WO1999014165A1 - Procede de regeneration de solutions acides metalliferes issues d'installations de traitement des surfaces - Google Patents

Procede de regeneration de solutions acides metalliferes issues d'installations de traitement des surfaces Download PDF

Info

Publication number
WO1999014165A1
WO1999014165A1 PCT/DE1998/002700 DE9802700W WO9914165A1 WO 1999014165 A1 WO1999014165 A1 WO 1999014165A1 DE 9802700 W DE9802700 W DE 9802700W WO 9914165 A1 WO9914165 A1 WO 9914165A1
Authority
WO
WIPO (PCT)
Prior art keywords
metal
acids
process stream
solution
metal salt
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.)
Ceased
Application number
PCT/DE1998/002700
Other languages
German (de)
English (en)
Other versions
WO1999014165B1 (fr
Inventor
Werner Sturm
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.)
Steuler Industriewerke GmbH
Original Assignee
Steuler Industriewerke 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 Steuler Industriewerke GmbH filed Critical Steuler Industriewerke GmbH
Priority to AU10221/99A priority Critical patent/AU1022199A/en
Publication of WO1999014165A1 publication Critical patent/WO1999014165A1/fr
Publication of WO1999014165B1 publication Critical patent/WO1999014165B1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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
    • C23G1/36—Regeneration of waste pickling liquors
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general

Definitions

  • the invention relates to a process for the preparation of metal-containing acid solutions from surface treatment plants, which in particular contain HN0 3 , HN0 3 / HF, H 2 S0 4 / HF, HF, HC1 etc.
  • the object of the invention is to provide a one- to multi-stage process with which the free and bound acids are practically completely recovered and returned to the surface treatment process.
  • the method according to the invention also improves the quality of the surface treatment solutions and thus also reduces the surface quality of the treated materials and the environmental impact.
  • inventive method is characterized by simplified handling and process control with a simultaneous reduction in operating and investment costs.
  • An acidic process stream that contains small residual amounts of dissolved metal salts and that directly or after further concentration or after use as an absorption and condensation solution in the Process step B or D is returned to the surface treatment process.
  • a metal salt-containing process stream which contains smaller residual amounts of free acids and which is fed to a further treatment, the free acids and also the bound acids present as metal salts being recovered.
  • the resulting filtrate which still contains dissolved metal salts, is returned to the 1st process stage and treated again.
  • the metal-containing salt stream from the 1st process stage and / or the separated metal salts from stage A are mixed with sulfuric acid.
  • the weaker acids such as HF, HC1 or HN0 3 are released from the metal salts.
  • the sulfuric acid-containing metal salt solution is then fed to a crystallization, the metals being crystallized out as metal sulfates.
  • the metal sulfate crystals are separated and disposed of or recycled as raw materials or sent for further processing.
  • the filtrate containing sulfuric acid, which still contains dissolved metal salts, is returned to the stripping / distillation process, where it is treated again.
  • stage B The metal sulfates from stage B are dissolved and subjected to electrolysis, z. B. the metals contained such as Ni, Cr, Cu, etc. are separated as elements.
  • the separated metals can be reused as raw materials in the metal manufacturing process.
  • the resulting highly concentrated Fe III sulfate solution can be used as a chemical in water or wastewater treatment.
  • the metal-containing process stream of the 1st process stage, the metal salt crystals of stage A and / or the metal sulfates of stage B are fed to a thermal process, e.g. the PYROMAS process or the fluidized bed process.
  • the metal salts are split into the respective metal oxides and the respective acids and / or sulfur trioxide or dioxide.
  • the metal oxides are separated and can be used as raw materials.
  • the exhaust gas / pyrolysis or roasting gas enriched with the acids and / or sulfur trioxide / dioxide is fed to a condensation / absorption process.
  • the respective acids or acid mixtures are formed by the condensation / absorption process can be returned directly or after an additional concentration in the surface treatment process or in the case of sulfuric acid in stage B.
  • the metal-containing process stream of the 1st process stage, the metal salt crystals of stage A and / or the metal sulfates of stage B are fed to a further treatment process in which in the 1st step neutralization with lye such as e.g. Potassium hydroxide solution, sodium hydroxide solution and / or sodium carbonate.
  • lye such as e.g. Potassium hydroxide solution, sodium hydroxide solution and / or sodium carbonate.
  • the metals are precipitated, separated and dewatered as metal hydroxides.
  • the metal-containing filter cake formed can then be used as a raw material immediately after washing to remove the residual salts, drying and / or calcining.
  • the filtrate obtained during the neutralization and separation of the solids, which contains the formed, dissolved salts of the respective acids and the neutralizing agents used, is then subjected to electrodialysis, based on bipolar membranes, the salts being split into the respective acids and alkalis .
  • the acids formed can be returned to the surface treatment process directly or after concentration.
  • the lye formed in each case can be used again as a neutralizing agent.
  • the different residues obtained as end products in the individual process steps can either be returned directly to production as raw materials or only after further processing.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un procédé d'au moins une opération permettant de régénérer des solutions acides métallifères issues d'un processus de traitement des surfaces. Ce procédé consiste a) à séparer les acides libres de la solution, ce qui permet d'obtenir un flux acide et un flux contenant un sel métallique et b) à régénérer le flux de traitement contenant un sel métallique.
PCT/DE1998/002700 1997-09-12 1998-09-11 Procede de regeneration de solutions acides metalliferes issues d'installations de traitement des surfaces Ceased WO1999014165A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU10221/99A AU1022199A (en) 1997-09-12 1998-09-11 Method for treating metal containing acid solutions from surface treatment installations

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19740164.3 1997-09-12
DE1997140164 DE19740164A1 (de) 1997-09-12 1997-09-12 Verfahren zur Aufbereitung von metallhaltigen Säurelösungen aus Oberflächenbehandlungsanlagen

Publications (2)

Publication Number Publication Date
WO1999014165A1 true WO1999014165A1 (fr) 1999-03-25
WO1999014165B1 WO1999014165B1 (fr) 1999-05-20

Family

ID=7842167

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1998/002700 Ceased WO1999014165A1 (fr) 1997-09-12 1998-09-11 Procede de regeneration de solutions acides metalliferes issues d'installations de traitement des surfaces

Country Status (3)

Country Link
AU (1) AU1022199A (fr)
DE (1) DE19740164A1 (fr)
WO (1) WO1999014165A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0968756A1 (fr) * 1998-07-02 2000-01-05 Umweltanalystisches Zentrum Gröditz GmbH Procédé de traitement d'acides mineraux contenant des métaux
DE102013108375A1 (de) * 2013-01-31 2014-07-31 Thomas König Verfahren zum Aufbereiten eines Beiz- und/oder Eloxalbades und Eloxieranordnung

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003035934A1 (fr) * 2001-10-25 2003-05-01 Eco-Tec Limited Procede et appareil de recyclage de solutions de decapage contenant du peroxyde
DE10231308C5 (de) * 2002-07-10 2009-10-15 Cmi Uvk Gmbh Verfahren und Vorrichtung zum Recyceln von Edelstahl-Beizbädern
DE102013105177A1 (de) 2013-05-21 2014-11-27 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Gewinnung metallischer Anteile sowie von metallabgereichertem Material aus metallhaltigen Materialien

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1546180A1 (de) * 1964-12-04 1970-10-08 Pawlek Dr Ing Franz Verfahren zur Regenerierung der Schwefelsaeure in verbrauchten Beizloesungen
DE2553416A1 (de) * 1975-11-27 1977-06-02 Hager & Elsaesser Verfahren zum abtrennen von geloesten stoffen aus einer loesung
US4382916A (en) * 1981-10-07 1983-05-10 Voss Steel Corporation Method of preparing hydrochloric acid and high purity ferrous sulfate hydrate crystals from hydrochloric acid waste pickle liquor
JPS62127485A (ja) * 1985-11-26 1987-06-09 Nisshin Steel Co Ltd 鉄鋼の塩酸酸洗廃液より酸化鉄を回収する方法
EP0269234A1 (fr) * 1986-10-14 1988-06-01 AlliedSignal Inc. Récupération d'acides de solutions contenant de l'acide et du sel
JPS63291608A (ja) * 1987-05-22 1988-11-29 Tokuyama Soda Co Ltd 酸廃液の再生方法
EP0398863A1 (fr) * 1989-05-17 1990-11-22 BÖHLER Gesellschaft m.b.H. Procédé de récupération de métaux ou d'oxydes de métaux et des acides à partir de solutions salines, en particulier à partir d'acides ou mélanges d'acides de décapage
US5562828A (en) * 1995-05-19 1996-10-08 Olsen; Douglas R. Method and apparatus for recovering acid and metal salts from pricklining liquors
EP0843025A1 (fr) * 1996-11-15 1998-05-20 Keramchemie GmbH Procédé de régénération de solutions de décapage usées

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1546180A1 (de) * 1964-12-04 1970-10-08 Pawlek Dr Ing Franz Verfahren zur Regenerierung der Schwefelsaeure in verbrauchten Beizloesungen
DE2553416A1 (de) * 1975-11-27 1977-06-02 Hager & Elsaesser Verfahren zum abtrennen von geloesten stoffen aus einer loesung
US4382916A (en) * 1981-10-07 1983-05-10 Voss Steel Corporation Method of preparing hydrochloric acid and high purity ferrous sulfate hydrate crystals from hydrochloric acid waste pickle liquor
JPS62127485A (ja) * 1985-11-26 1987-06-09 Nisshin Steel Co Ltd 鉄鋼の塩酸酸洗廃液より酸化鉄を回収する方法
EP0269234A1 (fr) * 1986-10-14 1988-06-01 AlliedSignal Inc. Récupération d'acides de solutions contenant de l'acide et du sel
JPS63291608A (ja) * 1987-05-22 1988-11-29 Tokuyama Soda Co Ltd 酸廃液の再生方法
EP0398863A1 (fr) * 1989-05-17 1990-11-22 BÖHLER Gesellschaft m.b.H. Procédé de récupération de métaux ou d'oxydes de métaux et des acides à partir de solutions salines, en particulier à partir d'acides ou mélanges d'acides de décapage
US5562828A (en) * 1995-05-19 1996-10-08 Olsen; Douglas R. Method and apparatus for recovering acid and metal salts from pricklining liquors
EP0843025A1 (fr) * 1996-11-15 1998-05-20 Keramchemie GmbH Procédé de régénération de solutions de décapage usées

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 011, no. 357 (C - 458) 20 November 1987 (1987-11-20) *
PATENT ABSTRACTS OF JAPAN vol. 013, no. 119 (C - 579) 23 March 1989 (1989-03-23) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0968756A1 (fr) * 1998-07-02 2000-01-05 Umweltanalystisches Zentrum Gröditz GmbH Procédé de traitement d'acides mineraux contenant des métaux
DE102013108375A1 (de) * 2013-01-31 2014-07-31 Thomas König Verfahren zum Aufbereiten eines Beiz- und/oder Eloxalbades und Eloxieranordnung

Also Published As

Publication number Publication date
WO1999014165B1 (fr) 1999-05-20
DE19740164A1 (de) 1999-03-18
AU1022199A (en) 1999-04-05

Similar Documents

Publication Publication Date Title
DE2714343C2 (de) Verfahren zur Naßreinigung von Gasen, die Schwefeldioxid, Halogene und Arsen enthalten
AT413697B (de) Verfahren zur behandlung säurehältiger abwässer
EP1521864B1 (fr) Procede et dispositif pour recycler des bains de decapage de metaux
DE69612674T2 (de) Verfahren zur entsalzung, und demineralisierung von säure und/oder metallsalzen enthaltenden lösungen
DE1467274B2 (de) Verfahren zur Aufbereitung von bei der Alkalibehandlung von Bauxit und ähnlichen Roherzen anfallenden Rotschlämmen unter Gewinnung der verwertbaren Bestandteile.-Anm: Mitsubishi Shipbuilding & Engineering Co. Ltd.. Tokio:
DE2948710A1 (de) Verfahren zum regenerieren von beizsaeure
DE4112339A1 (de) Verfahren zum herstellen von kupferarsenat
DE2546425B2 (de) Verfahren zur Gewinnung von technischem Molybdäntrioxid aus Molybdänitkonzentraten
CH632223A5 (de) Verfahren zur reinigung von abwasser.
WO1999014165A1 (fr) Procede de regeneration de solutions acides metalliferes issues d'installations de traitement des surfaces
DE4030707C2 (fr)
EP0263539B1 (fr) Procédé de traitement de résidus de l'hydrométallurgie du zinc
DE2256109A1 (de) Verfahren zur abtrennung von verunreinigungen
DE2729755C2 (de) Verfahren zur Herstellung von Titandioxid durch diskontinuierliches Aufschließen von Ilmeniterzen mit Schwefelsäure
DE2915129A1 (de) Verfahren zur grosstechnischen gewinnung von magnesiumoxid hoher reinheit
DE3136002C2 (de) Verfahren zur Reinigung des Abwassers, das bei der Laugung von vanadiumhaltigen Ausgangsstoffen anfällt
EP0320682B2 (fr) Procédé pour la fabrication du dioxyde de titane
WO1994024050A2 (fr) Procede d'epuration de solutions contenant des aluminates alcalins
EP0392211B1 (fr) Procédé de réutilisation d'acide sulfurique résiduaire
DE2750768A1 (de) Verfahren zur entfernung von chlorionen aus einem system zur behandlung von feuchtem abgas
DE293967C (fr)
DE3314877A1 (de) Verfahren zur behandlung einer entnahmeloesung, insbesondere fuer ein zinkextraktionsverfahren auf elektrolytischem weg
DE2042785B2 (fr)
DE4218554C2 (de) Verfahren und Vorrichtung zur Aufbereitung von Behandlungslösungen
DD208963A1 (de) Verfahren zur aufbereitung und abtrennung von vanadiumsalzen aus waessrigen loesungen

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AL AM AT AU AZ BA BB BG BR BY CA CH CN CU CZ DE DK EE ES FI GB GE GH GM HR HU ID IL IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MD MG MK MN MW MX NO NZ PL PT RO RU SD SE SG SI SK SL TJ TM TR TT UA UG US UZ VN YU ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): GH GM KE LS MW SD SZ UG ZW AM AZ BY KG KZ MD RU TJ TM AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE BF BJ CF CG CI CM GA GN GW ML MR NE SN TD TG

AK Designated states

Kind code of ref document: B1

Designated state(s): AL AM AT AU AZ BA BB BG BR BY CA CH CN CU CZ DE DK EE ES FI GB GE GH GM HR HU ID IL IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MD MG MK MN MW MX NO NZ PL PT RO RU SD SE SG SI SK SL TJ TM TR TT UA UG US UZ VN YU ZW

AL Designated countries for regional patents

Kind code of ref document: B1

Designated state(s): GH GM KE LS MW SD SZ UG ZW AM AZ BY KG KZ MD RU TJ TM AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE BF BJ CF CG CI CM GA GN GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
DFPE Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101)
NENP Non-entry into the national phase

Ref country code: KR

122 Ep: pct application non-entry in european phase
NENP Non-entry into the national phase

Ref country code: CA