EP1013800B1 - Verfahren zum Beizen von Edelstahl - Google Patents
Verfahren zum Beizen von Edelstahl Download PDFInfo
- Publication number
- EP1013800B1 EP1013800B1 EP99123620A EP99123620A EP1013800B1 EP 1013800 B1 EP1013800 B1 EP 1013800B1 EP 99123620 A EP99123620 A EP 99123620A EP 99123620 A EP99123620 A EP 99123620A EP 1013800 B1 EP1013800 B1 EP 1013800B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- pickling
- added
- process according
- acid
- electrolyte 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.)
- Expired - Lifetime
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
-
- 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
- C23G1/081—Iron or steel solutions containing H2SO4
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
- C25F1/06—Iron or steel
Definitions
- the invention relates to a method for chemical and / or electrochemical pickling of stainless steel in a nitric acid-free and acidic liquid.
- Fe 3+ salts sulfate, chloride, nitrate or fluoride salts
- Chromate detoxification is very costly. As reducing agent mostly Na 2 S 2 O 5 or similar sulfur compounds are used.
- the aim of the invention is the disadvantages of both methods, in particular the costly "chromate detoxification", to avoid.
- the invention is therefore characterized in that spent electrolyte solution is metered in from electrochemical neutral salt pickling lines, preferably sodium sulphate pickling lines.
- electrochemical neutral salt pickling lines preferably sodium sulphate pickling lines.
- a favorable development of the invention is characterized in that that the redox potential in the pickling liquid by the amount of added Electrolyte solution is set to a predetermined value, wherein the reduction-oxidation potential (redox potential) of the pickling liquid measured and the amount of spent electrolyte solution dosed in accordance with electrochemical Natriumsulfatbeizlinien accordingly can be.
- the pickling effect for the Stainless steel band can be adjusted in the acid pickling liquid.
- An advantageous embodiment of the invention is characterized in that that in a new batch of acid pickling a divalent and a trivalent iron salt, preferably iron sulfates, may be added.
- An advantageous development of the invention is characterized in that that, in addition to the spent electrolyte, another oxidizing agent, preferably hydrogen peroxide, fed to the pickling liquid becomes. Should the amount of accumulated spent neutral electrolyte amount are not sufficient to the desired or necessary redox potential for To adjust the pickling process, so this redox potential in a simple Be achieved manner.
- another oxidizing agent preferably hydrogen peroxide
- a favorable embodiment of the invention is characterized in that that inhibitors are added. In this way, the corrosion attack be better controlled on the pickling material.
- a favorable development of the invention is characterized in that that acidic and neutral electrochemical etching stages with each other be combined, the used electrolyte solution from the neutral electrolyte stage can be added to the acidic stage.
- the advantage of the method can be achieved in a pickling line.
- An advantageous embodiment of the invention is characterized in that the acidic pickling liquid is neutralized by means of sodium hydroxide (NaOH) or sodium carbonate (Na 2 CO 3 ), that subsequently the resulting metal hydroxides are separated off, preferably filtered off, for example by means of microfiltration, and that the resulting sodium sulfate (Na 2 SO 4 ) is recycled again as a neutral electrolyte.
- NaOH sodium hydroxide
- Na 2 CO 3 sodium carbonate
- Na 2 SO 4 sodium sulfate
- a favorable development of the invention is characterized in that that the consumed electrolyte solution of one or more cold strip pickling line (s) removed and the nitric acid-free and acidic pickling liquid one or more hot strip pickling line (s) is added.
- This can be the For a stainless steel plant cheapest option in terms of investment costs and operating costs are chosen.
- the spent electrolyte solution contains the trivalent iron in the form of suspended hydroxide sludge (Fe (OH) 3 ) and contains the hexavalent chromium (Cr 6+ ), which reacts directly with the bivalent iron (Fe 2+ ) produced by the pickling process, thereby causing Fe 3+ and Cr 3+ arise.
- the electrolytic treatment with a charge density of 200 A * sec / dm 2 was carried out in the acidified electrolytic solution in which the redox potential was set to 440 mV, and then the sample sheet was further electrochemically treated in the neutral electrolyte.
- This combined pickling method has the advantage over a conventional neutral electrolyte treatment that with the same charge density of, for example, 600 A * sec / dm 2, about 20% more pickling loss could be achieved with a slightly lower gloss.
- a large-scale plant consisting of six electrochemical pickling cells can be optimized so that the first two cells can be operated with acidic electrolyte at exactly set redox potential and the subsequent four with neutral electrolyte.
- the resulting advantages are: higher pickling losses in the electrochemical pickling part, ie shorter after-treatment in the following mixed chemical acid (HF + HNO 3 ) pickling part.
- the final product has the same gloss level.
- the most important advantage, however, is that the entire chromate-containing neutral electrolyte solution can be recycled and thus no longer incur the costs for the Cr 6+ reduction.
- a further advantage of this optimization is that the sodium sulfate solution (Na 2 SO 4 ) required for pickling in the neutral pH range is obtained by neutralization of the acidic electrolyte solution (H 2 SO 4 , Na 2 SO 4 , Fe 2+ , Fe 3+ , Cr 3+ , Ni 2+ ) with sodium hydroxide (NaOH) or sodium carbonate (Na 2 CO 3 ) and subsequent separation of the metal hydroxides (Fe (OH) 2 , Fe (OH) 3 , Cr (OH) 3 , Ni (OH) 2 ) by filtration, can be recovered.
- the filtration is advantageously carried out as microfiltration.
- the experiments are only examples of process control as defined in the claims.
Description
Claims (10)
- Verfahren zum chemischen und/oder elektrochemischen Beizen von Edelstahl in einer salpetersäurefreien und sauren Flüssigkeit, dadurch gekennzeichnet, daß verbrauchte Elektrolytlösung aus elektrochemischen Neutralsalzbeizlinien, bevorzugt Natriumsulfatbeizlinien, zudosiert wird.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Redoxpotential in der Beizflüssigkeit durch die Menge an zugegebener Elektrolytlösung auf einen vorgegebenen Wert eingestellt wird.
- Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß das Reduktions-Oxidationspotential (Redoxpotential) der Beizflüssigkeit gemessen und die Menge der verbrauchten Elektrolytlösung aus elektrochemischen Natriumsulfatbeizlinien entsprechend zudosiert wird.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß bei einem Neuansatz der Beizflüssigkeit ein zweiwertiges und ein dreiwertiges Eisensalz, bevorzugt Eisensulfate, zugesetzt werden.
- Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß zusätzlich zum verbrauchten Elektrolyten ein anderes Oxidationsmittel, vorzugsweise Wasserstoffperoxid, der Beizflüssigkeit zugeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß Inhibitoren zugesetzt werden.
- Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß saure und neutrale elektrochemische Beizstufen miteinander kombiniert werden.
- Verfahren nach Anspruch 7, dadurch gekennzeichnet, daß die gebrauchte Elektrolytlösung aus der Neutralelektrolytstufe in die saure Stufe zudosiert wird.
- Verfahren nach Anspruch 7 oder 8, dadurch gekennzeichnet, daß die saure Beizflüssigkeit mittels Natronlauge (NaOH) oder Natriumcarbonat (Na2CO3) neutralisiert wird, daß anschließend die entstandenen Metallhydroxide abgetrennt, vorzugsweise abfiltriert werden, beispielsweise mittels einer Mikrofiltration, und daß das entstandene Natriumsulfat (Na2SO4) wieder als Neutralelektrolyt rückgeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß die verbrauchte Elektrolytlösung einer oder mehreren Kaltbandbeizlinie(n) entnommen und der salpetersäurefreien und sauren Beizflüssigkeit einer oder mehrerer Warmbandbeizlinie(n) zudosiert wird.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT99123620T ATE247182T1 (de) | 1998-12-22 | 1999-11-27 | Verfahren zum beizen von edelstahl |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT212998 | 1998-12-22 | ||
AT0212998A AT406486B (de) | 1998-12-22 | 1998-12-22 | Verfahren zum beizen von edelstahl |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1013800A2 EP1013800A2 (de) | 2000-06-28 |
EP1013800A3 EP1013800A3 (de) | 2000-11-15 |
EP1013800B1 true EP1013800B1 (de) | 2003-08-13 |
Family
ID=3528401
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP99123620A Expired - Lifetime EP1013800B1 (de) | 1998-12-22 | 1999-11-27 | Verfahren zum Beizen von Edelstahl |
Country Status (8)
Country | Link |
---|---|
US (1) | US6398876B1 (de) |
EP (1) | EP1013800B1 (de) |
KR (1) | KR100562094B1 (de) |
CN (1) | CN1195898C (de) |
AT (2) | AT406486B (de) |
BR (1) | BR9905932A (de) |
DE (1) | DE59906582D1 (de) |
ZA (1) | ZA997788B (de) |
Families Citing this family (21)
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AT413697B (de) * | 2001-11-07 | 2006-05-15 | Andritz Ag Maschf | Verfahren zur behandlung säurehältiger abwässer |
CN100451174C (zh) * | 2004-05-28 | 2009-01-14 | 高桥金属株式会社 | 金属氧化皮膜或锈的去除水及该去除水的使用方法 |
JP4911920B2 (ja) * | 2005-05-18 | 2012-04-04 | 英夫 吉田 | 六価クロムの抽出方法 |
KR100650887B1 (ko) * | 2005-12-26 | 2006-11-28 | 주식회사 포스코 | 저크롬 페라이트 스테인레스강의 고속전해 산세방법 |
CN101922039B (zh) * | 2010-09-08 | 2012-01-04 | 西安航空动力股份有限公司 | 一种去除涡轮盘封严齿机加表面缺陷的方法 |
PL2761063T3 (pl) * | 2011-09-26 | 2017-03-31 | Ak Steel Properties, Inc. | Trawienie stali nierdzewnej w utleniającej, elektrolitycznej kąpieli kwasowej |
US9089887B2 (en) | 2012-12-10 | 2015-07-28 | Samuel Steel Pickling Company | Line threading device and method |
ITMI20130494A1 (it) * | 2013-03-29 | 2014-09-30 | Tenova Spa | Metodo per trattare in continuo la superficie di un laminato di acciaio inossidabile in una soluzione a base di acido cloridrico |
JP6137089B2 (ja) * | 2014-09-02 | 2017-05-31 | Jfeスチール株式会社 | 冷延鋼板の製造方法および冷延鋼板の製造設備 |
AT517710B1 (de) * | 2016-04-13 | 2017-04-15 | Andritz Ag Maschf | Verfahren zum elektrolytischen beizen von metallbändern |
US11312048B2 (en) * | 2017-01-10 | 2022-04-26 | Guangdong Everwin Precision Technology Co., Ltd. | Surface treatment method of material, material product and composite material |
CN107299201B (zh) * | 2017-07-21 | 2019-09-03 | 首钢集团有限公司 | 消除碳含量在0.40%以上的冷轧锯片钢表层裂纹的方法 |
CN107350744A (zh) * | 2017-07-25 | 2017-11-17 | 江苏星河阀门有限公司 | 一种用于核电机组的双卡套式管接头的生产工艺 |
JP7058537B2 (ja) * | 2018-03-30 | 2022-04-22 | 日鉄ステンレス株式会社 | 耐塩害腐食性に優れたフェライト系ステンレス鋼 |
CN109267142A (zh) * | 2018-09-26 | 2019-01-25 | 中国民航大学 | 一种沉淀硬化型不锈钢常温电解酸洗方法 |
BE1026907B1 (nl) * | 2018-12-20 | 2020-07-22 | Aperam Stainless Belgium | Werkwijze voor het produceren van op ten minste drie verschillende manieren afgewerkt roestvast plaatstaal |
BE1026906B1 (nl) * | 2018-12-20 | 2020-07-22 | Aperam Stainless Belgium | Werkwijze voor het produceren van op ten minste drie verschillende manieren afgewerkt roestvast plaatstaal |
EP3980381A4 (de) * | 2019-06-07 | 2023-08-02 | Evoqua Water Technologies LLC | Behandlungsschema für pfas mit trennung und elektrochemischer eliminierung |
CN111057935B (zh) * | 2019-12-25 | 2021-04-02 | 浦项(张家港)不锈钢股份有限公司 | 一种耐热不锈钢的制备方法 |
CN112831794B (zh) * | 2020-12-30 | 2023-04-28 | 中冶南方工程技术有限公司 | 酸洗废液处理系统、不锈钢酸洗系统及工艺 |
CN113215646A (zh) * | 2021-05-11 | 2021-08-06 | 山西太钢工程技术有限公司 | 一种电解硫酸钠溶液循环利用智能控制系统 |
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US2172041A (en) * | 1937-10-07 | 1939-09-05 | Stephen F Urban | Pickling solution |
US2564549A (en) * | 1945-07-02 | 1951-08-14 | Albert R Stargardter | Pickling treatment |
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US4197139A (en) * | 1978-08-23 | 1980-04-08 | Hjersted Norman B | Process for the reclamation of acid from spent pickle liquor |
US4391685A (en) * | 1981-02-26 | 1983-07-05 | Republic Steel Corporation | Process for electrolytically pickling steel strip material |
US4415415A (en) * | 1982-11-24 | 1983-11-15 | Allegheny Ludlum Steel Corporation | Method of controlling oxide scale formation and descaling thereof from metal articles |
HUT53398A (en) * | 1987-01-19 | 1990-10-28 | Borsodi Vegyi Komb | Process for descaling and deoxidating metals and metal alloys, particularly alloyed steels, high-alloyed steels and carbon steels, in pickling bath containing iron(iii)ion active ingredient |
JPS63216986A (ja) * | 1987-03-03 | 1988-09-09 | Sumitomo Metal Ind Ltd | 低Cr鋼の高速酸洗方法 |
AT387406B (de) * | 1987-05-07 | 1989-01-25 | Andritz Ag Maschf | Verfahren zum elektrolytischen beizen von chromhaeltigem edelstahl |
AT391486B (de) * | 1988-09-14 | 1990-10-10 | Andritz Ag Maschf | Verfahren zum elektrolytischen beizen von edelstahlband |
US5076884A (en) * | 1990-07-19 | 1991-12-31 | Westinghouse Electric Corp. | Process of precipitating zirconium or hafnium from spent pickling solutions |
JPH0762279B2 (ja) * | 1991-08-02 | 1995-07-05 | 日本冶金工業株式会社 | ステンレス鋼の中性塩電解脱スケール方法 |
US5213667A (en) * | 1991-08-05 | 1993-05-25 | Hozer Norman R | Electrolytic bath solution and method for improving the surface wear resistance of tools |
JP3377533B2 (ja) * | 1992-03-30 | 2003-02-17 | 新日本製鐵株式会社 | 酸洗廃液中のPt、Pd、Rh金属回収方法 |
AT401183B (de) * | 1995-02-15 | 1996-07-25 | Andritz Patentverwaltung | Verfahren zur regeneration von elektrolyten, insbesondere na2so4 aus abbeizen von edelstahl, insbesondere edelstahlbändern |
AT404030B (de) * | 1995-02-15 | 1998-07-27 | Andritz Patentverwaltung | Verfahren zur beize von materialien aus stahl, insbesondere edelstahl |
JPH0913200A (ja) * | 1995-06-30 | 1997-01-14 | Mitsubishi Heavy Ind Ltd | ステンレス鋼板用酸洗液の再生方法及びその装置 |
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 |
US5702534A (en) * | 1996-05-24 | 1997-12-30 | Armco Inc. | Hydrogen peroxide pickling of stainless steel |
IT1288407B1 (it) * | 1996-12-09 | 1998-09-22 | Sviluppo Materiali Spa | Metodo per il decapaggio di prodotti in lega metallica contenente ferro e di titanio e sue leghe |
-
1998
- 1998-12-22 AT AT0212998A patent/AT406486B/de not_active IP Right Cessation
-
1999
- 1999-11-27 AT AT99123620T patent/ATE247182T1/de not_active IP Right Cessation
- 1999-11-27 DE DE59906582T patent/DE59906582D1/de not_active Expired - Lifetime
- 1999-11-27 EP EP99123620A patent/EP1013800B1/de not_active Expired - Lifetime
- 1999-12-20 KR KR1019990059281A patent/KR100562094B1/ko not_active IP Right Cessation
- 1999-12-21 CN CNB991229452A patent/CN1195898C/zh not_active Expired - Fee Related
- 1999-12-21 ZA ZA9907788A patent/ZA997788B/xx unknown
- 1999-12-21 US US09/467,376 patent/US6398876B1/en not_active Expired - Fee Related
- 1999-12-22 BR BR9905932-0A patent/BR9905932A/pt not_active Application Discontinuation
Also Published As
Publication number | Publication date |
---|---|
CN1261630A (zh) | 2000-08-02 |
EP1013800A2 (de) | 2000-06-28 |
AT406486B (de) | 2000-05-25 |
EP1013800A3 (de) | 2000-11-15 |
ATE247182T1 (de) | 2003-08-15 |
KR100562094B1 (ko) | 2006-03-17 |
BR9905932A (pt) | 2000-09-12 |
KR20000048256A (ko) | 2000-07-25 |
ATA212998A (de) | 1999-10-15 |
ZA997788B (en) | 2000-06-30 |
DE59906582D1 (de) | 2003-09-18 |
CN1195898C (zh) | 2005-04-06 |
US6398876B1 (en) | 2002-06-04 |
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