EP0138801B1 - Procédé d'affinage électrolytique de l'argent - Google Patents

Procédé d'affinage électrolytique de l'argent Download PDF

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Publication number
EP0138801B1
EP0138801B1 EP84890159A EP84890159A EP0138801B1 EP 0138801 B1 EP0138801 B1 EP 0138801B1 EP 84890159 A EP84890159 A EP 84890159A EP 84890159 A EP84890159 A EP 84890159A EP 0138801 B1 EP0138801 B1 EP 0138801B1
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EP
European Patent Office
Prior art keywords
silver
electrolyte
contaminating metals
extraction
extracted
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
Application number
EP84890159A
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German (de)
English (en)
Other versions
EP0138801A1 (fr
Inventor
Adalbert Dr. Prior
Rolf Prof.Dipl.-Ing.Dr. Marr
Hans J. Dr. Bart
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.)
Ogussa Osterreichische Gold- und Silber-Scheideanstalt Scheid und Roessler & Co Kg GmbH
Original Assignee
Ogussa Osterreichische Gold- und Silber-Scheideanstalt Scheid und Roessler & Co Kg GmbH
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Publication of EP0138801A1 publication Critical patent/EP0138801A1/fr
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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

Definitions

  • the invention relates to an electrolytic silver refining process in which crude silver is anodically dissolved and raffinate silver is deposited cathodically, with accompanying metals being extracted selectively from the used electrolyte and separately being cathodically deposited after being converted into an aqueous phase, and the regenerated, low-accompanying-metal electrolyte is returned to silver electrolysis .
  • electrolytic silver refining which is usually carried out according to the Möbius or Balbach / Thum process
  • the less noble accompanying metals present in the anode raw silver, in particular the copper are a significant burden on the process, since they are dissolved and accumulate in the electrolyte.
  • a Cu content of around 60 g / l is considered the highest permissible value;
  • a cathodic copper deposition can occur above this, but at least copper salts are enclosed by the raffinate silver, so that the fineness requirements are no longer met.
  • the used electrolyte must therefore be regenerated or replaced from time to time.
  • the electrolyte cycle has already been used, with the used electrolyte being withdrawn from the refining cell, Cu being removed therefrom on the extraction path and the thus regenerated, low-Cu electrolyte being returned to the refining cell.
  • the extracted Cu was transferred into an aqueous phase and cathodically separated.
  • a large number of organic reagents have become known as selective extractants for Cu; this is how z.
  • B the known method described above according to the principle of solvent extraction with chelating agents such as phenonoximes or quinolines.
  • the used electrolyte is extracted in mixer / settler systems and the Cu is stripped from the organic extract phase with an acidic stripping solution.
  • the loaded stripping solution is electrolyzed, with Cu and optionally also Ni being able to be deposited cathodically. Depending on the chelating agent and the working conditions, it is possible to extract accompanying metals more or less selectively.
  • the organic phase (solvent + extractant) is washed.
  • the organic phase, the stripping solution regenerated by electrolysis and the regenerated electrolyte are circulated.
  • the object was therefore to create a process of the type mentioned at the outset in which there is a continuous complete regeneration of the electrolyte, in which the silver deficiency is also compensated for without the addition of silver nitrate solution.
  • the electrolyte used is anodically enriched with silver in a common electrolysis process and accompanying metals are cathodically deposited from the aqueous phase.
  • the system according to the invention for carrying out this method accordingly has, in addition to at least one refining cell, at least one electrolysis cell for cathodic deposition of the accompanying metals and at least one extraction device for extracting the accompanying metals from the used electrolyte and for transferring the extracted accompanying metals into an aqueous phase, at least one common electrolysis cell for enrichment of the used electrolyte with silver and for the cathodic deposition of accompanying metals in the form of a diaphragm cell with a silver anode.
  • Ag is anodically dissolved in the common electrolysis cell, a crude silver anode advantageously being used, since the accompanying metal content does not have to be completely eliminated, but only has to be reduced.
  • the current released during the cathodic deposition of the accompanying metals on the cathode supports the dissolution of the silver anodes.
  • the task of the anionic diaphragm is to prevent silver from getting into the cathode compartment where it would be excreted together with the accompanying metals, and to maintain the desired large concentration gradient of nitrate ions between the cathode and anode compartments.
  • a solvent extraction is usually carried out in the process according to the invention, the refining electrolyte used first being treated with a solvent / extractant phase and then stripping with an ionic (N0 3 ) stripping solution.
  • the solvent / extractant phase serves as a separating membrane between the used refining electrolyte and the acidic stripping solution, which is emulsified in the separating membrane.
  • the emulsion phase is separated off and, in a known manner, integrated into an aqueous phase (loaded stripping solution) and an organic phase (solvent / extractant).
  • the loaded stripping solution is regenerated by subsequent accompanying metal electrolysis or separation of valuable materials without electrolysis and emulsified again in the organic phase.
  • the organic phase only serves as a selective separation medium between the aqueous phases (used refining electrolyte and stripping solution), so that it does not have to absorb the accompanying metal as in liquid / liquid extraction. This results in a significantly reduced solvent expenditure as well as high enrichment rates, e.g. B. in the range of 1: 100.
  • FIG. 1 shows a flow diagram of a system according to the invention for its implementation
  • Fig. 2 is a schematic elevation of a diaphragm cell in section
  • Fig. 3 is a corresponding plan.
  • the used electrolyte E 1 flows from the refining cell 1 into the anode space 2 of a diaphragm electrolysis cell 2, 8, where it is enriched with silver by anodic dissolution of a silver anode.
  • the silver-enriched electrolyte E2 then arrives in the collecting tank 3, where it is adjusted to a pH value suitable for the extraction by passing it over Cu / Ag scrap, by adding lye or the like.
  • the pH-adjusted electrolyte E3. then reaches a two-stage extraction system 4.5, z. B. a mixer / setter, where it is extracted in countercurrent with a regenerated solvent / extractant phase (short solvent phase) S.
  • the pH-adjusted electrolyte E3 gets into the mixer of the first extraction stage 4, is extracted there with the solvent phase S 2 already loaded in the second extraction stage 5 and arrives from the settler of the first extraction stage 4 as pre-extracted electrolyte E 4 into the mixer of the second Extraction level 5, where accompanying metal is extracted with the unloaded, regenerated solvent phase S.
  • the now regenerated electrolyte E 5 is returned from the settler of the second extraction stage 5 to the refining cell.
  • the solvent phase S 3 which is loaded twice with accompanying metal, passes from the settler of the second extraction stage into the mixer of a washing system 6, where the silver content is reduced by washing with a washing solution W containing copper.
  • the silver is replaced by copper in the solvent phase S 3 and the silver-laden washing solution W 2 is returned to the collecting tank 3.
  • the arrangement of a washing system 6 is not absolutely necessary.
  • the now low-silver solvent phase S 4 enters the mixer of a stripping plant 7 and is freed of accompanying metal with the regenerated acid stripping solution A, by re-extraction, or the accompanying metal content is reduced to the desired extent.
  • the now regenerated solvent phase S is returned from the settler of the stripping system 7 to the mixer of the second extraction stage 5.
  • the stripping solution A 2 loaded with accompanying metal passes from the settler of the stripping system into the cathode chamber 8 of the diaphragm electrolysis cell 2 , 8, where accompanying metal is deposited cathodically.
  • the stripping solution A 1 thus regenerated is returned to the mixer of the stripping system 7.
  • a closed circuit for electrolyte, solvent phase and stripping solution is also possible.
  • the overall arrangement of the process stages can also be such that the used electrolyte is enriched with silver only after the accompanying metal extraction by anodic dissolution of a silver electrode.
  • the used electrolyte E is first fed into the extraction stages 4, 5 and then reaches the anode space 2 of the diaphragm electrolysis cell, where it is enriched with silver and then goes back to the electrolysis cell 1.
  • the cycle of the solvent phase and the stripping phase remains unchanged. This way of driving has the advantage that not so much Ag in the Extract S 3 is carried along.
  • a partial stream E 1 'of the used refining electrolyte E 1 is branched off and fed to a permeator P, where the partial stream E 1 ' by selective mass transfer with a Emulsion of a stripping solution in an organic solvent / complexing agent phase is freed of W or the W content is reduced accordingly.
  • the low-heat electrolyte E 1 "is fed back into the electrolyte stream E 1. Similar arrangements can be made with regard to the other accompanying metals.
  • extraction or permeation stages for the selective separation of different accompanying metals can also be connected in series, with or without a partial current mode of operation.
  • the preparation of the stripping solutions loaded with accompanying metal for the recovery of valuable materials can be carried out electrolytically, by other known processing methods or by a combination of the methods specified.
  • FIGS. 2 and 3 schematically show the diaphragm cell with an anionic membrane M, the Cu cathode CA and the crude silver anode AN, the electrolytes, the processes in the cell and with the guidance of electrolyte E and stripping solution: A.
  • an Ag-enriched used electrolyte E2 with 37.7 g / I Cu and 67 g / l Ag reaches the storage tank 3 and is drawn off from there at 1 I / h and in the two extraction stages 4.5 with 2 l / h of an extractant S 1 , which consists of 20 parts by volume of Acorga PT 5050 (Acorga Ltd.) as complexing agent and 80 parts by volume of Shellsol AB (aromatic solvent from Shell Intern.) As a diluent .
  • the complexing agent Acorga PT 5050 is a mixture of 2 parts of 2-hydroxy-5-nonylbenzaldoxime and 1 part of Tridecanoi.
  • the organic extract S 3 contains 10.4 g / I Cu and 10 ppm Ag and is regenerated either directly in the stripper 7 with an aqueous stripping solution A 1 (30 g / l Cu, 2 mol / l HN0 3 , 1 I / h) or previously washed in scrubber 6 using an aqueous 1 mol / l Cu (N0 3 ) 2 solution (1 l / h) Ag-free or Ag-poor.
  • the loaded stripping solution A 2 contains 59.5 g / l Cu, the regenerated extractant S 1 3.2 g / l Cu.
  • the used washing solution W 2 was, as can be seen in FIG. 1, fed to the storage tank 3 and the low-copper electrolyte E 5 to the refining cell 1 (Möbius).
  • Example 2 The procedure was as in Example 1 with the modification that the extractant S 1 from 20 parts by volume SME 529 (2-hydroxy-5-nonylaceo-tophenonoxime) as a complexing agent and 80 parts by volume MSB 529 (aromatic solvent of the shell Intern.) Existed as a diluent.
  • the extract S 3 contained 7.6 g / l Cu and 750 ppm Ag and was washed in scrubber 6 with an aqueous 1.0 m Cu (NO 3 ) 2 solution.
  • the Ag-arm washed extract S 4 (12 g / I Cu, 10 ppm Ag) was treated in the stripper 7 with an aqueous stripping solution A 1 (30 g / l Cu, 2 mol / l HNO 3, 1 I / h).
  • the regenerated extractant S 1 contained 1.9 g / l Cu
  • the loaded stripping solution A 2 entered the cathode compartment 8 of the diaphragm cell, where 20.2 g / l Cu was deposited and the equivalent amount of Ag was dissolved anodically.
  • Example 1 The procedure was as in Example 1 with the modification that the extractant S 1 consisted of 20 parts by volume of HS-LIX 64 as a complexing agent and 80 parts by volume of MSB 529 (aromatic solvent from Shell Intern.) As a diluent.
  • the complexing agent HS-LIX 64 contains 20 parts of 3-hydroxy-5-nonylbenzophenonoxime and 1 part of 5,8-diethyl-7-hydroxy-6-dodecano-noxime as active ingredients.
  • the extract S 3 contained 6.9 g / l Cu and 1.5 g / l Ag and was in the scrubber 6 with an aqueous 2 mol / l Cu (NO 3 ) 2 solution to a content of 10.5 g / l Cu and washed with 230 ppm Ag.
  • the washed extract S 4 was then stripped in the stripper 7 in the phase ratio extract S 4 : stripping solution A 1 of 2: with an aqueous stripping solution which contained 30 g / l Cu and 2 mol / l HN0 3 . From the loaded stripping solution A 2 2.8 19.2 g / l Cu were deposited in the cathode compartment 8 of the diaphragm cell 2.8 and the equivalent amount of Ag was dissolved in the anode compartment.
  • the extract S 3 contained 11.0 g / I Cu, 2 ppm Ag and 300 ppm Pd and was stripped in the stripper 7 with an aqueous stripping solution A 1 (35 g / l Cu, 2 mol / l HN0 3 ).
  • the regenerated extractant S 1 contained 3.2 g / l of Cu and 300 ppm Pd and was not entirely returned to extraction stage 5, but a partial stream was branched off in an amount of 1/10 of its total volume and in a separate extraction stage with the same volume 6 n HCl extracted and completely freed of Cu and Pd. After on closing washing with water to remove the chlorine ions, the regenerated partial stream was added to the extractant S 1 again; the Pd was precipitated as Pd (NH 3 ) 2 Cl 2 from the hydrochloric acid stripping solution.
  • the extract was stripped first with m HN0 3 and then with 2.5 n HN0 3 ; the extractant then contained 30 ppm of Cd.
  • the strip solutions were worked up in the usual way.
  • the extract was extracted in an extraction column with half the volume of water at 80 ° C., 3 ppm Pt remaining in the extract and the water phase being worked up in the usual manner with 91 ppm Pt as nitrate.
  • the electrolyte was freed of Cu, Ag and Pd as in Example 5b).
  • the electrolyte then contained 0.5 g / IW and was subjected to liquid membrane permeation.
  • a solvent / extractant phase containing an aliphatic solvent, 5% M tertiary amine, namely Alamin 336 or Hostarex 327, as a complexing agent and 3% M ECA 4360 (surfactant from Esso), in a volume ratio of 2: 1 with a aqueous stripping solution, consisting of saturated ammonium nitrate, emulsified.
  • Alamin 336 (Henkel) is a mixture of tertiary n-alkylamines with C 8 -C 10 alkyl chains, where C8 chains predominate.
  • Hostarex 327 (Hoechst) is a 1: 1 mixture of tri-n-octylamine and tri-n-decylamine.
  • a used Möbius electrolyte is regenerated in a system as described above, in which the extraction stage 4, 5 is designed as a conventional liquid membrane permeation unit:
  • an extractant phase consisting of kerosene as solvent, 3 vol.% Acorga P 5100 (1 Part 2-hydroxy-5-nonylbenzaldoxim + 1 part nonylphenol) as complexing agent and 3% ECA 4360 (surfactant based on polyamine), in a volume ratio of 2: 1 emulsified with an aqueous stripping solution containing 30 g / I Cu and 2 mol / 1 HN0 3 contained.
  • the permeator was operated with a throughput of 10 1 / h Ag-enriched used electrolyte E2 or used electrolyte E 1 and 3 I / h liquid membrane. In both cases, a Cu content of about 60 g / l was achieved in the aqueous stripping solution obtained after the emulsion had been cleaved. Further processing can be carried out analogously to Examples 1-5.
  • Examples 1 to 6 a diaphragm cell was used with a plastic-based anion exchange membrane with the trade name MA3148 from IONAC Chemical Co., New Jersey.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Claims (11)

1. Procédé d'affinage électrolytique d'argent dans lequel de l'argent cru est dissous anodique- ment et l'argent affiné est déposé cathodiquement et au même temps, les métaux contaminants sont extraits sélectivement de l'électrolyte usé et sont déposés cathodiquement suivant le transfert dans une phase aqueuse et l'électrolyte régénéré dépourvu de métaux contaminants est recyclé dans le procédé d'affinage, caractérisé en ce que dans une opération commune d'électrolyse, l'électrolyte usé est enrichi en argent et les métaux contaminants sont déposés cathodiquement de la phase aqueuse.
2. Le procédé selon la revendication 1, caractérisé en ce que les opérations d'électrolyse sont effectuées au moyen de solutions de parité ionique, en particulier de solutions d'acide nitrique.
3. Le procédé selon la revendication 1 ou 2, caractérisé en ce que du Cu est extrait de l'électrolyte et est déposé cathodiquement simultanément avec l'enrichissement anodique en argent.
4. Le procédé selon la revendication 3, caractérisé en ce que le Cu est extrait de l'électrolyte en premier lieu et l'enrichissement en argent est ajourné jusqu'avant le recyclage dans le procédé d'affinage.
5. Le procédé selon la revendication 4, caractérisé en ce que d'autres métaux contaminants, en particulier le Cd, Ni, Pd, Pt et/ou W sont extraits de l'électrolyte usé après le dépôt du Cu, mais avant l'enrichissement en argent.
6. Le procédé selon une des revendications 1 à 5, caractérisé en ce que l'extraction des métaux contaminants est effectuée sous forme de perméation membrane liquide, de préférence en combinaison avec une extraction de solvant.
7. Le procédé selon la revendication 5, caractérisé en ce que les autres métaux contaminants sont traités de manière non électrolytique après leur extraction sélective.
8. Dispositif pour la mise en oeuvre du procédé selon une des revendications 1 à 6, pourvu d'au moins une cellule d'affinage, au moins un moyen d'extraction pour extraire des métaux contaminants de l'électrolyte usé et pour le transfert des métaux contaminants extraits dans une phase aqueuse, et au moins une cellule d'électrolyse pour le dépôt cathodique de métaux contaminants de la phase aqueuse, caractérisé en ce qu'au moins une cellule commune d'électrolyse pour l'enrichissement de l'électrolyte usé en argent et pour le dépôt cathodique de métaux contaminants est pourvue sous forme d'une cellule à diaphragme avec une anode en argent.
9. Le dispositif selon la revendication 8, caractérisé en ce qu'un diaphragme anionique, en particulier sous forme d'une membrane d'échange anionique sur base de matières plastiques, est pourvu.
10. Le dispositif selon la revendication 8 ou 9, caractérisé en ce que la cellule à diaphragme est pourvue d'une anode en argent cru.
11. Le dispositif selon une des revendications 8 à 10, caractérisé en ce que le moyen d'extraction est un moyen de perméation membrane liquide.
EP84890159A 1983-08-29 1984-08-23 Procédé d'affinage électrolytique de l'argent Expired EP0138801B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT0307383A AT380032B (de) 1983-08-29 1983-08-29 Elektrolytisches silberraffinationsverfahren
AT3073/83 1983-08-29

Publications (2)

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EP0138801A1 EP0138801A1 (fr) 1985-04-24
EP0138801B1 true EP0138801B1 (fr) 1987-04-15

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EP84890159A Expired EP0138801B1 (fr) 1983-08-29 1984-08-23 Procédé d'affinage électrolytique de l'argent

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US (1) US4670115A (fr)
EP (1) EP0138801B1 (fr)
AT (1) AT380032B (fr)
DE (1) DE3463163D1 (fr)
ES (1) ES8602966A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT383372B (de) * 1985-07-24 1987-06-25 Oegussa Elektrolytisches silberraffinationsverfahren
CA2017032C (fr) * 1990-05-17 1995-10-10 Khay Gie J. Tan Raffinage hydrometallurgique de l'argent
US5409582A (en) * 1993-01-29 1995-04-25 Monsanto Company Silver bath waste treatment apparatus and method
FR2761085B1 (fr) * 1997-03-24 1999-04-16 Commissariat Energie Atomique Procede electrolytique de recuperation et de recyclage de l'argent a partir d'une solution nitrique
AT2421U1 (de) * 1997-11-06 1998-10-27 Prior Eng Ag Anlage zur silberraffination
CN109666952B (zh) * 2017-10-16 2020-12-04 中国科学院过程工程研究所 一种电沉积生产金属银的方法
CN109023433A (zh) * 2018-09-04 2018-12-18 安阳市岷山有色金属有限责任公司 一种粗银电解精炼工艺

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3224873A (en) * 1963-02-25 1965-12-21 Gen Mills Inc Liquid-liquid recovery of copper values using alpha-hydroxy oximes
US3410794A (en) * 1966-01-20 1968-11-12 Exxon Research Engineering Co Separating hydrocarbons with liquid membranes
GB1479324A (en) * 1974-09-23 1977-07-13 Brookside Metal Co Ltd Electrolytic refining of silver
US3975244A (en) * 1975-09-10 1976-08-17 Brookside Metal Company Limited Electrolytic refining
US4374713A (en) * 1981-06-01 1983-02-22 Gte Laboratories Incorporated Process for separating tungsten from coinage metals
US4468303A (en) * 1981-12-04 1984-08-28 Norcim Investments Pty Ltd. Metal recovery
US4443305A (en) * 1983-05-02 1984-04-17 Western Electric Company, Inc. Emulsion electrowinning

Also Published As

Publication number Publication date
ES535772A0 (es) 1985-12-16
US4670115A (en) 1987-06-02
ATA307383A (de) 1985-08-15
DE3463163D1 (en) 1987-05-21
ES8602966A1 (es) 1985-12-16
EP0138801A1 (fr) 1985-04-24
AT380032B (de) 1986-03-25

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