WO2004005586A1 - Electrolytic method of the extraction of metals - Google Patents

Electrolytic method of the extraction of metals Download PDF

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Publication number
WO2004005586A1
WO2004005586A1 PCT/AM2003/000002 AM0300002W WO2004005586A1 WO 2004005586 A1 WO2004005586 A1 WO 2004005586A1 AM 0300002 W AM0300002 W AM 0300002W WO 2004005586 A1 WO2004005586 A1 WO 2004005586A1
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WO
WIPO (PCT)
Prior art keywords
extraction
metals
electrodialysis
solution
cathode
Prior art date
Application number
PCT/AM2003/000002
Other languages
French (fr)
Inventor
Gagik Martoyan
Sahak Intsheyan
Sukias Tonikyan
Manuk Demirchyan
Zaven Guiragossian
Original Assignee
Gagik Martoyan
Sahak Intsheyan
Sukias Tonikyan
Manuk Demirchyan
Zaven Guiragossian
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.)
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Application filed by Gagik Martoyan, Sahak Intsheyan, Sukias Tonikyan, Manuk Demirchyan, Zaven Guiragossian filed Critical Gagik Martoyan
Priority to AU2003238535A priority Critical patent/AU2003238535A1/en
Publication of WO2004005586A1 publication Critical patent/WO2004005586A1/en

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Classifications

    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
    • C02F1/4678—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction of metals
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/16—Processing by fixation in stable solid media
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/006—Radioactive compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00—Apparatus for treatment of water, waste water or sewage
    • C02F2201/46—Apparatus for electrochemical processes
    • C02F2201/461—Electrolysis apparatus
    • C02F2201/46105—Details relating to the electrolytic devices
    • C02F2201/46115—Electrolytic cell with membranes or diaphragms
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention pertains to the field of electrochemistry, especially to the methods for the complete extraction of metals from electrolytic solutions.
  • the invention applies to the full extraction of metals from mineral ore concentrates, to the large reduction of volume of radioactive and other hazardous wastes, to the production of chemical compounds in pure form and to the desalination of water sources.
  • the electrodialysis method to extract ions was disclosed in an Armenia patent[l], in which ions were extracted in a three-chamber electrodialysis unit, having a mercury cathode, and cation exchange and anion-exchange membranes. This exploited the skin currents induced on the mercury cathode's surface, which assured the deep extraction of ions from solutions and their accumulation on the top surface of the cathode.
  • the disclosed invention is aimed to increase the productivity, efficiency and processing rate of this method.
  • the essence of the invention is that the extraction of metals from electrolytic solutions is performed by the coordinated use of both the electrodialysis and electrolysis methods.
  • a three-chamber electrodialysis unit the metal-containing aqueous solution is separated into a base and an acid solution.
  • the ion concentrations in the anode and cathode chambers are held constant.
  • the extraction of metals is made in a separate electrolysis unit, at the top surface of its mercury cathode, which is isolated from its electrolyte-processing chamber by a dielectric barrier.
  • Figure 1 shows the schematic flow chart of the method's implementation, where the extraction of chosen metals from electrolytic solutions is accomplished.
  • the metal-containing electrolytic solution(l) is filled at a specified rate into the water tank(2).
  • the water-diluted solution is pumped through the circulation loop(7), entering the processing chamber(4) of the electrodialysis separator and is returned back into the tank(2).
  • the salts dissociate in the processing chamber of the electrodialysis separator, the cations circulate through the loop(5) entering the base-solution tank(8), while the anions circulate via the loop(6) entering the tank(3) reserved for the acid solution.
  • the depth of the extraction of ions in the electrodialysis unit is limited by the diffusion current of ions, from the unit's side chambers back into the electrolyte-processing chamber.
  • the irreversible extraction and removal of cations make it possible to increase the efficiency of metal extraction through the electrodialysis unit.
  • the extraction of cations from the resulting base solution is accomplished in the following manner. From the base solution tank(8) the solute simultaneously circulates through the loop(l ⁇ ) passing through the processing chamber(12) of the electrolysis apparatus(ll), which has a mercury cathode(9). The thick solute of the extracted metal is then accumulated in a separate container(13).
  • FIG. 2 shows the schematic of the electrolysis unit, in which the one-way extraction of cations from the base solution is accomplished.
  • cations are transported through the ion-exchange membrane(15), and due to the skin currents produced on the surface of the mercury cathode(9), are driven to the top layer of the cathode, where due to the action of the dielectric separator(14), the possibility of their diffusion back into the processing chamber(12) is excluded.
  • the speed of skin current is typically 25 m/s, which many times exceed the speed of ions to dissolve in the mercury cathode. Therefore, in this method, this is the reason why an insignificant amount (about 1%) of amalgam may be formed.
  • the phenomenon of accumulation of ions at the top surface of the mercury cathode makes it possible, following simple operations, easily to collect and extract elements from the electrolytic solution in a uniformly solid phase.
  • the process efficiency is expressed by the fact that the collection of the same amount of ions in the system is accomplished in a much smaller electrolysis unit, and consequently, using much smaller amount of mercury, the handling of which is manageable, for a high throughput system.
  • Example 1 In the equipment shown in Figure 1, the water tank(2) was filled with liquid radioactive waste having the following properties, which was then pumped into the working chamber of the electrodialysis unit, filling it at a rate of 50 liters per hour.
  • the capacity of the base solution tank(8) was approximately 5 liters.
  • the cathode chamber(9) of the electrolysis concentrator-extractor unit was filled with mercury, which served as the cathode, while the anode was a plate of stainless steel.
  • the current in the electrodialysis unit dropped to the initial value of 0.007 A, from the peak value of 5.0 A, which corresponded to the current baseline when the electrolytic solution was not yet introduced into the electrodialysis unit. Subsequently, spraying the mercury cathode's top surface with a weak water jet, and processing the extracted metal with nitric acid reconstituted 19.77 gram of the original CsNO 3 . The difference (0.23 g or 1%) is attributed to measurement errors and processing losses.

Abstract

The invention pertains to the complete extraction of metals from electrolytic solutions by the combined means of electrodialysis and electrolysis. The invention solves the problem on how to extract metals from these solutions at high efficiency. To assure the high efficiency extraction of elements, the problem is solved first by separating the electrolytic solution into base and acid solutions via electrodialysis processing. At the same time the elements found in the base solution are selectively extracted in an electrolyzer that contains an ion-exchange membrane and a mercury cathode. Selected elements are made to migrate at the top surface of the mercury cathode, which is isolated from the processing chamber of the electrolysis unit by a dielectric barrier.

Description

C25C 5/02
Electrolytic Method of the Extraction of Metals
The invention pertains to the field of electrochemistry, especially to the methods for the complete extraction of metals from electrolytic solutions. The invention applies to the full extraction of metals from mineral ore concentrates, to the large reduction of volume of radioactive and other hazardous wastes, to the production of chemical compounds in pure form and to the desalination of water sources.
The electrodialysis method to extract ions was disclosed in an Armenia patent[l], in which ions were extracted in a three-chamber electrodialysis unit, having a mercury cathode, and cation exchange and anion-exchange membranes. This exploited the skin currents induced on the mercury cathode's surface, which assured the deep extraction of ions from solutions and their accumulation on the top surface of the cathode.
The deficiency of this method is that, as the electrodialysis unit's production volume is increased, in parallel it also becomes necessary to increase the volume of the mercury, which practically limits the possibilities of the method for higher throughput.
Hence, the disclosed invention is aimed to increase the productivity, efficiency and processing rate of this method.
The essence of the invention is that the extraction of metals from electrolytic solutions is performed by the coordinated use of both the electrodialysis and electrolysis methods. In a three-chamber electrodialysis unit, the metal-containing aqueous solution is separated into a base and an acid solution. The ion concentrations in the anode and cathode chambers are held constant. The extraction of metals is made in a separate electrolysis unit, at the top surface of its mercury cathode, which is isolated from its electrolyte-processing chamber by a dielectric barrier.
Figure 1 shows the schematic flow chart of the method's implementation, where the extraction of chosen metals from electrolytic solutions is accomplished.
The metal-containing electrolytic solution(l) is filled at a specified rate into the water tank(2). The water-diluted solution is pumped through the circulation loop(7), entering the processing chamber(4) of the electrodialysis separator and is returned back into the tank(2). As the salts dissociate in the processing chamber of the electrodialysis separator, the cations circulate through the loop(5) entering the base-solution tank(8), while the anions circulate via the loop(6) entering the tank(3) reserved for the acid solution.
The depth of the extraction of ions in the electrodialysis unit is limited by the diffusion current of ions, from the unit's side chambers back into the electrolyte-processing chamber. Thus, the irreversible extraction and removal of cations make it possible to increase the efficiency of metal extraction through the electrodialysis unit.
The extraction of cations from the resulting base solution is accomplished in the following manner. From the base solution tank(8) the solute simultaneously circulates through the loop(lθ) passing through the processing chamber(12) of the electrolysis apparatus(ll), which has a mercury cathode(9). The thick solute of the extracted metal is then accumulated in a separate container(13).
Figure 2 shows the schematic of the electrolysis unit, in which the one-way extraction of cations from the base solution is accomplished. Under the influence of the applied electric field, cations are transported through the ion-exchange membrane(15), and due to the skin currents produced on the surface of the mercury cathode(9), are driven to the top layer of the cathode, where due to the action of the dielectric separator(14), the possibility of their diffusion back into the processing chamber(12) is excluded. The speed of skin current is typically 25 m/s, which many times exceed the speed of ions to dissolve in the mercury cathode. Therefore, in this method, this is the reason why an insignificant amount (about 1%) of amalgam may be formed. The phenomenon of accumulation of ions at the top surface of the mercury cathode makes it possible, following simple operations, easily to collect and extract elements from the electrolytic solution in a uniformly solid phase.
Since the earlier version of the method severely limited the quantity of electrolytic solution passing through a fixed size electrodialysis unit[l], by localizing easily and reliably a separate electrolysis unit containing metallic mercury, it became possible to concentrate and extract the chosen metals, while also a minimal amount of mercury is used.
Therefore, as compared to the initial version of the method[l], in the present case, the process efficiency is expressed by the fact that the collection of the same amount of ions in the system is accomplished in a much smaller electrolysis unit, and consequently, using much smaller amount of mercury, the handling of which is manageable, for a high throughput system.
Example 1 In the equipment shown in Figure 1, the water tank(2) was filled with liquid radioactive waste having the following properties, which was then pumped into the working chamber of the electrodialysis unit, filling it at a rate of 50 liters per hour.
Figure imgf000004_0001
Characteristics of the three-chamber electrodialysis unit were:
• Voltage between Electrodes 10 V
• Type of Membranes Used MK-40 and MA-40 for cathode and anode sides
• Membrane Surface Area 500 cm2
• Number of Membranes 3 of each type (a total of 6)
• Separation of Membranes 0.3 cm
Stainless steel plates were used as electrodes.
The capacity of the base solution tank(8) was approximately 5 liters. The cathode chamber(9) of the electrolysis concentrator-extractor unit was filled with mercury, which served as the cathode, while the anode was a plate of stainless steel.
Characteristics of the electrolysis concentrator-extractor(l 1) were:
• Current Density in Electrolysis 15 mA/cm^ Concentrator-Extractor(l 1)
• Type of Membrane Used MK-40
• Membrane Surface Area 100 cm2
• Volume of Chambers (9 and 12) 30 cm3 with Electrodes, Each The base solution from tank-(8) was also simultaneously processed in the electrolysis unit, in which the isotopes are entirely accumulated on the mercury cathode's top surface. Washing the cathode's top surface with a weak water jet and measuring the specific activity verified this. The collected isotopes in the solution of the wash were easily brought to a solid phase. Example 2
An amount of 20.0 gram of CsNO3 was dissolved in 100 ml of water. Subsequently, the solution(l) filled the water tank(2) at a rate of 10 ml/min, which was pumped into the electrodialysis separator's central processing chamber. As a result of the electrodialysis process, the initial solution separated into an acid solution accumulated in tank-(3) and a base solution in tank-(8). At the same time, the base solution in tank-(8) was processed by the separate electrolysis unit containing mercury cathode, where the amount of extracted metal was monitored by the magnitude of the current passing through the electrodialysis separator.
After 15 minutes of operation, the current in the electrodialysis unit dropped to the initial value of 0.007 A, from the peak value of 5.0 A, which corresponded to the current baseline when the electrolytic solution was not yet introduced into the electrodialysis unit. Subsequently, spraying the mercury cathode's top surface with a weak water jet, and processing the extracted metal with nitric acid reconstituted 19.77 gram of the original CsNO3. The difference (0.23 g or 1%) is attributed to measurement errors and processing losses.
References
1. Armenian Patent No. 1069, G.A. Martoyan, S.G. Intsheyan, S.G. Tonikyan and M. Demirchyan "The Electrolytic Processing Mode of Liquid Radioactive Wastes" (in Armenian), 2001
2. US Patent No. 4,931,153, "Electrolytic Treatment of Radioactive Liquid Waste to Remove Sodium"

Claims

The electrolytic method of the extraction of metals includes separation of the metal- containing aqueous solution into a base and an acid solution by means of the electrodialysis method, following which the metals are removed from the base solution by means of an especial electrolysis unit having mercury cathode, wherein the improvement comprises the separation of the electrolytic solution in a stand-alone three-chamber electrodialysis unit, in which the ion concentrations in the anode and cathode chambers are held constant, while the extraction of chosen metals is made in a separate electrolysis unit, at the top surface of its mercury cathode, which is isolated from its electrolyte-processing chamber by a dielectric barrier.
PCT/AM2003/000002 2002-07-09 2003-06-27 Electrolytic method of the extraction of metals WO2004005586A1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006053336A (en) * 2004-08-11 2006-02-23 Bridgestone Corp Method of manufacturing panel for image display
US20130233720A1 (en) * 2011-10-27 2013-09-12 Gagik Martoyan Extraction of metals
US20180079663A1 (en) * 2015-03-31 2018-03-22 Kurita Water Industries Ltd. Method and apparatus for treating acidic liquid containing metal ions
AT521985A2 (en) * 2018-11-16 2020-06-15 Ustav Chemickych Procesu Av Cr V V I Process for isolating mercury from the solution and device for carrying out this process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4931153A (en) * 1987-08-21 1990-06-05 Doryokuro Kakunenryo Kaihatsu Jigyodan Electrolytic treatment of radioactive liquid waste to remove sodium
EP0568408A1 (en) * 1992-04-21 1993-11-03 Framatome Separation and confinement vessel for radio-active products contained in liquid effluents and device and process for treating those effluents

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4931153A (en) * 1987-08-21 1990-06-05 Doryokuro Kakunenryo Kaihatsu Jigyodan Electrolytic treatment of radioactive liquid waste to remove sodium
EP0568408A1 (en) * 1992-04-21 1993-11-03 Framatome Separation and confinement vessel for radio-active products contained in liquid effluents and device and process for treating those effluents

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006053336A (en) * 2004-08-11 2006-02-23 Bridgestone Corp Method of manufacturing panel for image display
JP4614711B2 (en) * 2004-08-11 2011-01-19 株式会社ブリヂストン Manufacturing method of image display panel
US20130233720A1 (en) * 2011-10-27 2013-09-12 Gagik Martoyan Extraction of metals
US20180079663A1 (en) * 2015-03-31 2018-03-22 Kurita Water Industries Ltd. Method and apparatus for treating acidic liquid containing metal ions
AT521985A2 (en) * 2018-11-16 2020-06-15 Ustav Chemickych Procesu Av Cr V V I Process for isolating mercury from the solution and device for carrying out this process
AT521985A3 (en) * 2018-11-16 2020-10-15 Ustav Chemickych Procesu Av Cr V V I Process for the isolation of mercury from the solution and apparatus for carrying out this process
AT521985B1 (en) * 2018-11-16 2020-12-15 Ustav Chemickych Procesu Av Cr V V I Process for the isolation of mercury from the solution and apparatus for carrying out this process

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