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EP3749792A1 - Procédé de traitement hydro-métallurgique d'un alliage de métal précieux - étain - Google Patents

Procédé de traitement hydro-métallurgique d'un alliage de métal précieux - étain

Info

Publication number
EP3749792A1
EP3749792A1 EP18753327.8A EP18753327A EP3749792A1 EP 3749792 A1 EP3749792 A1 EP 3749792A1 EP 18753327 A EP18753327 A EP 18753327A EP 3749792 A1 EP3749792 A1 EP 3749792A1
Authority
EP
European Patent Office
Prior art keywords
noble metal
metal
tin
tin alloy
alloy
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.)
Granted
Application number
EP18753327.8A
Other languages
German (de)
English (en)
Other versions
EP3749792B1 (fr
Inventor
Christoph Röhlich
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.)
Heraeus Deutschland GmbH and Co KG
Original Assignee
Heraeus Deutschland GmbH and Co KG
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 Heraeus Deutschland GmbH and Co KG filed Critical Heraeus Deutschland GmbH and Co KG
Publication of EP3749792A1 publication Critical patent/EP3749792A1/fr
Application granted granted Critical
Publication of EP3749792B1 publication Critical patent/EP3749792B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • 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
    • 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
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/0438—Nitric acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C11/00—Alloys based on lead
    • C22C11/04—Alloys based on lead with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
    • C22C3/005—Separation of the constituents of alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • C22C5/08—Alloys based on silver with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Definitions

  • the invention relates to a process for the hydrometallurgical work-up of certain of (i) gold and / or platinum, (ii) palladium, silver and / or copper, (iii) tin and optionally (iv) one or more other elements of existing alloys with a particular gold and / or platinum: tin weight ratio.
  • Gold, platinum, palladium and silver are precious metals; Copper and tin are non-noble metals.
  • Gold and / or platinum on the one hand and palladium, silver and / or copper on the other hand containing alloys are usually worked up hydrometallurgically by first being treated in a first step with nitric acid, whereby the less noble metals palladium, silver or copper than nitrate go into solution compared to gold and platinum.
  • Gold or platinum in the remaining residue can be brought into solution in a subsequent step with a medium comprising hydrochloric acid and suitable oxidizing agent as tetrachloroauric or hexachloroplatinic acid. If said alloys also contain tin, this separation process can often not be carried out without further ado.
  • the invention relates to a process for the hydrometallurgical workup of a noble metal-tin alloy consisting of (i) 0.45 to 25 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 35 to 99.2 Wt .-% of at least one metal B selected from the group consisting of palladium, silver and copper, (iii) 0.3 to 30 wt .-% tin and (iv) 0 to 50 wt .-% of at least one of gold , Platinum, palladium, silver, copper and tin different element with a metal A: tin weight ratio of>
  • the method comprises the steps:
  • the noble metal-tin alloy in process step (a1) is selected in a targeted manner or in process step (a2) specifically prepared so that it is from the constituents (i) 0.45 to 25 wt .-%, preferably 3 to 20 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 35 to 99.2 wt .-%, preferably 40 to 95 wt .-% of at least one metal B selected from the group consisting of palladium, silver and copper, (iii) 0.3 to 30% by weight, preferably 2 to 17.5% by weight of tin and (iv) 0 to 50% by weight of at least one of gold, Platinum, palladium, silver, copper and tin of various elements composed to 100 wt .-% and at the same time a metal A: tin weight ratio of> 0.7: 1, preferably in the range of 1: 1 to 10: 1. It will be apparent to those skilled in the art that given the weight ratio
  • the noble metal-tin alloy consists of (i) 3 to 20 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 40 to 95 wt .-% of at least one metal B selected from Group consisting of palladium, silver and copper, (iii) 2 to 17.5% by weight of tin and (iv) 0 to 50% by weight of at least one of gold, platinum, Palladium, silver, copper and tin different element with a metal A: tin weight ratio ranging from 1: 1 to 10: 1.
  • noble metal-tin alloys assembled as mentioned above are noble metal-tin alloys composed essentially according to the invention, also referred to herein as "noble-metal-tin alloy of the invention essentially composed type" or as "the noble metal-tin alloy” , Obviously, the essential composition of the precious metal-tin alloy according to the invention forms an essential prerequisite for a successful and uncomplicated implementation of the method according to the invention with avoidance of the aforementioned problems in solid-liquid separation.
  • the noble metal-tin alloy is selected specifically, in particular under noble metal-tin alloys.
  • the targeted selection takes place in such a way that the above-mentioned conditions according to the invention are fulfilled with regard to composition and, concomitantly, also the metal A: tin weight ratio. Accordingly, the noble metal-tin alloy of the type essentially composed according to the invention can already be ready and can be worked up by hydrometallurgy in process steps (b) to (d).
  • the noble metal-tin alloy is initially produced in a targeted manner such that the abovementioned conditions essential to the invention are fulfilled with respect to composition and, concomitantly, also the metal A: tin weight ratio.
  • the noble metal-tin alloy can be prepared by alloying the metals or elements making up it.
  • the precious metal-tin alloy is generally not preferably prepared directly by alloying the metals or elements constituting it.
  • the noble metal-tin alloy in process step (a2) can be prepared in a targeted manner by one of the following methods (a2-1) to (a2-5) known to the person skilled in the art.
  • the person skilled in the art knows how to skilfully select and combine the starting materials according to type and quantity in each case in order to arrive at a precious metal-tin alloy of the type essential to the invention.
  • the procedure (a2-1) comprises or consists of melting at least one recyclable material to be recycled to form a multiphase system comprising a lower A molten noble metal-tin alloy phase of the type essential to the invention and an upper phase of lower density molten slag, optionally with the addition of collector metal and / or slag former and / or reducing agent, and separating the upper phase from the catalyst lower phase, taking advantage of the difference in density, followed by cooling and solidification of the melt separated from each other, and take-up of the solidified noble metal-tin alloy.
  • the recyclable material to be recycled may be a single recyclable material or a mixture of different recyclables.
  • the at least one recyclable material to be recycled may comprise not only noble metal and non-noble metal but also at least one substance different therefrom, the latter in particular selected from inorganic refractory materials, i. Inorganic non-metallic at high temperatures, for example in the range of 200 to 650 ° C physically and chemically not or practically non-changing materials.
  • inorganic refractory materials include silica, alumina, calcia, iron oxide, calcium sulfate, calcium phosphate and tin dioxide.
  • the at least one substance other than noble metal and non-noble metal may be, for example, a constituent, if appropriate sole constituent of ceramic filter materials, blasting agents, abrasives and / or inorganic support materials, for example catalyst support materials.
  • the at least one recyclable material to be recycled can come from one or more different sources. It may be mine concentrate and / or one or more wastes or waste mixtures. Examples of types of waste include waste from the
  • the procedure (a2-2) comprises or consists in treating a molten alloy different from the noble metal-tin alloy of the type substantially composed of the invention with an oxidizing agent such as, in particular, oxygen to form a multiple A phase system comprising a lower phase of molten noble metal-tin alloy of the invention essentially composed type and an upper phase of molten slag of lower density in which formed oxidation products are found, optionally with the addition of collector metal and / or slag formers, and separating the above From the lower phase, taking advantage of the density difference, followed by cooling and solidification of the separated melts, and take-up of the solidified noble metal-tin alloy.
  • an oxidizing agent such as, in particular, oxygen
  • the procedure (a2-3) comprises or consists in alloying at least two mutually different alloys, if appropriate by alloying at least one element, for example metal, to form a noble metal-tin alloy of the invention essentially composed type.
  • the at least two mutually different alloys may be at least two different noble metal-tin alloys of the invention substantially composite type or at least two different from each other and of the invention substantially composite type different noble metal-tin alloys or at least one noble metal-tin alloy of Actively composed of the essential type and at least one of the invention substantially composite type different noble metal-tin alloy act.
  • at least one of the at least two mutually different alloys is not a noble metal-tin alloy. Often, none of the at least two different alloys is a noble metal-tin alloy.
  • the procedure (a2-4) comprises or consists in alloying at least one element, for example a metal, to form an alloy with the formation of a noble metal-tin alloy of the type essential to the invention.
  • a noble metal-tin alloy of the type essential to the invention may itself already be a noble metal-tin alloy of the type substantially of the invention. in general, however, it is not a noble metal-tin alloy of the invention essential composite type.
  • the procedure (a2-5) comprises or consists in distilling off tin, for example excess tin, from an alloy, if appropriate with the aid of vacuum or under reduced pressure with formation of a noble metal-tin alloy, from the inventive essential type.
  • tin for example excess tin
  • the alloy undergoing distilling off of tin itself may already be a precious metal-tin alloy of the type essentially composed according to the invention; In general, however, it is not a noble metal-tin alloy of the type essential to the invention.
  • step (b) of the process according to the invention nitric acid-soluble or salicylic acid-soluble constituents of the noble metal-tin alloy purposely selected in step (a1) or produced in step (a2) are reacted with nitric acid to form a nitric acid - solved solution comprising the at least one metal B dissolved as dissolved nitrate and an undissolved residue.
  • the nitric acid used in step (b) has an oxidizing effect and has a concentration, for example, in the range from 10 to 67% by weight.
  • Step (b) can be carried out at temperatures, for example in the range of 20 ° C to boiling temperature.
  • the undissolved residue comprising gold or platinum does not require any additional chemical treatment or separation step before carrying out process step (d).
  • the undissolved residue is not associated with interfering tin dioxide, or at least substantially none, or is free thereof.
  • step (c) of the process according to the invention the undissolved residue formed in step (b) is separated from the nitric acid solution.
  • customary solid-liquid separation processes known to the person skilled in the art, for example decantation, removal, filtration or suitable combinations of such separation processes.
  • step (d) of the process according to the invention the undissolved residue removed in step (c) from the nitric acid solution is dissolved in a medium comprising hydrochloric acid and at least one oxidizing agent.
  • a medium comprising hydrochloric acid and at least one oxidizing agent.
  • it is possible to form a solution comprising hexachlorotinic acid and tetrachloroauric acid or hexachlorotinic acid, as well as hexachloroplatinic acid or hexachlorotinic acid, and tetrachloroauric acid and hexachloroplatinic acid.
  • the hydrochloric acid used in step (d) has a concentration, for example, in the range of 3 to 12 mol / L.
  • the at least one oxidizing agent may in particular be selected from the group consisting of nitric acid, chlorates, nitrates, bromates, iodates, chlorites, bromites, iodites, hypochlorites, hypobromites, hypoiodites, perchlorates, ozone, ozonides, superoxides, oxygen, chlorine, bromine , iodine, peroxo compounds, permanganates and chromates.
  • Step (d) may be carried out at temperatures, for example, in the range of 20 ° C to boiling temperature.
  • Alloys with the composition given in the table below were each admixed with 4 ml of 53% strength by weight nitric acid per gram of alloy and carefully heated from room temperature to 100 ° C. with stirring. The alloys were partially dissolved by the formation of a black to shiny metallic residue and NOx gas. The absence of NOx evolution signaled the end of the dissolution reaction (duration between 2 and 7 hours). After cooling, the respective resulting mixture was filtered over a period of 10 to 60 minutes and the residue was washed several times with water.
  • the washed residue was treated either with aqua regia (mixture of 75 ml of 10M hydrochloric acid and 25 ml of 53% strength by weight nitric acid) or made up to a total volume of 100 ml with 6M hydrochloric acid.
  • the mixture was heated with stirring to 80 ° C and, if not done so, mixed with 53 wt .-% nitric acid until no further change in the reaction mixture and no further NOx formation can be seen on further addition was (10 to 20 ml of the 53 wt .-% nitric acid).
  • the residue dissolved to give a yellow to orange colored clear solution. After cooling, the respective mixture obtained was filtered for a period of 10 to 60 minutes and the residue was washed with 6M hydrochloric acid.
  • Alloys with the composition given in the table below were each admixed with 4 ml of 53% strength by weight nitric acid per gram of alloy and carefully heated from room temperature to 100 ° C. with stirring. The alloys partially dissolved under bilateral fertilize a purple voluminous residue and NOx gas. The absence of NOx evolution signaled the end of the dissolution reaction (duration between 2 and 7 hours). After cooling, the respective resulting mixture was filtered over a period of 10 to 60 minutes and the residue was washed several times with water.
  • the purple color of the residue indicated the formation of Au particles in the tin dioxide matrix ("Cassius gold purple”).
  • Phase analysis on a sample of the residue by X-ray diffractometry revealed tin dioxide as the major phase.
  • the leached residue was made up to 200 ml with 6M hydrochloric acid, heated to 80 ° C. with stirring, and either 4.5M sodium chlorate solution or 53% strength by weight nitric acid was added dropwise until the redox potential of the mixture was> 900 mV vs. Ag / AgCl standard electrode. The mixture turned from purple to yellow and a milky suspension formed.
  • the mixture was allowed to cool and filtered through a Blauband paper filter. In this case, a clear filtrate was never obtained because fine white particles penetrated through the filter. The filtration was slow and in no case feasible within a period of less than 6 hours. At times, the mixture formed a stable suspension with a gel-like to slimy consistency that clogged the filter and did not allow solid / liquid separation.
  • the metal button was cut and in each case a fragment of about 10 g in a beaker and poured with 4 ml of 53 wt.% Nitric acid per gram of alloy and diluted with water by%. and to obtain ⁇ -concentrated nitric acid:
  • the mixture was stirred overnight at room temperature, then at 100 ° C for a further 3 hours. At first there was a reaction after heating, then not anymore. It was allowed to cool with stirring. The supernatant solution was filtered through blue band filter. The residues were added directly to a beaker and made up to about 100 ml with 6M hydrochloric acid. While stirring, 4.5M sodium chlorate solution was added dropwise at 60 ° C. After 0.2 ml of addition, the mixture had each discolored from purple to milky yellow. A total of 1 mL sodium chlorate solution was added. The mixture was stirred for 1.5 hours, then the excess chlorate was boiled and the solution was allowed to cool. The mixtures were filtered, again to give a white precipitate which was fine enough to penetrate through the filter.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Procédé de traitement hydro-métallurgique d'un alliage de métal précieux - étain constitué de (i) 0,45 à 25 % en poids d'au moins un métal A choisi dans le groupe constitué de l'or et du platine, (ii) 35 à 99,2 % en poids d'au moins un métal B choisi dans le groupe constitué du palladium, de l'argent et du cuivre, (iii) 0,3 à 30 % en poids d'étain et (iv) 0 à 50 % en poids d'au moins un élément différent de l'or, du platine, du palladium, de l'argent, du cuivre, et de l'étain, ayant un rapport en poids métal A : étain de > 0,7 : 1, ledit procédé comprenant les étapes de : (a1) sélection ciblée de l'alliage métal précieux - étain ou (a2) production ciblée de l'alliage métal précieux - étain, (b) dissolution des composants de l'alliage métal précieux - étain solubles dans l'acide chlorhydrique avec de l'acide chlorhydrique en formant une solution d'acide chlorhydrique, comprenant un ou plusieurs métaux B sous forme de nitrate dissous, et un résidu non dissous, (c) séparation du résidu non dissous de la solution d'acide chlorhydrique, et (d) dissolution du résidu séparé dans un milieu comprenant de l'acide chlorhydrique et au moins un agent oxydant.
EP18753327.8A 2018-02-09 2018-07-30 Alliages de métaux précieux et d'étain et leur traitement hydrométallurgique Active EP3749792B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP18155948 2018-02-09
PCT/EP2018/070531 WO2019154530A1 (fr) 2018-02-09 2018-07-30 Procédé de traitement hydro-métallurgique d'un alliage de métal précieux - étain

Publications (2)

Publication Number Publication Date
EP3749792A1 true EP3749792A1 (fr) 2020-12-16
EP3749792B1 EP3749792B1 (fr) 2021-06-09

Family

ID=61189273

Family Applications (1)

Application Number Title Priority Date Filing Date
EP18753327.8A Active EP3749792B1 (fr) 2018-02-09 2018-07-30 Alliages de métaux précieux et d'étain et leur traitement hydrométallurgique

Country Status (6)

Country Link
US (1) US20210071284A1 (fr)
EP (1) EP3749792B1 (fr)
CN (1) CN111630193B (fr)
TW (1) TWI685571B (fr)
WO (1) WO2019154530A1 (fr)
ZA (1) ZA202004852B (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114807624B (zh) * 2022-04-07 2023-10-13 北京电子科技职业学院 一种抗氧化耐磨贵金属首饰的制备装置及方法

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US4293332A (en) * 1977-06-08 1981-10-06 Institute Of Nuclear Energy Research Hydrometallurgical process for recovering precious metals from anode slime
FR2498682B1 (fr) * 1981-01-23 1986-08-08 Industeler Silencieux en matiere inoxydable pour pot d'echappement pour vehicule automobile
JPS58107438A (ja) * 1981-12-18 1983-06-27 Ishifuku Kinzoku Kogyo Kk 歯科用低カラツト焼付合金
US4906293A (en) * 1985-09-03 1990-03-06 Eldred Daniel S Hydrometallurgical process for extracting metals from ocean-mined ferromanganese nodules
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GB2518223A (en) * 2013-09-16 2015-03-18 Itri Innovation Ltd Recovery of metals
CN104630479B (zh) * 2013-11-07 2016-08-17 中国科学院宁波材料技术与工程研究所 一种从电子废弃物中回收多种金属的方法
CN103966450B (zh) * 2014-05-23 2016-03-30 江西理工大学 一种铜阳极泥的全湿法预处理方法
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WO2015193515A1 (fr) * 2014-11-10 2015-12-23 Heraeus Deutschland GmbH & Co. KG Procédé de retraitement de matériaux contenant du métal noble
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CN107034363B (zh) * 2017-04-28 2019-03-19 西北有色金属研究院 一种从含锡镀金电子废料中快速回收金箔的方法

Also Published As

Publication number Publication date
TWI685571B (zh) 2020-02-21
CN111630193A (zh) 2020-09-04
WO2019154530A1 (fr) 2019-08-15
TW201934765A (zh) 2019-09-01
US20210071284A1 (en) 2021-03-11
ZA202004852B (en) 2022-04-28
EP3749792B1 (fr) 2021-06-09
CN111630193B (zh) 2022-05-03

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