WO2013057700A1 - Method of electrolytic deposition of arsenic from industrial electrolytes including waste electrolytes used in electrorefining of copper after prior decopperisation of electrolyte - Google Patents
Method of electrolytic deposition of arsenic from industrial electrolytes including waste electrolytes used in electrorefining of copper after prior decopperisation of electrolyte Download PDFInfo
- Publication number
- WO2013057700A1 WO2013057700A1 PCT/IB2012/055717 IB2012055717W WO2013057700A1 WO 2013057700 A1 WO2013057700 A1 WO 2013057700A1 IB 2012055717 W IB2012055717 W IB 2012055717W WO 2013057700 A1 WO2013057700 A1 WO 2013057700A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cathode
- arsenic
- copper
- anode
- electrolyte
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 73
- 239000003792 electrolyte Substances 0.000 title claims abstract description 42
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 39
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical group [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000010949 copper Substances 0.000 title claims abstract description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 32
- 230000008021 deposition Effects 0.000 title claims description 8
- 239000002699 waste material Substances 0.000 title abstract description 6
- 238000002955 isolation Methods 0.000 claims abstract description 16
- 229910000831 Steel Inorganic materials 0.000 claims description 33
- 239000010959 steel Substances 0.000 claims description 33
- 238000004070 electrodeposition Methods 0.000 claims description 29
- 238000007670 refining Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910000978 Pb alloy Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000012993 chemical processing Methods 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims 2
- 238000005868 electrolysis reaction Methods 0.000 description 26
- 239000000203 mixture Substances 0.000 description 7
- 230000001419 dependent effect Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 3
- JEMGLEPMXOIVNS-UHFFFAOYSA-N arsenic copper Chemical compound [Cu].[As] JEMGLEPMXOIVNS-UHFFFAOYSA-N 0.000 description 3
- 229910000070 arsenic hydride Inorganic materials 0.000 description 3
- 150000001879 copper Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000559 atomic spectroscopy Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- MKOYQDCOZXHZSO-UHFFFAOYSA-N [Cu].[Cu].[Cu].[As] Chemical compound [Cu].[Cu].[Cu].[As] MKOYQDCOZXHZSO-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000009867 copper metallurgy Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009852 extractive metallurgy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
-
- 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
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
-
- 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
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
Definitions
- the subject of the present invention is a novel method of the electrolytic isolation of arsenic from waste electrolytes from the electrorefining of copper, a method of preparing electrolyte by its decopperisation as well as a method of isolation of arsenic from copper industry electrolytes with their prior decopperisation .
- arsenic is a significant component of Polish copper concentrates. Annually, material processing is supplemented by about 2500 tons of arsenic. According to the same literature source, there are at least two material streams from which the reclamation and stabilization of arsenic are not fully mastered.
- the first subject of the present invention is a method of electrolytic isolation of arsenic from a post-refining electrolyte characterised in that it is embodied using a single- stage potentiostatic arsenic isolation process, preferably on a steel cathode, in the cathode potential range of from -1.20 V to -1.70 V in relation to the anode, preferably of acid-resistant steel, wherein the electrolyte is not chemically processed.
- the isolation is conducted without any chemical processing of the electrolyte which, for contrast, is required in the solvent extraction (SX) as used at present in the isolation of copper salts from the post-refinement solution.
- a method according to the present invention is characterised in that the electrodeposition is conducted at room temperature from 18°C to 50°C, preferably from 18°C to 30°C.
- a method according to the present invention is characterised in that the electrodeposition process makes use of an anode of a lead alloy, or based on titanium oxide and iridium wherein the cathode and anode surface areas are comparable.
- the example anodes are already used in the galvanic industry in the electrodeposition of copper. More preferably a method according to the present invention is characterised in that the electrodeposition process is conducted using an anode of acid- resistant steel and then the anode surface area is at least 5- fold that of the cathode. Equally preferably, a method according to the present invention is characterised in that the electrodeposition is conducted using a cathode of acid-resistant steel or of copper. Most preferably, a method according to the present invention is characterised in that the process of electrodeposition is conducted with constant circulation of the electrolyte or with electrolyte mixing.
- the second subject of the present invention is a method of decopperisation of a post-refining electrolyte, characterised in that it is embodied using a single-stage potentiostatic process isolation of copper on a cathode with a cathode potential range of from -1.00 V to -1.50 V in relation to the acid-resistant steel anode, wherein the electrolyte is not subjected to. chemical processing.
- Equally preferably a method according to the present invention is characterised in that the electrodeposition process is conducted at room temperature from 18°C to 50°C, preferably from 18°C to 30°C.
- a method according to the present invention is characterised in that the electrodeposition process makes use of a lead alloy anode, or one based on titanium oxide and iridium, wherein the surface areas of the cathode and anode are comparable. More preferably, a method according to the present invention is characterised in that the electrodeposition process is conducted using an acid-resistant steel anode, wherein the anode surface area is at least 5-fold greater than the cathode surface area. W the next preferable embodiment of the present invention, the method is characterised in that the electrodeposition process is conducted using a cathode of acid-resistant steel or of copper. Also preferably, a method according to the present invention is characterised in that the electrodeposition process is conducted with constant electrolyte circulation or mixing.
- the third subject of the present invention is a method of electrolytic isolation of arsenic from a post-refining electrolyte, characterised in that it encompasses
- the present invention relates to a method of electrolytic and potentistatic production of arsenic from electrolytes, in which the concentration of copper is about 1 mg/1.
- -a post-refining electrolyte is decopperised to a concentration of about 1 mg/1, preferably according to the second subject of the present invention
- the cathode is exchanged as well as increasing the cathode potential by at least -200 mV such that the isolation of arsenic proceeds at a commercially effective rate
- the deposited arsenic is such that it may be a commercial product, and not a copper-arsenic sponge which is a troublesome waste product in need of further processing,
- the arsenic deposited during the above process is finally removed from the material cycle and does not require further processing or manipulation, -during the potentiostatic isolation of arsenic the toxic arsenous gas AsH 3 is not produced.
- the process of decopperisation via the electrodeposition of copper from post- refining electrolytes is carried out using potentiostatic electrolysis: potentiostatic electrolysis with a cathode potential range of from -1.20 V to -1.70 V, in relation to an acid-resistant steel anode, wherein the time of electrolysis is dependent on an initial concentration of arsenic, the final concentration of arsenic that is to be achieved, the applied cathode potential, electrolyte mixing or flow rate as well as temperature. If the value of the resistance in Ohms IR is negligible, the range of cathode potentials in relation to the acid-resistant steel anode is from -1.20 V to -1.45 V. Due to the differing construction of the electrolysers , and the industrial electrolytes used (of varying conductivity and resistance) , the potential drop entailed by the ohmic resistance can be from -0.2 to -0.5 V
- the maximum value of the applied cathode potential is -1.70 V.
- the present invention defined in the second subject of the present invention, has an advantage over the above-defined methods in that the proposed decopperisation method is based solely on potentistatic electrodeposition, wherein:
- the post-refining electrolyte is decopperised to a concentration level of about 1 ppm (lmg/dm 3 , thus the concentration of copper in the decoppered solution is at least 200 times smaller than in the presently used process) which has an economic, technical and ecological significance;
- the cathodic copper produced throughout the concentration range thus from about 50 g/dm 3 to 1 mg/dm 3 has a commercial purity, meaning >99.9% by mass;
- Example 1 In an electrochemical vessel thermoregulated to 25°C there is an indicator electrode of steel plate with a surface area of about 2.5 cm2. which is the cathode, as well as a reference electrode 10 (anode) in the form of a steel plate with a surface area of about 50 cm2 and a thickness of 0.15 cm.
- the vessel is filled with an industrial electrolyte after a presently used industrial decopperisation, and then according to the decopperisation method defined in the second subject of the present invention (example 3 and 4), therefore of the following composition: 0.001 g/dm 3 Cu, 170 g/dm 3 H 2 S0 4 as well as 0.102 g/dm 3 Fe, 0.147 g/dm 3 Sb, 0.032 g/dm 3 Co, 5,1 g/dm 3 Ni, as well as 2.9 g/dm 3 As.
- the electrodes are connected to a measurement device - a commercially available galvanostat /potentiostat which can be programmed to perform an electrolysis. During the electrolysis we measure current changes dependent on electrolysis duration. The size of the recorded current is connected to the changes in the concentration of arsenide ions in solution. The solution is not mixed.
- the vessel is filled with an industrial electrolyte after a presently used industrial decopperisation, and then according to the decopperisation method defined in the second subject of the present invention (example 3 and 4), therefore of the following composition: 0.001 g/dm 3 Cu, 170 g/dm 3 H 2 S0 4 as well as 0.102 g/dm 3 Fe, 0.147 g/dm 3 Sb, 0.032 g/dm 3 Co, 5,1 g/dm 3 Ni, as well as 2.9 g/dm 3 As.
- the electrodes are connected to a measurement device - a commercially available galvanostat/potentiostat which can be programmed to perform an electrolysis.
- a measurement device - a commercially available galvanostat/potentiostat which can be programmed to perform an electrolysis.
- the electrolysis we measure current changes dependent on electrolysis duration.
- the size of the recorded current is connected to the changes in the concentration of arsenide ions in solution.
- the vessel is filled with an industrial electrolyte after an industrial decopperisation according to a presently used decopperisation method, meaning galvanostatic cascade deposition, with the following composition: 0.102 g/dm 3 Cu, 170 g/dm 3 H 2 S0 4 as well as 0.102 g/dm 3 Fe, 0.147 g/dm 3 Sb, 0.032 g/dm 3 Co, 5,1 g/dm 3 Ni, as well as 2.9 g/dm 3 As.
- the electrodes are connected to a measurement device - a commercially available galvanostat/potentiostat which can be programmed to perform an electrolysis.
- the electrolysis we measured current changes dependent on the progress of the electrolysis.
- the size of the recorded current is connected to the changes in the concentration of copper ions in solution.
- the solution is mixed at a rate of 50 RPM.
- the potentiostatic electrolysis parameters are:
- the resulting cathodic copper thus has a purity of > 99.9% by mass.
- the solution was analyzed using absorption atomic spectroscopy and we observed that the concentration of copper is 0.004 g/dm 3 (4 ppm) .
- an indicator electrode of steel plate with a surface area of about 2.5 cm 2 which is the cathode, as well as a reference electrode (anode) in the form of a copper plate with a surface area of about 50 cm 2 and a thickness of 0.15 cm.
- the vessel is filled with an industrial electrolyte after an industrial decopperisation according to a presently used decopperisation method, meaning galvanostatic cascade deposition, with the following composition: 0.102 g/dm 3 Cu, 170 g/dm 3 .
- the electrodes are connected to a measurement device - a commercially available galvanostat/potentiostat which can be programmed to perform an electrolysis.
- a measurement device a commercially available galvanostat/potentiostat which can be programmed to perform an electrolysis.
- the electrolysis we measured current changes dependent on the progress of the electrolysis. The size of the recorded current is connected to the changes in the concentration of copper ions in solution. The solution is not mixed.
- the resulting cathode copper thus has a purity of >99.9% by mass.
- the solution was analyzed using absorption atomic spectroscopy and observed that the concentration of copper is 0.002 g dm-3 (2 ppm) .
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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)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP12795068.1A EP2769004A1 (en) | 2011-10-19 | 2012-10-19 | Method of electrolytic deposition of arsenic from industrial electrolytes including waste electrolytes used in electrorefining of copper after prior decopperisation of electrolyte |
| CN201280063161.4A CN104204305A (zh) | 2011-10-19 | 2012-10-19 | 从包括电解液预先脱铜后的用于铜电解精炼的废电解液的工业电解液电解沉积砷的方法 |
| MX2014004770A MX2014004770A (es) | 2011-10-19 | 2012-10-19 | Metodo para la deposicion electrolitica de arsenico a partir de electrolitos industriales incluyendo electrolitos residuales utilizados en la electrorrefinacion de cobre despues de la descobrizacion previa del electrolito. |
| US14/352,729 US20140246326A1 (en) | 2011-10-19 | 2012-10-19 | Method Of Electrolytic Deposition Of Arsenic From Industrial Electrolytes Including Waste Electrolytes Used In Electrorefining Of Copper After Prior Decopperisation Of Electrolyte |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL39669311A PL396693A1 (pl) | 2011-10-19 | 2011-10-19 | Nowa metoda odmiedziowania elektrolitów przemyslu miedziowego |
| PLPL396693 | 2011-10-19 | ||
| PLPL396882 | 2011-11-07 | ||
| PL396882A PL226513B1 (pl) | 2011-11-07 | 2011-11-07 | Sposób elektrolitycznego wydzielania arsenu z elektrolitów porafinacyjnych miedzi zawierających wysokie stężenie kwasu siarkowego |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2013057700A1 true WO2013057700A1 (en) | 2013-04-25 |
Family
ID=47278915
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IB2012/055717 WO2013057700A1 (en) | 2011-10-19 | 2012-10-19 | Method of electrolytic deposition of arsenic from industrial electrolytes including waste electrolytes used in electrorefining of copper after prior decopperisation of electrolyte |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP2769004A1 (es) |
| CN (1) | CN104204305A (es) |
| CL (1) | CL2014001004A1 (es) |
| MX (1) | MX2014004770A (es) |
| WO (1) | WO2013057700A1 (es) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020087189A1 (es) * | 2018-10-29 | 2020-05-07 | Gallegos Riedemann Alejo Ivan | Nuevo proceso electroquimico basado en factor adimensional |
| WO2020245619A1 (en) * | 2019-06-06 | 2020-12-10 | Przemyslaw Los | Method for copper and zinc separation from industrial electrolytes including waste industrial electrolytes |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079826B (zh) * | 2019-05-07 | 2021-04-06 | 昆明理工大学 | 一种从铜冶炼高杂质高镍阳极铜板中回收硫酸镍的方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2742415A (en) * | 1953-03-27 | 1956-04-17 | American Smelting Refining | Electrodeposition of arsenic from acid electrolytes |
| US4146447A (en) * | 1976-08-02 | 1979-03-27 | Noranda Mines Limited | Arsenic removal from electrolytes |
| US20060226024A1 (en) * | 2004-06-22 | 2006-10-12 | Phelps Dodge Corporation | Method and apparatus for electrowinning copper using the ferrous/ferric anode reaction and a flow-through anode |
| WO2009117354A2 (en) * | 2008-03-19 | 2009-09-24 | Eltron Research & Development, Inc. | Electrowinning apparatus and process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857918A (zh) * | 2009-04-07 | 2010-10-13 | 国立云林科技大学 | 废弃物砷化镓的镓及砷纯化回收方法 |
-
2012
- 2012-10-19 WO PCT/IB2012/055717 patent/WO2013057700A1/en active Application Filing
- 2012-10-19 MX MX2014004770A patent/MX2014004770A/es unknown
- 2012-10-19 CN CN201280063161.4A patent/CN104204305A/zh active Pending
- 2012-10-19 EP EP12795068.1A patent/EP2769004A1/en not_active Withdrawn
-
2014
- 2014-04-17 CL CL2014001004A patent/CL2014001004A1/es unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2742415A (en) * | 1953-03-27 | 1956-04-17 | American Smelting Refining | Electrodeposition of arsenic from acid electrolytes |
| US4146447A (en) * | 1976-08-02 | 1979-03-27 | Noranda Mines Limited | Arsenic removal from electrolytes |
| US20060226024A1 (en) * | 2004-06-22 | 2006-10-12 | Phelps Dodge Corporation | Method and apparatus for electrowinning copper using the ferrous/ferric anode reaction and a flow-through anode |
| WO2009117354A2 (en) * | 2008-03-19 | 2009-09-24 | Eltron Research & Development, Inc. | Electrowinning apparatus and process |
Non-Patent Citations (3)
| Title |
|---|
| ANDRZEJ CHMIELARZ: "Copper Metallurgy", 50TH ANNIVERSARY OF KGHM POLSKA MIEDZ SA KRAKOW, 2011, pages 87,88 |
| NANSEU-NJIKI ET AL: "Electrolytic arsenic removal for recycling of washing solutions in a remediation process of CCA-treated wood", SCIENCE OF THE TOTAL ENVIRONMENT, ELSEVIER, AMSTERDAM, NL, vol. 384, no. 1-3, 24 August 2007 (2007-08-24), pages 48 - 54, XP022210519, ISSN: 0048-9697, DOI: 10.1016/J.SCITOTENV.2007.04.043 * |
| W.G. DAVENPORT; M. KING; M. SCHLESINGER: "Extractive Metallurgy of Copper", 2002, ELSEVIER SCIENCE LTD. |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020087189A1 (es) * | 2018-10-29 | 2020-05-07 | Gallegos Riedemann Alejo Ivan | Nuevo proceso electroquimico basado en factor adimensional |
| WO2020245619A1 (en) * | 2019-06-06 | 2020-12-10 | Przemyslaw Los | Method for copper and zinc separation from industrial electrolytes including waste industrial electrolytes |
Also Published As
| Publication number | Publication date |
|---|---|
| CL2014001004A1 (es) | 2014-10-10 |
| CN104204305A (zh) | 2014-12-10 |
| EP2769004A1 (en) | 2014-08-27 |
| MX2014004770A (es) | 2015-01-16 |
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