EP0188975B2 - Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen - Google Patents

Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen Download PDF

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Publication number
EP0188975B2
EP0188975B2 EP85420013A EP85420013A EP0188975B2 EP 0188975 B2 EP0188975 B2 EP 0188975B2 EP 85420013 A EP85420013 A EP 85420013A EP 85420013 A EP85420013 A EP 85420013A EP 0188975 B2 EP0188975 B2 EP 0188975B2
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EP
European Patent Office
Prior art keywords
solution
process according
scouring
ions
steels
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
EP85420013A
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English (en)
French (fr)
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EP0188975B1 (de
EP0188975A1 (de
EP0188975B8 (de
Inventor
S.A. Ugine
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.)
Ugine SA
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Ugine SA
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Application filed by Ugine SA filed Critical Ugine SA
Priority to DE3588013T priority Critical patent/DE3588013T3/de
Priority to EP85420013A priority patent/EP0188975B8/de
Priority to AT85420013T priority patent/ATE121804T1/de
Publication of EP0188975A1 publication Critical patent/EP0188975A1/de
Publication of EP0188975B1 publication Critical patent/EP0188975B1/de
Publication of EP0188975B2 publication Critical patent/EP0188975B2/de
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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

Definitions

  • the present invention relates to a new method for carrying out the pickling of steel parts, and it relates more particularly, although not exclusively, to the acid pickling of steels stainless.
  • the ultimate operation for carrying out the stripping consists in applying to the steel parts, mixtures composed of nitric acid HNO 3 at approximately 150 g per liter and hydrofluoric acid HF at a concentration between 10 and 30 g per liter. Processing temperatures are often in the range of 40 to 60 ° C.
  • the present invention aims to avoid these drawbacks by eliminating the use of nitric acid as a pickling oxidizer.
  • the subject of the present invention is a process for pickling steel parts, and in particular stainless steel, consisting in applying an aqueous pickling solution consisting of hydrofluoric acid, fluoride ions and ferric pickling ions in solution in l water and, in order to maintain a constant pickling power in the aqueous hydrofluoric acid solution having a pH of 0 to 3, to maintain the concentration of Fe 3+ ions, present in the form of fluorinated complexes, at an Fe value 3+ between 1 and 150 g per liter, by reoxidation of Fe 2+ ions formed during pickling with oxygen or an oxygen-containing gas, maintaining the REDOX potential at a value between -200 and +800 mV, potential measured between a platinum electrode and an Ag / AgCl reference electrode placed in the solution.
  • an aqueous pickling solution consisting of hydrofluoric acid, fluoride ions and ferric pickling ions in solution in l water and, in order to maintain a constant pickling power in the a
  • the solution has an acid concentration hydrofluoric between 5 and 50 g per liter, for a pH between 0 and 3.
  • the treating solution is applied at a temperature between 10 and 70 ° C, for a residence time between 30 seconds and 5 minutes.
  • REDOX potential is the difference in potential measured between a non- corrodable (eg platinum) and a reference electrode (eg Ag / AgCl or calomel saturated), these two electrodes being immersed in the bath to be studied. The value thus measured allows characterize the oxidizing power of the chemical solution.
  • a non- corrodable eg platinum
  • a reference electrode eg Ag / AgCl or calomel saturated
  • the new process consists in replacing the oxidant HNO 3 by the oxidant Fe 3+ introduced in the form of fluorinated complexes.
  • This process can be used not only to pickle stainless steels, but also read most mild steels, especially silicon steels (which are currently often pickled with hydrochloric acid or sulfuric acid, acids requiring regeneration facilities or very important treatment).

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  • 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)

Claims (11)

  1. Verfahren zum Beizen von Stücken aus Stahl und insbesondere aus rostfreiem Stahl, bestehend aus dem Auftragen einer wässrigen Beizlösung, bestehend aus Fluorwasserstoffsäure, Fluoridionen und Eisen(III)-lonen vom Beizen in wässriger Lösung und, um ein konstantes Beizvermögen in der wässrigen Fluorwasserstoffsäure-Lösung mit einem pH-Wert von 0 bis 3 beizubehalten, dem Aufrechterhalten der Konzentration der in Form von Fluorkomplexen vorhandenen Fe3+-lonen bei einem Fe3+-Wert zwischen 1 und 150 g/l durch Rückoxidation der bei dem Beizen durch Oxidation mit Sauerstoff oder einem Sauerstoff enthaltenden Gas gebildeten Fe2+-lonen und dem Aufrechterhalten des Redox-Potentials auf einem Wert zwischen -200 und +800 mV, wobei das Potential zwischen einer Platin-Elektrode und einer Ag/AgCl-Referenzelektrode, angeordnet in der Lösung, gemessen wird.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Rückoxidation der Fe2+-lonen durch Oxidation mit Sauerstoff durch geeignete Belüftung der Beizlösung durchgeführt wird.
  3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass die Belüftung der Lösung durch den Kontakt der Lösungsoberfläche mit Luft erzielt wird.
  4. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass die Belüftung der Beizlösung durch Pumpen und Aufstauen der Behandlungslösung an der freien Luft erzielt wird.
  5. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass die Belüftung der Lösung durch Einspritzen eines Sauerstoff enthaltenden Gases erzielt wird.
  6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, dass das Einspritzen des Gases bei einem Druck zwischen 0,1 und 5 bar durchgeführt wird.
  7. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Rückoxidation durch Zugabe von H2O2 vervollständigt wird.
  8. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Lösung bei einem pH-Wert zwischen 0 und 3 eine Konzentration an Fluorwasserstoff-Säure zwischen 5 und 50 g/l aufweist.
  9. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Behandlungslösung bei einer Temperatur zwischen 10 und 70 °C bei einer Verweilzeit zwischen 30 Sekunden und 5 Minuten angewandt wird.
  10. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass man das Redox-Potential durch das Regulieren des Gas-Durchsatzes auf den gewünschten Wert einstellt.
  11. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es für kaltgewalzten und geglühten Stahl folgenden Daten entspricht: HF 20 bis 25 g/l pH 1 bis 1,5 Fe3+ 30 g/l Redox-Potential = 100 bis 250 mV, bezogen auf Ag/AgCl, Temperatur 50 bis 55 °C Behandlungsdauer 1 bis 2 Minuten Einspritzen von Luft 80 Nm3/h pro Bad mit 25 bis 30 m3.
EP85420013A 1985-01-22 1985-01-22 Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen Expired - Lifetime EP0188975B8 (de)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE3588013T DE3588013T3 (de) 1985-01-22 1985-01-22 Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen.
EP85420013A EP0188975B8 (de) 1985-01-22 1985-01-22 Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen
AT85420013T ATE121804T1 (de) 1985-01-22 1985-01-22 Verfahren zum säuren beizen von stahlen, insbesondere von rostfreien stahlen.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP85420013A EP0188975B8 (de) 1985-01-22 1985-01-22 Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen

Publications (4)

Publication Number Publication Date
EP0188975A1 EP0188975A1 (de) 1986-07-30
EP0188975B1 EP0188975B1 (de) 1995-04-26
EP0188975B2 true EP0188975B2 (de) 2001-10-24
EP0188975B8 EP0188975B8 (de) 2002-01-09

Family

ID=8194569

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85420013A Expired - Lifetime EP0188975B8 (de) 1985-01-22 1985-01-22 Verfahren zum säuren Beizen von Stahlen, insbesondere von rostfreien Stahlen

Country Status (3)

Country Link
EP (1) EP0188975B8 (de)
AT (1) ATE121804T1 (de)
DE (1) DE3588013T3 (de)

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2587369B1 (fr) * 1985-09-19 1993-01-29 Ugine Gueugnon Sa Procede de decapage acide de produits en acier inoxydable
US5154774A (en) * 1985-09-19 1992-10-13 Ugine Aciers De Chatillon Et Gueugnon Process for acid pickling of stainless steel products
US4872919A (en) * 1988-01-28 1989-10-10 The Procter & Gamble Company Method for removing precipitated calcium citrate from juice pasteurization or sterilization equipment
DE3937438C2 (de) * 1989-02-23 1998-01-29 Wilfried Simmer Verfahren zum Beizen von Stahl
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.
IT1245594B (it) * 1991-03-29 1994-09-29 Itb Srl Processo di decapaggio e di passivazione di acciaio inossidabile senza acido nitrico
IT1255655B (it) * 1992-08-06 1995-11-09 Processo di decapaggio e passivazione di acciaio inossidabile senza impiego di acido nitrico
IT1276955B1 (it) * 1995-10-18 1997-11-03 Novamax Itb S R L Processo di decapaggio e passivazione di acciaio inossidabile senza impiego di acido nitrico
IT1276954B1 (it) * 1995-10-18 1997-11-03 Novamax Itb S R L Processo di decapaggio e di passivazione di acciaio inossidabile senza impiego di acido nitrico
FR2745301B1 (fr) * 1996-02-27 1998-04-03 Usinor Sacilor Procede de decapage d'une piece en acier et notamment d'une bande de tole en acier inoxydable
FR2772050B1 (fr) * 1997-12-10 1999-12-31 Imphy Sa Procede de decapage d'acier et notamment d'acier inoxydable
GB9807286D0 (en) 1998-04-06 1998-06-03 Solvay Interox Ltd Pickling process
DE19850524C2 (de) * 1998-11-03 2002-04-04 Eilenburger Elektrolyse & Umwelttechnik Gmbh Nitratfreies Recycling-Beizverfahren für Edelstähle
IT1312556B1 (it) 1999-05-03 2002-04-22 Henkel Kgaa Processo di decapaggio di acciaio inossidabile in assenza di acidonitrico ed in presenza di ioni cloruro
RU2154696C1 (ru) * 1999-06-08 2000-08-20 Московский государственный вечерний металлургический институт Способ обработки окисленных металлических материалов
DE10160318A1 (de) * 2001-12-07 2003-06-18 Henkel Kgaa Verfahren zum Beizen von martensitischem oder ferritischem Edelstahl
CN101631895B (zh) * 2007-02-12 2013-05-08 汉高股份及两合公司 处理金属表面的方法
KR101373975B1 (ko) * 2008-11-14 2014-03-12 에이케이 스틸 프로퍼티즈 인코포레이티드 제2철 이온을 함유하는 산성 산세척액으로 규소강을 산세척하는 방법
DE102012004907A1 (de) 2012-03-02 2013-09-05 Sms Siemag Ag Verfahren zum Beizen von Standard Stählen

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2474526A (en) 1940-06-15 1949-06-28 Monsanto Chemicals Picking of stainless steels
US2564549A (en) * 1945-07-02 1951-08-14 Albert R Stargardter Pickling treatment
DE899890C (de) * 1952-03-18 1953-12-17 Deutsche Edelstahlwerke Ag Verfahren zum Regenerieren von Beizbaedern
JPS549120A (en) 1977-06-24 1979-01-23 Tokai Electro Chemical Co Method of controlling acid cleaning liquid for stainless steel

Also Published As

Publication number Publication date
EP0188975B1 (de) 1995-04-26
DE3588013T2 (de) 1995-09-14
EP0188975A1 (de) 1986-07-30
DE3588013T3 (de) 2002-06-06
ATE121804T1 (de) 1995-05-15
EP0188975B8 (de) 2002-01-09
DE3588013D1 (de) 1995-06-01

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