EP0442775A1 - Verfahren zum Beizen von Gegenständen aus Stahl, insbesondere aus rostfreiem Stahl - Google Patents

Verfahren zum Beizen von Gegenständen aus Stahl, insbesondere aus rostfreiem Stahl Download PDF

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Publication number
EP0442775A1
EP0442775A1 EP91400252A EP91400252A EP0442775A1 EP 0442775 A1 EP0442775 A1 EP 0442775A1 EP 91400252 A EP91400252 A EP 91400252A EP 91400252 A EP91400252 A EP 91400252A EP 0442775 A1 EP0442775 A1 EP 0442775A1
Authority
EP
European Patent Office
Prior art keywords
solution
chosen
pickling
acid
ions
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.)
Granted
Application number
EP91400252A
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English (en)
French (fr)
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EP0442775B1 (de
Inventor
Dominique Henriet
Didier Paul
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.)
USINOR SA
Original Assignee
Ugine Aciers SA
Ugine Aciers de Chatillon et Guegnon
Ugine SA
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Filing date
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Application filed by Ugine Aciers SA, Ugine Aciers de Chatillon et Guegnon, Ugine SA filed Critical Ugine Aciers SA
Publication of EP0442775A1 publication Critical patent/EP0442775A1/de
Application granted granted Critical
Publication of EP0442775B1 publication Critical patent/EP0442775B1/de
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
    • 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
    • C23G1/088—Iron or steel solutions containing organic acids

Definitions

  • the invention relates to a process for pickling metallic steel materials, in particular stainless steel.
  • the pickling process can be implemented on metallic steel materials, in particular stainless steel in an industrial environment, before leaving the factory, for example for descaling but also by non-professionals in metallurgy for cleaning stainless steel elements.
  • the pickling operation consists of immersing the materials in pickling baths composed of nitric acid and hydrofluoric acid in a proportion of 6 to 16% of HNO3 per liter and 1 at 5% HF per liter, the temperature of use of the baths being between 40 ° C and 60 ° C.
  • nitric acid leads to the release of particularly toxic oxide or nitrogen dioxide vapors, and to the release of nitro compounds such as nitrites and nitrates in the effluents. If the maximum authorized content of nitrates is relatively high, that relating to nitrites is much lower because nitrites lead to the formation of harmful nitrosamines.
  • FR-A-2 587 369 further describes a process for pickling stainless steel materials in which a pickling bath composed of hydrofluoric acid, dissolved ferric iron is used, the balance being water.
  • the bath is used at a temperature between 15 and 70 ° C.
  • the ferric iron content of the bath is maintained by means of an injection of air, or by circulation in the open air.
  • hydrofluoric acid-based process has the drawback that, since hydrofluoric acid can be dangerous to handle, it cannot be suitable for all cleaning operations by spraying or spraying metallic elements such as, for example, a tank or a tank.
  • Document JP-A-7547826 also discloses a process for pickling metallic materials of stainless steel, consisting of the use of a bath composed of a mixture of halogenated acids containing in a determined proportion of hydrochloric acid.
  • the main agent entering into the chemical reaction is hydrochloric acid which reacts with the material to be pickled to give a ferrous chloride with evolution of hydrogen according to the reaction: 2 HCl + Fe ------ FeCl2 + H2
  • the object of the invention is to propose a non-polluting process which can be used in the metallurgy industry as well as by non-metallurgical professionals.
  • the inventors of the present invention have discovered that the pickling of metallic steel materials, in particular stainless steel could be carried out without the need to use an oxidizing corrosive acid such as HF or HCl, by oxidation with a Fe2+ mixture. / Fe3+, the redox potential of which is maintained between determined values, the Fe2+ and Fe3+ ions being maintained in aqueous solution by an organic acid presenting no danger to humans during its use.
  • the subject of the invention is therefore a process for pickling steel materials, in particular stainless steel, characterized in that the materials are treated with an aqueous solution containing ferrous ions and ferric ions as well as a non-organic acid. oxidizing iron in an amount sufficient to keep the Fe2+ and Fe3+ ions in solution, the ferrous and ferric ions being present in the solution in an Fe2+ / Fe3+ ratio between 10/90 and 40/60, and in this that the Fe2+ / Fe3+ ratio is maintained in the interval defined by the addition of hydrogen peroxide.
  • the acid in the solution by a secondary reaction, during pickling, will give either easily recyclable salts in an industrial environment, or non-toxic salts so that the process can be used easily and without danger.
  • the organic acid is preferably a compound represented by the general formula
  • R (COOH) n in which R represents a C1-C4 alkyl, C1-C4 hydroxyalkyl group or an aryl, aralkyl or C6-C14 alkaryl group, optionally substituted by one or more substituents chosen from C1-C4 alkyl groups and atoms of halogen and n represents 1, 2 or 3.
  • organic acids mention may be made of formic, acetic, propionic, butanoic, lactic, benzoic, phthalic and naphthoic acid.
  • the Fe2+ / Fe3+ ratio is between 10/90 and 40/60, preferably between 10/90 and 25/75, and even better is around 20/80.
  • the ratio and therefore the reaction kinetics are maintained by regenerating the Fe3+ ion by the addition of hydrogen peroxide.
  • the peracid is advantageously chosen from perboric, peracetic, percarbonic, perbenzoic, persulfuric, perphosphoric, periodic and perphthalic acids.
  • the persalt is advantageously chosen from sodium percarbonate and magnesium perborate and the organic peroxide is preferably urea peroxide.
  • the process implementation temperature is advantageously between 10 and 90 ° C.
  • the invention also relates to a pickling product for steel materials, in particular stainless steel, characterized in that it comprises on the one hand a solution containing ferrous ions and ferric ions, the ratio Fe++ / Fe +++ being between 10/90 and 40/60 as well as a quantity sufficient to maintain in solution the ions Fe2+ and Fe3+ of an organic acid non oxidizing of iron, and on the other hand a source of peroxide d hydrogen intended to be added to the solution to maintain the ratio Fe2+ / Fe3+ in the defined range.
  • the organic acid and the source of hydrogen peroxide are as defined above.
  • the pickling and cleaning product can be transported without special packaging to the place of its use, and can be used without any particular precaution anywhere, including for pickling closed containers such as tanks, fixed or mobile tanks, or containers.
  • the method according to the invention can be used for the pickling of metallic steel materials, in particular stainless steel and in particular for descaling, polishing and cleaning of said materials, the treatment being able to be carried out in a bath, by spraying or spraying.
  • organic acids are that they decompose into CO2, H2O and H2, decomposition residues which do not harm the ecological environment when they are released into the atmosphere, in effluents or even at sea.
  • Another advantage is that the organic medium allows the formation of a passive film reducing the corrosion of the metal.
  • the pickling solution used in the invention avoids the redeposition of certain metals, such as Cu, Ni, Cr, Sn, Zn during pickling, this thanks to the high value of the redox potential of the solution.
  • the formation of the Fe3+ ion is controlled by measuring the redox potential of the pickling bath.
  • the redox potential or REDOX is the potential difference measured between a non-corrodable electrode (for example made of platinum) and a reference electrode / (for example Hg / HgCl or saturated calomel), these two electrodes being immersed in the pickling solution.
  • the measured value makes it possible, on the one hand to characterize the oxidizing power of the pickling bath and on the other hand, to readjust the bath by the introduction of H2O2 or of the compound capable of supplying H2O2.
  • the source of H2O2 introduced into the base pickling solutlon can be the peracid homologous to the acid of the solution, which has the advantage of not modifying the initial composition of the solution.
  • organic acid / peracid pairs which can be used for implementing the process can be the following: acetic acid / peracetic acid, benzoic acid / perbenzoic acid, phthalic acid / perphthalic acid.
  • H202 an organic oxidizing agent such as percarbonic acid (H4 (CO3) 2, 3H202) or even peroxide urea (CO (NH2) 2, H2O2) which breaks down into CO2, H20 and N2.
  • organic oxidizing agent such as percarbonic acid (H4 (CO3) 2, 3H202) or even peroxide urea (CO (NH2) 2, H2O2) which breaks down into CO2, H20 and N2.
  • the advantages of the process also reside in the fact that the oxidant is created "in situ" without the addition of toxic or polluting substances and without the effluents and used acid solutions being a danger for humans. Also the product according to the invention comprising the acid solution and its liquid or solid oxidant, can be used in all environments, even in confined environments.

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)
  • ing And Chemical Polishing (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
  • Detergent Compositions (AREA)
EP91400252A 1990-02-08 1991-02-01 Verfahren zum Beizen von Gegenständen aus Stahl, insbesondere aus rostfreiem Stahl Expired - Lifetime EP0442775B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9001481A FR2657888B1 (fr) 1990-02-08 1990-02-08 Procedes de decapage de materiaux en acier inoxydable.
FR9001481 1990-02-08

Publications (2)

Publication Number Publication Date
EP0442775A1 true EP0442775A1 (de) 1991-08-21
EP0442775B1 EP0442775B1 (de) 1995-04-26

Family

ID=9393510

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91400252A Expired - Lifetime EP0442775B1 (de) 1990-02-08 1991-02-01 Verfahren zum Beizen von Gegenständen aus Stahl, insbesondere aus rostfreiem Stahl

Country Status (13)

Country Link
US (1) US5164016A (de)
EP (1) EP0442775B1 (de)
JP (1) JPH04218685A (de)
KR (1) KR100189579B1 (de)
AT (1) ATE121805T1 (de)
CA (1) CA2035847A1 (de)
CZ (1) CZ281613B6 (de)
DE (1) DE69109147T2 (de)
ES (1) ES2072560T3 (de)
FI (1) FI96519C (de)
FR (1) FR2657888B1 (de)
NO (1) NO303788B1 (de)
RU (1) RU2072397C1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0776256A1 (de) * 1994-09-26 1997-06-04 Calgon Vestal, Inc. Säurebehandlung von rostfreiem stahl

Families Citing this family (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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.
US5244000A (en) * 1991-11-13 1993-09-14 Hughes Aircraft Company Method and system for removing contaminants
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
USH2087H1 (en) * 1998-05-19 2003-11-04 H. C. Starck, Inc. Pickling of refractory metals
DE19833990A1 (de) * 1998-07-29 2000-02-10 Metallgesellschaft Ag Beizmittel für Edelstähle
TW529041B (en) * 2000-12-21 2003-04-21 Toshiba Corp Chemical decontamination method and treatment method and apparatus of chemical decontamination solution
AU2002252617B2 (en) 2001-04-09 2007-05-31 Ak Steel Properties, Inc. Hydrogen peroxide pickling scheme for stainless steel grades
CA2443687C (en) 2001-04-09 2009-08-11 Vijay N. Madi Hydrogen peroxide pickling of silicon-containing electrical steel grades
WO2002081380A1 (en) * 2001-04-09 2002-10-17 Ak Properties, Inc. Apparatus and method for removing hydrogen peroxide from spent pickle liquor
US7964085B1 (en) 2002-11-25 2011-06-21 Applied Materials, Inc. Electrochemical removal of tantalum-containing materials
US20060105182A1 (en) * 2004-11-16 2006-05-18 Applied Materials, Inc. Erosion resistant textured chamber surface
WO2005003273A1 (en) * 2003-07-01 2005-01-13 William A. Barnstead Engineering Corporation Method, process, chemistry and apparatus for treating a substrate
US7910218B2 (en) * 2003-10-22 2011-03-22 Applied Materials, Inc. Cleaning and refurbishing chamber components having metal coatings
US7579067B2 (en) * 2004-11-24 2009-08-25 Applied Materials, Inc. Process chamber component with layered coating and method
US8617672B2 (en) 2005-07-13 2013-12-31 Applied Materials, Inc. Localized surface annealing of components for substrate processing chambers
US7762114B2 (en) 2005-09-09 2010-07-27 Applied Materials, Inc. Flow-formed chamber component having a textured surface
US7981262B2 (en) 2007-01-29 2011-07-19 Applied Materials, Inc. Process kit for substrate processing chamber
US7942969B2 (en) 2007-05-30 2011-05-17 Applied Materials, Inc. Substrate cleaning chamber and components
WO2010056825A2 (en) * 2008-11-14 2010-05-20 Ak Steel Properties, Inc. Ferric pickling of silicon steel
JP2012180562A (ja) * 2011-03-01 2012-09-20 Yushiro Chemical Industry Co Ltd さび除去剤水溶液
US8734586B2 (en) 2012-02-02 2014-05-27 Sematech, Inc. Process for cleaning shield surfaces in deposition systems
US8734907B2 (en) 2012-02-02 2014-05-27 Sematech, Inc. Coating of shield surfaces in deposition systems
KR102013528B1 (ko) * 2018-10-10 2019-10-21 (주)스템코코리아 스테인레스강 세정용 조성물 및 이를 이용한 스테인레스강 세정 방법
CN111519225B (zh) * 2018-11-27 2021-09-14 广州三孚新材料科技股份有限公司 Abs塑料的无铬无锰粗化液及其使用方法
CN114086181B (zh) * 2021-10-19 2023-11-10 富联裕展科技(深圳)有限公司 蚀刻液以及制备铝合金工件的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1109389A (en) * 1966-03-03 1968-04-10 Montedison Spa Process for cleaning and/or pickling ferrous metallic surfaces
FR2262099A1 (en) * 1974-02-27 1975-09-19 Pfizer Rust removal process for steel - esp for ships holds, comprising treatment with ammonia and org. acid, then adding an oxidant
GB2000196A (en) * 1977-06-24 1979-01-04 Tokai Electro Chemical Co Controlling stainless steel pickling solution by hydrogen peroxide and sulphuric acid addition
BE891163A (fr) * 1981-11-17 1982-05-17 Centre Rech Metallurgique Perfectionnements aux procedes de traitement de produits en acier
FR2551465A3 (fr) * 1983-09-02 1985-03-08 Gueugnon Sa Forges Procede de decapage acide des aciers inoxydables et solution acide pour sa mise en oeuvre

Family Cites Families (4)

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Publication number Priority date Publication date Assignee Title
US3873362A (en) * 1973-05-29 1975-03-25 Halliburton Co Process for cleaning radioactively contaminated metal surfaces
BE871631A (fr) * 1978-10-27 1979-04-27 Centre Rech Metallurgique Procede de decapage continu de toles en acier.
JPS5839234B2 (ja) * 1981-10-26 1983-08-29 住友金属工業株式会社 鋼線材の酸洗脱スケ−ル方法
FR2563824B1 (fr) * 1984-05-04 1986-09-12 Atochem Stabilisation de solutions aqueuses acides contenant du peroxyde d'hydrogene et des ions metalliques

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1109389A (en) * 1966-03-03 1968-04-10 Montedison Spa Process for cleaning and/or pickling ferrous metallic surfaces
FR2262099A1 (en) * 1974-02-27 1975-09-19 Pfizer Rust removal process for steel - esp for ships holds, comprising treatment with ammonia and org. acid, then adding an oxidant
GB2000196A (en) * 1977-06-24 1979-01-04 Tokai Electro Chemical Co Controlling stainless steel pickling solution by hydrogen peroxide and sulphuric acid addition
BE891163A (fr) * 1981-11-17 1982-05-17 Centre Rech Metallurgique Perfectionnements aux procedes de traitement de produits en acier
FR2551465A3 (fr) * 1983-09-02 1985-03-08 Gueugnon Sa Forges Procede de decapage acide des aciers inoxydables et solution acide pour sa mise en oeuvre

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN, vol. 7, no. 167 (C-177)[1312], 22 juillet 1983; & JP-A-58 073 778 (SUMITOMO KINZOKU KOGYO K.K.) 04-05-1983 *
PATENT ABSTRACTS OF JAPAN, vol. 7, no. 167 (C-177)[1312], 22 juillet 1983; & JP-A-58 073 779 (SUMITOMO KINZOKU KOGYO K.K.) 04-05-1983 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0776256A1 (de) * 1994-09-26 1997-06-04 Calgon Vestal, Inc. Säurebehandlung von rostfreiem stahl
EP0776256A4 (de) * 1994-09-26 1998-05-20 Squibb & Sons Inc Säurebehandlung von rostfreiem stahl

Also Published As

Publication number Publication date
EP0442775B1 (de) 1995-04-26
CA2035847A1 (en) 1991-08-09
KR100189579B1 (ko) 1999-06-01
US5164016A (en) 1992-11-17
KR910015721A (ko) 1991-09-30
CS31691A3 (en) 1992-04-15
NO910448L (no) 1991-08-09
ATE121805T1 (de) 1995-05-15
FI910594A (fi) 1991-08-09
FR2657888A1 (fr) 1991-08-09
RU2072397C1 (ru) 1997-01-27
CZ281613B6 (cs) 1996-11-13
NO910448D0 (no) 1991-02-06
NO303788B1 (no) 1998-08-31
ES2072560T3 (es) 1995-07-16
FI96519C (fi) 1996-07-10
DE69109147T2 (de) 1995-08-31
DE69109147D1 (de) 1995-06-01
FR2657888B1 (fr) 1994-04-15
FI96519B (fi) 1996-03-29
FI910594A0 (fi) 1991-02-07
JPH04218685A (ja) 1992-08-10

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