FI126880B - Method and Arrangements for Monitoring a Hydrometallurgical Liquid-Liquid Extraction Process - Google Patents
Method and Arrangements for Monitoring a Hydrometallurgical Liquid-Liquid Extraction Process Download PDFInfo
- Publication number
- FI126880B FI126880B FI20156035A FI20156035A FI126880B FI 126880 B FI126880 B FI 126880B FI 20156035 A FI20156035 A FI 20156035A FI 20156035 A FI20156035 A FI 20156035A FI 126880 B FI126880 B FI 126880B
- Authority
- FI
- Finland
- Prior art keywords
- liquid
- ray
- clarification basin
- settler
- arrangement according
- Prior art date
Links
Classifications
-
- 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
- B01D11/0446—Juxtaposition of mixers-settlers
- B01D11/0453—Juxtaposition of mixers-settlers with narrow passages limited by plates, walls, e.g. helically coiled tubes
-
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
-
- 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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
- C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
- C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
- C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
-
- 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
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/24—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by observing the transmission of wave or particle radiation through the material
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Environmental & Geological Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Toxicology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
A METHOD AND AN ARRANGEMENT FOR MONITORING OF A HYDROMETAL-LURGICAL LIQUID-LIQUID EXTRACTION PROCESS
FIELD OF THE INVENTION
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.
BACKGROUND OF THE INVENTION
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.
Under normal operating conditions the amount of entrainment is quite low but in the event of process disturbances, which can take place for several possible reasons, the phase disengagement rate in the settler may decrease and result in an increase in entrainment. In liquid-liquid extraction processes there is currently no automated online measurement used for acquiring adequate measurement data for monitoring the liquid-liquid extraction process. 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.
In general, there are several problems with the prior art solutions for monitoring the hydrometallurgical liquid-liquid extraction process. So far, the measuring solutions are relatively troublesome and difficult to process. The presence of solids has been difficult to detect. Previously there has not been any means for the monitoring of accumulation of solids and the scaling of equipment surfaces in the hydrometallurgical liquid-liquid 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.
There is a demand in the market for a method for monitoring the hydrometallurgical liquid-liquid extraction process which method would be continuous, reliable and informative measurement when compared to the prior art solutions. Likewise, there is a demand in the market for an arrangement for monitoring the hydrometallurgical liquid-liquid extraction process which arrangement would be more reliable and informative measurement when compared to the prior art solutions.
BRIEF DESCRIPTION OF THE INVENTION
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 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 the said two or more phases being in liquid state, which method comprises the steps of: - transmitting X-ray radiation into of a settler cell of said settler by an at least one X-ray tube unit arranged in said settler, said at least one X-ray tube unit comprising an at least one X-ray transmission source; and - detecting X-ray radiation travelling inside said settler cell by an at least one X-ray sensor unit.
Preferably, said method comprises the step of providing a two- or three-dimensional image related to the attenuation of X-rays by the multiphase liquid-liquid system inside the said settler cell based on the detected X-ray radiation data.
Preferably, said method comprises the step of controlling the said hydrometallurgical liquid-liquid extraction process based on the detected X-ray radiation data.
Preferably in the method, said settler is a loading settler. Alternatively in the method, said settler is a stripping settler, a washing settler, a scrubbing settler or an after-settler.
Furthermore, the objects of the invention are achieved by an arrangement for monitoring of a hydrometallurgical liquid-liquid extraction process, said 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 the said two or more phases being in liquid state, which arrangement comprises: - an at least one X-ray tube unit, said at least one X-ray tube unit comprising an 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, and - an at least one X-ray sensor unit arranged to detect X-ray radiation travelling inside said at least one settler cell.
Preferably, said arrangement comprises 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. Preferably, said arrangement comprises a sensor data processing unit, which said sensor data processing unit controls the said hydrometallurgical liquid-liquid extraction process based on the detected X-ray radiation data.
Preferably, 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. Preferably, 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. Preferably, the crud formation in said at least one settler cell is calculated based on the detected X-ray radiation data. Preferably, 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.
Preferably, the X-rays from said at least one X-ray transmission source of the said X-ray tube are collimated into a narrow beam in at least one dimension when propagating inside said at least one settler cell. Preferably, said at least one X-ray tube unit is arranged to move or turn in order to transmit X-ray radiation in multiple directions. Preferably, said at least one X-ray sensor unit is arranged to move or turn.
Preferably, said at least one X-ray tube unit is attached at a first wall structure of the said at least one settler cell, and that the said at least one X-ray sensor unit attached at a second wall structure of the said at least one settler cell, the said second wall structure being on the side opposing the said at least one X-ray tube unit. Alternatively, said at least one X-ray tube unit and the said at least one X-ray sensor unit are attached inside the said at least one settler cell the said at least one X-ray sensor unit opposing the said at least one X-ray tube unit.
Preferably, said at least one X-ray tube unit and the 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 the said at least one X-ray sensor unit. Preferably, said at least one X-ray measurement unit is a movable X-ray measurement unit.
Preferably, said settler comprises an at least one X-ray measurement unit and one or more double gate type fence structures, so that the said an at least one X-ray measurement unit is attached before, after or inside the at least one of the said one or more double gate type fence structure inside the settler.
Preferably, said settler comprises one or more double gate type fence structures and an at least one X-ray tube unit attached to one first fence structure inside at least one of the said one or more double gate type fence structure inside the settler settler and an at least one X-ray sensor unit attached to one second fence structure inside at least one of the said one or more double gate type fence structure inside the settler. Alternatively, said settler comprises one or more double gate type fence structures and an at least one X-ray sensor unit attached to one first fence structure inside at least one of the said one or more double gate type fence structure inside the settler settler and an at least one X-ray tube unit attached to one second fence structure inside at least one of the said one or more double gate type fence structure inside the settler. More preferably, 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 the said double gate type fence structure inside the settler. More preferably, said X-ray sensor unit detects crud formation on the said double gate type fence structure from said two- or three-dimensional image.
Preferably in the arrangement, said settler is a loading settler. Alternatively in the arrangement, said settler is a stripping settler, a washing settler, a scrubbing settler or an after-settler.
BRIEF DESCRIPTION OF THE DRAWINGS
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 embodiment 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.
In the following, the invention will be described in greater detail by means of preferred embodiments with reference to the accompanying drawings of Figures 1 to 10.
DETAILED DESCRIPTION OF THE 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. There are a number of leaching process options available for the hydrometallurgical treatment of ores and concentrates. In the leaching process, oxidation potential, temperature, and pH of the solution are important parameters. There are several 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.
After the leaching process, in the solution purification, which can be a liquid-liquid extraction process, 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.
After the loading process, is 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.
Figure 1 shows a flow diagram of a hydrometallurgical process according 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.
In a hydrometallurgical process according to the present invention the leach-ing process 1 is carried out first. The leaching process provides a pregnant leach solution for the liquid-liquid extraction process 2. In the loading stage of 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. In the stripping stage 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. In a hydrometallurgical process according to the present invention after the liquid-liquid extraction process 2 the recovery process 3 is carried out.
Figure 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.
In another hydrometallurgical process according to the present invention the leaching process 4 is carried out first. Leaching 4 involves the use of aqueous solutions, which contain a lixiviant brought into contact with a material containing a valuable metal. There are a number of leaching process options available for the hydrometallurgical treatment of ores and concentrates. In the leaching process, oxidation potential, temperature, and pH of the solution are important parameters. There are several versatile leaching methods ranging from sulfuric acid to chloride leaching and from atmospheric to pressure leaching. 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.
In 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.
In the stripping process 6 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 11 to the electrowinning process 7 and the stripped organic phase stream is returned in a hydrometallurgy pipe 12 back to the extraction process 5.
In the electrowinning process 7 the rich electrolyte is taken to an electrowinning settler of the electrowinning process 7. In 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.
Many hydrometallurgical liquid-liquid extraction processes include also some washing and scrubbing stages to remove impurity elements from the organic phase. 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.
In a hydrometallurgical process there are process blocks, in which different incoming hydrometallurgical fluid streams are combined or mixed and thereafter separated further into different outgoing hydrometallurgical fluid streams. Very often the incoming pregnant leach solution contains suspended solids such as silica and gypsum which tend to accumulate in the liquid- liquid process in various places such as equipment surfaces and on the liquid-liquid interface. The accumulated solid material may also suddenly continue downstream in the process and end up in the raffinate or electrolyte. Currently there are no suitable arrangements for measuring the characteristics of the incoming or the outgoing hydrometallurgical fluid stream or of the hydrometallurgical fluid stream in the liquid- liquid process for a proper controlling of the said process block or the entire hydrometallurgical process
For example, in the extraction process 5 the settler separates the phases in the liquid-liquid dispersed pregnant leach solution. The phases exiting 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 electrowinning process 7 following the extraction process 5 and the stripping process 6.
Under normal operating conditions the amount of entrainment is quite low but in the event of process disturbances, which can take place for several possible reasons, the phase disengagement rate in the settler may decrease and result in an increase in entrainment. In extraction process 5 there is currently no automated online measurement used for acquiring adequate measurement data for controlling the extraction process 5. 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.
Figure 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 invention 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. The rectangular cuboid volumes between the fence structures 15-18 are typically called settler cells.
Figure 4 shows a partial cross-sectional view of a settler of a hydrometallurgical liquid-liquid extraction process according to the present invention. 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. 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. Likewise 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. As shown in Figure 4 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.
In the liquid-liquid extraction process 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. The phases exiting the settler 19, i.e. the separated organic phase 22 and the separated aqueous phase 24, 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 organic phase 22 typically contains impurities which can impair the purity of the product, cause degradation of the organic phase and lower the current efficiency of the electrowinning 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.
In a typical hydrometallurgical process 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. Typically the purpose of after settler is to give more settling time in order to remove organic droplets. Typically aftersettlers 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.
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. 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 the 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 according to the present embodiment comprises an at least one X-ray tube unit 28. In the present embodiment 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. In Figure 5 the X-ray radiation travelling inside settler cell 25 is marked with a reference number 33.
The settler cell 25 according to the present embodiment 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, the said at least one X-ray sensor unit 34 opposing the said at least one X-ray tube unit 28.
In the settler cell 25 according to the present embodiment the X-rays from said at least one X-ray tube 29-32 of the 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. Furthermore, the said at least one X-ray transmission source 29-32 of the 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.
In the embodiment presented in Figure 5 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 the 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, the 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.
The 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 the 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. The 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 accumulated solids phase present in the 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. 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 according to the presented embodiment comprises several X-ray measurement units 41-45 arranged at the said several settler cells. Each of the several X-ray measurement units 41-45 arranged at the said several settler cells comprises an at least one X-ray tube unit and an at least one X-ray sensor unit so that the said least one X-ray sensor unit is arranged to detect an X-ray radiation transmitted by the said at least one X-ray tube unit.
From the said detected X-ray radiation data 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. The 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 liquid-liquid system inside the respective settler cell. Furthermore, the water content of organic phase at different heights and crud formation in the respective settler cell may be calculated based on the said image provided by said at least one X-ray measurement units 41-45.
Measuring the water content of the organic layer online gives an opportunity to follow the process behaviour in several settler cells, to detect abnormal situations and to make corrective actions in time. Online measurement will also give a long time average measurement result instead of an instantaneous indication. 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 thicknesses 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.
Figure 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 the 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. Likewise 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 according to the present invention comprises an at least one X-ray tube unit 47 attached before or after at least one first fence structure 20 of the 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 the said one or more double gate type fence structure 20-21 inside the settler 46, so that the said least one X-ray sensor unit 48 is arranged to detect an X-ray radiation transmitted by the said at least one X-ray tube unit 47, said X-ray radiation having travelled through the said one or more double gate type fence structure 20-21 inside the settler 46. Alternatively, an at least one X-ray sensor unit may be attached before or after at least one first fence structure 20 of the 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 the said one or more double gate type fence structure 20-21 inside the settler 46.
From the said detected X-ray radiation data 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 the said double gate type fence structure 20-21 inside the settler 46 based on the detected X-ray radiation data. Furthermore, from the said two- or three-dimensional image crud formation and scaling, on the said double gate type fence structure 20-21 can be detected.
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. 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 the 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. Likewise 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 according to the present invention comprises an at least one X-ray tube unit 50 attached to one first fence structure 20 inside at least one of the 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 the said one or more double gate type fence structure 20-21 inside the settler 49, so that the said least one X-ray sensor unit 51 is arranged to detect an X-ray radiation transmitted by the said at least one X-ray tube unit 50, said X-ray radiation having travelled upwards through the said one or more double gate type fence structure 20-21 inside the settler 49. Alternatively, an at least one X-ray sensor unit may be attached to one first fence structure 20 inside at least one of the 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 the said one or more double gate type fence structure 20- 21 inside the settler 49.
From the said detected X-ray radiation data a sensor data processing unitcan provide a two- or three-dimensional image related to the attenuation of X-rays by the liquid-liquid system traveling through the said double gate type fence structure 20-21 inside the settler 49 based on the detected X-ray radiation data. Furthermore, from the said two- or three-dimensional image crud formation on the said double gate type fence structure 20-21 can be detected.
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. 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 the 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 according to the present embodiment comprises an at least one movable X-ray measurement unit 52. The 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, the said at least one X-ray sensor unit 54 opposing the said at least one X-ray tube unit 53.
In the present embodiment the 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 the said at least one X-ray sensor unit 54 is arranged to detect X-ray radiation 59 travelling inside the settler cell 25.
In the settler cell 25 according to the present embodiment the X-rays from said at least one X-ray transmission source 55-58 of the 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. Furthermore, the said at least one X-ray transmission source 55-58 of the said X-ray tube unit 53 may be arranged to move or turn, e.g. horizontally, in order to transmit X-ray radiation in multiple directions. The said at least one movable X-ray measurement unit 52 according to the present embodiment may also be used together with the said one or more double gate type fence structure 20-21 where the 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.
In the embodiment presented in Figure 10 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 the 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, the 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.
The 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 the 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. Many hydrometallurgical liquid-liquid extraction processes include also some washing and scrubbing stages to remove impurity elements from the organic phase. Again furthermore, 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 insensitive 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.
With the help of the solution according to the present invention 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.
It will be obvious to a person skilled in the art that, as the technology advances, the inventive concept can be implemented in various ways. The invention and its embodiments are not limited to the examples described above but may vary within the scope of the claims.
Claims (24)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/FI2016/050920 WO2017109294A1 (en) | 2015-12-23 | 2016-12-23 | A method and an arrangement for monitoring of a hydrometallurgical liquid-liquid extraction process |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FI20156003 | 2015-12-23 |
Publications (2)
Publication Number | Publication Date |
---|---|
FI20156035A FI20156035A (en) | 2017-06-24 |
FI126880B true FI126880B (en) | 2017-07-14 |
Family
ID=59285522
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
FI20156035A FI126880B (en) | 2015-12-23 | 2015-12-30 | Method and Arrangements for Monitoring a Hydrometallurgical Liquid-Liquid Extraction Process |
Country Status (1)
Country | Link |
---|---|
FI (1) | FI126880B (en) |
-
2015
- 2015-12-30 FI FI20156035A patent/FI126880B/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
FI20156035A (en) | 2017-06-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Szymanowski | Hydroxyoximes and copper hydrometallurgy | |
Sarangi et al. | Separation of iron (III), copper (II) and zinc (II) from a mixed sulphate/chloride solution using TBP, LIX 84I and Cyanex 923 | |
Bonggotgetsakul et al. | Recovery of gold from aqua regia digested electronic scrap using a poly (vinylidene fluoride-co-hexafluoropropene)(PVDF-HFP) based polymer inclusion membrane (PIM) containing Cyphos® IL 104 | |
Marchese et al. | Transport of molybdenum with Alamine 336 using supported liquid membrane | |
Surucu et al. | Selective separation of cobalt and nickel by flat sheet supported liquid membrane using Alamine 300 as carrier | |
Annane et al. | Polymer inclusion membrane extraction of cadmium (II) with Aliquat 336 in micro-channel cell | |
KR20130041080A (en) | Method for recovering gold by solvent extraction | |
Torkaman et al. | Reactive extraction of cobalt sulfate solution with D2EHPA/TBP extractants in the pilot plant Oldshue–Rushton column | |
US20180282887A1 (en) | Solvent extraction and stripping system | |
Lin et al. | Mass-transfer in hollow-fiber modules for extraction and back-extraction of copper (II) with LIX64N carriers | |
Gameiro et al. | Extraction of copper from ammoniacal medium by emulsion liquid membranes using LIX 54 | |
CN103459622A (en) | Extraction of gold | |
Shakib et al. | The performance of pulsed scale-up column for permeable of selenium and tellurium ions to organic phase, case study: Disc and doughnut structure | |
Jantunen et al. | Removal and recovery of arsenic from concentrated sulfuric acid by solvent extraction | |
Sole | Solvent extraction in the hydrometallurgical processing and purification of metals: process design and selected applications | |
Aktas | Cementation of rhodium from waste chloride solutions using copper powder | |
Artzer et al. | Removal of antimony and bismuth from copper electrorefining electrolyte: Part II—An investigation of two proprietary solvent extraction extractants | |
Pandey et al. | Recovery of Hf and Zr from slurry waste of zirconium purification plant using solvent extraction | |
Liu et al. | Enhancing the separation performance of vanadium from a black shale leaching solution by supported liquid membrane using trialkylamine | |
Estay et al. | Enhancing the effectiveness of copper and cyanide recovery in gold cyanidation: A new integrated membrane process | |
FI126880B (en) | Method and Arrangements for Monitoring a Hydrometallurgical Liquid-Liquid Extraction Process | |
Jantunen et al. | Separation of zinc and iron from secondary manganese sulfate leachate by solvent extraction | |
Cole et al. | Understanding aqueous-in-organic entrainment in copper solvent extraction | |
WO2017109294A1 (en) | A method and an arrangement for monitoring of a hydrometallurgical liquid-liquid extraction process | |
US5000927A (en) | Method of regulating a purex solvent extraction process |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
FG | Patent granted |
Ref document number: 126880 Country of ref document: FI Kind code of ref document: B |
|
MM | Patent lapsed |