JP2014088620A - Autoclave apparatus in high-pressure acid leaching step - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an autoclave which can be efficiently operated and reduces the control value of a free sulfuric acid concentration after discharge in a high-pressure acid leaching step of a nickel oxidized ore.SOLUTION: Each partition wall of an autoclave apparatus 100 in a high-pressure acid leaching step of allowing leaching of heated and pressurized raw material slurry and sulfuric acid to proceed by stirring machines 30A to G included in each of compartments 20A to G in an autoclave body 110 sectioned into plural compartments with partition walls 10A to F is provided with feeding liquid ports 52A to F for transporting slurry which are allowed to be reclosable by feeding liquid port doors 51A to F for transporting slurry. The feeding liquid port for transporting slurry is placed at a position where a height from the bottom of the autoclave to the center of the gravity of each feeding liquid port door for transporting slurry is 0.1 time to 0.3 time the diameter of the autoclave and a distance from the central line of each partition wall to the center of the gravity of each feeding liquid port door for transporting slurry is 0.05 time to 0.25 time the diameter of the autoclave. The upper ends of the partition walls are provided with notches 12A to F which adjust an overflow amount.

Description

  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.

In recent years, due to the development of materials with effective corrosion resistance under high temperature and high pressure, high pressure acid leaching (HPAL) using sulfuric acid has attracted attention as a hydrometallurgical method for nickel oxide ore. ing. Unlike the conventional dry smelting method, which is a conventional nickel oxide ore smelting method, 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, which is the main impurity, is leached in the form of hematite (Fe ₂ O ₃ ) by controlling the redox 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.

  For example, a high-pressure acid leaching method using an autoclave is adopted as a wet smelting method of nickel oxide ore.

  In the high pressure acid leaching method for obtaining the nickel / cobalt mixed sulfide, for example, as shown in FIG. 7, 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).

  In the pretreatment step (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).

  In the 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. Similarly, 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 with high-temperature and pressurized acid, and the resulting leached slurry is cooled and depressurized to normal temperature and normal pressure with a flash vessel.

  In the solid-liquid separation step (3), 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.

  In the neutralization step (4), the leachate obtained in the solid-liquid separation step (3) is neutralized.

  In the zinc removal step (5), hydrogen sulfide gas is added to the leachate neutralized in the neutralization step (4) to precipitate and remove zinc as zinc sulfide.

  In the sulfidation 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.

  In the detoxification step (7), the leaching residue generated in the solid-liquid separation step (3) and the nickel poor solution generated in the sulfidation step (6) are detoxified.

  Here, in the autoclave in the high-pressure acid leaching step (2), 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.

  By the way, when the slurry is transferred to the next room in the autoclave, the slurry is transferred by overflowing the upper part of the partition wall, and is also transferred through a liquid passage port provided at the lower part of the partition wall (see, for example, Patent Document 2). ).

  There is usually a difference in the residence time between the overflowed slurry and the slurry at the bottom of each chamber, depending 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.

  In addition, 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 maintained 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.

  When this operation is performed, it takes a long time to return to normal operation, which results in a significant loss of operating time. Therefore, even if it stops urgently, the discharge valve is not fully closed, and the slurry inside the autoclave is continuously discharged at a very small flow rate. At this time, the liquid passage ports are provided so that the slurry in each chamber can be supplied to the last chamber through the liquid passage ports and the slurry discharge can be maintained as much as possible.

  Therefore, in steady 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. For this purpose, it is an important point in design to make the size of the liquid passage as large as possible, and it is appropriately adjusted according to the flow rate in actual operation and the size of the autoclave.

  However, this balance is lost, the slurry transfer from the liquid passage port provided at the lower part of the partition wall becomes dominant, and the slurry transfer from the overflow may be almost lost, and the slurry residence time is biased toward the bottom part. Therefore, there is a problem that efficient operation is hindered.

  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 the predetermined leaching rate in operation (usually 90 to 95%). Excess sulfuric acid is charged in the autoclave compared to the amount. In order to maintain this operation, 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.

  In addition, since the leachate obtained in the solid-liquid separation step (3) is neutralized in the next neutralization step (4), free sulfuric acid is neutralized without contributing to the leaching, so it is unnecessary. Moreover, since the cost of the neutralizing agent for neutralization is required, there is a problem that the amount of free sulfuric acid is desired to be reduced as much as possible. However, the present situation is that the above-mentioned free sulfuric acid is used to maintain a predetermined leaching rate. It is a situation that must be made in quantity.

  For example, in the first compartment in the autoclave, 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. There has been proposed a technique for maintaining the optimum temperature condition without performing the process (see, for example, Patent Document 3).

  In addition, a technique has been proposed in which sulfuric acid is regenerated and the amount of added sulfuric acid is reduced by a combined implementation of two or more successive leaching stages, including a normal pressure leaching stage and a pressure leaching stage. (For example, refer to Patent Document 4).

  However, the disclosed technique of Patent Document 3 is intended for sulfide raw materials, and the disclosed technique of Patent Document 4 requires an atmospheric pressure leaching process, and thus cannot be applied to the above problems.

  In addition, in an autoclave device divided into a plurality of partitions by a partition wall, 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.

  In consideration of the strength of the partition wall, 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 device 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.

  Other objects of the present invention and specific advantages obtained by the present invention will become more apparent from the description of embodiments described below.

  In order to achieve the above object, 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.

  That is, 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. 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 liquid passage port is provided, and the height of the slurry transfer passage port from the lowest part of the autoclave to the gravity center of the slurry transfer passage port is 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. , The upper end of the partition wall, wherein the notch portion and adjustable overflow amount by setting height position of the adjusting plate is provided.

In the autoclave according to the present invention, the downstream partition has a ratio of the amount of liquid passing through the notch and the amount of liquid passing through the slurry transfer opening of 55:45, and the other partitions pass through the notch. The ratio between the amount of liquid to be transferred and the amount of liquid passing through the slurry transfer opening may be 84:16 and operated at a flow rate of 500 m ³ / hour.

  In the autoclave apparatus according to the present invention, 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.

  In the autoclave apparatus according to the present invention, the slurry transfer port may be a rectangular opening that does not reach the end of the partition wall.

  Moreover, the autoclave apparatus which concerns on this invention WHEREIN: The said fluid transfer opening for slurry transfer shall be installed in the door of a manway opening part.

  Moreover, the autoclave apparatus which concerns on this invention WHEREIN: The said fluid transfer port for slurry transfer shall be a rectangular opening of 30 cm square-50 cm square.

  According to the present invention, in the high-pressure acid leaching step, mixing of the raw slurry and sulfuric acid can be promoted, and the management value of the free sulfuric acid concentration after discharge can be reduced.

BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows the principal part structural example of the autoclave apparatus to which this invention is applied, (A) is the cross-sectional top view which showed the internal structure typically by cut | disconnecting an autoclave apparatus horizontally, (B) is a figure showing an autoclave apparatus FIG. 3 is a longitudinal side view schematically showing an internal structure by cutting vertically along a line BB shown in FIG. FIG. 2 is a longitudinal sectional front view schematically showing the internal structure of the autoclave device cut vertically along the line AA shown in FIG. It is the vertical front view which showed typically the other example of installation of the opening for manways, and the liquid passing port for slurry transfer. It is a schematic diagram which shows the simulation result of the indoor convection in the said autoclave apparatus. It is a figure which shows typically the transfer state of the slurry in the said autoclave apparatus. It is a schematic diagram which shows the result of having simulated the distribution of the pressure difference (1st tank-2nd tank) between the tanks in the said autoclave apparatus. It is process drawing which shows the leaching procedure of nickel and cobalt by the high pressure acid leaching method of nickel oxide ore.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

  The present invention is implemented by an autoclave apparatus 100 having a structure as shown in FIGS. 1A and 1B and FIG.

  FIG. 1 is a diagram illustrating an exemplary configuration of a main part of an autoclave apparatus 100. FIG. 1A is a cross-sectional plan view schematically showing an internal structure by horizontally cutting the autoclave apparatus 100, and FIG. FIG. 3 is a longitudinal side view schematically showing the internal structure by cutting vertically along the line BB shown in FIG. 2. FIG. 2 is a longitudinal sectional front view schematically showing the internal structure of the autoclave device 100 cut vertically along the line AA shown in FIG.

  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. In the autoclave apparatus 100, 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. Further, 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.

  Further, 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.

  Further, 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.

  Moreover, in this autoclave apparatus 100, each stirrer 30A, 30B ... 30G with which each compartment 20A, 20B ... 20G was each rotated clockwise, and forms the downward flow of a slurry.

  Further, the uppermost end compartment 20A of the autoclave apparatus 100 is provided with a manhole 41 closed on the floor wall portion near the partition wall 10A by an open / close lid. Further, in the compartment 20F on the downstream end side, a manhole 42 closed by an opening / closing lid is provided on the floor wall portion in the vicinity of the partition wall 10F. Further, 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.

Here, 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.

  Here, the slurry transfer ports 52A, 52B,... 52F provided in the partition walls 10A, 10B,... 10F in the autoclave main body 110 can flow about 10% to 45% with respect to the total flow rate. It is formed in a shape that does not reach the end of the partition wall in size. .. 52F for the slurry transfer in the autoclave apparatus 100 are representative of the partition walls 10A, 10B,... 10F, as shown in the longitudinal front view of FIG. A rectangular shape having a height of 170 mm and a width of 240 having a center of gravity at a position where the distance C = 600 mm from the center line of FIG.

  Further, the manway openings 50A, 50B,... 50F are arranged in the center as much as possible without interfering with the pipes inserted into the respective compartments 20A, 20B,. It is a rectangle with a height H580 mm and a width W 600 mm with the position of the center of gravity at a position H2 = 890 mm from the bottom.

  As shown in FIG. 3, 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.

  Further, 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.

  In this autoclave apparatus 100, the convection simulation result in the autoclave chamber is shown in FIG. 4 for the slurry flow in each of the compartments 20A, 20B... 20G generated by the clockwise rotation of the stirrers 30A, 30B. As shown in the schematic diagram (color drawing is submitted as reference figure 1), there is a bias, and the convection speed is fast in the right direction of the figure regardless of the position of the slurry transfer opening. The color drawing in Reference FIG. 1 shows slurry streamlines in the vicinity of the partition walls. The red line indicates that there is more slurry with a shorter residence time than the blue line.

  In this autoclave apparatus 100, 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.

  For this reason, conventionally, if the free sulfuric acid concentration of the leachate is not 50 to 55 g / L, the predetermined leach rate 90 to 95% could not be maintained. Even if it manages to 50-50 g / L and a half, a predetermined | prescribed leaching rate can be maintained.

  Here, 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,. However, even if the opening is narrowed, 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.

  If 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.

  In this autoclave device 100, 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.

In this autoclave apparatus 100, as shown in FIG. 5, 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,. When the ratio was 84:16 and the operation was performed at a flow rate of 500 m ³ / hour, the overflow amount of the slurry was surely maintained, the residence time of the slurry was increased by 20%, and the required free sulfuric acid concentration was reduced to about It was possible to manage and operate in a state reduced to 45 g / L.

  When 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 for the adjusted area, but is preferably 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.

  Here, in a two-tank model in which one tank and two tanks are connected via a partition wall having a diameter of 6 m, the slurry is passed through so as to be located downstream in the stirring direction of the slurry by the stirrer in the first tank on the upstream side. A fluid analysis is performed when the port is provided in the partition wall, and the result of simulating the distribution of the pressure difference between the tanks (first tank-second tank) is presented as a schematic diagram of FIG. ). In the color drawing of Reference FIG. 2, the region from yellow to red indicates a high pressure on the first tank side and shows a tendency to easily flow from the first tank to the second tank. On the other hand, the light blue to brown and blue regions have a small pressure difference and are 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 indicates that the pressure difference is zero, that is, is balanced. From this figure, the area around the calculated opening for transferring the slurry is a distribution area of yellow color (that is, a pressure difference of about 1400 Pa at the maximum), which is an area that easily flows from the first tank to the second tank. Yes.

When the slurry transfer port is translated from the above position to the upstream side in the direction of stirring the slurry, the pressure difference at this location is about 600 Pa at maximum, which is a half of the initial position. Speed installation since it is proportional to the square root of the pressure difference ^{(P = ρu 2/2)} , that the pressure is 1/2 the slurry-conveying flow-through openings of the same size on the upstream side of the stirring direction of the slurry Then, the flow rate is reduced to (1/2) ^0.5 , that is, 70%, and it becomes difficult to flow into the second tank.

  From this result, it was found that in order to install a slurry transfer port as large as possible while maintaining overflow, it should be shifted downstream from the upstream side in the rotation direction of the stirring blade. It was done.

  From FIG. 6, the region where the pressure difference is small is distributed at a height of 100 ± 20 cm from the lowest part and 50 cm away from the center of the partition wall, and it is desirable to install a slurry transfer port at this position.

  Therefore, in the slurry transfer liquid passage ports 52A, 52B,... 52F, the height from the lowest part of the autoclave to the gravity center of the slurry transfer liquid 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 liquid transfer port door for slurry transfer is set at a position 0.05 to 0.25 times the autoclave diameter D and does not reach the end of the partition wall. It was supposed to have. At this time, 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.

  Further, the shape of the slurry transfer ports 52A, 52B,... 52F is not particularly limited, but a rectangular shape is preferable because processing is easy.

  Moreover, the liquid transfer port for slurry transfer can secure an overflow even if it has a large shape by being arranged in a region where the pressure difference is small, and by forming a rectangular opening of 30 cm square to 50 cm square, It functions as a manway while ensuring overflow.

  Moreover, in this autoclave apparatus 100, since the slurry transfer ports 52A, 52B,... 52F are installed in the doors 51A, 51B,... 51F that close the manway openings 50A, 50B,. As the entire partition wall, the opening portions are gathered into one place, and strength reduction can be prevented. In this case, the manway openings 50A, 50B,... 50F are moved from the central part to both sides, so the inclination of the autoclave becomes slightly tight. If prepared, it can be passed without problems. In addition, although 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., a 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. .

  In this operation, HPAL operation was performed using the autoclave apparatus 100 to which the present invention was applied.

  As a result, the leaching rate of nickel was 92.5%. At this time, the free sulfuric acid in the leachate could be managed at 45 to 50 g / L.

[Comparative Example 1]
The present invention is not applied, and the HPAL operation is performed by using a conventional autoclave apparatus in which the partition walls 10A, 10B,... The same operation as in Example 1 was performed except that the operation was performed.

  As a result, the leaching rate of nickel was 92.0%. At this time, 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 seven 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 from the downstream side of the rotation and operated in an overflow state.

  As a result, the leaching rate of nickel was a good result of 92.0%.

[Comparative 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).

  As a result, a short path of sulfuric acid was generated from the first tank to the second tank, and ore insufficiently leached out from the slurry transfer port to the second tank, and the leaching rate of nickel decreased.

  1A, 1B Raw material slurry supply pipe, 2A, 2B sulfuric acid supply pipe, 3 high pressure steam supply pipe, 4 sulfuric acid supply pipe, 5 PSV vent pipe, 6 TAIL gas vent pipe, 7 slurry extraction pipe, 8 spare pipe, 10A, 10B ... 10F Bulkhead, 11C Adjustment weir plate, 12A, 12B ... 12F Notch, 20A, 20B ... 20G Compartment, 30A, 30B ... 30G Stirrer, 41, 42, 43 Manhole, 50A , 50B ... 50F Manway opening, 51A, 51B ... 51F Door, 52A, 52B ... 52F Slurry transfer port, 100 Autoclave device, 110 Autoclave body

Claims (6)

The leaching progresses by stirring the heated and pressurized raw slurry and sulfuric acid with a stirrer provided in each compartment in the autoclave divided into a plurality of partitions by the partition, and the downstream compartment from the upstream compartment An autoclave device in a high-pressure acid leaching process in which slurry is transferred to a chamber and leaching is sequentially advanced,
Each partition wall is provided with a slurry transfer passage opening that can be opened and closed by a slurry transfer passage door.
The slurry transfer port is 0.1 to 0.3 times the autoclave diameter from the lowest part of the autoclave to the center of gravity of the slurry transfer port door, and the slurry is transferred from the center line of the partition wall. The distance to the center of gravity of the liquid inlet door is set at a position 0.05 to 0.25 times the diameter of the autoclave and has a shape that does not reach the end of the partition wall,
An autoclave device, wherein an upper end portion of the partition wall is provided with a notch portion that allows an overflow amount to be adjusted depending on an installation height position of the adjustment plate. The downstream partition has a 55:45 ratio of the amount of liquid passing through the notch and the amount of liquid passing through the slurry transfer opening, and the other partition is the amount of liquid passing through the notch and the slurry transfer opening. The autoclave apparatus according to claim 1, wherein the ratio of the amount of liquid passing through the section is 84:16, and the autoclave apparatus is operated at a flow rate of 500 m ³ / hour.   The said partition is provided with the said liquid flow port for said slurry transfer in the downstream position of the stirring direction of the slurry by the stirrer in the upstream compartment, respectively. 2. The autoclave apparatus according to 2.   The autoclave device according to any one of claims 1 to 3, wherein the slurry transfer port is a rectangular opening that does not reach an end of the partition wall.   The autoclave device according to claim 4, wherein the slurry transfer port is installed at a door of a manway opening.   The autoclave device according to claim 4, wherein the slurry transfer port is a rectangular opening of 30 to 50 cm square.