for the Guaranteed pickling process required pickling agent. It is particularly advantageous to use the magnesium in metallic Form, as magnesium oxide, hydroxide, carbonate or sulfate add.
  • the mordant in its application as Spray stain with a content of 9.5 to 15.5% by weight Sulfuric acid or 15.0 to 30.0% by weight phosphoric acid, and 4.0 to 11.0 wt% hydrogen fluoride, 4.5 to 11.5 % By weight acid-soluble aromatic nitro compound and 2.5 up to 4.5% by weight of magnesium compound (calculated as Mg) use.
  • mordant in its application as a brush stain 12.0 to 16.0% by weight sulfuric acid or 18.0 to 30.0% by weight Phosphoric acid and 4.5 to 12.0% by weight of hydrogen fluoride, 2.5 to 9.5% by weight of acid-soluble aromatic Nitro compound and 3.0 to 5.5% by weight magnesium compound (calc. as Mg).
  • Suitable acid-soluble aromatic nitro compounds are those that have at least one nitro and at least one acidic group, especially a carboxyl or Have sulfonic acid group. It is particularly advantageous it, as an acid-soluble aromatic nitro compound Use m-nitrobenzenesulfonate and / or 3-nitrophthalate.
  • the temperatures at which the invention Pickling agents are used depending on the type of Different application. When used as a bath stain it is set to a value in the range of 15 to 80 ° C. Depending on the degree of scaling or Oxide coating of the pickling material 5 to 90 min., The shorter ones Pickling times for the higher pickling temperatures and the longer pickling times for the lower pickling temperatures be valid.
  • the pickling agent When using the pickling agent as a spray or Brush stains are usually through the pickling temperatures the prevailing room or ambient temperatures specified. They are generally between 15 and 35 ° C. The required pickling time is about 15 to 180 min.
  • the plate pairs were spaced 2 minutes apart. optically on Descaling the weld and removing Tarnished colors checked.
  • the sheet pair made of material 1.4511 was after 10 min made of material 1.4462 after 24 min. clean.
  • the clear, viscous liquid obtained was applied to metal sheets of steel grade 1.4301, which is a hand drawn Welded seam, with a pressure of 6 bar sprayed.
  • the obtained 1 to 2 mm thick film flowed due to its thixotropy also on vertical surfaces Not.
  • the spray stain was rinsed.
  • the weld was descaled.
  • the entire sheet surface was uniformly light and weak angebeizt.
  • a non-flowable, opaque paste was created that with a brush on the weld of a sheet of metal Stainless steel quality 1.4571 in a thickness of 2 to 3 mm was applied.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Detergent Compositions (AREA)
  • Glass Compositions (AREA)
  • Catalysts (AREA)

Claims (6)

  1. Agent de décapage aqueux, exempt d'agents émulsifiants et d'agents mouillants, pour acier fin, à base d'acide sulfurique ou d'acide phosphorique et d'acide fluorhydrique, caractérisé par le fait qu'il contient (pour 100 % en poids de substance)
    de 1,5 à 16 % en poids d'acide sulfurique ou
    de 2,0 à 30 % en poids d'acide phosphorique, ainsi que
    de 0,5 à 14 % en poids d'acide fluorhydrique et
    de 0,5 à 15,5 % en poids d'un composé nitré aromatique soluble en milieu acide
    auquel on n'ajoute pas de composé de fer III, et auquel on peut ajouter seulement pendant la phase de démarrage un agent oxydant capable d'oxyder le fer II en fer III.
  2. Agent de décapage selon la revendication 1, caractérisé par le fait que, lorsqu'il est utilisé sous forme de bain, il contient
    de 5,0 à 11 % en poids d'acide sulfurique ou
    de 8,0 à 20 en poids d'acide phosphorique, ainsi que
    de 4,0 à 10 % en poids d'acide fluorhydrique et
    de 4,5 à 11 % en poids d'un composé nitré aromatique soluble en milieu acide.
  3. Agent de décapage selon la revendication 1, caractérisé par le fait que, lorsqu'il est appliqué par pulvérisation ou au pinceau, il contient en outre de 2,5 à 5,5 % en poids d'un composé de magnésium (calculé comme Mg).
  4. Agent de décapage selon la revendication 3, caractérisé par le fait que, lorsqu'il est appliqué par pulvérisation, il contient
    de 9,5 à 15,5 en poids d'acide sulfurique ou
    de 15,0 à 30,0 % en poids d'acide phosphorique, ainsi que
    de 4,0 à 11,0 % en poids d'acide fluorhydrique,
    de 4,5 à 11,5 % en poids d'un composé nitré aromatique soluble en milieu acide, et
    de 2,5 à 4,5 % en poids d'un composé de magnésium (calculé comme Mg).
  5. Agent de décapage selon la revendication 3, caractérisé par le fait que, lorsqu'il est appliqué au pinceau, il contient
    de 12,0 à 16,0 % en poids d'acide sulfurique ou
    de 18,0 à 30,0 % en poids d'acide phosphorique, ainsi que
    de 4,5 à 12,0 % en poids d'acide fluorhydrique,
    de 2,5 à 9,5 % en poids d'un composé nitré aromatique soluble en milieu acide, et
    de 3,0 à 5,5 % en poids d'un composé de magnésium (calculé comme Mg).
  6. Agent de décapage selon une ou plusieurs des revendications 1 à 5, caractérisé par le fait qu'il contient, en tant que composé nitré aromatique soluble en milieu acide, du m-nitrobenzènesulfonate et/ou du 3-nitrophtalate.
EP99942796A 1998-07-29 1999-07-22 Decapant pour aciers speciaux Expired - Lifetime EP1100982B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19833990 1998-07-29
DE19833990A DE19833990A1 (de) 1998-07-29 1998-07-29 Beizmittel für Edelstähle
PCT/EP1999/005226 WO2000006797A1 (fr) 1998-07-29 1999-07-22 Decapant pour aciers speciaux

Publications (2)

Publication Number Publication Date
EP1100982A1 EP1100982A1 (fr) 2001-05-23
EP1100982B1 true EP1100982B1 (fr) 2002-12-04

Family

ID=7875604

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99942796A Expired - Lifetime EP1100982B1 (fr) 1998-07-29 1999-07-22 Decapant pour aciers speciaux

Country Status (6)

Country Link
US (1) US7041629B2 (fr)
EP (1) EP1100982B1 (fr)
AT (1) ATE229098T1 (fr)
CA (1) CA2338484A1 (fr)
DE (2) DE19833990A1 (fr)
WO (1) WO2000006797A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10160318A1 (de) * 2001-12-07 2003-06-18 Henkel Kgaa Verfahren zum Beizen von martensitischem oder ferritischem Edelstahl
DE102009038795A1 (de) * 2009-08-25 2011-05-05 Poligrat Gmbh Beizverfahren für Edelstahl
DE102013101629A1 (de) 2013-02-19 2014-08-21 Wolfgang DAMBACHER Vorrichtung und Verfahren zur Oberflächenbehandlung von Werkstücken

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2339467A (en) * 1942-02-13 1944-01-18 Hoe & Co R Mechanism for registering printing plates
US2698781A (en) * 1953-04-27 1955-01-04 Enthone Accelerating action of acids on metals
US3239467A (en) * 1962-02-15 1966-03-08 Lord Corp Metal cleaning and treating compositions
GB1279834A (en) * 1968-10-07 1972-06-28 Chugai Kasei Co Ltd Improvements in metal cleaning and etching compositions
DE2507059A1 (de) * 1975-02-19 1976-09-02 Basf Ag Verfahren zur reinigung von eisen enthaltenden metallgegenstaenden
JPS5610396A (en) * 1979-07-07 1981-02-02 Nobuo Miyazawa Additive for acid bath for descaling of stainless steel
DE3105508A1 (de) * 1981-02-14 1982-09-02 Metallgesellschaft Ag, 6000 Frankfurt Beiz- und entrostungspaste fuer metalle
CA1185152A (fr) * 1982-01-22 1985-04-09 Thomas W. Bleeks Decapage selectif par voie chimique des surfaces enduites des substrats en super-alliage
DE3530132A1 (de) * 1985-08-23 1987-02-26 August Wittig Oberflaechen beiz- und entrostungspaste zum reinigen von metalloberflaechen insbesondere aus edelstahl und/oder aluminium u. aluminiumlegierungen
US4971631A (en) * 1988-03-07 1990-11-20 Bernard Lietaer Compositions and methods for cleaning hard surfaces
FR2657888B1 (fr) * 1990-02-08 1994-04-15 Ugine Aciers Procedes de decapage de materiaux en acier inoxydable.
FR2673200A1 (fr) * 1991-02-25 1992-08-28 Ugine Aciers Procede de surdecapage de materiaux en acier tels que les aciers inoxydables et les aciers allies.
FR2683551B1 (fr) * 1991-11-07 1994-09-16 Ugine Sa Procede de decapage de materiaux en acier en continu sur une ligne de traitement.
DE4237021C1 (de) * 1992-11-02 1994-02-10 Poligrat Gmbh Mittel zum Beizen der Oberfläche von Chromnickelstählen und Chromstählen sowie Verwendung des Mittels
FR2721328B1 (fr) * 1994-06-15 1996-09-06 Ugine Sa Procédé de décapage de matériaux métalliques, notamment en acier allié, en acier inoxydable ou en alliage de titane, par une solution du type contenant des ions ferriques en milieu acide.
SE504733C2 (sv) * 1994-06-17 1997-04-14 Ta Chemistry Ab Förfarande för betning
US5711996A (en) * 1995-09-28 1998-01-27 Man-Gill Chemical Company Aqueous coating compositions and coated metal surfaces
US5702534A (en) * 1996-05-24 1997-12-30 Armco Inc. Hydrogen peroxide pickling of stainless steel

Also Published As

Publication number Publication date
EP1100982A1 (fr) 2001-05-23
US7041629B2 (en) 2006-05-09
DE19833990A1 (de) 2000-02-10
WO2000006797A1 (fr) 2000-02-10
DE59903669D1 (de) 2003-01-16
ATE229098T1 (de) 2002-12-15
US20040053801A1 (en) 2004-03-18
CA2338484A1 (fr) 2000-02-10

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