WO2013191020A1 - 高圧酸浸出工程におけるオートクレーブ装置 - Google Patents
高圧酸浸出工程におけるオートクレーブ装置 Download PDFInfo
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- WO2013191020A1 WO2013191020A1 PCT/JP2013/065959 JP2013065959W WO2013191020A1 WO 2013191020 A1 WO2013191020 A1 WO 2013191020A1 JP 2013065959 W JP2013065959 W JP 2013065959W WO 2013191020 A1 WO2013191020 A1 WO 2013191020A1
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- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/006—Baffles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0223—Moving bed of solid material
- B01D11/0234—Moving bed of solid material using other slow rotating arms or elements, whereby the general transport direction of the solids is not parallel to the rotation axis, e.g. perpendicular
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0253—Fluidised bed of solid materials
- B01D11/0257—Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
- B01F33/813—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles mixing simultaneously in two or more mixing receptacles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/50—Mixing receptacles
- B01F35/52—Receptacles with two or more compartments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- 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
- C22B3/02—Apparatus therefor
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- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
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- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
- B01J2219/00763—Baffles
- B01J2219/00765—Baffles attached to the reactor wall
- B01J2219/00768—Baffles attached to the reactor wall vertical
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/182—Details relating to the spatial orientation of the reactor horizontal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/19—Details relating to the geometry of the reactor
- B01J2219/194—Details relating to the geometry of the reactor round
- B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
- B01J2219/1943—Details relating to the geometry of the reactor round circular or disk-shaped cylindrical
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present invention relates to an autoclave apparatus through which a sulfide material continuously passes in a high-pressure acid leaching process of nickel oxide ore. More specifically, in an autoclave used for high-pressure acid leaching of nickel oxide ore, the inside of the autoclave is divided into a plurality of chambers by partition walls, and when performing an operation in which the charge is leached while being sequentially transferred through each chamber, The present invention relates to a technique capable of maintaining the same leaching rate as before even if the amount of free sulfuric acid, which is the control value of the autoclave final solution, is reduced by defining the position of the liquid passage port provided in the partition wall.
- This application claims priority in Japan based on Japanese Patent Application No. 2012-137883 filed on June 19, 2012 and Japanese Patent Application No. 2012-260294 filed on November 28, 2012 This application is incorporated herein by reference.
- HPAL high pressure acid leaching
- this method does not include dry processes such as reduction and drying processes, and is a consistent wet process. It has the advantage of being advantageous. That is, in the high-pressure acid leaching method, iron as the main impurity is leached in the form of hematite (Fe 2 O 3 ) by controlling the oxidation-reduction potential and temperature of the leaching solution in the pressure leaching reactor in the leaching step. By fixing to the residue, nickel and cobalt can be leached selectively with respect to iron, so that there is a very great merit.
- a high-pressure acid leaching method using an autoclave is adopted as a wet smelting method of nickel oxide ore.
- a pretreatment step (1), a high pressure acid leaching step (2), and a solid-liquid separation step (3) The neutralization process (4), the dezincification process (5), the sulfurization process (6), and the detoxification process (7) are included (for example, refer patent document 1).
- the nickel oxide ore is pulverized and classified using a pulverization facility and a sieving facility to prepare a raw slurry having a predetermined slurry concentration containing ores of 2 mm or less.
- the raw slurry is supplied to the next high pressure acid leaching step (2).
- the raw material slurry obtained in the pretreatment step (1) is heated and boosted stepwise by a pre-heater (temperature rising / pressurizing equipment) and then supplied to the autoclave.
- a pre-heater temperature rising / pressurizing equipment
- sulfuric acid that has been heated and increased in pressure is added to the raw material slurry, and stirred at 220 to 280 ° C., the valuable metal is leached at high pressure under high pressure.
- the leaching slurry of the valuable metal obtained in the leaching step (2) is subjected to solid-liquid separation, and the leaching solution (crude nickel sulfate aqueous solution) containing nickel and cobalt as the valuable metals and the leaching residue are obtained. obtain.
- the leachate obtained in the solid-liquid separation step (3) is neutralized.
- step (6) hydrogen sulfide gas is added to the final zinc removal solution obtained in the dezincification step (5) to obtain a nickel / cobalt composite sulfide and a nickel poor solution.
- the leaching residue generated in the solid-liquid separation process (3) and the nickel poor liquid generated in the sulfidation process (6) are detoxified.
- the heated and pressurized raw slurry and sulfuric acid are supplied to the first compartment in the autoclave divided into a plurality of partitions, and the first compartment is prepared.
- the leaching proceeds with stirring by the agitator, and the slurry is transferred to the second compartment and beyond by overflow or the like, and the leaching is further advanced in the same manner sequentially.
- the slurry that overflows and the slurry at the bottom of each chamber usually have a difference in the residence time in the chamber, although it depends on the state of slurry flow in the chamber by stirring. Therefore, by transferring the overflow slurry and the bottom slurry in a balanced manner to the next room, the balance of the residence time is balanced, and the overall residence time is averaged, aiming for efficient operation. Yes.
- the slurry in each chamber is supplied to the last chamber in order to continue the slurry discharge from the autoclave as much as possible as a role of the liquid inlet when the operation is urgently stopped due to some trouble rather than the steady operation. It is possible to make it possible.
- the amount of slurry discharged from the autoclave is controlled to be kept at the set liquid level of the autoclave by a valve installed between the autoclave and the flash vessel. If the slurry supply to the autoclave is stopped due to some trouble, it is necessary to close the discharge valve to keep the autoclave liquid level, but once the discharge valve is fully closed, to open the discharge valve again. In order to prevent equipment damage due to rapid evaporation in the discharge pipe and in the flash tank, it is necessary to lower the temperature and pressure in the autoclave much more than the normal operation.
- the size of the liquid inlet is made as small as possible in order to maintain the overflow state in which the overflow slurry and the bottom slurry are transferred to the next room in a well-balanced manner.
- This problem has the effect of lowering the overall leaching rate of the autoclave, which is commensurate with the valuable metals contained in the raw slurry in order to maintain a predetermined leaching rate in operation (usually 90 to 95%).
- Excess sulfuric acid is charged in the autoclave compared to the amount.
- the amount of free sulfuric acid (unreacted sulfuric acid remaining in the leachate) is controlled, and this value is usually about 50 to 55 g / L.
- external heating or cooling can be carried out by means such as maintaining a reactive slurry having a volume 50 to 200% larger than the volume of the reactive slurry contained in any of the downstream compartments.
- a technique for maintaining the optimum temperature condition without performing the process see, for example, Patent Document 3).
- Patent Document 3 is intended for sulfide raw materials, and the disclosed technique of Patent Document 4 requires a normal pressure leaching process, and thus cannot be applied to the above problems.
- an opening for a manway that is used when a worker inspects the interior of the autoclave such as a periodic inspection is provided in each partition wall. Is closed by a door.
- the slurry transfer port is provided with a slurry transfer port door as a set in the manway door member, and the manway door is closed during normal operation. The door for the slurry transfer port is opened and used.
- the manway is used when workers check the inside of the autoclave during regular inspections, etc.
- the inside bottom of the autoclave is the least inclined as a foothold in the inside of the autoclave, so the manway door is provided near the center bottom of the bulkhead. ing. Therefore, it is common to provide the door for the slurry transfer port at the center bottom of the partition wall.
- JP-A-2005-350766 JP 2003-84220 A Japanese Patent Publication No. 07-084623 Special table 2009-515044 gazette
- An object of the present invention is to provide an autoclave device capable of promoting efficient operation and reducing the control value of free sulfuric acid concentration after discharge in the high-pressure acid leaching process in view of the conventional problems as described above. There is to do.
- Another object of the present invention is to provide an autoclave apparatus having a slurry transfer port that can function as a manway in a partition wall while ensuring overflow in a high-pressure acid leaching process.
- the present inventors have found the effective installation position of the slurry transfer port provided in the partition wall of the autoclave by examining the flow rate (stirring pressure) of each indoor slurry by stirring.
- the autoclave device has been completed, which can promote efficient operation by averaging the residence time and reduce the control value of the free sulfuric acid concentration after discharge.
- the present invention advances the leaching by agitating the heated and pressurized raw material slurry and sulfuric acid with a stirrer provided in each compartment in the autoclave partitioned into a plurality of partitions, and the upstream partition.
- a stirrer provided in each compartment in the autoclave partitioned into a plurality of partitions, and the upstream partition.
- It is an autoclave device in a high-pressure acid leaching process in which slurry is transferred from a chamber to a downstream compartment and the leaching proceeds in sequence, and each partition wall can be opened and closed by a slurry transfer opening door.
- a fluid passage port is provided, and the slurry transport passage port has a height from the lowest part of the autoclave to the center of gravity of the slurry transport passage door being 0.1 to 0.3 times the autoclave diameter,
- the distance from the center line of the partition wall to the center of gravity of the fluid transfer door for transferring the slurry is set at a position 0.05 to 0.25 times the diameter of the autoclave and does not reach the end of the partition wall. Characterized in that it.
- each of the partition walls is provided with the slurry transfer port at the downstream position in the stirring direction of the slurry by the stirrer in the upstream compartment. be able to.
- the slurry transfer port may be a rectangular opening that does not reach the end of the partition wall.
- the slurry transfer port may be installed at a door of the manway opening.
- the slurry transfer port may be a rectangular opening of 30 to 50 cm square.
- a notch portion that allows an overflow amount to be adjusted by an installation height position of the adjustment plate may be provided at an upper end portion of the partition wall.
- the downstream partition has a ratio of the amount of liquid passing through the notch portion and the amount of liquid passing through the slurry transfer port, 55:45, and the other partitions are notches.
- the ratio of the amount of liquid passing through the section and the amount of liquid passing through the slurry transfer port can be 84:16, and can be operated at a flow rate of 500 m 3 / hour.
- the mixing of the raw slurry and sulfuric acid can be promoted, and the control value of the free sulfuric acid concentration after discharge can be reduced.
- FIG. 1 is a diagram showing a configuration example of a main part of an autoclave apparatus to which the present invention is applied.
- FIG. 1A is a cross-sectional plan view schematically showing an internal structure by horizontally cutting the autoclave apparatus.
- FIG. 3B is a longitudinal side view schematically showing the internal structure of the autoclave apparatus cut vertically along the line BB shown in FIG.
- FIG. 2 is a longitudinal front view schematically showing the internal structure of the autoclave apparatus cut vertically along the line AA shown in FIG. 1 (A).
- FIG. 3 is a longitudinal front view schematically showing another installation example of a manway opening and a slurry transfer port.
- FIG. 4 is a schematic diagram showing a simulation result of indoor convection in the autoclave apparatus.
- FIG. 1A is a cross-sectional plan view schematically showing an internal structure by horizontally cutting the autoclave apparatus.
- FIG. 3B is a longitudinal side view schematically showing the internal structure of the autoclave apparatus cut vertically
- FIG. 5 is a diagram schematically showing the state of slurry transfer in the autoclave apparatus.
- FIG. 6 is a schematic diagram showing the result of simulating the distribution of the pressure difference between the tanks (first tank-second tank) in the autoclave apparatus.
- FIG. 7 is a process diagram showing a leaching procedure of nickel and cobalt by high pressure acid leaching of nickel oxide ore.
- the present invention is implemented by an autoclave apparatus 100 having a structure as shown in FIGS. 1 and 2, for example.
- FIG. 1 is a diagram showing a configuration example of a main part of an autoclave device 100.
- FIG. 1A is a cross-sectional plan view schematically showing an internal structure by horizontally cutting the autoclave device 100
- FIG. FIG. 3 is a longitudinal side view schematically showing the internal structure of the autoclave device 100 cut perpendicularly along the line BB shown in FIG. 2.
- FIG. 2 is a longitudinal front view schematically showing the internal structure of the autoclave apparatus 100 cut vertically along the line AA shown in FIG. 1 (A).
- This autoclave apparatus 100 is an autoclave apparatus in a high-pressure acid leaching process in which heated and pressurized raw material slurry and sulfuric acid are stirred to leach valuable metals at high temperature and pressure, and is a horizontally installed cylindrical autoclave body.
- 110 includes a plurality of compartments 20A, 20B,... 20G that are partitioned by partition walls 10A, 10B,... 10F, and agitators 30A, 30B,. is set up.
- the raw slurry and sulfuric acid are mixed by the stirrers 30A, 30B,... 30G provided in each of the compartments 20A, 20B,.
- the leaching is advanced by agitating the slurry, the slurry is transferred from the upstream compartment to the downstream compartment, and the leaching is advanced sequentially.
- the autoclave main body 110 includes two raw material slurry supply pipes 1A and 1B each having a raw material slurry discharge port around a stirring blade of a stirrer 30A provided in the upstreammost compartment 20A.
- Two sulfuric acid supply pipes 2A and 2B having outlets are alternately arranged.
- the raw material slurry outlet and the sulfuric acid outlet are higher than the uppermost part of the stirring blade and lower than the content liquid level L.
- the partition chamber 20A is provided with a high-pressure steam supply pipe 3 having a high-pressure steam discharge port in the vicinity of the partition wall 10A.
- a sulfuric acid supply pipe 4 having a sulfuric acid discharge port is provided in the vicinity of a stirring blade of a stirrer 30B provided in the next compartment 20B.
- a PSV vent pipe 5 having a suction port is provided in the vicinity of the stirring blade of the stirrer 30F provided in the compartment 20F on the downstream end side.
- a TAIL gas vent pipe 6 having a suction port, a slurry extraction pipe 7 having a slurry extraction port, and a spare pipe 8 are provided around the stirring blades of the stirrer 30G provided in the most downstream compartment 20G. ing.
- Each pipe is inserted into the autoclave main body 110 from above.
- stirrers 30A, 30B,... 30G provided in the compartments 20A, 20B,... 20G rotate clockwise, respectively, to form a downward flow of slurry.
- a manhole 41 closed by an opening / closing lid is provided on the floor wall portion in the vicinity of the partition wall 10A.
- a manhole 42 closed by an opening / closing lid is provided on the floor wall portion in the vicinity of the partition wall 10F.
- the most downstream compartment 20G is provided with a manhole 43 that is closed by an open / close lid on the ceiling near the partition wall 10F.
- the autoclave main body 110 in the autoclave apparatus 100 has a capacity of about 1000 m 3 in a shape in which both ends of a cylindrical body having a diameter D of about 5500 mm and a total length L of about 35000 mm are closed by a hemisphere.
- the autoclave main body 110 is provided with manway openings 50A, 50B,... 50F, which are used when workers check the inside of the autoclave, such as periodic inspections, in the partition walls 10A, 10B,.
- the doors 51A, 51B,... 51F for closing the manway openings 50A, 50B,... 50F are provided with the liquid passing ports 52A, 52B,.
- the above-mentioned slurry transfer ports 52A, 52B,... 52F are opened and closed by opening / closing lids (not shown), and the manway openings 50A, 50B,. It is closed with 51A, 51B ... 51F, and the doors of the fluid passing ports 52A, 52B ... 52F for slurry transfer are opened and used.
- the manway openings 50A, 50B,... 50F are installed in the center, and only the slurry transfer ports 52A, 52B,. You may set it off from.
- each of the partition walls 10A, 10B,..., 10F in the autoclave main body 110 can be adjusted in the overflow amount according to the installation height position of the adjustment weir plate 11C as in the partition wall 10C shown in the longitudinal front view of FIG.
- the notch portion 12C is provided at the upper end portion.
- FIG. 4 shows the convection simulation result in the autoclave chamber.
- the convection velocity is fast in the right direction in the figure regardless of the position of the slurry transfer opening.
- FIG. 4 shows slurry streamlines in the vicinity of the partition walls. This indicates that the red line R has more slurry with a shorter residence time than the blue line B.
- the slurry transfer liquid inlets 52A, 52B,... 52F are caused to rotate in the respective compartments 20A, 20B,. Since it is provided at a position away from the center line of the autoclave main body 110 by shifting to the downstream side of the flow, the pressure applied to the partition generated by the flow of the slurry is lower than that in the prior art, and the slurry is supplied to the slurry transfer liquid passage 52A. , 52B... 52F is not dominant and can be balanced with the overflow transfer.
- the predetermined leach rate of 90 to 95% could not be maintained. Even if it is controlled to 45 to 50 g / L, it is possible to maintain a predetermined leaching rate.
- the transfer amount from the slurry transfer ports 52A, 52B,... 52F is controlled by reducing the opening area without changing the position of the slurry transfer ports 52A, 52B,.
- the effect is small and the balance cannot be maintained. It is a slurry that becomes a target in the operation of nickel oxide ore, and when stirring necessary for leaching is performed, it is considered that the pressure applied to the center exceeds the range that can be controlled by adjusting the area of the opening.
- the positions of the slurry transfer ports 52A, 52B,... 52F are moved from the center as in the autoclave apparatus 100, the controllable low pressure is obtained, so the opening area is the slurry to be transferred to the next room. What is necessary is just to adjust suitably according to the ratio of the quantity, ie, the amount of slurry overflow, and the ratio of the slurry quantity which passes the liquid flow port for slurry transfer.
- the overflow amount can be adjusted by the installation height position of the adjustment weir plate at 12A, 12B... 12F provided at the upper end of each partition wall 10A, 10B.
- the opening areas of the liquid inlets 52A, 52B,... 52F are constant.
- the downstream partition 10F has a ratio of the amount of slurry passing through the notch portion 12F and the amount of slurry passing through the slurry transfer port 52F to 55:45.
- the other partition walls 10A, 10B,... 10E include an overflow amount of the slurry passing through the notches 12A, 12B,... 12E and an amount of slurry passing through the slurry transfer liquid passing ports 52A, 52B,.
- the slurry transfer liquid passage ports 52A, 52B,... 52F are installed on the side where the discharge port of the steam pipe is located, the temperature becomes higher than the surroundings due to the steam, and the slurry for preventing the temperature drop in each chamber is next. Since it will be transferred to a chamber, it is not preferable.
- the shape of the slurry transfer liquid passage ports 52A, 52B,... 52F is not particularly limited except that the adjusted area is used, but it is preferable to have a shape that does not reach the end of the partition wall. A reduction in the fixing strength of the partition wall can be prevented when it reaches the end of the partition wall, that is, when the end of the partition wall body is firmly fixed to the autoclave wall surface.
- FIG. 6 is a schematic diagram showing the result of simulating the distribution of the pressure difference between the tanks (first tank-second tank) by performing a fluid analysis when the port is provided in the partition wall.
- a region A1 from yellow to red indicates a place where the pressure on the first tank side is high, and tends to easily flow from the first tank to the two tanks.
- the light blue to brown and blue region A2 has a small pressure difference and is difficult to flow from the first tank to the second tank.
- the gray to black region indicates that the pressure difference is reversed, and the reddish pink region A3 indicates that the pressure difference is zero, that is, a balanced state.
- the area around the calculated position of the slurry transfer opening is a distribution area A1 of a yellow color (that is, a pressure difference of about 1400 Pa at the maximum), and is an area that easily flows from the first tank to the second tank. ing.
- the pressure difference at this location is about 600 Pa at maximum, which is a half of the initial position.
- the region with a small pressure difference is distributed at a height of 100 ⁇ 20 cm from the bottom and 50 cm away from the center of the partition wall, and it is desirable to install a slurry transfer port at this position.
- the height from the lowest part of the autoclave to the center of gravity of the slurry transfer passage door is 0.1 to 0.3 times the autoclave diameter D or less.
- the distance from the center line of the partition wall to the center of gravity of the slurry transfer passage door is 0.05 to 0.25 times the autoclave diameter D, and the shape does not reach the end of the partition wall. It was supposed to have.
- the direction deviating from the center is the left when facing the partition wall from the downstream compartment if the rotation direction of the stirrer is right rotation. The reverse is true when the stirrer rotates counterclockwise. At this time, the rotation direction of the stirrer in each compartment is the same direction. That is, each partition wall is provided with the above-described slurry transfer port at a downstream position in the agitating direction of the slurry by the agitator in the upstream compartment.
- the shape of the slurry transfer ports 52A, 52B,... 52F is not particularly limited, but is preferably rectangular because processing is easy.
- the slurry transfer port is provided in a region having a small pressure difference, thereby ensuring an overflow even when the shape is large, and by forming a rectangular opening of 30 cm square to 50 cm square, It functions as a manway while ensuring overflow.
- the slope is gentle at the lowest part of the autoclave, it is also a place where the leach residue is most likely to accumulate even if the slurry is discharged because the worker enters the inside, so it is preferable to prepare the above countermeasures, so that a preferable work situation Can be produced.
- Example 1 The autoclave was operated at a pressure of 4.7 MPaG, a temperature of 250 ° C., an Ni grade in the ore of 1.0 to 1.4% by weight, and an amount of slurry flowing into the autoclave of about 300 to 700 m 3 / hour.
- HPAL operation was performed using the autoclave apparatus 100 to which the present invention was applied.
- the leaching rate of nickel was 92.5%.
- the free sulfuric acid in the leachate could be managed at 45 to 50 g / L.
- Example 1 The present invention is not applied, and the HPAL operation is performed using the autoclave apparatus having a conventional structure in which the partition walls 10A, 10B,. The same operation as in Example 1 was performed except that the operation was performed.
- the leaching rate of nickel was 92.0%.
- the free sulfuric acid in the leachate could not be operated unless it was controlled at 50 to 55 g / L.
- Example 2 In the autoclave apparatus 100 divided into 7 tanks by a diameter of 6 m, a total length of 40 m, and partition walls 10A, 10B,... 10F, each partition wall 10A, 10B,.
- the slurry transfer ports 52A, 52B,... 52F were installed at positions 50 cm away on the downstream side of the rotation and operated in an overflow state.
- the leaching rate of nickel was 92.0%, which was a good result.
- Example 2 The operation was performed in the same manner as in Example 2 except that a slurry transfer port was provided at a position 50 cm away from the upstream side in the rotation direction of the stirring blade (clockwise as viewed from above).
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Abstract
Description
オートクレーブ装置内の圧力が4.7MPaG、温度が250℃、鉱石中のNi品位が1.0~1.4重量%、オートクレーブへのスラリー流入量が300~700m3/時間程度の操業を行った。
本発明を適用せず、上記オートクレーブ装置100における各隔壁10A,10B・・・10Fをオートクレーブ本体110の中心線から間隔C=0としたものに置き換えた従来構造のオートクレーブ装置を用いてHPAL操業を行った以外は、実施例1と同様に操業した。
直径6m、全長40m、隔壁10A,10B・・・10Fにより7槽に分割されたオートクレーブ装置100において、各隔壁10A,10B・・・10Fに最下部から100cmの高さで、隔壁中央から撹拌翼回転の下流側に50cm離れた位置に上記スラリー移送用通液口52A,52B・・・52Fを設置し、オーバーフローの状態で操業した。
撹拌翼の回転方向(上から見て時計回り)の上流側に50cm離れた位置にスラリー移送用通液口を設置した以外は、実施例2と同様に操業した。
Claims (5)
- 加熱、加圧された原料スラリー及び硫酸を、隔壁で複数に区画されたオートクレーブ内の各区画室に備えられた撹拌機によって撹拌することにより浸出を進行させ、上流側の区画室から下流側の区画室にスラリーを移送し、順次、浸出を進行させる高圧酸浸出工程におけるオートクレーブ装置であって、
各隔壁には、それぞれスラリー移送用通液口扉により開閉自在なスラリー移送用通液口が設けられ、
上記スラリー移送用通液口は、オートクレーブ最低部からスラリー移送用通液口扉の重心までの高さがオートクレーブ直径の0.1倍~0.3倍であって、隔壁の中心線からスラリー移送用通液口扉の重心までの距離がオートクレーブ直径の0.05倍~0.25倍の位置に設置され、隔壁の端部に届かない形状を有する
ことを特徴とするオートクレーブ装置。 - 上記各隔壁には、それぞれ上流側の区画室における撹拌機によるスラリーの撹拌方向の下流側の位置に、上記スラリー移送用通液口が設けられていることを特徴とする請求項1に記載のオートクレーブ装置。
- 上記スラリー移送用通液口は、隔壁の端部に届かない矩形状の開口であることを特徴とする請求項1又は請求項2に記載のオートクレーブ装置。
- 上記スラリー移送用通液口は、マンウェイ開口部の扉に設置されることを特徴とする請求項3に記載のオートクレーブ装置。
- 上記スラリー移送用通液口は、30cm角~50cm角の矩形状の開口であることを特徴とする請求項3に記載のオートクレーブ装置。
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CA2876915A CA2876915C (en) | 2012-06-19 | 2013-06-10 | Autoclave apparatus used during high-pressure acid leaching process |
US14/406,492 US9732400B2 (en) | 2012-06-19 | 2013-06-10 | Autoclave apparatus used during high-pressure acid leaching process |
AU2013278507A AU2013278507B2 (en) | 2012-06-19 | 2013-06-10 | Autoclave apparatus used during high-pressure acid leaching process |
EP13807230.1A EP2862951B1 (en) | 2012-06-19 | 2013-06-10 | Autoclave apparatus used during high-pressure acid leaching process |
PH12014502773A PH12014502773A1 (en) | 2012-06-19 | 2014-12-10 | Autoclave apparatus used during high-pressure acid leaching process |
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