Fused salt extraction zirconium and hafnium separation equipment and separation method

Abstract

The invention provides zirconium and hafnium separation equipment and a separation method through fused salt extraction, and relates to the technical field of zirconium and hafnium separation. The fused salt extraction zirconium and hafnium separation equipment comprises a separation tank, a feeding pipe is fixedly connected to the upper side of the separation tank, a discharging pipe is fixedly connected to the lower side of the separation tank, a valve is arranged on the outer side of the discharging pipe, supporting plates are fixedly connected to the left side and the right side of the separation tank, a stirring unit is arranged on the inner side of the separation tank, and the stirring unit is connected with the valve. The stirring unit comprises a rotating rod, the rotating rod is rotationally connected to the inner side of the separation tank, and two fixing blocks are fixedly connected to the outer side of the rotating rod. By arranging a rotating rod, a stirring plate, a control rod, a rotating disc, a sliding rod, a square frame, an L-shaped plate and a filter cartridge, molten salt and a zirconium-hafnium mixture can be fully mixed conveniently through the stirring plate on the rotating rod, materials are filtered through the filter cartridge at the bottom, precipitates generated by reaction are filtered, and the situation that the separation effect is affected by large precipitates is avoided.

Description

Technical Field

[0001] The invention relates to the technical field of zirconium and hafnium separation, in particular to molten salt extraction zirconium and hafnium separation equipment and a separation method. Background Art

[0002] Molten salt extraction uses molten salt as an extractant to convert certain substances in liquid metal into salts and extract them into the molten salt phase. Corresponding compounds that are easier to reduce than the metal compounds to be extracted are often added to the molten salt phase to increase the distribution coefficient of the metal elements in the molten salt. Zirconium (Zr) and hafnium (Hf) are both important metal elements that often coexist in nature and have similar chemical properties, which makes their separation a challenge.

[0003] When separating zirconium and hafnium, molten salt extraction is often used. During the separation, molten salt is added to the zirconium and hafnium mixture and stirred to fully mix the molten salt and the zirconium and hafnium mixture, which is convenient for separation operation. Precipitates are easily generated during separation. If these precipitates are not handled in time, the purity of the separated zirconium and hafnium mixture is not high and the separation effect is not good. Summary of the invention

[0004] Technical issues solved

[0005] In view of the shortcomings of the prior art, the present invention provides a molten salt extraction zirconium-hafnium separation device and a separation method, which solves the problem of poor separation effect of zirconium-hafnium mixture.

[0006] Technical Solution

[0007] To achieve the above objectives, the present invention is implemented through the following technical solutions: a molten salt extraction zirconium and hafnium separation device, comprising a separation tank, a feed pipe is fixedly connected to the upper side of the separation tank, a discharge pipe is fixedly connected to the lower side of the separation tank, a valve is arranged on the outer side of the discharge pipe, support plates are fixedly connected to the left and right sides of the separation tank, and a stirring unit is arranged on the inner side of the separation tank;

[0008] The stirring unit comprises a rotating rod, which is rotatably connected to the inner side of the separation tank, two fixed blocks are fixedly connected to the outer side of the rotating rod, the left and right sides of the fixed block are fixedly connected to the connecting block 1, the outer sides of the connecting blocks 1 on the left and right sides are rotatably connected to stirring plates, the stirring plate is fixedly connected to a vertical plate on one side close to the inner wall of the separation tank, the outer side of the separation tank is fixedly connected to a mounting block, the outer side of the mounting block is rotatably connected to a control rod, the outer side of the upper end of the control rod and the outer side of the rotating rod are fixedly connected to pulleys, and a belt is provided between the two pulleys. The lower end of the control rod is fixedly connected to bevel gear 1, the lower side of the separation tank is fixedly connected to a mounting plate, the outer side of the mounting plate is rotatably connected to a rotating shaft, the right end of the rotating shaft is fixedly connected to bevel gear 2, the left end of the rotating shaft is fixedly connected to a turntable, the left side of the turntable is fixedly connected to a sliding rod, the outer side of the sliding rod is slidably connected to a square frame, the lower side of the separation tank is fixedly connected to a telescopic rod, the lower end of the telescopic rod is fixedly connected to a fixing ring, the lower side of the fixing ring is fixedly connected to a filter cartridge, and an L-shaped plate is fixedly connected between the filter cartridge and the square frame.

[0009] Preferably, the bevel gear one is meshingly connected with the bevel gear two.

[0010] Preferably, the upper end of the rotating rod passes through the upper side of the separation tank, the upper side of the separation tank is fixedly connected to a fixing rod, the upper end of the fixing rod is fixedly connected to a top plate, the upper side of the top plate is fixedly connected to a motor, and the outer side of the motor output end and the outer side of the rotating rod are both fixedly connected to a gear part.

[0011] Preferably, the outer sides of the stirring plates on both sides are fixedly connected with connecting blocks 2, the outer sides of the connecting blocks 2 are rotatably connected with a rotating plate, the outer sides of the rotating plates on both sides are rotatably connected with connecting blocks 3, the outer sides of the connecting blocks 3 are fixedly connected with a control block, the middle part of the rotating rod is fixedly connected with two fixed cylinders, the inner sides of the two fixed cylinders are provided with piston plates, a moving rod is fixedly connected between the piston plates and the control blocks, a spring is fixedly connected between the outer sides of the piston plates and the inner walls of the fixed cylinders, a U-shaped tube is fixedly connected between the two fixed cylinders, a conveying tube is fixedly connected to the upper side of the U-shaped tube, a fixing frame and an air pump are fixedly connected to the upper side of the top plate, a connecting tube is fixedly connected to the upper side of the air pump, a pressure relief valve is provided on the outer side of the connecting tube.

[0012] Preferably, the connecting pipe is communicated with the delivery pipe.

[0013] Preferably, the piston plate is slidably connected to the fixed cylinder.

[0014] Preferably, the rotating plate is arranged in an inclined structure.

[0015] The method for separating zirconium and hafnium by molten salt extraction comprises the following steps:

[0016] S1. Adding raw materials and molten salt: adding zirconium-hafnium mixture and molten salt into the separation tank through a feed pipe;

[0017] S2, stirring and separating: start the motor and control the stirring plate to rotate for stirring;

[0018] S3, sedimentation filtration: control the valve to filter the sediment;

[0019] S4. Collection: Collect the precipitate and separated metals.

[0020] Beneficial Effects

[0021] The present invention provides a molten salt extraction zirconium and hafnium separation device and separation method. It has the following beneficial effects:

[0022] 1. The rotating rod, stirring plate, control rod, rotating disk, sliding rod, square frame, L-shaped plate and filter cartridge are provided to facilitate the stirring plate on the rotating rod to fully mix the molten salt and the zirconium-hafnium mixture, and filter the material through the filter cartridge at the bottom to filter the precipitate produced by the reaction, thereby preventing large precipitates from affecting the separation effect.

[0023] 2. By arranging the rotating rod, the stirring plate, the vertical plate, the rotating plate, the control block, the fixed cylinder, the piston plate and the air pump, it is convenient to control the swing of multiple stirring plates, so that the stirring effect of the stirring plates is increased and the separation effect is increased. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is the overall three-dimensional structure diagram of the present invention;

[0025] Figure 2 It is a partial three-dimensional structural diagram of the stirring unit in the present invention;

[0026] Figure 3 It is a partially cutaway three-dimensional structural diagram of the stirring unit in the present invention;

[0027] Figure 4 for Figure 3 The enlarged view of point A in the middle;

[0028] Figure 5 It is a partial three-dimensional structural diagram of the upper part of the stirring unit in the present invention;

[0029] Figure 6 A three-dimensional structural diagram of a control rod of a stirring unit in the present invention;

[0030] Figure 7 for Figure 6 Enlarged view of point B in the middle.

[0031] Among them, 1. separation tank; 2. support plate; 3. feed pipe; 4. discharge pipe; 5. valve; 6. stirring unit; 601. rotating rod; 602. fixed block; 603. connecting block 1; 604. stirring plate; 605. vertical plate; 606. connecting block 2; 607. rotating plate; 608. connecting block 3; 609. control block; 610. fixed cylinder; 611. moving rod; 612. piston plate; 613. spring; 614. U-shaped tube; 615. conveying pipe; 616. gear parts; 617. fixing rod; 618. top plate; 619. motor; 620. air pump; 621. connecting pipe; 622. pressure relief valve; 623. fixing frame; 624. control rod; 625. mounting block; 626. pulley; 627. belt; 628. telescopic rod; 629. bevel gear 1; 630. bevel gear 2; 631. mounting plate; 632. rotating shaft; 633. turntable; 634. sliding rod; 635. square frame; 636. L-shaped plate; 7. fixing ring; 8. filter cartridge. DETAILED DESCRIPTION

[0032] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0033] Embodiment 1:

[0034] like Figure 1 , Figure 5 - Figure 7 As shown, the molten salt extraction zirconium-hafnium separation equipment includes a separation tank 1, a feed pipe 3 is fixedly connected to the upper side of the separation tank 1, a discharge pipe 4 is fixedly connected to the lower side of the separation tank 1, a valve 5 is arranged on the outer side of the discharge pipe 4, support plates 2 are fixedly connected to the left and right sides of the separation tank 1, a stirring unit 6 is arranged on the inner side of the separation tank 1, and the stirring unit 6 is convenient for stirring the zirconium-hafnium mixture and the molten salt, the raw materials are added into the separation tank 1 through the feed pipe 3, and then the materials are discharged through the valve 5 in the discharge pipe 4.

[0035] The stirring unit 6 includes a rotating rod 601, which is rotatably connected to the inner side of the separation tank 1, and two fixed blocks 602 are fixedly connected to the outer side of the rotating rod 601, and the left and right sides of the fixed block 602 are fixedly connected to the connecting block 1 603, and the outer sides of the connecting blocks 1 603 on the left and right sides are rotatably connected to stirring plates 604, and the stirring plate 604 is fixedly connected to the side of the inner wall of the separation tank 1. A mounting block 625 is fixedly connected to the outer side of the separation tank 1, and a control rod 624 is rotatably connected to the outer side of the mounting block 625. The outer side of the upper end of the control rod 624 and the outer side of the rotating rod 601 are fixedly connected with a pulley 626, and a belt 627 is provided between the two pulleys 626. The lower end of the control rod 624 is fixedly connected to a cone Gear 1 629, a mounting plate 631 is fixedly connected to the lower side of the separation tank 1, a rotating shaft 632 is rotatably connected to the outer side of the mounting plate 631, a bevel gear 2 630 is fixedly connected to the right end of the rotating shaft 632, a turntable 633 is fixedly connected to the left end of the rotating shaft 632, a slide bar 634 is fixedly connected to the left side of the turntable 633, a square frame 635 is slidably connected to the outer side of the slide bar 634, a telescopic rod 628 is fixedly connected to the lower side of the separation tank 1, a fixing ring 7 is fixedly connected to the lower end of the telescopic rod 628, a filter cartridge 8 is fixedly connected to the lower side of the fixing ring 7, an L-shaped plate 636 is fixedly connected between the filter cartridge 8 and the square frame 635, a bevel gear 1 629 is meshedly connected to a bevel gear 2 630, and the upper end of the rotating rod 601 passes through the separation tank 1, a fixing rod 617 is fixedly connected to the upper side of the separation tank 1, a top plate 618 is fixedly connected to the upper end of the fixing rod 617, a motor 619 is fixedly connected to the upper side of the top plate 618, a gear 616 is fixedly connected to the outer side of the output end of the motor 619 and the outer side of the rotating rod 601, when the raw materials are stirred, the motor 619 is started, the motor 619 drives the gear 616 to rotate, and because the two gears 616 are meshed and connected, the motor 619 drives the rotating rod 601 to rotate, and the rotating rod 601 drives the stirring plate 604 to rotate, so that the stirring plate 604 stirs the material, so that the zirconium-hafnium mixture and the molten salt are fully mixed together, when the extraction is completed, the valve 5 is controlled to discharge the material to the bottom of the discharge pipe 4, and the material falls The rotating rod 601 drives the pulley 626 to rotate. Under the action of the belt 627, the rotating rod 601 drives the control rod 624 to rotate. The control rod 624 drives the bevel gear 1 629 to rotate. The bevel gear 1 629 drives the bevel gear 2 630 to rotate. The bevel gear 2 630 drives the rotating shaft 632 to rotate. The rotating shaft 632 drives the rotating disk 633 to rotate. The rotating disk 633 drives the sliding rod 634 to rotate. The sliding rod 634 drives the square frame 635 to move up and down repeatedly. The square frame 635 drives the L-shaped plate 636 to move. The L-shaped plate 636 drives the fixing ring 7 to move. The fixing ring 7 drives the filter cartridge 8 to vibrate up and down repeatedly, so that the filter screen in the filter cartridge 8 filters the material sediment, thereby increasing the separation purity of the zirconium-hafnium mixture.

[0036] Embodiment 2:

[0037] Based on the first embodiment, Figure 2 - Figure 4 As shown, the outer sides of the stirring plates 604 on both sides are fixedly connected with the connecting block 2 606, the outer side of the connecting block 2 606 is rotatably connected with the rotating plate 607, the outer sides of the rotating plates 607 on both sides are rotatably connected with the connecting block 3 608, the outer side of the connecting block 3 608 is fixedly connected with the control block 609, the middle part of the rotating rod 601 is fixedly connected with two fixed cylinders 610, the inner sides of the two fixed cylinders 610 are provided with piston plates 612, the moving rod 611 is fixedly connected between the piston plate 612 and the control block 609, the outer side of the piston plate 612 and the inner wall of the fixed cylinder 610 are fixedly connected with a spring 613, a U-shaped tube 614 is fixedly connected between the two fixed cylinders 610, the upper side of the U-shaped tube 614 is fixedly connected with a conveying pipe 615, the upper side of the top plate 618 is fixedly connected with a fixing frame 623 and an air pump 620, the upper side of the air pump 620 is fixedly connected with a connecting pipe 621, and the outer side of the connecting pipe 621 is provided with a drain The pressure relief valve 622, the connecting pipe 621 is connected with the conveying pipe 615, the piston plate 612 is slidably connected with the fixed cylinder 610, and the rotating plate 607 is set as an inclined structure. When stirring, the air pump 620 is started, and gas is introduced into the U-shaped tube 614 under the action of the connecting pipe 621 and the conveying pipe 615, and distributed to the fixed cylinder 610 on both sides. Under the action of air pressure, the piston plate 612 moves, the piston plate 612 drives the moving rod 611 to move, and the moving rod 611 drives the control block 609 to move, and the control block 609 drives the rotating plate 607 to rotate, and the rotating plates 607 on both sides gather together, and the rotating plate 607 drives the stirring plate 604 to rotate, so that the stirring plates 604 on both sides rotate, and then the pressure relief valve 622 is controlled to start, so that the gas in the fixed cylinder 610 is discharged, and the piston plate 612 is reset under the elastic force of the spring 613, and the above operation is repeated to make the stirring plate 604 swing repeatedly to increase the material stirring effect.

[0038] The method for separating zirconium and hafnium by molten salt extraction comprises the following steps:

[0039] S1, adding raw materials and molten salt: adding the zirconium-hafnium mixture and the molten salt into the separation tank 1 through the feed pipe 3;

[0040] S2, stirring and separating: starting the motor 619 to control the stirring plate 604 to rotate for stirring;

[0041] S3, sedimentation filtration: control the valve 5 to filter the sediment;

[0042] S4. Collection: Collect the precipitate and separated metals.

[0043] Working principle: when in use, the material is added into the separation tank 1 through the feed pipe 3, and the motor 619 is started. Under the action of the gear part 616, the stirring plate 604 on the rotating rod 601 is controlled to rotate, so as to facilitate the stirring of the material and the extraction. The air pump 620 is started. Under the action of the connecting pipe 621, the conveying pipe 615 and the U-shaped pipe 614, the gas is filled into the fixed cylinder 610. Under the action of the piston plate 612, the moving rod 611, the control block 609 and the rotating plate 607, the stirring plates 604 on both sides are controlled to swing to increase the material stirring effect. After the extraction is completed, the valve 5 is controlled to make the material enter the filter cylinder 8. The rotating rod 601 drives the control rod 624 to rotate. Under the action of the bevel gear 1 629 and the bevel gear 2 630, the rotating shaft 632 is controlled to rotate. Under the action of the turntable 633, the slide bar 634, the square frame 635 and the L-shaped plate 636, the filter cylinder 8 is controlled to vibrate repeatedly up and down, so as to facilitate the filtering of the sediment and increase the separation effect.

[0044] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A molten salt extraction zirconium and hafnium separation device, comprising a separation tank (1), characterized in that: A feed pipe (3) is fixedly connected to the upper side of the separation tank (1), a discharge pipe (4) is fixedly connected to the lower side of the separation tank (1), a valve (5) is arranged on the outer side of the discharge pipe (4), support plates (2) are fixedly connected to the left and right sides of the separation tank (1), and a stirring unit (6) is arranged on the inner side of the separation tank (1); The stirring unit (6) comprises a rotating rod (601), wherein the rotating rod (601) is rotatably connected to the inner side of the separation tank (1), and two fixed blocks (602) are fixedly connected to the outer side of the rotating rod (601), and the left and right sides of the fixed block (602) are fixedly connected to the connecting block 1 (603), and the outer sides of the connecting block 1 (603) on the left and right sides are rotatably connected to stirring plates (604), and the stirring plates (604) are fixedly connected to the side close to the inner wall of the separation tank (1) with a vertical plate (605), and the outer side of the separation tank (1) is fixedly connected to a mounting block (625), and the outer side of the mounting block (625) is rotatably connected to a control rod (624), and the outer side of the upper end of the control rod (624) and the outer side of the rotating rod (601) are fixedly connected to pulleys (626), and a belt (627) is provided between the two pulleys (626). The lower end of the control rod (624) is fixedly connected to a bevel gear 1 (629); the lower side of the separation tank (1) is fixedly connected to a mounting plate (631); the outer side of the mounting plate (631) is rotatably connected to a rotating shaft (632); the right end of the rotating shaft (632) is fixedly connected to a bevel gear 2 (630); the left end of the rotating shaft (632) is fixedly connected to a rotating disk (633); the left side of the rotating disk (633) is fixedly connected to a sliding rod (634); the outer side of the sliding rod (634) is slidably connected to a square frame (635); the lower side of the separation tank (1) is fixedly connected to a telescopic rod (628); the lower end of the telescopic rod (628) is fixedly connected to a fixing ring (7); the lower side of the fixing ring (7) is fixedly connected to a filter cartridge (8); an L-shaped plate (636) is fixedly connected between the filter cartridge (8) and the square frame (635).

2. The molten salt extraction zirconium and hafnium separation equipment according to claim 1, characterized in that: The bevel gear one (629) is meshedly connected with the bevel gear two (630).

3. The molten salt extraction zirconium and hafnium separation equipment according to claim 1, characterized in that: The upper end of the rotating rod (601) passes through the upper side of the separation tank (1); the upper side of the separation tank (1) is fixedly connected to a fixing rod (617); the upper end of the fixing rod (617) is fixedly connected to a top plate (618); the upper side of the top plate (618) is fixedly connected to a motor (619); and the outer side of the output end of the motor (619) and the outer side of the rotating rod (601) are both fixedly connected to a gear member (616).

4. The molten salt extraction zirconium and hafnium separation equipment according to claim 3 is characterized in that: The outer sides of the stirring plates (604) on both sides are fixedly connected with connecting blocks 2 (606), the outer sides of the connecting blocks 2 (606) are rotatably connected with rotating plates (607), the outer sides of the rotating plates (607) on both sides are rotatably connected with connecting blocks 3 (608), the outer sides of the connecting blocks 3 (608) are fixedly connected with control blocks (609), the middle part of the rotating rod (601) is fixedly connected with two fixed cylinders (610), the inner sides of the two fixed cylinders (610) are provided with piston plates (612), and the piston plates (612) are fixedly connected with the control blocks (609). A moving rod (611) is fixedly connected to the top plate (618); a spring (613) is fixedly connected between the outer side of the piston plate (612) and the inner wall of the fixed cylinder (610); a U-shaped tube (614) is fixedly connected between the two fixed cylinders (610); a delivery tube (615) is fixedly connected to the upper side of the U-shaped tube (614); a fixing frame (623) and an air pump (620) are fixedly connected to the upper side of the top plate (618); a connecting tube (621) is fixedly connected to the upper side of the air pump (620); a pressure relief valve (622) is arranged on the outer side of the connecting tube (621).

5. The molten salt extraction zirconium and hafnium separation equipment according to claim 4 is characterized in that: The connecting pipe (621) is in communication with the delivery pipe (615).

6. The molten salt extraction zirconium and hafnium separation equipment according to claim 4, characterized in that: The piston plate (612) is slidably connected to the fixed cylinder (610).

7. The molten salt extraction zirconium and hafnium separation equipment according to claim 4, characterized in that: The rotating plate (607) is arranged in an inclined structure.

8. A method for separating zirconium and hafnium by extracting zirconium and hafnium from molten salt, according to the device for separating zirconium and hafnium by extracting zirconium and hafnium from molten salt according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1. Adding raw materials and molten salt: adding the zirconium-hafnium mixture and the molten salt into the separation tank (1) through the feed pipe (3); S2, stirring and separating: starting the motor (619) and controlling the stirring plate (604) to rotate for stirring; S3, sedimentation filtration: control valve (5) to filter the sediment; S4. Collection: Collect the precipitate and separated metals.

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