WO2002081777A1 - Hydrogen peroxide pickling scheme for stainless steel grades - Google Patents
Hydrogen peroxide pickling scheme for stainless steel grades Download PDFInfo
- Publication number
- WO2002081777A1 WO2002081777A1 PCT/US2002/011135 US0211135W WO02081777A1 WO 2002081777 A1 WO2002081777 A1 WO 2002081777A1 US 0211135 W US0211135 W US 0211135W WO 02081777 A1 WO02081777 A1 WO 02081777A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- tank
- solution
- pickling
- pickling tank
- hydrogen peroxide
- Prior art date
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
- 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
-
- 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
- C23G1/36—Regeneration of waste pickling liquors
-
- 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
- C23G3/00—Apparatus for cleaning or pickling metallic material
- C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
- C23G3/021—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously by dipping
-
- 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
- C23G3/00—Apparatus for cleaning or pickling metallic material
- C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
- C23G3/027—Associated apparatus, e.g. for pretreating or after-treating
Definitions
- This invention relates to a process for pickling ferrous alloy steels
- this invention relates to a process for pickling hot rolled and annealed stainless steel strip using a pickling solution comprising hydrogen peroxide.
- the annealing of stainless steel strip can result in the formation of oxides on the surface of the steel.
- oxides comprised of iron, chromium, nickel and other associated metal oxides, must be removed prior to utilizing the steel.
- the oxides of stainless steel are resistant to most of the common acid treatments. These oxides adhere tightly to the base metal, thus requiring mechanical scale cracking such as shot blasting, roll bending or leveling of the steel strip or electrolytic and/or molten salt bath treatment in order to either loosen these oxides or make the surface more porous prior to pickling.
- the oxides on the surface of the stainless steel have been removed, or "pickled off," using nitric acid in combination with hydrofluoric acid.
- the present invention relates to a process for pickling hot rolled, hot rolled
- the process comprises immersing the stainless steel strip in a pre-pickling tank comprising a solution of sulfuric acid and hydrofluoric acid.
- the strip is then immersed in a pickling tank comprising a solution of sulfuric acid, hydrofluoric acid and hydrogen peroxide.
- the pre-pickling tank (Tank 1 in Figure 1) contains from about 90 g/1 to about 200 g/1 sulfuric acid and from about 10 g/1 to about 60 g/1 hydrofluoric acid.
- the solution in the pre-pickling tank is maintained at a temperature of from about 54°C to about 77°C.
- the pickling tank (Tank 3 in Figure 1) is comprised of a mixture of stabilized hydrogen peroxide, sulfuric acid, and hydrofluoric acid.
- the pickling tank (Tank 3 in Figure 1) is comprised of a mixture of stabilized hydrogen peroxide in a concentration of about 5 g/1 to about 50 g/1, sulfuric acid in a concentration of about 20 g/1 to about 60 g/1, and hydrofluoric acid in a concentration of about 2 g/1 to about 50 g/1.
- the concentration of stabilized hydrogen peroxide is from about 20 g/L to about 40 g/L.
- the concentration of stabilized hydrogen peroxide is from about 25 g/L to about 35 g/L.
- the concentration of hydrogen peroxide is from about 5 g/L to less than 10 g/L.
- the solution in the pickling tank is maintained at a temperature of from about 20°C to about 60°C and is preferably at a temperature of from about 35 °C to about 50°C.
- the strip Prior to immersing the steel strip in the pickling tank, the strip may be scrubbed, preferably using a scrubber-brush machine. In addition, the strip may also be immersed in a de-smutting tank immediately prior to being scrubbed.
- the de-smutting tank contains a solution comprising hydrogen peroxide, sulfuric acid and hydrofluoric acid, which is the overflow pickle solution form the pickling tank that is channeled back into the de-smutting tank.
- a filtration device and a heat exchanger are external to and coupled to the pickling tank.
- the filtration system and heat exchanger are arranged in a re-circulating loop so that at any time, a portion of the solution from the pickling tank is routed through the filtration system and heat exchanger.
- the resulting solution is deposited back into the pickling tank through at least one nozzle located inside the pickling tank.
- Figure 1 Scheme 1 : Basic two-tank scheme for hydrogen peroxide pickling of stainless steel.
- Figure 2 Scheme 2: Scheme for hydrogen peroxide pickling of stainless steel with intermediate treatment of a de-smutting tank followed by a scrubber-brush machine.
- Figure 3 Scheme 3: Scheme for hydrogen peroxide pickling of stainless steel with intermediate treatment of a de-smutting tank followed by a scrubber-brush apparatus and where Tank 3 is equipped with a filtration unit and heat exchanger.
- the present invention relates to a process for pickling hot rolled, hot rolled
- the process comprises at least one pre-pickling tank and at least one pickling tank, and optionally includes a scrubber-brush tank, a de- smutting tank, a filtration unit and a heat exchanger.
- the steel strip is first immersed into at least one pre-pickling tank (Tank 1 in Figure 1).
- the solution contained in the pre-pickling tank (Tank 1 in Figure 1) is comprised of a mixture of sulfuric acid and hydrofluoric acid.
- the sulfuric acid is in a concentration of from about 90 g/1 to about 200 g/1 and hydrofluoric acid, in a concentration of about 10 g/1 to about 60 g/1.
- This solution is maintained at an elevated temperature of about 54°C to about 77°C.
- the pickling tank (Tank 3 in Figure 1) is comprised of a mixture of stabilized hydrogen peroxide, sulfuric acid, and hydrofluoric acid.
- the pickling tank (Tank 3 in Figure 1) is comprised of a mixture of stabilized hydrogen peroxide in a concentration of about 5 g/1 to about 50 g/1, sulfuric acid in a concentration of about 20 g/1 to about 60 g/1, and hydrofluoric acid in a concentration of about 2 g/1 to about 50 g/1.
- the concentration of stabilized hydrogen peroxide is from about 20 g/L to about 40 g/L.
- the concentration of stabilized hydrogen peroxide is from about 25 g/L to about 35 g/L.
- the concentration of hydrogen peroxide is from about 5 g/L to less than 10 g/L.
- This pickling tank is maintained at a temperature of about 20°C to about 60°C, with a preferred temperature range of about 35 °C to about 50°C.
- FIG. 1 further optional steps may also be added to this pickling process.
- One embodiment includes the addition of a scrubber-brush tank and a de- smutting tank to the pickling process.
- the scrubber-brush tank serves to mechanically remove, at least in part, oxides (scale) from the stainless steel strip.
- the de-smutting tank (Tank 2 in Figure 2) receives the pickle solution overflow from Tank 3.
- oxide on the steel strip, received from Tank 1 can start to react with the hydrogen peroxide- containing pickle solution.
- the subsequent scrubber-brush step (Scrubber Brush- 1 in Figure 2) mechanically removes the oxide from the strip surface.
- the pickling process in Tank 3 is an exothermic reaction.
- the heat produced by the pickling process may be due in part to the reaction of loose oxide particles in the tank with the pickling solution. Accordingly, in order to minimize the rise in temperature and degradation of hydrogen peroxide in Tank 3, it is desirable to keep the loose oxide particles out of the pickling tank and control the tank temperature to below 54°C and preferably below 43°C.
- the following hot rolled stainless steels are processed on a continuous anneal pickle line. Before pickling as per the conditions below, the steel is annealed at proper temperature depending on the alloy and then mechanically de-scaled
- the steel strip surface is also subjected to
- the strip is also subjected to
- Tank-3 is also subjected to temperature control by a heat exchanger and
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)
- Heat Treatment Of Sheet Steel (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
Description
Claims
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE60215629T DE60215629T2 (en) | 2001-04-09 | 2002-04-09 | PROCESS FOR STAINLESS STEEL STAIN USING HYDROGEN PEROXIDE |
KR1020037013175A KR100681099B1 (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades |
JP2002579536A JP4175463B2 (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grade |
BRPI0208749-9A BR0208749B1 (en) | 2001-04-09 | 2002-04-09 | process for continuously stripping stainless steel strip. |
EP02721700A EP1381714B8 (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades |
AU2002252617A AU2002252617B2 (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades |
MXPA03009219A MXPA03009219A (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades. |
CA002443695A CA2443695C (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US28256501P | 2001-04-09 | 2001-04-09 | |
US60/282,565 | 2001-04-09 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002081777A1 true WO2002081777A1 (en) | 2002-10-17 |
Family
ID=23082082
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2002/011135 WO2002081777A1 (en) | 2001-04-09 | 2002-04-09 | Hydrogen peroxide pickling scheme for stainless steel grades |
Country Status (14)
Country | Link |
---|---|
US (1) | US6645306B2 (en) |
EP (1) | EP1381714B8 (en) |
JP (1) | JP4175463B2 (en) |
KR (1) | KR100681099B1 (en) |
CN (1) | CN1244717C (en) |
AT (1) | ATE343663T1 (en) |
AU (1) | AU2002252617B2 (en) |
BR (1) | BR0208749B1 (en) |
CA (1) | CA2443695C (en) |
DE (1) | DE60215629T2 (en) |
ES (1) | ES2272699T3 (en) |
MX (1) | MXPA03009219A (en) |
WO (1) | WO2002081777A1 (en) |
ZA (1) | ZA200307743B (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6599371B2 (en) * | 2001-04-09 | 2003-07-29 | Ak Steel Corporation | Hydrogen peroxide pickling scheme for silicon-containing electrical steel grades |
US6645306B2 (en) * | 2001-04-09 | 2003-11-11 | Ak Steel Corporation | Hydrogen peroxide pickling scheme for stainless steel grades |
DE102006042416B4 (en) * | 2006-09-06 | 2009-04-23 | Sms Demag Ag | Method for pickling metal strips and apparatus for carrying out the method |
EP2470689A1 (en) * | 2009-08-25 | 2012-07-04 | Poligrat GmbH | Pickling process for high-grade steel |
EP2612957A4 (en) * | 2010-08-31 | 2015-04-08 | Jfe Steel Corp | Method for producing cold-rolled steel sheet, cold-rolled steel sheet, and vehicle member |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10160318A1 (en) * | 2001-12-07 | 2003-06-18 | Henkel Kgaa | Process for pickling martensitic or ferritic stainless steel |
US7396559B2 (en) * | 2003-08-11 | 2008-07-08 | General Motors Corporation | Method of making an electrically conductive element for use in a fuel cell |
US20050037935A1 (en) | 2003-08-11 | 2005-02-17 | Abd Elhamid Mahmoud H. | Composition and method for surface treatment of oxidized metal |
ES2331663T3 (en) * | 2007-04-19 | 2010-01-12 | Straumann Holding Ag | PROCESS TO PROVIDE A TOPOGRAPHY TO THE SURFACE OF A DENTAL IMPLANT. |
PL2352861T3 (en) * | 2008-11-14 | 2018-10-31 | Ak Steel Properties, Inc. | Process for pickling silicon-containing electrical steel with an acidic pickling solution containing ferric ions |
CN102337547B (en) * | 2010-07-15 | 2013-09-04 | 宝山钢铁股份有限公司 | Pickling method for hot rolled double-phase stainless steel plates |
KR101242990B1 (en) | 2010-12-28 | 2013-03-12 | 주식회사 포스코 | Pickling process to improve surface quality of ferritic stainless cold strip |
KR101289147B1 (en) * | 2010-12-28 | 2013-07-23 | 주식회사 포스코 | Environmental-Friendly and High Speed Pickling Process for Ferritic Stainless Cold Strip with Good Surface Quality |
KR101243021B1 (en) | 2010-12-28 | 2013-03-12 | 주식회사 포스코 | Pickling method and pickling solution for preventing and removing defects of low-chrome ferritic stainless steel in the pickling process |
KR20160022931A (en) | 2011-09-26 | 2016-03-02 | 에이케이 스틸 프로퍼티즈 인코포레이티드 | Stainless steel pickling in an oxidizing, electrolytic acid bath |
US10125425B2 (en) | 2013-07-01 | 2018-11-13 | General Electric Company | Method for smut removal during stripping of coating |
KR101461815B1 (en) * | 2013-07-31 | 2014-11-13 | 주식회사 포스코 | High Speed Pickling Method for Surface Improvement of High Chromium Ferritic Stainless Cold Steel Strip |
CN103882455A (en) * | 2014-03-18 | 2014-06-25 | 浙江大学 | Nitric-acid-free stainless steel acid washing solution and preparation method thereof |
CN106435607B (en) * | 2016-06-30 | 2021-05-18 | 宝钢德盛不锈钢有限公司 | Environment-friendly continuous annealing and pickling production method for stainless steel hot-rolled coil and pickling solution |
CN112275714A (en) * | 2020-09-21 | 2021-01-29 | 山东宏旺实业有限公司 | Method and device for cleaning titanium-plated stainless steel |
CN115386880B (en) * | 2022-09-02 | 2024-03-15 | 中国第一汽车股份有限公司 | Treatment fluid for stripping steel product surface as well as preparation method and application thereof |
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GB910356A (en) * | 1959-06-26 | 1962-11-14 | Fakler & Cie O | Method of automatically controlling a sulphuric acid treatment plant for ferrous materials |
US4002489A (en) * | 1973-06-21 | 1977-01-11 | Nyby Bruk Ab | Method of pickling metallic material |
US5908511A (en) * | 1992-08-06 | 1999-06-01 | Itb S.R.L. | Process for stainless steel pickling and passivation without using nitric acid |
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-
2002
- 2002-04-09 US US10/118,765 patent/US6645306B2/en not_active Expired - Lifetime
- 2002-04-09 EP EP02721700A patent/EP1381714B8/en not_active Revoked
- 2002-04-09 AT AT02721700T patent/ATE343663T1/en not_active IP Right Cessation
- 2002-04-09 ES ES02721700T patent/ES2272699T3/en not_active Expired - Lifetime
- 2002-04-09 CN CNB02808828XA patent/CN1244717C/en not_active Expired - Fee Related
- 2002-04-09 WO PCT/US2002/011135 patent/WO2002081777A1/en active IP Right Grant
- 2002-04-09 AU AU2002252617A patent/AU2002252617B2/en not_active Ceased
- 2002-04-09 BR BRPI0208749-9A patent/BR0208749B1/en not_active IP Right Cessation
- 2002-04-09 JP JP2002579536A patent/JP4175463B2/en not_active Expired - Fee Related
- 2002-04-09 DE DE60215629T patent/DE60215629T2/en not_active Expired - Lifetime
- 2002-04-09 CA CA002443695A patent/CA2443695C/en not_active Expired - Fee Related
- 2002-04-09 KR KR1020037013175A patent/KR100681099B1/en active IP Right Grant
- 2002-04-09 MX MXPA03009219A patent/MXPA03009219A/en active IP Right Grant
-
2003
- 2003-10-03 ZA ZA200307743A patent/ZA200307743B/en unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB910356A (en) * | 1959-06-26 | 1962-11-14 | Fakler & Cie O | Method of automatically controlling a sulphuric acid treatment plant for ferrous materials |
US4002489A (en) * | 1973-06-21 | 1977-01-11 | Nyby Bruk Ab | Method of pickling metallic material |
US5908511A (en) * | 1992-08-06 | 1999-06-01 | Itb S.R.L. | Process for stainless steel pickling and passivation without using nitric acid |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6599371B2 (en) * | 2001-04-09 | 2003-07-29 | Ak Steel Corporation | Hydrogen peroxide pickling scheme for silicon-containing electrical steel grades |
US6645306B2 (en) * | 2001-04-09 | 2003-11-11 | Ak Steel Corporation | Hydrogen peroxide pickling scheme for stainless steel grades |
DE102006042416B4 (en) * | 2006-09-06 | 2009-04-23 | Sms Demag Ag | Method for pickling metal strips and apparatus for carrying out the method |
EP2470689A1 (en) * | 2009-08-25 | 2012-07-04 | Poligrat GmbH | Pickling process for high-grade steel |
EP2612957A4 (en) * | 2010-08-31 | 2015-04-08 | Jfe Steel Corp | Method for producing cold-rolled steel sheet, cold-rolled steel sheet, and vehicle member |
Also Published As
Publication number | Publication date |
---|---|
US6645306B2 (en) | 2003-11-11 |
CN1244717C (en) | 2006-03-08 |
ES2272699T3 (en) | 2007-05-01 |
EP1381714B1 (en) | 2006-10-25 |
DE60215629D1 (en) | 2006-12-07 |
ATE343663T1 (en) | 2006-11-15 |
AU2002252617B2 (en) | 2007-05-31 |
DE60215629T2 (en) | 2007-09-06 |
MXPA03009219A (en) | 2005-03-07 |
EP1381714B8 (en) | 2007-01-03 |
JP2004524448A (en) | 2004-08-12 |
ZA200307743B (en) | 2004-10-04 |
KR20030088127A (en) | 2003-11-17 |
CA2443695C (en) | 2009-02-24 |
BR0208749B1 (en) | 2012-08-07 |
CN1505696A (en) | 2004-06-16 |
KR100681099B1 (en) | 2007-02-08 |
US20020174880A1 (en) | 2002-11-28 |
CA2443695A1 (en) | 2002-10-17 |
EP1381714A1 (en) | 2004-01-21 |
JP4175463B2 (en) | 2008-11-05 |
BR0208749A (en) | 2004-06-22 |
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