WO2017109294A1 - Procédé et agencement de surveillance d'un processus d'extraction liquide-liquide hydrométallurgique - Google Patents

Procédé et agencement de surveillance d'un processus d'extraction liquide-liquide hydrométallurgique Download PDF

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Publication number
WO2017109294A1
WO2017109294A1 PCT/FI2016/050920 FI2016050920W WO2017109294A1 WO 2017109294 A1 WO2017109294 A1 WO 2017109294A1 FI 2016050920 W FI2016050920 W FI 2016050920W WO 2017109294 A1 WO2017109294 A1 WO 2017109294A1
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Prior art keywords
settler
liquid
ray
cell
unit
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English (en)
Inventor
Erkki Paatero
Kari Saloheimo
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Outotec Finland Oy
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Outotec Finland Oy
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Priority claimed from FI20156035A external-priority patent/FI126880B/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0484—Controlling means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/12—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the material being a flowing fluid or a flowing granular solid
    • G01N23/125—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the material being a flowing fluid or a flowing granular solid with immerged detecting head
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • G01N33/202—Constituents thereof
    • G01N33/2022—Non-metallic constituents
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • G01N33/205—Metals in liquid state, e.g. molten metals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/322—Accessories, mechanical or electrical features immerged detecting head
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/40—Imaging
    • G01N2223/419—Imaging computed tomograph
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/605—Specific applications or type of materials phases
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/637—Specific applications or type of materials liquid

Definitions

  • the present invention relates to the field of mineral engineering and metallurgy and hydrometallurgical technologies in general and to extraction of metal compounds from ores or concentrates by wet processes, and more particularly to a method and an arrangement for monitoring of a hydrometallurgical liquid-liquid extraction process.
  • Hydrometallurgical technologies are used for obtaining or extracting metal compounds from their ores.
  • the phases exiting a hydrometallurgical extraction process should be clean of the other liquid phase and solids but in practice some residue of the other phase, commonly called entrainment, will remain in the solutions.
  • Entrainment consists of isolated droplets of the other liquid phase that settle slowly by gravity due to the very small size of the droplets or due to solids.
  • a typical practice for providing measurement data for monitoring of a hydrometallurgical liquid-liquid extraction process is that the plant personnel take samples manually from the process and use instrumental or chemical analysis in the laboratory to measure the water and solid content. These methods are, however, time consuming, prone to human errors and, as being based on a single sample taken from a single point will only give an instantaneous indication of the status of the liquid-liquid extraction process.
  • the problem therefore is to find a solution for an adequate measuring arrangement in a hydrometallurgical liquid-liquid extraction process which can provide continuously reliable measurement data for monitoring the hydro- metallurgical liquid-liquid extraction process.
  • An object of the present invention is thus to provide a method and an apparatus for implementing the method so as to overcome the above problems and to alleviate the above disadvantages.
  • the objects of the invention are achieved by a method for monitoring of a hydrometallurgical liquid-liquid extraction process, said process com- prising multiphase liquid-liquid system in at least one settler cell, said multiphase liquid-liquid system comprising two or more phases, at least two of said two or more phases being in liquid state, which method comprises the steps of:
  • said method comprises the step of controlling said hydrometallurgical liquid-liquid extraction process based on the detected X-ray radiation data.
  • said settler is a loading settler.
  • said settler is a stripping settler, a washing settler, a scrubbing settler or an after-settler.
  • an ar- rangement for monitoring of a hydrometallurgical liquid-liquid extraction process comprising multiphase liquid-liquid system in an at least one settler cell, said multiphase liquid-liquid system comprising two or more phases, at least two of said two or more phases being in liquid state, which arrangement comprises:
  • At least one X-ray tube unit comprising at least one X-ray transmission source, said at least one X-ray transmission source being arranged to transmit X-ray radiation into said at least one settler cell,
  • At least one X-ray sensor unit arranged to detect X-ray radiation travelling inside said at least one settler cell
  • a sensor data processing unit which said sensor data processing unit provides a two- or three-dimensional image related to the attenuation of X- rays by the liquid-liquid system inside the settler cell.
  • said arrangement comprises a sensor data processing unit, which said sensor data processing unit controls said hydrometallurgical liquid-liquid extraction process based on the detected X-ray radiation data.
  • phase volumes, particle densities and/or particle sizes in the multiphase solution of the liquid-liquid system is/are calculated based on the detected X-ray radiation data.
  • the water content of organic phase at different heights in said at least one settler cell is/are calculated based on the detected X-ray radiation data.
  • the crud formation in said at least one settler cell is calculated based on the detected X-ray radiation data.
  • the thickness of the separated organic phase layer and/or the thickness of the system layer in said at least one settler cell is/are calculated based on the detected X-ray radiation data.
  • the X-rays from said at least one X-ray transmission source of said X-ray tube are collimated into a narrow beam in at least one dimension when propagating inside said at least one settler cell.
  • said at least one X-ray tube unit is arranged to move or turn in order to transmit X-ray radiation in multiple directions.
  • said at least one X-ray sensor unit is arranged to move or turn.
  • said at least one X-ray tube unit is attached to a first wall structure of said at least one settler cell, and that said at least one X-ray sensor unit is attached to a second wall structure of said at least one settler cell, said second wall structure being on the side opposing said at least one X-ray tube unit.
  • said at least one X-ray tube unit and said at least one X-ray sensor unit are attached inside said at least one settler cell said at least one X-ray sensor unit opposing said at least one X-ray tube unit.
  • said at least one X-ray tube unit and said at least one X-ray sensor unit are realized as an at least one X-ray measurement unit, each of said at least one X-ray measurement unit comprising at least one X-ray tube unit and said at least one X-ray sensor unit.
  • said at least one X-ray measurement unit is a movable X-ray measurement unit.
  • said settler comprises at least one X-ray measurement unit and one or more double gate type fence structures, so that said at least one X-ray measurement unit is attached before, after or inside the at least one of said one or more double gate type fence structure inside the settler.
  • said settler comprises one or more double gate type fence structures and at least one X-ray tube unit attached to one first fence structure inside at least one of said one or more double gate type fence struc- tures inside the settler and at least one X-ray sensor unit attached to one second fence structure inside at least one of said one or more double gate type fence structures inside the settler.
  • said settler comprises one or more double gate type fence structures and at least one X-ray sensor unit attached to one first fence structure inside at least one of said one or more dou- ble gate type fence structures inside the settler and at least one X-ray tube unit attached to one second fence structure inside at least one of said one or more double gate type fence structures inside the settler.
  • said X-ray sensor unit provides a two- or three-dimensional image related to the attenuation of X-rays by the liquid-liquid system traveling through said double gate type fence structure inside the settler. More preferably, said X-ray sensor unit detects crud formation on said double gate type fence structure from said two- or three-dimensional image.
  • said settler is a loading settler.
  • said settler is a stripping settler, a washing settler, a scrubbing settler or an after-settler.
  • Figure 1 shows a flow diagram of a hydrometallurgical process according to the present invention
  • Figure 2 shows a flow diagram of another hydrometallurgical liquid- liquid extraction process according to the present invention
  • Figure 3 shows a top view of a settler of a hydrometallurgical liquid- liquid extraction process according to the present invention
  • Figure 4 shows a partial cross-sectional view of a settler of a hydrometallurgical liquid-liquid extraction process according to the present invention
  • Figure 5 shows a perspective view of one embodiment of a settler cell of a hydrometallurgical liquid-liquid extraction process according to the present invention
  • Figure 6 shows a picture based on an X-ray image from a settler of a hydrometallurgical liquid-liquid extraction process according to the present invention
  • Figure 7 shows a partial cross-sectional view of one embodiment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention
  • Figure 8 shows a partial cross-sectional view of another embodi- ment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention
  • Figure 9 shows a partial cross-sectional view of a third embodiment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • Figure 10 shows a perspective view of another embodiment of a settler cell of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • the present invention relates to a method and an arrangement monitoring of a hydrometallurgical liquid-liquid extraction process in a settler.
  • Hydrometallurgical technologies are used for obtaining or extracting metal compounds from their ores. Hydrometallurgical processes involve the use of aqueous chemistry for the recovery of metals from ores, concentrates, and recycled or residual materials. Hydrometallurgy is typically divided into three general areas: leaching, solution purification and recovery technologies.
  • Leaching involves the use of aqueous solutions, which contain a lix- iviant brought into contact with a material containing a valuable metal.
  • aqueous solutions which contain a lix- iviant brought into contact with a material containing a valuable metal.
  • leaching process options available for the hydrometallurgical treatment of ores and concentrates.
  • oxidation potential, temperature, and pH of the solution are important parameters.
  • leaching methods utilizing lixiviants such as sulfuric acid, chloride and cyanide at atmospheric or elevated pressure.
  • Leaching technologies include the leaching of e.g. zinc, copper, nickel, cobalt, gold, silver, rare earth elements, molybdenum, manganese and synthetic rutile.
  • the pregnant leach solution is first mixed with an organic stream to form a liquid-liquid system when the metal ion is transferred to the organic phase. After mixing the phase disengagement takes place in a settler. The resulting streams will be a loaded organic phase stream and a raffinate stream.
  • the stripping process where the loaded organic phase is mixed as a liquid-liquid system with stripping liquor and allowed to separate in a settler. In stripping the metal will be transferred from the organic phase to the stripping liquor. The resulting streams will be a stripped organic phase stream and a rich stripping liquor stream.
  • FIG. 1 shows a flow diagram of a hydrometallurgical process ac- cording to the present invention.
  • a hydrometallurgical process according to the present invention comprises the process blocks for leaching process 1 , liquid- liquid extraction process 2, and recovery process 3.
  • the leach-ing process 1 is carried out first.
  • the leaching process provides a pregnant leach solution for the liquid-liquid extraction process 2.
  • the pregnant leach solution is first mixed into liquid-liquid system with an organic stream in a mixer tank.
  • the resulting mixed liquid-liquid system is taken from the mixer tank to a settler of the liquid-liquid extraction process 2 for separation.
  • the loading stage of the liquid-liquid extraction process provides a loaded organic phase stream and a raffinate stream as output of the loading process.
  • the loaded organic phase stream from the loading stage of the liquid-liquid extraction process 2 is provided as an input for the stripping stage of the liquid-liquid extraction process 2.
  • the loaded organic phase is then mixed into liquid-liquid system with e.g. a lean electrolyte in a mixer tank.
  • the resulting mixed liquid-liquid system is taken to a stripping settler for separation.
  • the stripping stage of the liquid-liquid extraction process provides a stripped organic phase stream and a rich electrolyte stream as output of the stripping process.
  • the recovery pro- cess 3 is carried out after the liquid-liquid extraction process 2 the recovery pro- cess 3 is carried out.
  • FIG. 2 shows a flow diagram of another hydrometallurgical liquid- liquid extraction process according to the present invention.
  • Another hydro- metallurgical process according to the present invention comprises the process blocks for a leaching process 4, an extraction process 5, a stripping process 6, and an electrowinning process 7.
  • Leaching 4 involves the use of aqueous solutions, which contain a lixiviant brought into contact with a material containing a valuable metal.
  • leaching process op- tions available for the hydrometallurgical treatment of ores and concentrates.
  • oxidation potential, temperature, and pH of the solution are important parameters.
  • Leaching technologies include the leaching of e.g. zinc, copper, nickel, cobalt, gold, silver, rare earth elements, molybdenum, manganese and synthetic rutile.
  • the leaching process 4 provides a pregnant leach solution, which pregnant leach solution is carried in a hydrometallurgy pipe 8 to the extraction process 5.
  • the pregnant leach solution is typically first mixed with an organic stream in a mixer tank to form a liquid-liquid disys- temspersion when the metal ion is transferred to the organic phase.
  • the resulting liq-uid-liquid system is taken from the mixer tank to a liquid-liquid extraction settler of the extraction process 5 for separation.
  • the loading stage of the extraction process 5 provides a loaded organic phase stream and a barren leach solution stream as output of the loading stage of the extraction process 5.
  • the loaded organic phase stream is carried in a hydrometallurgy pipe 9 to the stripping process 6 and the barren leach solution stream is returned in a hydrometallurgy pipe 10 back to the leaching process 4.
  • the loaded organic phase is then mixed into liquid-liquid system with e.g. a lean electrolyte in a mixer tank.
  • the resulting mixed liquid-liquid system is taken to a stripping settler of the stripping process 6 for separation.
  • the stripping stage of the stripping process 6 provides a stripped organic phase stream and a rich electrolyte stream as output of the stripping process 6.
  • the rich electrolyte stream is carried in a hydrometallurgy pipe 1 1 to the electrowinning process 7 and the stripped organic phase stream is returned in a hydrometallurgy pipe 12 back to the extraction process 5.
  • the rich electrolyte is taken to an electrowinning settler of the electrowinning process 7.
  • a current is passed from an inert anode through the rich electrolyte solution containing the metal so that the metal is extracted as it is deposited in an electroplating process onto the cathode.
  • the electrowinning process 7 provides cathodes containing the metal and a spent electrolyte stream as output of the electrowinning process 7.
  • the cathodes containing the metal are taken out as the output of the hydrometallurgical process and the spent electrolyte stream is returned in a hydrometallurgy pipe 13 back to the stripping process 6.
  • hydrometallurgical liquid-liquid extraction processes include also some washing and scrubbing stages to remove impurity elements from the organic phase.
  • Some plants use after settlers for the aqueous raffinate and/or for the rich electrolyte.
  • Such equipment utilizes similar settlers as used in the actual liquid-liquid extraction stages.
  • the settler separates the phases in the liquid-liquid dispersed pregnant leach solution.
  • the phases exit- ing the liquid-liquid extraction settler i.e. the separated loaded organic phase and the separated aqueous raffinate phase, should be clean of the other liquid phase and solids but in practice some residue of the other phase, commonly called entrainment, will remain in the solutions.
  • Entrainment consists of isolated droplets of the other liquid phase that settle slowly by gravity due to the very small size of the droplets or due to solids.
  • the entrained aqueous liquid in the separated loaded organic phase typically contains impurities which can impair the purity of the product, cause degradation of the organic phase and lower the current efficiency of the elec- trowinning process 7 following the extraction process 5 and the stripping pro- cess 6.
  • a typical practice for providing measurement data for controlling of a hydrometallurgical process is that the plant personnel take samples manually from the process and use a centrifuge in the laboratory to measure the water content. Also the content of solids is measured based on samples. These methods, however, are time consuming, prone to human errors and, as being based on a single sample taken from a single point will only give an instantaneous indication of the status of the hydrometallurgical process.
  • FIG. 3 shows a top view of a settler of a hydrometallurgical liquid- liquid extraction process according to the present invention.
  • a settler 14 according to the present invention comprises several fence structures 15-18, said fence structures 15-18 enabling the proper and controlled flow of the hydro- metallurgical liquid-liquid extraction process.
  • the fence structures 15-18 of the a settler 14 according to the present invention may be regular present inven- tion fence structures 15-18, or even DDG-type fence structures 15-18 (DDG, System Depletor Gate). Such constructions are often objects for scaling by e.g. gyp-sum.
  • DDG System Depletor Gate
  • FIG 4 shows a partial cross-sectional view of a settler of a hy- drometallurgical liquid-liquid extraction process according to the present inven- tion.
  • a settler 19 according to the present invention comprises several double gate type fence structures 20-21 , and one such said double gate type fence structure 20-21 is shown in Figure 4.
  • the flow direction is from left to right and the separated organic phase 22 flows on the top from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • the separated aqueous phase 24 flows on the bottom from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • the flow of the system 23 is restricted by the top part of the left fence 20 of the double gate type fence structure 20-21 and the bottom part of the right fence 21 of the double gate type fence structure 20-21 .
  • the thickness of the system layer 23 of one left side settler cell before the fence structure 20-21 is noticeably larger than the thickness of the system layer 23 of the other right side settler cell after the fence structure 20-21 as the system breaks up along the path through the settler.
  • the settler 19 part of a mixer- settler separates the phases after the liquid-liquid contact, in which the two immiscible solutions are mixed to system.
  • Entrainment consists of isolated droplets of the other liquid phase that settle slowly by gravity due to the very small size of the droplets or due to solids.
  • the entrained aqueous liquid in the separated organic phase 22 typical- ly contains impurities which can impair the purity of the product, cause degradation of the organic phase and lower the current efficiency of the elec- trowinning process following the liquid-liquid extraction.
  • the separated organic phase 22 layer lies on top of the settler 19 and when this phase is to be the pure one of the two exiting phases, as in the case where the separated organic phase 22 is loaded with the target element, it should contain a minimum amount of entrained aqueous.
  • a pregnant leach solution is a sulfuric acid solution with a pH between 1 .5 and 3.
  • the organic phase typically contains an extractant diluted with a kerosene type solvent.
  • the lean electrolyte used for stripping is sulfuric acid solution containing 170 g/L to 210 g/L H2S04.
  • the wash and scrubbing stages are for removing impurities from the organic phase using aqueous solutions.
  • after settler typically the purpose of after settler is to give more settling time in order to remove organic droplets.
  • after- settlers are installed for the rich electrolyte after the stripping stage and before the solution enters the electrowinning tankhouse and for the raffinate leaving the extraction stages and before entering the raffinate pond.
  • FIG. 5 shows a perspective view of one embodiment of a settler cell of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • a settler cell 25 comprises a multiphase liquid-liquid system 26 received from a mixer tank said liquid-liquid system 26 including the preg- nant leach solution.
  • Said multiphase liquid-liquid system 26 comprises two or more phases so that at least two of said two or more phases is in liquid state.
  • Said multiphase liquid-liquid system 26 is in a smooth flow in the settler cell 25 and the flow direction across the settler cell 25 is indicated with an arrow 27.
  • a settler cell 25 comprises an at least one X-ray tube unit 28.
  • said X-ray tube unit 28 is attached inside the settler cell 25.
  • the X-ray tube unit 28 includes an at least one X-ray transmission source 29-32 said at least one X-ray transmission source 29-32 being arranged to transmit X-ray radiation inside the of the settler cell 25.
  • the X-ray radiation travelling inside settler cell 25 is marked with a reference number 33.
  • the settler cell 25 also comprises an at least one X-ray sensor unit 34 attached inside the settler cell 25 and arranged to detect X-ray radiation 33 travelling inside the settler cell 25, said at least one X-ray sensor unit 34 opposing said at least one X-ray tube unit 28.
  • the X- rays from said at least one X-ray tube 29-32 of said X-ray tube unit 28 may be collimated into a narrow beam in at least one dimension when propagating, e.g. horizontally, into the of the settler cell 25 thus minimizing the amount of radiation to other directions other directions than the detector.
  • said at least one X-ray transmission source 29-32 of said X-ray tube unit 28 may be arranged to move or turn, e.g. horizontally, in order to transmit X-ray radiation in multiple directions.
  • an at least one X-ray sensor unit 34 attached inside the settler cell 25 detects an X-ray radiation 33 transmitted by an opposing at least one X-ray tube unit 28, said X-ray radiation 33 travelling inside the settler cell 25. From said detected X-ray radiation data a sensor data processing unit can provide a two-dimensional image related to the attenuation of X-rays by the liquid-liquid system 26 inside the settler cell 25 based on the detected X-ray radiation data. Furthermore, said at least one X- ray sensor unit 34 may be arranged to move or turn, e.g. horizontally, in order to sense and provide a two- or three-dimensional image.
  • Said image provided by said at least one X-ray sensor unit 34 gives information for the calculation of phase volumes, particle densities and particle sizes in the multiphase solution of the liquid-liquid system 26. Furthermore, the water content of organic phase at different heights and crud formation in said settler cell 25 may be calculated based on said image provided by said at least one X-ray sensor unit 34.
  • Figure 6 shows a picture based on an X-ray image from a settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • the picture presented in Figure 6 shows a visual presentation of a copper solvent extraction process based on an X-ray image. Said X-ray image is taken in a laboratory from an experiment measurement in a 10 liter settler.
  • the picture presented in Figure 6 shows the two different liquid phases, i.e. the copper loaded organic phase and the aqueous phase, as well as the accumu- lated solids phase present in the settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • FIG. 7 shows a partial cross-sectional view of one embodiment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • a loading settler 35 according to the presented embodiment comprises several settler cells and several double gate type fence structures 36-40 arranger between said several settler cells, said several double gate type fence structures 36-40 enabling the proper and controlled flow of the hydrometallurgical liquid-liquid extraction process.
  • a loading settler 35 com- prises several X-ray measurement units 41 -45 arranged at said several settler cells.
  • Each of the several X-ray measurement units 41 -45 arranged at said several settler cells comprises an at least one X-ray tube unit and an at least one X-ray sensor unit so that said least one X-ray sensor unit is arranged to detect an X-ray radiation transmitted by said at least one X-ray tube unit.
  • a sensor data processing unit can provide a two- or three-dimensional image related to the attenuation of X-rays by the liquid-liquid system inside the respective settler cell based on the detected X-ray radiation data.
  • Said images provided by said several X-ray measurement units 41 -45 give information for the calculation of phase volumes, particle densities and particle sizes in the multiphase solution of the liq- uid-liquid system inside the respective settler cell.
  • the water content of organic phase at different heights and crud formation in the respective settler cell may be calculated based on said image provided by said at least one X-ray measurement units 41 -45.
  • the X-ray measurement units 41 -45 can be arranged in said several settler cells so that they also can be used to measure the thick- nesses of the separated organic phase layer.
  • a loading settler according to the present invention may also comprise an at least one X-ray measurement units in the first settler cell before the first fence structure.
  • a loading settler according to the present invention may also comprise several X-ray measurement units 41 -45 in one settler cell.
  • FIG 8 shows a partial cross-sectional view of another embodiment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • Another embodiment of a loading settler 46 according to the present invention comprises one or more double gate type fence structure 20-21 , each of said double gate type fence structure 20-21 comprising one first fence structure 20 and one second fence structure 21 , an example of one such said double gate type fence structure 20-21 being shown in Figure 8.
  • the flow direction is from left to right and the separated organic phase 22 flows on the top from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • the flow of the system 23 is restricted by the top part of the left fence 20 of the double gate type fence structure 20-21 and the bottom part of the right fence 21 of the double gate type fence structure 20-21 .
  • the separated aqueous phase 24 flows on the bottom from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • a loading settler 46 comprises an at least one X-ray tube unit 47 attached before or after at least one first fence structure 20 of said one or more double gate type fence structure 20-21 inside the settler 46 and an at least one X-ray sensor unit 48 attached before or after at least one second fence structure 21 of said one or more double gate type fence structure 20-21 inside the settler 46, so that said least one X-ray sensor unit 48 is arranged to detect an X-ray radiation transmitted by said at least one X-ray tube unit 47, said X-ray radiation having travelled through said one or more double gate type fence structure 20-21 inside the settler 46.
  • an at least one X-ray sensor unit may be attached before or after at least one first fence structure 20 of said one or more double gate type fence structure 20-21 inside the settler 46 and, respectively, an at least one X-ray tube unit attached before or after at least one second fence structure 21 of said one or more double gate type fence structure 20-21 inside the settler 46.
  • a sensor data processing unit can provide a two- or three-dimensional image related to the attenuation of X-rays by the liquid-liquid system traveling through said double gate type fence structure 20-21 inside the settler 46 based on the detected X-ray radiation data. Furthermore, from said two- or three-dimensional image crud formation and scaling, on said double gate type fence structure 20-21 can be detected.
  • FIG 9 shows a partial cross-sectional view of a third embodiment of a loading settler of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • Another embodiment of a loading settler 49 according to the present invention comprises one or more double gate type fence structure 20-21 , each of said double gate type fence structure 20-21 comprising one first fence structure 20 and one second fence structure 21 , an example of and one such said double gate type fence structure 20-21 being shown in Figure 9.
  • the flow direction is from left to right and the separated organic phase 22 flows on the top from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • the flow of the system 23 is restricted by the top part of the left fence 20 of the double gate type fence structure 20-21 and the bottom part of the right fence 21 of the double gate type fence structure 20-21 .
  • the separated aqueous phase 24 flows on the bottom from left to right and from one settler cell before the fence structure 20-21 to another settler cell after the fence structure 20-21 .
  • a loading settler 49 comprises an at least one X-ray tube unit 50 attached to one first fence structure 20 inside at least one of said one or more double gate type fence structure 20-21 inside the settler 49 and an at least one X-ray sensor unit 51 attached to one second fence structure 21 inside at least one of said one or more double gate type fence structure 20-21 inside the settler 49, so that said least one X-ray sensor unit 51 is arranged to detect an X-ray radiation transmitted by said at least one X-ray tube unit 50, said X-ray radiation having travelled upwards through said one or more double gate type fence structure 20-21 inside the settler 49.
  • an at least one X-ray sensor unit may be attached to one first fence structure 20 inside at least one of said one or more double gate type fence structure 20-21 inside the settler 49 and, respectively, an at least one X-ray tube unit may be attached to one second fence structure 21 inside at least one of said one or more double gate type fence structure 20-21 inside the settler 49.
  • a sensor data processing unit can provide a two- or three-dimensional image related to the attenuation of X-rays by the liquid-liquid system traveling through said double gate type fence structure 20-21 inside the settler 49 based on the detected X-ray radiation data. Furthermore, from said two- or three-dimensional image crud formation on said double gate type fence structure 20-21 can be detected.
  • FIG 10 shows a perspective view of another embodiment of a settler cell of a hydrometallurgical liquid-liquid extraction process according to the present invention.
  • a settler cell 25 comprises a multiphase liquid-liquid system 26 received from a mixer tank said liquid-liquid system 26 including the pregnant leach solution.
  • Said multiphase liquid-liquid system 26 comprises two or more phases so that at least two of said two or more phases is in liquid state.
  • Said multiphase liquid-liquid system 26 is in a smooth flow in the settler cell 25 and the flow direction across the settler cell 25 is indicated with an arrow 27.
  • a settler cell 25 comprises an at least one movable X-ray measurement unit 52.
  • Said at least one movable X-ray measurement unit 52 comprises an at least one X-ray tube unit 53 and an at least one X-ray sensor unit 54, said at least one X-ray sensor unit 54 opposing said at least one X-ray tube unit 53.
  • said X-ray tube unit 53 includes an at least one X-ray transmission source 55-58, said at least one X-ray transmission source 55-58 being arranged to transmit X-ray radiation inside the of the settler cell 25.
  • Respectively said at least one X-ray sensor unit 54 is arranged to detect X-ray radiation 59 travelling inside the settler cell 25.
  • the X- rays from said at least one X-ray transmission source 55-58 of said X-ray tube unit 53 may be collimated into a narrow beam in at least one dimension when propagating intothe settler cell 25 thus minimizing the amount of radiation to other directions other directions than the detector.
  • said at least one X-ray transmission source 55-58 of said X-ray tube unit 53 may be ar- ranged to move or turn, e.g. horizontally, in order to transmit X-ray radiation in multiple directions.
  • Said at least one movable X-ray measurement unit 52 may also be used together with said one or more double gate type fence structure 20-21 where said at least one movable X-ray measurement unit 52 can be moved e.g. in the direction parallel to the fence structure and/or in the direction perpendicular to the fence structure.
  • an at least one X-ray sensor unit 54 attached inside the settler cell 25 detects an X-ray radiation 33 transmitted by an opposing at least one X-ray tube unit 53, said X-ray radiation 33 travelling inside the settler cell 25. From said detected X-ray radiation data a sensor data processing unit can provide a two-dimensional image related to the attenuation of X-rays by the liquid-liquid system 26 inside the settler cell 25 based on the detected X-ray radiation data. Furthermore, said at least one X- ray sensor unit 54 may be arranged to move or turn, e.g. horizontally, in order to sense and provide a two- or three-dimensional image.
  • Said image provided by said at least one X-ray sensor unit 54 gives information for the calculation of phase volumes, particle densities and particle sizes in the multiphase solution of the liquid-liquid system 26. Furthermore, the water content of organic phase at different heights and crud formation in said settler cell 25 may be calculated based on said image provided by said at least one X-ray sensor unit 54. Any one of the embodiments of the present invention may also be used in a stripping settler. In the stripping settler the metal will be exchanged from the organic phase to the electrolyte. Furthermore, any one of the embodiments of the present invention may also be used in a washing settler or in a scrubbing settler.
  • hydrometallurgical liquid-liquid extraction processes include also some washing and scrubbing stages to remove impurity elements from the organic phase.
  • any one of the embodiments of the present invention may also be used in an after settler.
  • To remove small amounts of organics some plants use after settlers for the aqueous raffinate and/or for the rich electrolyte. Such equipment utilizes similar settlers as used in the actual liquid-liquid extraction stages.
  • the solution for monitoring of a hydrometallurgical liquid-liquid extraction process according to the present invention provides a continuous measurement of a liquid-liquid system in a settler cell, which is highly insensi- tive to dirt or contamination of the measurement system, e.g. insensitive to contamination of the optical surfaces of the measurement system.
  • the solution for monitoring of a hydrometallurgical liquid-liquid extraction process according to the present invention provides reliable, online measurement data for the monitoring of the hydrometallurgical liquid-liquid extraction process containing information from both the liquid phases as well as about the solids.
  • the manufacturers and owners of settlers will be able to provide settler with a measurement arrangement producing more reliable measurement data for monitoring of a hydrometallurgical liquid-liquid extraction process in a settler with said measurement data containing information from both the liquid phases as well as about the solids.
  • the solution according to the present invention may be utilised in any kind of a settler.

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Abstract

La présente invention concerne le domaine du génie minéral et des technologies de la métallurgie et de l'hydrométallurgie en général, et l'extraction de composés métalliques à partir de minerais ou de concentrés par des processus en phase humide, et plus particulièrement un procédé et un agencement pour surveiller un processus d'extraction liquide-liquide hydrométallurgique. Un agencement de surveillance d'un processus d'extraction liquide-liquide hydrométallurgique selon la présente invention comprend au moins une unité de tube à rayons X (28), (53), ladite unité de tube à rayons X, (28), (53) comprenant au moins une source d'émission de rayons X (29-32), (55-58), ladite source d'émission de rayons X (29-32), (55-58) étant conçu pour émettre un rayonnement de rayons X dans au moins une cellule de décantation (25), et au moins une unité de capteur de rayons X (34), (54) conçue pour détecter un rayonnement de rayons X (33), (59) se déplaçant à l'intérieur de ladite cellule de décantation (25), et une unité de traitement de données de capteur, ladite unité de traitement de données de capteur fournissant une image bidimensionnelle ou tridimensionnelle associée à l'atténuation des rayons X par le système liquide-liquide (26) à l'intérieur de la cellule de décantation (25).
PCT/FI2016/050920 2015-12-23 2016-12-23 Procédé et agencement de surveillance d'un processus d'extraction liquide-liquide hydrométallurgique Ceased WO2017109294A1 (fr)

Applications Claiming Priority (4)

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FI20156003 2015-12-23
FI20156003 2015-12-23
FI20156035A FI126880B (en) 2015-12-23 2015-12-30 A method and arrangement for controlling a hydrometallurgical fluid-liquid extraction process
FI20156035 2015-12-30

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1171795A (en) * 1965-12-16 1969-11-26 Incentive Ab Device for the Determination of Distribution Factors.
US4023022A (en) * 1974-08-05 1977-05-10 Mitsui Mining & Smelting Co., Ltd. System for automatically and continuously measuring zinc and sulfuric acid concentration in circulating electrolyte
WO2011119045A1 (fr) * 2010-03-24 2011-09-29 Institutt For Energiteknikk Procédé de réalisation de mesures par tomodensitométrie de flux multiphases contenant du pétrole à travers une conduite
US20120114097A1 (en) * 2009-07-07 2012-05-10 Stepan Polikhov Apparatus and method for measuring multi-phase fluid flow
WO2014074002A1 (fr) * 2012-11-06 2014-05-15 Siemens Aktiengesellschaft Procédé et système pour la détection d'inclusions métalliques dans des scories en fusion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1171795A (en) * 1965-12-16 1969-11-26 Incentive Ab Device for the Determination of Distribution Factors.
US4023022A (en) * 1974-08-05 1977-05-10 Mitsui Mining & Smelting Co., Ltd. System for automatically and continuously measuring zinc and sulfuric acid concentration in circulating electrolyte
US20120114097A1 (en) * 2009-07-07 2012-05-10 Stepan Polikhov Apparatus and method for measuring multi-phase fluid flow
WO2011119045A1 (fr) * 2010-03-24 2011-09-29 Institutt For Energiteknikk Procédé de réalisation de mesures par tomodensitométrie de flux multiphases contenant du pétrole à travers une conduite
WO2014074002A1 (fr) * 2012-11-06 2014-05-15 Siemens Aktiengesellschaft Procédé et système pour la détection d'inclusions métalliques dans des scories en fusion

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SOLYMAR K ET AL: "CHARACTERISTICS AND SEPARABILITY OF RED MUD", LIGHT METALS. SAN DIEGO, MAR. 1 - 5, 1992; [PROCEEDINGS OF THE TMS ANNUAL MEETING], WARRENDALE, TMS, US, vol. MEETING 121, 1 March 1992 (1992-03-01), pages 209 - 223, XP000366149 *

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