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US20030136685A1 - Process for electrochemical decomposition of superalloys - Google Patents

Process for electrochemical decomposition of superalloys Download PDF

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Publication number
US20030136685A1
US20030136685A1 US10/292,321 US29232102A US2003136685A1 US 20030136685 A1 US20030136685 A1 US 20030136685A1 US 29232102 A US29232102 A US 29232102A US 2003136685 A1 US2003136685 A1 US 2003136685A1
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US
United States
Prior art keywords
electrolysis
superalloys
process according
superalloy
rhenium
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.)
Abandoned
Application number
US10/292,321
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English (en)
Inventor
Viktor Stoller
Armin Olbrich
Juliane Meese-Marktscheffel
Wolfgang Mathy
Michael Erb
Georg Nietfeld
Gerhard Gille
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HC Starck GmbH
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Individual
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.)
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Publication date
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Assigned to H.C. STARCK GMBH reassignment H.C. STARCK GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MATHY, WOLFGANG, NIETFELD, GEORG, ERB, MICHAEL, GILLE, GERHARD, MEESE-MARKTSCHEFFEL, JULIANE, OLBRICH, ARMIN, STOLLER, VIKTOR
Publication of US20030136685A1 publication Critical patent/US20030136685A1/en
Assigned to H.C. STARCK GMBH & CO. KG reassignment H.C. STARCK GMBH & CO. KG CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: H.C. STARCK GMBH
Assigned to H. C. STARCK GMBH & CO. KG reassignment H. C. STARCK GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH
Priority to US11/741,347 priority Critical patent/US20080110767A1/en
Assigned to BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH reassignment BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH CORRECTIVE ASSIGNMENT TO CORRECT THE THE ASSIGNEE NEED TO BE CHANGED TO BAYER BETEILIGUNGSVERWALTUNG GOSLAR GMBH PREVIOUSLY RECORDED ON REEL 018766 FRAME 0488. ASSIGNOR(S) HEREBY CONFIRMS THE CHANGE OF NAME. Assignors: H.C. STARK GMBH
Assigned to H.C. STARCK GMBH reassignment H.C. STARCK GMBH MERGER (SEE DOCUMENT FOR DETAILS). Assignors: H.C. STARCK GMBH & CO. KG
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/045—Leaching using electrochemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a process for electrochemical decomposition of superalloys, in particular superalloy scrap, with the particular purpose of recovering rare and valuable metals such as rhenium, platinum, tantalum and hafnium.
  • Superalloys are high melting, high strength and extremely wear-resistant alloys of a comparatively large number of metals, which are used predominantly in turbine construction, especially aircraft turbines. Their special properties are owed in part to the addition of very rare and expensive elements, for example tantalum, hafnium or even rhenium/platinum. Because of their tough nature, it is difficult to recycle them, and to date they are not recycled economically, after their service life.
  • the actual decomposition of the alloy is in turn carried out wet-chemically by heat treatment in mineral acids of suitable concentration and composition (see, for example, Potter et al., Eff. Technol. Recycling Metal 1971, 35).
  • solvent extraction combined with sulphide precipitation reactions and electrodeposition reactions may, for example, be used (see, for example, Churchwood et al., J. Metals, September, 1963, 648).
  • a decomposition process which is based on anodic oxidation of the alloy in an electrolysis bath with a protic, organic solvent component, is used in order to recover the metallic constituents from superalloys.
  • This patent specification states that at most 10% water may be added to the electrolyte solution, so that the process still functions according to the invention (otherwise formation of a gel which is difficult to process and passivation of the anode surface and therefore termination of the electrolysis).
  • the electrolytically obtained filtration residue is processed, for example, thermally by calcination after mixing into milk of lime, the calcination product, for its part, being subsequently processed further by customary hydrometallurgical separating operations.
  • the present invention therefore relates to a process for decomposition of superalloys, wherein both electrodes of an electrochemical cell are formed by the superalloy to be decomposed, and the polarity of the electrolysis current is reversed with a frequency of from 0.005 to 5 Hz, preferably from 0.08 to 2 Hz, and particularly preferably from 0.01 to 1 Hz.
  • superalloys are alloys which contain from 50 to 75 wt. % of nickel as the major component, respectively from 3 to 15 wt. % of at least one of the elements cobalt, chromium and optionally aluminium, as well as from 1 to 10 wt. % of one or more of the elements tantalum, niobium, tungsten, molybdenum, rhenium, platinum and hafnium.
  • Such superalloys are not susceptible to decomposition by means of direct-current electrolysis in aqueous solutions, since a superficial passivation layer is formed after only a short electrolysis time, which then brings the electrolysis current to a standstill.
  • FIG. 1 is a schematic representation of the process from the identification of the superalloy scrap ( 1 ), electrolytic dissolving ( 2 ), suspension ( 3 ), filtration/washing ( 4 ) and further processing variants ( 5 ) and ( 6 ) respectively in order to recover valuable materials, in particular rhenium, platinum, tantalum and hafnium.
  • FIG. 2 is a schematic representation of three variants for the processing ( 6 ) of the filtrate ( 4 . 2 ) containing Ni/Co/Cr/Al/part of the Re/majority of the Mo.
  • an inorganic acid is used as the electrolyte, preferably hydrochloric acid, and particularly preferably a hydrochloric acid solution with an HCl content of from 15 to 25 wt. %. Nevertheless, mixtures of hydrochloric acid and sulphuric acid may also be used advantageously if subsequent stages and refluxes are taken into account.
  • the electrolysis is advantageously conducted with an electrolysis-current density of from 80 to 600 mA/cm 2 of cross-sectional area of the electrolysis cell.
  • the electrolysis voltage between the electrodes is between 2 and 6 volts, depending on the electrolyte conductivity, the current density and the spacing of the electrodes.
  • the electrochemical decomposition is preferably carried out at a constant electrolysis current.
  • the temperature in the electrolysis cell is from 20 to 100° C., and particularly preferably from 60 to 80° C.
  • the superalloy electrochemically decomposed according to the invention is subsequently processed, in a manner which is known per se, in order to recover the valuable materials, in particular rhenium, platinum, tantalum and hafnium.
  • This aspect of the invention is further described with particular reference to the drawings. This is represented schematically in the appended FIGS. 1 and 2.
  • the superalloy which may contain the elements rhenium, tantalum, hafnium, platinum, chromium, molybdenum, tungsten, nickel and cobalt, is electrochemically decomposed according to the invention ( 2 ); a suspension ( 3 ) is produced, from which a filter residue ( 4 .
  • the filter residue ( 4 . 1 ) is further decomposed of oxidising leaching ( 5 ) by suspending in fully deionised water, adding sodium hydroxide solution, heating to a temperature of from 65 to 90° C. supplementing with hydrogen peroxide while stirring.
  • the cooled suspension is filtered ( 5 . 1 ) and the filter residue is washed.
  • the filtrate ( 5 . 3 ) which contains the tungsten, molybdenum and part of the rhenium and a little Pt, can be separated further, in a manner which is known per se, by means of strongly basic ion exchangers.
  • the residue of the HF decomposition ( 5 . 4 ) contains the valuable platinum ( 5 . 5 ).
  • the filtrate ( 5 . 6 ) contains the valuable tantalum/hafnium, which can be separated further by extraction with MIBK.
  • variants which are explained in FIG. 2, are available for the processing ( 6 ) of the filtrate ( 4 . 2 ) which has been obtained from the filtration ( 4 ).
  • the filtrate ( 4 . 2 ) from FIG. 1 is sent through an ion exchanger ( 7 . 1 ) and the rhenium is obtained as an eluate ( 8 . 1 ).
  • the nickel/cobalt units can be separated ( 10 . 1 ) via a solvent-extraction (SX) system.
  • the filtrate ( 4 . 2 ) is subjected to fractional hydroxide precipitation ( 7 . 2 ); after filtration ( 8 . 2 ), a residue ( 10 . 2 ) containing aluminium and chromium is obtained and a filtrate ( 9 . 2 ), from which rhenium is separated by means of an ion exchanger ( 11 . 2 ) and is recovered by elution ( 12 . 2 ).
  • the raffinate ( 13 . 2 ) consists of a nickel/cobalt solution.
  • the 0.422 kg of filtration residue ( 1 ) contains wt. %: 39.5 Ta 2 O 5 , 6.2 ReO 2 , 27.8 WO 3 , 1.6 MoO 3 and 25 H 2 O.
  • the filtrate is purified with the wash water and wt. %: 0.3 HReO 4 , 0.4 H 2 MoO 4 , 2.8 CoCl 2 , 17.6 NiCl 2 , 1.9 CrCl 3 , 3.3 AlCl 3 and 0.2 HCl are found in solution ( 1 ).
  • the wet filtration residue is suspended in 195 g of fully deionised water in a 2-litre beaker while stirring, supplemented with 160 g of 50% strength sodium hydroxide solution and heated to 80° C. 41 g of 30% strength hydrogen peroxide solution are then introduced. After 2 hours of stirring at 80° C., the suspension is cooled, filtered and the residue is washed with 0.370 kg of fully deionised water.
  • the 0.222 kg of filtration residue ( 2 ) contains wt. %: 74.9 Ta 2 O 5 , 0.1 ReO 2 , 1.0 WO 3 and 23.0 H 2 O.
  • the filtrate is purified with the wash water and wt. %: 2.3 NaReO 4 , 10.6 Na 2 Wo 4 , 0.7 Na 2 MoO 4 and 2.2 NaOH are found in solution ( 2 ).
  • Tungsten and rhenium are separated in a known manner by means of strongly basic ion-exchange resins, and can thereafter be sent to the further value chain as precursors for the production of tungsten and rhenium products.
  • Molybdenum and rhenium are separated in a known manner by means of strongly basic ion-exchange resins, and can thereafter be used as precursors for the production of molybdenum and rhenium products.
  • the filtration residue can be reprocessed in a known manner, for example reducing melt to form Ni—Co alloys.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
US10/292,321 2001-11-14 2002-11-12 Process for electrochemical decomposition of superalloys Abandoned US20030136685A1 (en)

Priority Applications (1)

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US11/741,347 US20080110767A1 (en) 2001-11-14 2007-06-21 Process for electrochemical decomposition of superalloys

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2001155791 DE10155791C1 (de) 2001-11-14 2001-11-14 Verfahren zum elektrochemischen Aufschluss von Superlegierungen
DE10155791.4 2001-11-14

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US (2) US20030136685A1 (es)
EP (1) EP1312686B1 (es)
JP (1) JP4716398B2 (es)
KR (2) KR20030040117A (es)
CN (1) CN1285769C (es)
AT (1) ATE384144T1 (es)
CA (1) CA2411444C (es)
DE (2) DE10155791C1 (es)
MX (1) MXPA02011143A (es)
PE (1) PE20030504A1 (es)
RU (1) RU2313589C2 (es)
TW (1) TW200303374A (es)

Cited By (8)

* Cited by examiner, † Cited by third party
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US20090255372A1 (en) * 2006-06-30 2009-10-15 H.C. Starck Gmbh Recycling of superalloys with the aid of an alkali metal salt bath
EP2081685A4 (en) * 2006-11-13 2010-12-15 In-Soo Jin PROCESS FOR EXTRACTING PLATINUM GROUP METALS FROM USED CATALYSTS BY ELECTROCHEMICAL PROCESS
US20110126673A1 (en) * 2009-11-30 2011-06-02 General Electric Company Rhenium recovery from superalloys and associated methods
US20120058029A1 (en) * 2009-03-13 2012-03-08 Neo Performance Materials Limited Rhenium recovery
KR101600334B1 (ko) 2014-09-22 2016-03-10 한국지질자원연구원 용매추출에 의한 레늄함유 용액으로부터 레늄의 선택적인 분리방법
WO2017075015A1 (en) 2015-10-26 2017-05-04 Techemet, Llc A method for platinum recovery from materials containing rhenium and platinum metals
US10399166B2 (en) 2015-10-30 2019-09-03 General Electric Company System and method for machining workpiece of lattice structure and article machined therefrom
CN120230915A (zh) * 2025-06-03 2025-07-01 中南大学 一种从高温合金中综合回收有价金属的方法

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JP2011500962A (ja) 2007-10-15 2011-01-06 ハイ−テンプ・スペシャルティー・メタルス・インコーポレーテッド 再生スクラップを原材料として使用したタンタル粉末の生産方法
RU2437836C1 (ru) * 2010-04-23 2011-12-27 Учреждение Российской академии наук Институт неорганической химии им. А.В. Николаева Сибирского отделения РАН Способ извлечения и очистки рения из растворов от переработки жаропрочных сплавов
US9322081B2 (en) 2011-07-05 2016-04-26 Orchard Material Technology, Llc Retrieval of high value refractory metals from alloys and mixtures
RU2484159C1 (ru) * 2012-04-12 2013-06-10 Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук Способ электрохимической переработки отходов жаропрочных никелевых сплавов, содержащих рений, вольфрам, тантал и другие ценные металлы
RU2505612C1 (ru) * 2012-06-28 2014-01-27 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Российский химико-технологический университет им. Д.И. Менделеева (РХТУ им. Д.И. Менделеева) Способ извлечения молибдена из вольфрамсодержащих растворов
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CN106757156B (zh) * 2016-12-08 2018-08-10 江苏鼎杰合金科技有限公司 一种从含Re高温合金废料中回收Re的方法
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090255372A1 (en) * 2006-06-30 2009-10-15 H.C. Starck Gmbh Recycling of superalloys with the aid of an alkali metal salt bath
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PE20030504A1 (es) 2003-07-13
TW200303374A (en) 2003-09-01
DE50211544D1 (de) 2008-03-06
CN1285769C (zh) 2006-11-22
RU2313589C2 (ru) 2007-12-27
DE10155791C1 (de) 2003-07-17
HK1055998A1 (en) 2004-01-30
CA2411444A1 (en) 2003-05-14
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EP1312686A2 (de) 2003-05-21
CA2411444C (en) 2011-08-16
EP1312686A3 (de) 2003-10-08
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US20080110767A1 (en) 2008-05-15
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