CA2663652A1 - Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes - Google Patents
Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes Download PDFInfo
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- CA2663652A1 CA2663652A1 CA002663652A CA2663652A CA2663652A1 CA 2663652 A1 CA2663652 A1 CA 2663652A1 CA 002663652 A CA002663652 A CA 002663652A CA 2663652 A CA2663652 A CA 2663652A CA 2663652 A1 CA2663652 A1 CA 2663652A1
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- iron
- process according
- electrochemical process
- metal chloride
- chloride solution
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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
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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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)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
An electrochemical process for the concurrent recovery of iron metal and chlorine gas from an iron-rich metal chloride solution, comprising electrolysing the iron-rich metal chloride solution in an electrolyser comprising a cathodic compartment equipped with a cathode having a hydrogen overpotential higher than that of iron and containing a catholyte having a pH below about 2, an anodic compartment equipped with an anode and containing an anolyte, and a separator allowing for anion passage, the electrolysing step comprising circulating the iron-rich metal chloride solution in a non-anodic compartment of the electrolyser, thereby causing iron to be electrodeposited at the cathode and chlorine gas to evolve at the anode, and leaving an iron-depleted solution. The iron-rich metal chloride solution may originate from carbo-chlorination wastes, spent acid leaching liquors or pickling liquors.
Claims (36)
1. An electrochemical process for the recovery of metallic iron and chlorine gas from an iron-rich metal chloride solution, which process comprises:
a) providing an iron-rich metal chloride solution;
b) electrolysing said iron-rich metal chloride solution in an electrolyser comprising a cathodic compartment equipped with a cathode having a hydrogen overpotential higher than that of iron and containing a catholyte having a pH below about 2, an anodic compartment equipped with an anode and containing an anolyte, and a separator allowing for anion passage, said electrolysing step comprising circulating said iron-rich metal chloride solution in a non-anodic compartment of said electrolyser, thereby causing iron to be electrodeposited at the cathode and chlorine gas to evolve at the anode, and leaving an iron-depleted solution; and c) separately recovering said electrodeposited iron and said chlorine gas.
a) providing an iron-rich metal chloride solution;
b) electrolysing said iron-rich metal chloride solution in an electrolyser comprising a cathodic compartment equipped with a cathode having a hydrogen overpotential higher than that of iron and containing a catholyte having a pH below about 2, an anodic compartment equipped with an anode and containing an anolyte, and a separator allowing for anion passage, said electrolysing step comprising circulating said iron-rich metal chloride solution in a non-anodic compartment of said electrolyser, thereby causing iron to be electrodeposited at the cathode and chlorine gas to evolve at the anode, and leaving an iron-depleted solution; and c) separately recovering said electrodeposited iron and said chlorine gas.
2. The electrochemical process of claim 1, wherein step a) of providing an iron-rich metal chloride solution includes the following steps:
a1) leaching a solid carbo-chlorination waste with a hot aqueous solution, thereby forming an aqueous slurry; and a2) subjecting said aqueous slurry to a separation of solids, thereby forming an insoluble cake and isolating an iron-rich metal chloride solution.
a1) leaching a solid carbo-chlorination waste with a hot aqueous solution, thereby forming an aqueous slurry; and a2) subjecting said aqueous slurry to a separation of solids, thereby forming an insoluble cake and isolating an iron-rich metal chloride solution.
3. The electrochemical process according to claim 1 or 2, wherein the pH of the catholyte is adjusted to range between about 0.3 and about 1.8, preferably between about 0.6 and about 1.5, more preferably between about 0.6 and about 1.1, most preferably between about 0.9 and about 1.1.
4. The electrochemical process according to any one of claims 1 to 3, wherein the cathode has an overvoltage, at 200 A.m-2, greater than about 425 mV
in 0.5 mol.dm-3 HCl at 25°C.
in 0.5 mol.dm-3 HCl at 25°C.
5. The electrochemical process according to claim 4, wherein the cathode is constructed from or coated with a material selected from the group consisting of titanium, titanium alloy, zirconium, zirconium alloy, zinc, zinc alloy, cadmium, cadmium alloy, tin, tin alloy, copper, copper alloy, lead, lead alloy, niobium, niobium alloy, gold, gold alloy, mercury and metallic amalgam with mercury.
6. The electrochemical process according to claim 5, wherein the material consists of titanium or titanium alloy, preferably titanium palladium ASTM
grade 7.
grade 7.
7. The electrochemical process according to any one of claims 1 to 6, wherein the cathode is pretreated before the electrolysing step, preferably chemically etched by immersion into a fluoro-nitric acid mixture, and thorough rinsing with deionised water to eliminate traces of acid, said fluoro-nitric acid mixture preferably having the following composition: about 70 vol% conc. HNO3, about 20 vol.% conc. HF and about 10 vol.% H2O.
8. The electrochemical process according to any one of claims 1 to 7, wherein said anolyte is circulated in loop within the anodic compartment of the electrolyser.
9. The electrochemical process according to any one of claims 1 to 8, wherein said anolyte comprises HCl, preferably about 10 to about 37 wt.%, more preferably about 20%, a salt selected from the group consisting of MgCl2, NaCl, LiCl, KCl, CaCl2 and mixtures thereof, preferably 1 to about 20 wt.%, more preferably about 16 wt.%, and Fe(III) as a corrosion inhibitor, preferably 10 to about 12,000 ppm wt, more preferably about 8000 to about 10000 ppm wt.
10. The electrochemical process according to any one of claims 1 to 9, wherein the anode is a dimensionally stable anode of the type [M/M x O y-A z O
t], wherein M is a refractory metal or an alloy with a valve action property, including titanium, titanium alloy, zirconium, zirconium alloy, hafnium, hafnium alloy, vanadium, vanadium alloy, niobium, niobium alloy, tantalum or tantalum alloy, wherein M x O y is a metallic oxide of a valve metal forming a thin and impervious layer protecting the base metal, including TiO2, ZrO2, HfO2, NbO2, Nb2O5, TaO2, or Ta2O5, and wherein A z O t is an electrocatalytic metal oxide of a noble metal, an oxide of the platinum group metals including RuO2, IrO2 or P t O x, or a metallic oxide, including SnO2, Sb2O5 or Bi2O3.
t], wherein M is a refractory metal or an alloy with a valve action property, including titanium, titanium alloy, zirconium, zirconium alloy, hafnium, hafnium alloy, vanadium, vanadium alloy, niobium, niobium alloy, tantalum or tantalum alloy, wherein M x O y is a metallic oxide of a valve metal forming a thin and impervious layer protecting the base metal, including TiO2, ZrO2, HfO2, NbO2, Nb2O5, TaO2, or Ta2O5, and wherein A z O t is an electrocatalytic metal oxide of a noble metal, an oxide of the platinum group metals including RuO2, IrO2 or P t O x, or a metallic oxide, including SnO2, Sb2O5 or Bi2O3.
11. The electrochemical process according to any one of claims 1-9, wherein the anode is constructed from bulk electronically conductive ceramics, including sub-stoichiometric titanium oxides having as a general formula Ti n O2n-1, wherein n is an integer equal to or above 3; conductive oxides with a spinel structure AB2O4, wherein A is Fe(II), Mn(II) or Ni(II), and B is Al, Fe(III), Cr(III) or Co(III); or conductive oxides with a perovskite structure ABO3 , wherein A is Fe(II), Mn(II), Co(II) or Ni(II), and B is Ti(IV) or with a pyrochlore structure AB2O7.
12. The electrochemical process according to any one of claims 1-9, wherein the anode is constructed from carbon-based materials such as graphite, impervious graphite, or vitreous carbon.
13. The electrochemical process according to any one of claims 1 to 12, wherein the electrolysing step is performed in a two-compartment electrolyser in which the separator is an ion-exchange membrane, preferably an anion-exchange membrane, and wherein said iron-rich metal chloride solution is circulated in loop within the cathodic compartment of the electrolyser, acting as the catholyte.
14. The electrochemical process according to claim 13, wherein the iron-rich metal chloride solution is adjusted to a pH below 2, preferably ranging between about 0.3 and about 1.8, preferably between about 0.6 and about 1.5, more preferably between about 0.6 and about 1.1, most preferably between about 0.9 and about 1.1, prior to the electrolysing step.
15. The electrochemical process according to any one of claims 1 to 12, wherein the electrolysing step is performed in a three-compartment electrolyser in which the anodic and cathodic compartments are separated from a central compartment by an anion and a cation exchange membranes, respectively, and wherein the iron-rich metal chloride solution is circulated within the central compartment of the electrolyser.
16. The electrochemical process according to claim 15, wherein said catholyte is circulated in loop within the cathodic compartment.
17. The electrochemical process according to claim 15 or 16, wherein the catholyte comprises about 1 to about 450 g/L of iron (II) chloride, preferably about 335 g/L, about 1 to about 350 g/L MgCl2 or CaCl2 or a mixture thereof, preferably about 250 g/L, preferably MgCl2, and 0 to about 10 g/L of free HCl.
18. The electrochemical process according to any one of claims 1 to 17, wherein a volume flow rate of both anolyte and catholyte ranges between about 0.1 L/min and about 100 L/min, preferably between about 0.1 L/min to about 30 L/min, and more preferably is of about 2 L/min.
19. The electrochemical process according to any one of claims 1 to 18, wherein the electrolysing step is performed under constant current at a current density ranging from about 50 to about 5000 A/m2.
20. The electrochemical process according to claim 19, wherein the electrolysing step is performed under constant current at a current density ranging from about 50 to about 1000 A/m2, preferably about 500 A/m2, thereby obtaining an essentially dendrite-free smooth deposit of iron.
21. The electrochemical process according to claim 19, wherein the electrolysing step is performed under constant current at a current density ranging from about 3000 to about 5000 A/m2, preferably about 4000 A/m2, thereby obtaining an essentially powdered iron.
22. The electrochemical process according to any one of claims 1 to 21, wherein the electrolysing step is performed at an operating temperature ranging from about 40 to about 110°C, preferably from about 80°C to 95°C, more preferably equating about 85°C.
23. The electrochemical process according to claim 1, wherein the iron-rich metal chloride solution originates from carbo-chlorination wastes, spent acid leaching liquors or pickling liquors.
24. The electrochemical process according to any one of claims 1 to 23, wherein the iron-rich metal chloride solution comprises vanadium, said process further comprising a vanadium separation step before, during or after the electrolysing step.
25. The electrochemical process according to claim 24, wherein said vanadium separation step occurs before the electrolysing step.
26. The electrochemical process according to claim 25, wherein said vanadium separation step consists in removing vanadium from the iron-rich metal chloride solution concurrently with chromium by co-precipitation at a pH
ranging from about 0.5 to about 3Ø
ranging from about 0.5 to about 3Ø
27. The electrochemical process according to claim 24, wherein the pH of the catholyte ranges between about 0.3 and about 0.5, causing vanadium to precipitate at the cathode along with iron electrodeposition, and wherein the vanadium-separation step occurs after the electrolysing step.
28. The electrochemical process according to claim 24, wherein the pH of the catholyte ranges between about 0.6 and about 1.8, causing vanadium to essentially remain within the circulating iron-rich metal chloride solution while iron is electrodeposited at the cathode, and wherein vanadium is thereafter recovered from the iron-depleted solution exiting the electrolyser, whereby the vanadium separation step occurs during the electrolysing step.
29. The electrochemical process according to any one of claims 1 to 28, wherein chlorine gas recovered from the anode is further dried and liquefied.
30. The electrochemical process according to any one of claim 1 to 29, wherein the iron-depleted solution exiting the electrolyser is recovered and further treated in order to remove calcium and radioactivity by addition of sulphuric acid, thereby producing a magnesium- and aluminum-rich brine.
31. The process according to claim 30, further comprising a step of pyrohydrolysis of said magnesium- and aluminum-rich brine in a fluid-bed pyrohydrolyser, thereby producing azeotropic hydrochloric acid and spinel beads.
32. The process according to claim 31, further comprising recovery of said azeotropic hydrochloric acid for export.
33. The process according to claim 2, wherein leaching is performed with hot process water, hot diluted hydrochloric acid, hot spent leaching acid or spent pickling liquors.
34. The process according to claim 2, wherein the solid separation step is performed by physical separation method, preferably by decantation, filtration or centrifugation.
35. An electrochemical process for the recovery of metallic iron and chlorine gas from an iron-rich metal chloride solution, which process comprises:
a) providing an iron-rich metal chloride solution;
b) electrolysing said iron-rich metal chloride solution in a two-compartment electrolyser comprising a cathodic compartment equipped with a cathode having a hydrogen overpotential higher than that of iron, and an anodic compartment equipped with an anode and containing an anolyte, said cathodic and anodic compartments being separated by an anion-exchange membrane, said electrolysing step comprising circulating said iron-rich metal chloride solution, adjusted to a pH below 2, as a catholyte in said cathodic compartment of said electrolyser, thereby causing iron to be electrodeposited at the cathode and chlorine gas to evolve at the anode, and leaving an iron-depleted solution; and c) separately recovering said electrodeposited iron and said chlorine gas.
a) providing an iron-rich metal chloride solution;
b) electrolysing said iron-rich metal chloride solution in a two-compartment electrolyser comprising a cathodic compartment equipped with a cathode having a hydrogen overpotential higher than that of iron, and an anodic compartment equipped with an anode and containing an anolyte, said cathodic and anodic compartments being separated by an anion-exchange membrane, said electrolysing step comprising circulating said iron-rich metal chloride solution, adjusted to a pH below 2, as a catholyte in said cathodic compartment of said electrolyser, thereby causing iron to be electrodeposited at the cathode and chlorine gas to evolve at the anode, and leaving an iron-depleted solution; and c) separately recovering said electrodeposited iron and said chlorine gas.
36. An electrochemical process according to claim 35 wherein in step c) recovering iron is conducted by physically stripping said iron electrodeposited at the cathode and recovering chlorine is conducted by suctioning of chlorine gas above the anodic compartment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA2663652A CA2663652C (en) | 2006-09-21 | 2007-01-09 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US82645306P | 2006-09-21 | 2006-09-21 | |
| CA2560407 | 2006-09-21 | ||
| US60/826,453 | 2006-09-21 | ||
| CA2,560,407 | 2006-09-21 | ||
| CA2663652A CA2663652C (en) | 2006-09-21 | 2007-01-09 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
| PCT/CA2007/000026 WO2008034212A1 (en) | 2006-09-21 | 2007-01-09 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2663652A1 true CA2663652A1 (en) | 2008-03-27 |
| CA2663652C CA2663652C (en) | 2010-07-06 |
Family
ID=39200106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2663652A Expired - Fee Related CA2663652C (en) | 2006-09-21 | 2007-01-09 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US20100044243A1 (en) |
| EP (1) | EP2064369B1 (en) |
| JP (1) | JP2010504423A (en) |
| AU (1) | AU2007299519B2 (en) |
| CA (1) | CA2663652C (en) |
| WO (1) | WO2008034212A1 (en) |
| ZA (1) | ZA200900950B (en) |
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| CN102037160B (en) * | 2008-03-20 | 2013-11-13 | 力拓铁钛公司 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
| SI2268852T1 (en) * | 2008-04-11 | 2019-09-30 | Electrochem Technologies & Materials Inc. | Electrochemical process for the recovery of metallic iron and sulfuric acid values from iron-rich sulfate wastes, mining residues and pickling liquors |
| ITMI20111938A1 (en) * | 2011-10-26 | 2013-04-27 | Industrie De Nora Spa | ANODIC COMPARTMENT FOR CELLS FOR ELECTROLYTIC EXTRACTION OF METALS |
| US20130233720A1 (en) * | 2011-10-27 | 2013-09-12 | Gagik Martoyan | Extraction of metals |
| US9222147B2 (en) | 2012-01-12 | 2015-12-29 | Nichromet Extraction Inc. | Method for selective precipitation of iron, arsenic and antimony |
| EP2966035A1 (en) * | 2014-07-08 | 2016-01-13 | Kronos International, Inc. | Method for the recovery of hydrochloric acid from metal chloride solutions with a high iron chloride content |
| KR101723730B1 (en) * | 2015-06-03 | 2017-04-06 | 조범래 | High selective metals and acid recovery process from a multi-metallic solutio |
| CN105132936B (en) * | 2015-07-07 | 2017-12-22 | 昆明理工大学 | One kind prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder |
| US10364169B2 (en) * | 2015-11-30 | 2019-07-30 | The Board Of Trustees Of The University Of Illinois | Ultrafiltration TIO2 magnéli phase reactive electrochemical membranes |
| MA51025A (en) * | 2017-07-07 | 2021-04-07 | 9203 5468 Quebec Inc Dba Nmr360 | PROCESS FOR OXIDATION AND HYDROTHERMIC DISSOCIATION OF METAL CHLORIDES FOR THE SEPARATION OF METALS AND HYDROTHERMIC ACID |
| CN109628953B (en) * | 2018-12-26 | 2020-10-23 | 浙江工业大学 | Method for removing arsenic, antimony and bismuth in copper electrolyte |
| BR112023019059A2 (en) * | 2021-03-24 | 2023-10-17 | Electrasteel Inc | IMPURITIES REMOVAL IN AN IRON CONVERSION SYSTEM |
| CN113215589B (en) * | 2021-04-15 | 2023-03-17 | 中国恩菲工程技术有限公司 | Method for separating iron and other metal elements in iron alloy |
| CN114740143B (en) * | 2022-04-12 | 2023-10-27 | 四川大学 | Deep dechlorination method and device based on occurrence form of chloride ions in chlorination tailings |
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-
2007
- 2007-01-09 WO PCT/CA2007/000026 patent/WO2008034212A1/en active Application Filing
- 2007-01-09 AU AU2007299519A patent/AU2007299519B2/en not_active Ceased
- 2007-01-09 EP EP07701657A patent/EP2064369B1/en not_active Not-in-force
- 2007-01-09 JP JP2009528559A patent/JP2010504423A/en active Pending
- 2007-01-09 CA CA2663652A patent/CA2663652C/en not_active Expired - Fee Related
- 2007-01-09 US US12/442,367 patent/US20100044243A1/en not_active Abandoned
-
2009
- 2009-02-10 ZA ZA2009/00950A patent/ZA200900950B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CA2663652C (en) | 2010-07-06 |
| JP2010504423A (en) | 2010-02-12 |
| AU2007299519A1 (en) | 2008-03-27 |
| EP2064369A4 (en) | 2009-11-04 |
| EP2064369A1 (en) | 2009-06-03 |
| WO2008034212A1 (en) | 2008-03-27 |
| EP2064369B1 (en) | 2011-03-30 |
| US20100044243A1 (en) | 2010-02-25 |
| ZA200900950B (en) | 2009-12-30 |
| AU2007299519B2 (en) | 2011-12-15 |
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