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US20090255372A1 - Recycling of superalloys with the aid of an alkali metal salt bath - Google Patents

Recycling of superalloys with the aid of an alkali metal salt bath Download PDF

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Publication number
US20090255372A1
US20090255372A1 US12/306,853 US30685307A US2009255372A1 US 20090255372 A1 US20090255372 A1 US 20090255372A1 US 30685307 A US30685307 A US 30685307A US 2009255372 A1 US2009255372 A1 US 2009255372A1
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United States
Prior art keywords
melt
process according
metals
weight
superalloy
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Abandoned
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US12/306,853
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English (en)
Inventor
Armin Olbrich
Juliane Meese-Marktscheffel
Matthias Jahn
Rüdiger Zertani
Viktor Stoller
Michael Erb
Karl-Heinz Heine
Uwe Kutzler
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HC Starck GmbH
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HC Starck GmbH
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Assigned to H.C. STARCK GMBH reassignment H.C. STARCK GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KUTZLER, UWE, HEINE, KARL-HEINZ, ERB, MICHAEL, STOLLER, VIKTOR, JAHN, MATTHIAS, ZERTANI, RUEDIGER, MEESE-MARKTSCHEFFEL, JULIANE, OLBRICH, ARMIN
Publication of US20090255372A1 publication Critical patent/US20090255372A1/en
Abandoned legal-status Critical Current

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Classifications

    • 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
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/36—Obtaining tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G47/00—Compounds of rhenium
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/02—Obtaining nickel or cobalt by dry processes
    • C22B23/026—Obtaining nickel or cobalt by dry processes from spent catalysts
    • 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
    • C22B61/00—Obtaining metals not elsewhere provided for in this subclass
    • 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
    • C22B7/001—Dry processes
    • 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 the digestion of superalloys, in particular superalloy scrap, in a salt melt and subsequent recovery of the valuable metals.
  • Superalloys are alloys which have a complex composition, are stable at high temperatures and are based on nickel and cobalt, with additions of other metals, such as, for example, aluminium, chromium, molybdenum, tungsten, tantalum, niobium, manganese, rhenium, platinum, titanium, zirconium and hafnium, and nonmetals, such as boron and/or carbon.
  • the superalloys are high-strength and particularly hard-wearing alloys which are used in motor and engine construction, in energy technology and in aviation and space flight. The particular properties of these alloys are achieved in particular by the addition of rare and noble metals, such as rhenium, tantalum, niobium or even platinum.
  • the superalloys differ from the customary high-melting alloys, e.g. W—Re alloys or Mo—Re alloys, in their particular resistance to oxidation or corrosion.
  • W—Re alloys or Mo—Re alloys e.g. W—Re alloys or Mo—Re alloys
  • components comprising superalloys are used in the production of blades in aircraft turbines. After elapse of the duration of use, such parts are an important raw material source for recovering rare metals, in particular rhenium, tantalum, niobium, tungsten, molybdenum and platinum.
  • the recovery of the alloy metals of the superalloys is commercially very interesting owing to the high proportion of expensive metals.
  • special superalloys contain the metals rhenium in up to 12% by weight, tantalum in up to 12% by weight, niobium in up to 5% by weight and tungsten and molybdenum in up to 12% by weight.
  • Further metals which serve as base metals in the superalloys are nickel and cobalt.
  • the superalloys are a raw material source from which the recovery of these metals is commercially expedient.
  • the high-melting metals present in scraps of an Fe/Ni/Co/Cu base alloy e.g. tungsten, molybdenum and chromium
  • scraps of an Fe/Ni/Co/Cu base alloy e.g. tungsten, molybdenum and chromium
  • tungsten, molybdenum and chromium are first converted into borides, carbides, nitrides, silicides or phosphides via a melting process by addition of non-metallic compounds of group III, IV or V, melted to give anodes and then subjected to an anodic oxidation.
  • Those metals such as Co, Ni and Cu initially go into solution and are deposited from this at the cathode, while the high-melting metals, remain behind in the anode sludge, for example as borides, carbides, etc.
  • the metals Ni, Co, Cu are separated from the high-melting metals, such as W, Mo or chromium, but there is no information at all about whether complete separation of these metals takes place.
  • the document furthermore provides no information about the cost-efficiency of the process.
  • WO 96/14440 describes a process for the electrochemical digestion of superalloys by anodic oxidation of the alloy in an electrolysis bath with an organic solvent component.
  • the document discloses that up to 10% of water can be added to the electrolyte solution so that the process can still be carried out according to the invention. Otherwise, passivation of the anode occurs through formation of a gel or a firmly adhering oxide layer, which can lead to termination of the electrolysis.
  • the working-up and separation of the valuable substances from the suspension forming as a result of the electrolysis are initially effected by filtration.
  • the filtration residue separated off and containing a part of the alloy metals is then worked up thermally by calcination and subsequently by the customary hydrometallurgical processes.
  • DE 10155791C1 likewise discloses an electrochemical digestion process for superalloys.
  • the superalloys are first cast into sheets and then electrolytically digested in an oxygen-free inorganic acid.
  • the problem of anodic passivation is counteracted by reversal of the polarity of the electrodes.
  • the two last-mentioned processes can be implemented economically only under certain general conditions, in particular very high rhenium contents in superalloys.
  • DE 19521333 C1 discloses a pyrometallurgical digestion of tungsten-containing hard metal and heavy metal scraps. The digestion takes place at temperatures between 800 and 1000° C. in a salt melt which consists of NaOH and Na 2 SO 4 . In these processes, a sodium tungstate melt is produced, which is dissolved in water after subsequent cooling.
  • tungsten hard metal scrap is virtually completely digested there in alkaline, sulphate-containing melt under oxidizing conditions by formation of sodium tungstate. This is not surprising since the metallate is distinguished by high stability and dissolves in the NaOH melt under the reaction conditions. Thus, a complete dissolution process of the hard metal scrap is ensured.
  • the object was achieved by a process for the recovery of valuable metals from superalloys, the superalloys being digested in a salt melt consisting of 60-95% by weight of NaOH and 5-40% by weight of Na 2 SO 4 and the melt digestion product formed thereby then being worked up hydrometallurgically with the aim of simple separation of the individual valuable metals.
  • the digestion is preferably carried out in a salt melt consisting of 65-85% by weight of NaOH and 15-35% by weight of Na 2 SO 4 , particularly preferably of 70-80% by weight of NaOH and 20-30% by weight of Na 2 SO 4 .
  • Superalloys according to the present invention are alloys which contain, as main components, 50 to 80% of nickel, 3 to 15% by weight of at least one or more of the elements cobalt, chromium and optionally aluminium, and 1 to 12% by weight of one or more of the elements rhenium, tantalum, niobium, tungsten, molybdenum, hafnium and platinum.
  • the process according to the invention is suitable in particular for rhenium-containing superalloys which contain up to 12% by weight of rhenium.
  • the digestion according to the invention of superalloys is advantageously carried out in such a way that up to 10% by weight, preferably up to 8% by weight and particularly preferably up to 5% by weight of sodium carbonate (Na 2 CO 3 ), based on the weight of the salt melt, are added to the salt melt.
  • compositions of the salt melt are listed in Table 1.
  • the superalloys may be present both in lump form and in pulverulent form (grindings or grinding dusts).
  • the superalloy digestion can be carried out both in directly heated furnaces, e.g. in furnaces with gas or oil firing, and in indirectly heated furnaces, continuously or batchwise.
  • the furnaces suitable for this purpose are, for example, rotary furnaces and rotary tubular kilns.
  • the digestion of superalloys is preferably carried out in a moving alkaline melt in a directly fired rotary tubular kiln operated batchwise.
  • the digestion according to the invention is carried out in such a way that at least 1 kg of salt melt, preferably at least 1.5 kg and particularly preferably at least 2 kg are used per 1 kg of superalloy. In the case of certain superalloys which have rhenium contents greater than 8%, up to 5 kg of salt melt are used per kilogram of superalloy.
  • the digestion according to the invention of superalloys takes place particularly advantageously with regard to the space-time yield if air and/or oxygen, or a mixture thereof, is passed into the salt melt.
  • a mixture of air and oxygen consisting of 25 to 95% by volume of air and 5 to 75% by volume of oxygen, preferably of 35 to 80% by volume of air and 20 to 65% by volume of oxygen, is preferably passed into the salt melt.
  • the digestion according to the invention of superalloys is carried out at temperatures of 800 to 1200° C.
  • the digestion is carried out in the temperature range of 850 to 1100° C., particularly preferably at 900 to 1050° C.
  • Good digestion conditions are present if oxidizing agents are additionally introduced into the melt.
  • oxidizing agents for example, nitrates, peroxodisulphates, peroxides of the alkali metals and/or mixtures thereof can serve as such.
  • Potassium nitrate, sodium nitrate, sodium peroxide, potassium peroxide, sodium peroxodisulphate, potassium peroxodisulphate and/or mixtures thereof are advantageously used as oxidizing agents.
  • Particularly good digestion rates are achieved if 5 to 25% by weight of the oxidizing component, based on the weight of the melt, are added to the melt.
  • compositions of the salt melt are shown in Table 2.
  • the melt digestion is particularly advantageously carried out in such a way that a partial oxidation of the superalloy takes place or, after virtually complete oxidation, reducing conditions are established for a certain time.
  • three fractions are pre-formed in the melt itself, consisting of:
  • the present invention therefore relates to a process for working up the superalloy melt digestion product, comprising the following steps:
  • the process according to the invention is shown schematically in the attached FIG. 1 .
  • the superalloy melt digestion product ( 2 ) is crushed after cooling to room temperature, then comminuted in a mill and then leached in water.
  • the leaching is carried out at temperatures of less than 60° C. and particularly preferably at less than 40° C.
  • the particular feature of the melt digestion comprises the three fractions which are formed therein beforehand and are present during the water leaching as fractions which can be easily separated:
  • the rhenium can be separated off after the filtration from the filtrate ( 4 ) over strongly basic ion exchangers, as described in DE 10155791.
  • the rhenium-free solution containing substantially sodium molybdate and sodium tungstate can be added to the process for obtaining molybdenum and tungsten.
  • the nonmagnetic residue which contains up to 15% of tantalum, can be used as raw material in tantalum-metallurgy.
  • the magnetic residue is advantageously used for the production of cobalt and nickel.
  • the process according to the invention is suitable in particular for recovering rhenium from superalloys.
  • the present invention furthermore relates to a process for obtaining rhenium from superalloys, comprising the following steps:
  • the process according to the invention for obtaining rhenium from superalloys is advantageously carried out in a manner such that up to 10% by weight, preferably up to 8% by weight and particularly preferably up to 5% by weight of sodium carbonate (Na 2 CO 3 ), based on the weight of the salt melt, are added to the salt melt.
  • Na 2 CO 3 sodium carbonate
  • the removal of the rhenium from the aqueous suspension by means of strongly basic ion exchange resins is preferred.
  • An advantage of the process according to the invention is that the superalloy digestion in an NaOH—Na 2 SO 4 melt is exothermic. By passing in air or an air/oxygen mixture, the process is readily controllable. A further advantage is that the valuable substances can be virtually completely recovered.
  • the filter cake was suspended again in water, and the metallic, magnetic fractions were separated from the oxidic and hydroxidic fractions by circulating the suspension through a magnetic separator by means of a pump.
  • the substantially metal-free suspension was then separated again by means of a filter press, and the filtrates were initially introduced for the next leaching run. 1.46 t of metal sludge ( 5 ) and 0.56 t of hydroxide sludge ( 6 ) were obtained.
  • the hydroxide sludge ( 6 ) was sent to a tantalum facility for recovering the tantalum, and the metal sludge ( 5 ) was sent to a nickel facility for further working-up.
  • the rhenium-containing filtrate ( 3 ) was passed over ion exchange columns with strongly basic ion exchangers for recovering the rhenium.
  • the further enrichment and purification of the rhenium were effected by standard methods according to the prior art.
  • the rhenium-free outflow of the ion exchange columns was used in a tungsten facility as an initially taken material for the leaching of WO 3 .
  • the rhenium yield was 94%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)
US12/306,853 2006-06-30 2007-06-29 Recycling of superalloys with the aid of an alkali metal salt bath Abandoned US20090255372A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102006030731A DE102006030731A1 (de) 2006-06-30 2006-06-30 Recycling von Superlegierungen
DE102006030731.3 2006-06-30
PCT/EP2007/056527 WO2008000810A1 (de) 2006-06-30 2007-06-29 Recycling von superlegierungen unter verwendung einer alkalimetall- salzschmelze

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US (1) US20090255372A1 (de)
EP (1) EP2038438B1 (de)
JP (1) JP5550336B2 (de)
KR (1) KR101457713B1 (de)
CN (1) CN101479394B (de)
AT (1) ATE528415T1 (de)
CA (1) CA2654516C (de)
DE (1) DE102006030731A1 (de)
MX (1) MX2008015447A (de)
PL (1) PL2038438T3 (de)
RU (1) RU2447165C2 (de)
WO (1) WO2008000810A1 (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110229366A1 (en) * 2010-03-16 2011-09-22 Luederitz Eberhard Method for recovering rhenium and other metals from rhenium-bearing materials
US20120058029A1 (en) * 2009-03-13 2012-03-08 Neo Performance Materials Limited Rhenium recovery
US8632747B2 (en) 2009-03-11 2014-01-21 A.L.M.T. Corp. Method for producing sodium tungstate, method for collecting tungsten, apparatus for producing sodium tungstate, and method for producing sodium tungstate aqueous solution
US9322081B2 (en) 2011-07-05 2016-04-26 Orchard Material Technology, Llc Retrieval of high value refractory metals from alloys and mixtures
WO2017075015A1 (en) 2015-10-26 2017-05-04 Techemet, Llc A method for platinum recovery from materials containing rhenium and platinum metals
US10011890B2 (en) 2013-03-15 2018-07-03 A.L.M.T. Corp. Sodium tungstate production method
CN111876620A (zh) * 2020-07-21 2020-11-03 浙江今飞凯达轮毂股份有限公司 钛元素添加剂和钛元素添加剂制备方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108342583B (zh) * 2018-02-08 2020-01-14 河南科技大学 一种从钼精矿焙烧收尘灰中回收铼和钼的方法
JP7688842B2 (ja) * 2021-12-27 2025-06-05 三菱マテリアル株式会社 タングステン酸ナトリウムの製造方法

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US3649487A (en) * 1969-12-03 1972-03-14 Gullspangs Elektrokemiska Ab Process for the recovery from secondary material of such metals as nickel cobalt iron and copper said secondary material comprising in addition one or more metals having a high melting point
US4320094A (en) * 1980-04-15 1982-03-16 Cabot Corporation Partitioning of refractory metals from oxidation resistant scrap alloy
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US5993756A (en) * 1995-06-12 1999-11-30 H.C. Starck, Gmbh & Co. Kg Sodium tungstate preparation process
US20030136685A1 (en) * 2001-11-14 2003-07-24 Viktor Stoller Process for electrochemical decomposition of superalloys

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US3607236A (en) * 1969-09-22 1971-09-21 Parkman T Brooks Reclaiming of superalloy scrap
US3649487A (en) * 1969-12-03 1972-03-14 Gullspangs Elektrokemiska Ab Process for the recovery from secondary material of such metals as nickel cobalt iron and copper said secondary material comprising in addition one or more metals having a high melting point
US4320094A (en) * 1980-04-15 1982-03-16 Cabot Corporation Partitioning of refractory metals from oxidation resistant scrap alloy
US4521381A (en) * 1984-11-07 1985-06-04 Gte Products Corporation Recovery of rhenium
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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9512504B2 (en) 2009-03-11 2016-12-06 A.L.M.T Corp. Method for producing sodium tungstate, method for collecting tungsten, apparatus for producing sodium tungstate, and method for producing sodium tungstate aqueous solution
US9249479B2 (en) 2009-03-11 2016-02-02 A.L.M.T. Corp. Method for producing sodium tungstate, method for collecting tungsten, apparatus for producing sodium tungstate, and method for producing sodium tungstate aqueous solution
US8632747B2 (en) 2009-03-11 2014-01-21 A.L.M.T. Corp. Method for producing sodium tungstate, method for collecting tungsten, apparatus for producing sodium tungstate, and method for producing sodium tungstate aqueous solution
US8956582B2 (en) * 2009-03-13 2015-02-17 Maritime House Metals Inc. Rhenium recovery
US20120058029A1 (en) * 2009-03-13 2012-03-08 Neo Performance Materials Limited Rhenium recovery
CN103003455A (zh) * 2010-03-16 2013-03-27 世界资源公司 从含铼的材料中回收铼和其他金属的方法
US20110229366A1 (en) * 2010-03-16 2011-09-22 Luederitz Eberhard Method for recovering rhenium and other metals from rhenium-bearing materials
US8383070B2 (en) 2010-03-16 2013-02-26 World Resources Company Method for recovering rhenium and other metals from rhenium-bearing materials
US9322081B2 (en) 2011-07-05 2016-04-26 Orchard Material Technology, Llc Retrieval of high value refractory metals from alloys and mixtures
US10011890B2 (en) 2013-03-15 2018-07-03 A.L.M.T. Corp. Sodium tungstate production method
WO2017075015A1 (en) 2015-10-26 2017-05-04 Techemet, Llc A method for platinum recovery from materials containing rhenium and platinum metals
US9702021B2 (en) 2015-10-26 2017-07-11 Techemet, Llc Method for platinum recovery from materials containing rhenium and platinum metals
US9708690B2 (en) 2015-10-26 2017-07-18 Techemet, Llc Method for platinum recovery from materials containing rhenium and platinum metals
DE112016004897T5 (de) 2015-10-26 2018-07-05 Techemet, Llc Verfahren zur Platingewinnung aus Rhenium- und Platinmetalle enthaltenden Materialien
CN111876620A (zh) * 2020-07-21 2020-11-03 浙江今飞凯达轮毂股份有限公司 钛元素添加剂和钛元素添加剂制备方法

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RU2009102948A (ru) 2010-08-10
JP5550336B2 (ja) 2014-07-16
DE102006030731A1 (de) 2008-01-03
EP2038438B1 (de) 2011-10-12
CA2654516A1 (en) 2008-01-03
WO2008000810A1 (de) 2008-01-03
KR101457713B1 (ko) 2014-11-03
PL2038438T3 (pl) 2012-04-30
CN101479394A (zh) 2009-07-08
CN101479394B (zh) 2012-09-26
MX2008015447A (es) 2008-12-12
RU2447165C2 (ru) 2012-04-10
ATE528415T1 (de) 2011-10-15
CA2654516C (en) 2014-12-23
EP2038438A1 (de) 2009-03-25
JP2009541596A (ja) 2009-11-26
KR20090023692A (ko) 2009-03-05

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