A zirconium-hafnium solution crystallization separation device and separation method

Abstract

The present invention belongs to the technical field of chemical purification, and in particular to a zirconium-hafnium solution crystallization separation device and a separation method. In view of the fact that when the existing zirconium-hafnium solution crystallization separation device uses a solvent to dissolve a zirconium-hafnium solid compound, the solvent consumption is too high, and solvent waste occurs due to the uneven mixing of the solvent and the zirconium-hafnium solid compound, which reduces the economic benefits of the equipment in preparing and purifying zirconium metal. The following scheme is proposed, including a box body, and a top cover is fixedly connected to the upper side of the box body. The zirconium-hafnium solution crystallization separation device and a separation method disclosed by the present invention utilize a mixing synergistic module to fully mix the zirconium-hafnium solid compound with the solvent, accelerate the reaction speed of the zirconium-hafnium solid compound with the solvent, ensure the completion of the chemical reaction of the dissolution, allow the solvent to fully react, improve the dissolution efficiency, avoid excessive input of solvent, reduce consumption, and save resources.

Description

Technical Field

[0001] The invention relates to the technical field of chemical purification, and in particular to a zirconium-hafnium solution crystallization separation device and a separation method. Background Art

[0002] Zirconium is a chemical element. Its chemical symbol is Zr. Its atomic number is 40. It is a silvery white metal with a high melting point and a light gray color. Its density is 6.49 g / cm3. Its melting point is 1852±2℃ and its boiling point is 4377℃. Its valence is +2, +3 and +4. Its first ionization energy is 6.84 electron volts. Zirconium easily forms an oxide film on its surface, which is shiny, so its appearance is similar to that of steel. It is corrosion-resistant and soluble in hydrofluoric acid and aqua regia. At high temperatures, it can react with non-metallic elements and many metal elements to form solid solution compounds.

[0003] When the existing zirconium-hafnium solution crystallization separation equipment uses a solvent to dissolve the zirconium-hafnium solid compound, the solvent and the zirconium-hafnium solid compound are mixed unevenly, resulting in excessive solvent consumption and solvent waste, which reduces the economic benefits of the equipment in preparing purified zirconium metal. Summary of the invention

[0004] The invention discloses a zirconium-hafnium solution crystallization separation device and a separation method, aiming to solve the technical problem that the existing zirconium-hafnium solution crystallization separation device in the background technology cannot effectively mix the solvent and the zirconium-hafnium solid compound uniformly.

[0005] The invention provides a zirconium-hafnium solution crystallization separation device, comprising a box body, a top cover is fixedly connected to the upper side of the box body, and a mixing and synergistic module is arranged below the top cover, the mixing and synergistic module is located inside the box body, a reaction barrel is arranged inside the box body, the mixing and synergistic module comprises a connecting platform, a receiving groove is provided at the bottom of the connecting platform, a push rod is slidably connected in the receiving groove, a connecting rod is fixedly connected to the bottom of the push rod, and a motor 2 is fixedly connected to the inner wall of the bottom of the box body, the output end of the motor 2 is connected to a rotating rod through a coupling, and a rotating rod is provided on a side close to the connecting rod. There is a circular groove, and a hydraulic rod 2 is fixedly connected to the inner wall of the circular groove. The output end of the hydraulic rod 2 is fixedly connected to the side opposite to the connecting rod. An exhaust gas treatment module is arranged on the box body, and the exhaust gas treatment module is located outside the reaction barrel. An extraction module is arranged on the box body, and a notch is opened on one side of the box body. A sealing door is connected to the inner wall of one side of the notch through a hinge, and an observation window is opened on the sealing door. Two symmetrical circular holes are opened on the side of the box body close to the sealing door, and delivery pipes are fixedly connected in the circular holes. The two delivery pipes are connected to the side opposite to the reaction barrel through flanges.

[0006] By providing a sealing door, an observation window, a top cover, a conveying pipe, a mixing and efficiency enhancement module, an extraction module, an exhaust gas treatment module and a reaction barrel, the device utilizes the mixing and efficiency enhancement module to fully mix the zirconium and hafnium solid compound with the solvent, accelerate the reaction speed of the zirconium and hafnium solid compound with the solvent, ensure the completion of the chemical reaction of the dissolution, allow the solvent to fully react, improve the dissolution efficiency, avoid excessive input of the solvent, reduce consumption, and save resources.

[0007] In a preferred solution, a hydraulic rod 1 is fixedly connected to the bottom of the top cover, an output end of the hydraulic rod 1 is fixedly connected to a fixing box, a motor 1 is fixedly connected to the top inner wall of the fixing box, and a fine hole is provided at the bottom of the fixing box, a main shaft is movably connected in the fine hole, the upper side of the main shaft is connected to the output end of the motor 1 through a coupling, the main shaft is located inside the reaction barrel, and two symmetrical cross bars 1 are fixedly connected to the outside of the main shaft; two symmetrical secondary shafts are movably connected to the opposite sides of the two cross bars 1, and the outsides of the two secondary shafts are fixedly connected to gears, the gears are both located above the cross bar 1, and a shielding cover is fixedly connected to the outside of the fixing box, an inner wall of the shielding cover is fixedly connected to an inner gear ring, and the two gears are meshed with the inner gear ring; the outsides of the secondary shafts are fixedly connected There are two symmetrical cross bars 2, which are both located between the two cross bars 1, and the two cross bars 2 located on the same side are fixedly connected to the opposite sides with two symmetrical vertical bars, and the outsides of the vertical bars are fixedly connected with a plurality of stirring bars distributed at equal distances; the inner wall of the box body is fixedly connected with a mounting frame, the mounting frame is located outside the reaction barrel, the inner wall of the mounting frame is fixedly connected with a plurality of springs distributed at equal distances around the circumference, the ends of the springs away from the mounting frame are fixedly connected to the outside of the reaction barrel, and the inner wall of the box body is fixedly connected with a supporting plate, the supporting plate is located below the reaction barrel and outside the connecting platform, an annular groove is opened on the upper side of the supporting plate, and the bottom of the reaction barrel is fixedly connected with a plurality of spherical rollers distributed at equal distances around the circumference, and the outsides of the spherical rollers are in contact with the bottom inner wall of the annular groove.

[0008] By providing a mixing and synergistic module, the mixing and synergistic module can realize contactless stirring of the solution in the reaction barrel by using a connecting platform and a push rod, while ensuring the stirring and mixing effect, reducing direct contact with the solution in the reaction barrel, so that the zirconium compound in the reaction barrel will not be excessively attached to the device during crystallization and precipitation, that is, reducing the loss of the zirconium compound, reducing the corrosion of the compound to the device, and increasing the service life of the device.

[0009] In a preferred embodiment, the extraction module includes a fixed frame, which is fixedly connected to the side opposite to the inner wall of the box body, and a hole groove is provided on the fixed frame, in which a screw rod is movably connected, an isolation cover is fixedly connected to the upper side of the fixed frame, and a motor three is fixedly connected to the top inner wall of the isolation cover, the output end of the motor three is connected to the upper side of the screw rod through a coupling, and a movable block is arranged outside the screw rod, and the outside of the movable block is slidably connected to the inner wall of the fixed frame; a circular groove is provided on the movable block, in which an extraction tube is fixedly connected, one end of the extraction tube away from the movable block is located inside the reaction barrel, one end of the extraction tube close to the movable block is fixedly connected to a hose, and one end of the hose away from the extraction tube is fixedly connected to a discharge pipe, and a circular hole is provided on the inner wall of one side of the box body close to the fixed frame, and the inner wall of the circular hole is fixedly connected to the outside of the discharge pipe.

[0010] By providing an extraction module, the extraction module uses a screw rod and a movable block to enable the extraction tube to gradually extract the upper organic solvent according to the amount of organic solvent containing hafnium compounds, thereby avoiding the situation where the device accidentally extracts the lower inorganic solvent containing zirconium compounds, thereby ensuring the output of zirconium compounds in the device.

[0011] In a preferred embodiment, the exhaust gas treatment module includes two symmetrical air intake frames, the bottoms of the two air intake frames are fixedly connected to the upper side of the supporting plate, the air intake frames are provided with slots, the inner walls of the slots are fixedly connected to filters, and the top cover is provided with two symmetrical circular openings, the circular openings are fixedly connected to air pipes, the upper sides of the air intake frames are provided with holes, the inner walls of the two holes are respectively fixedly connected to the outsides of the two air pipes, the ends of the two air pipes away from the air intake frames are fixedly connected to air guide pipes, and the ends of the two air guide pipes away from the air pipes are fixedly connected to the same air collecting box; an air pump is fixedly connected to the upper side of the air collecting box, the input end of the air pump is connected to the outside of the air collecting box through a conduit, the output end of the air pump is connected to a collecting pipe through a circular pipe, the end of the collecting pipe away from the air pump is fixedly connected to an activated carbon canister, the end of the activated carbon canister away from the collecting pipe is fixedly connected to a transfer pipe, and an alkaline gas washing box is arranged on the outside of the end of the transfer pipe away from the activated carbon canister, and the bottom of the alkaline gas washing box is fixedly connected to the upper side of the top cover.

[0012] By setting up a waste gas treatment module, the waste gas treatment module uses an air intake frame to collect the toxic gases produced by the chemical reaction in the reaction barrel, and uses an activated carbon tank and an alkaline scrubbing box to harmlessly treat these harmful substances, thereby avoiding environmental pollution and harm caused by direct emissions.

[0013] A zirconium-hafnium solution crystallization separation method, using the zirconium-hafnium solution crystallization separation device as described above, comprises the following steps: Step 1: After the zirconium-hafnium solid compound is placed in a reaction barrel, a solvent is delivered to the reaction barrel through a delivery pipe to dissolve the zirconium-hafnium solid compound, and during the dissolution process, a mixing and synergistic module is used to stir the zirconium-hafnium solid compound; Step 2: Add the extractant, stir for a while, let it stand, and after the solution is separated into layers, use the extraction module to extract the upper layer of solution.

[0014] Step 3: Add sulfuric acid solution to the remaining solution in the reaction barrel through a delivery pipe. Stir the reaction barrel and let it stand to allow the solution to crystallize and precipitate. During the whole process, use the waste gas treatment module to absorb and wash the waste gas generated in the equipment.

[0015] As can be seen from the above, the zirconium-hafnium solution crystallization separation equipment provided by the present invention has the advantage of utilizing a mixing and synergistic module to fully mix the zirconium-hafnium solid compound with the solvent, thereby accelerating the reaction rate of the zirconium-hafnium solid compound with the solvent, ensuring the completion of the chemical reaction of the dissolution, allowing the solvent to fully react, thereby improving the dissolution efficiency, avoiding excessive input of the solvent, reducing consumption, and saving resources. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of the overall structure of a zirconium-hafnium solution crystallization separation device proposed by the present invention; Figure 2 This is a schematic cross-sectional view of a zirconium-hafnium solution crystallization and separation device proposed by the present invention; Figure 3 This is a schematic diagram of the reaction barrel structure of a zirconium-hafnium solution crystallization separation device proposed by the present invention; Figure 4 This is a schematic diagram of the shielding cover structure of a zirconium-hafnium solution crystallization separation device proposed by the present invention; Figure 5 A schematic diagram of the rotating rod structure of a zirconium-hafnium solution crystallization separation device proposed by the present invention; Figure 6 This is a schematic diagram of the structure of an extraction module of a zirconium-hafnium solution crystallization separation device proposed by the present invention; Figure 7 This is a schematic diagram of the structure of an exhaust gas treatment module of a zirconium-hafnium solution crystallization separation device proposed in the present invention.

[0017] In the figure: 1, box body; 2, sealing door; 3, observation window; 4, top cover; 5, conveying pipe; 6, hybrid efficiency module; 601, hydraulic rod 1; 602, fixing box; 603, shielding cover; 604, mounting frame; 605, spring; 606, connecting platform; 607, supporting plate; 608, main shaft; 609, motor 1; 610, cross bar 1; 611, secondary shaft; 612, gear; 613, inner gear ring; 614, cross bar 2; 615, vertical rod; 616, stirring rod; 617, annular groove; 618, spherical roller; 619, receiving groove; 620, push rod; 621. Connecting rod; 622. Rotating rod; 623. Hydraulic rod 2; 624. Motor 2; 7. Extraction module; 701. Fixed frame; 702. Screw rod; 703. Motor 3; 704. Isolation cover; 705. Movable block; 706. Extraction pipe; 707. Hose; 708. Exhaust pipe; 8. Waste gas treatment module; 801. Air intake frame; 802. Filter; 803. Air pipe; 804. Air guide pipe; 805. Air collecting box; 806. Air pump; 807. Collection pipe; 808. Activated carbon canister; 809. Transfer pipe; 810. Alkaline washing box; 9. Reaction barrel. DETAILED DESCRIPTION

[0018] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0019] The zirconium-hafnium solution crystallization separation device disclosed in the present invention is mainly used in the scenario where the existing zirconium-hafnium solution crystallization separation device cannot effectively mix the solvent and the zirconium-hafnium solid compound uniformly.

[0020] Reference Figure 1-7A zirconium-hafnium solution crystallization separation device comprises a box body 1, a top cover 4 is connected to the upper side of the box body 1 by bolts, and a mixing efficiency enhancement module 6 is arranged below the top cover 4, the mixing efficiency enhancement module 6 is located inside the box body 1, a reaction barrel 9 is arranged inside the box body 1, and the mixing efficiency enhancement module 6 comprises a connecting platform 606, a receiving groove 619 is opened at the bottom of the connecting platform 606, a push rod 620 is slidably connected in the receiving groove 619, a connecting rod 621 is connected to the bottom of the push rod 620 by bolts, and a motor 624 is connected to the inner wall of the bottom of the box body 1 by bolts, and the output end of the motor 624 is connected to a rotating rod 622 by a coupling, and the rotating rod 622 is close to the connecting rod 621. A circular groove is provided on one side of the rod 621, and a hydraulic rod 623 is connected to the inner wall of the circular groove by bolts. The output end of the hydraulic rod 623 is connected to the side opposite to the connecting rod 621 by bolts. A waste gas treatment module 8 is provided on the box body 1, and the waste gas treatment module 8 is located outside the reaction barrel 9. An extraction module 7 is provided on the box body 1. A notch is provided on one side of the box body 1, and a sealing door 2 is connected to the inner wall of one side of the notch by a hinge. An observation window 3 is provided on the sealing door 2, and two symmetrical circular holes are provided on the side of the box body 1 close to the sealing door 2, and delivery pipes 5 are connected to the circular holes by bolts, and the two delivery pipes 5 are connected to the side opposite to the reaction barrel 9 by flanges.

[0021] Specifically, after opening the sealing door 2 and placing the zirconium-hafnium solid compound into the reaction barrel 9, the sealing door 2 is closed, and the solvent is injected into the reaction barrel 9 through the delivery pipe 5, and the mixture in the reaction barrel 9 is stirred by the mixing and synergistic module 6 to dissolve the zirconium-hafnium solid compound, and the extractant is added, and the mixture is stirred for a period of time, and then the mixture is allowed to stand. After the solution is layered, the upper layer of the solution is extracted by the extraction module 7, and the sulfuric acid solution is added to the remaining solution in the reaction barrel 9 through the delivery pipe 5. After the reaction barrel 9 is stirred, the mixture is allowed to stand to allow the solution to crystallize and precipitate. During the whole process, the waste gas treatment module 8 is used to absorb and wash the waste gas generated in the equipment; the device uses the mixing and synergistic module 6 to fully mix the zirconium-hafnium solid compound with the solvent, accelerate the reaction speed of the zirconium-hafnium solid compound with the solvent, ensure the completion of the chemical reaction of the dissolution, and allow the solvent to fully react, thereby improving the dissolution efficiency, avoiding excessive input of the solvent, reducing the consumption, and saving resources.

[0022] Reference Figure 3 , Figure 4 and Figure 5In a preferred embodiment, the bottom of the top cover 4 is connected to a hydraulic rod 601 by bolts, the output end of the hydraulic rod 601 is connected to a fixed box 602 by bolts, the top inner wall of the fixed box 602 is connected to a motor 609 by bolts, and a fine hole is opened at the bottom of the fixed box 602, and a main shaft 608 is rotatably connected to the fine hole through a bearing, and the upper side of the main shaft 608 is connected to the output end of the motor 609 by a coupling, and the main shaft 608 is located inside the reaction barrel 9, and the outer side of the main shaft 608 is connected to the outer side of the main shaft 608. The fixing box 602 is provided with two symmetrical cross bars 610 connected by bolts; two symmetrical secondary shafts 611 are rotatably connected to the opposite sides of the two cross bars 610 through bearings, and the outsides of the two secondary shafts 611 are connected with gears 612 by bolts, and the gears 612 are located above the cross bars 610, and the outside of the fixing box 602 is connected with a shielding cover 603 by bolts, and the inner wall of the shielding cover 603 is connected with an inner gear ring 613 by bolts, and the two gears 612 are meshed with the inner gear ring 613; the outside of the secondary shaft 611 is connected with a gear 612 by bolts, and the gear 612 is .... The two cross bars 614 are connected to each other by bolts, and the two cross bars 614 are located between the two cross bars 610. The two cross bars 614 on the same side are connected to two symmetrical vertical bars 615 on opposite sides by bolts, and the outsides of the vertical bars 615 are connected to multiple stirring bars 616 distributed at equal distances by bolts; the inner wall of the box body 1 is connected to a mounting frame 604 by bolts, and the mounting frame 604 is located outside the reaction barrel 9. The inner wall of the mounting frame 604 is connected to multiple circular Springs 605 are evenly distributed around the circumference, and one end of the spring 605 away from the mounting frame 604 is connected to the outside of the reaction barrel 9 by bolts, and the inner wall of the box body 1 is connected to a supporting plate 607 by bolts, and the supporting plate 607 is located below the reaction barrel 9 and connected to the outside of the platform 606. An annular groove 617 is opened on the upper side of the supporting plate 607, and a plurality of spherical rollers 618 evenly distributed around the circumference are connected to the bottom of the reaction barrel 9 by bolts, and the outside of the spherical rollers 618 are in contact with the bottom inner wall of the annular groove 617.

[0023] Specifically, after the zirconium-hafnium solid compound is placed in the reaction barrel 9, the solvent is injected into the reaction barrel 9 through the delivery pipe 5, the hydraulic rod 1 601 is started, the hydraulic rod 1 601 drives the fixed box 602 to descend, and the main shaft 608 is lowered into the reaction barrel 9, the motor 1 609 is started, the motor 1 609 drives the main shaft 608 to rotate, so that the cross bar 1 610 connected to the main shaft 608 rotates, and the secondary shaft 611 on the cross bar 1 610 drives the cross bar 2 614 to rotate through the meshing of the gear 612 and the inner gear ring 613, so that the stirring rod 616 on the vertical rod 615 is rotated to the reaction barrel 9. The mixture in the barrel 9 is stirred. After the extractant is added to extract and separate the hafnium compound, the hydraulic rod 1 601 is started, so that the hydraulic rod 1 601 lifts and separates the main shaft 608 from the reaction barrel 9, and sulfuric acid solution is injected into the reaction barrel 9. The motor 2 624 is started, and the motor 2 624 drives the rotating rod 622 to rotate. The hydraulic rod 2 623 is started, and the output end of the hydraulic rod 2 623 is extended, so that the motor 2 624 connected to the hydraulic rod 2 623 drives the push rod 620 to squeeze the receiving groove 619 and rotate in the connecting platform 606, so that the solution in the reaction barrel 9 is continuously shaken.

[0024] In a specific application scenario, the mixing enhancement module 6 is mainly used in the mixing enhancement link in the mixing enhancement process, that is, the mixing enhancement module 6 can use the connecting platform 606 and the push rod 620 to realize contactless stirring of the solution in the reaction barrel 9. While ensuring the stirring and mixing effect, it reduces direct contact with the solution in the reaction barrel 9, so that the zirconium compound in the reaction barrel 9 will not be excessively attached to the device during crystallization and precipitation, that is, the loss of zirconium compounds is reduced, the corrosion of the compound to the device is reduced, and the service life of the device is increased.

[0025] Reference Figure 6 In a preferred embodiment, the extraction module 7 includes a fixed frame 701, the fixed frame 701 is connected to the inner wall of the box body 1 on one side by bolts, a hole groove is opened on the fixed frame 701, a screw rod 702 is rotatably connected in the hole groove through a bearing, an isolation cover 704 is connected to the upper side of the fixed frame 701 by bolts, a motor 3 703 is connected to the inner wall of the top of the isolation cover 704 by bolts, an output end of the motor 3 703 is connected to the upper side of the screw rod 702 by a coupling, and a movable block 705 is arranged outside the screw rod 702, and the movable block 70 5 is slidably connected to the inner wall of the fixed frame 701; a circular notch is opened on the movable block 705, and an extraction tube 706 is connected to the circular notch by bolts, and the end of the extraction tube 706 away from the movable block 705 is located inside the reaction barrel 9, and the end of the extraction tube 706 close to the movable block 705 is connected to a hose 707 by bolts, and the end of the hose 707 away from the extraction tube 706 is connected to a discharge pipe 708 by bolts, and a circular hole is opened on the inner wall of one side of the box body 1 close to the fixed frame 701, and the inner wall of the circular hole is connected to the outer side of the discharge pipe 708 by bolts.

[0026] Specifically, after the extraction agent is added to the device to extract the hafnium compound, the motor 3 703 is started, and the motor 3 703 drives the screw 702 to rotate, so that the movable block 705 on the screw 702 drives the extraction tube 706 to move downward on the fixed frame 701, so that one end of the extraction tube 706 contacts the upper layer of the organic solvent containing the hafnium compound and extracts it, so that only the lower layer of the inorganic solvent containing the zirconium compound exists in the reaction barrel 9.

[0027] In a specific application scenario, the extraction module 7 is mainly suitable for the extraction link in the extraction process, that is, the extraction module 7 uses the screw 702 and the movable block 705 to enable the extraction tube 706 to gradually extract the upper organic solvent according to the amount of organic solvent containing hafnium compounds, thereby avoiding the situation where the device accidentally extracts the lower inorganic solvent containing zirconium compounds, thereby ensuring the output of zirconium compounds in the device.

[0028] Reference Figure 7 In a preferred embodiment, the exhaust gas treatment module 8 includes two symmetrical air intake frames 801, the bottoms of the two air intake frames 801 are connected to the upper side of the support plate 607 by bolts, the air intake frames 801 are provided with slots, the inner walls of the slots are connected to the filter screen 802 by bolts, and the top cover 4 is provided with two symmetrical round openings, the round openings are connected to the air delivery pipes 803 by bolts, the upper side of the air intake frames 801 are provided with holes, the inner walls of the two holes are respectively connected to the outside of the two air delivery pipes 803 by bolts, and the ends of the two air delivery pipes 803 away from the air intake frames 801 are connected to the air guide pipes 804 by bolts, and the two air guide pipes 804 are away from the air intake frames 801. One end of the air pipe 803 is connected to the same air collecting box 805 by bolts; the upper side of the air collecting box 805 is connected to the air pump 806 by bolts, the input end of the air pump 806 is connected to the outside of the air collecting box 805 by a conduit, the output end of the air pump 806 is connected to the collecting pipe 807 by a round tube, the end of the collecting pipe 807 away from the air pump 806 is connected to the activated carbon tank 808 by bolts, the end of the activated carbon tank 808 away from the collecting pipe 807 is connected to the transfer pipe 809 by bolts, and the end of the transfer pipe 809 away from the activated carbon tank 808 is provided with an alkaline washing box 810 on the outside, and the bottom of the alkaline washing box 810 is connected to the upper side of the top cover 4 by bolts.

[0029] Specifically, during the entire separation process, the air pump 806 is kept turned on. The air pump 806 drives the gas collecting box 805 to collect harmful substances such as hydrogen sulfide and hydrocyanic acid extracted from the bottom of the device by the air intake frame 801 into the gas collecting box 805 through the air guide pipe 804, and transports them to the activated carbon tank 808 through the collecting pipe 807. After the activated carbon in the activated carbon tank 808 absorbs the hydrogen sulfide, it is transported to the alkaline washing box 810 through the transfer pipe 809, so that the alkaline solution in the alkaline washing box 810 can clean and absorb the hydrocyanic acid.

[0030] In specific application scenarios, the waste gas treatment module 8 is mainly suitable for the waste gas treatment link in the waste gas treatment process, that is, the waste gas treatment module 8 uses the air intake frame 801 to collect the toxic gas produced by the chemical reaction in the reaction barrel 9, and uses the activated carbon tank 808 and the alkaline washing box 810 to harmlessly treat these harmful substances, thereby avoiding environmental pollution and harm caused by direct emissions.

[0031] A zirconium-hafnium solution crystallization separation method, using the zirconium-hafnium solution crystallization separation device as described above, comprises the following steps: Step 1: After the zirconium-hafnium solid compound is placed in the reaction barrel 9, a solvent is transported into the reaction barrel 9 through the transport pipe 5 to dissolve the zirconium-hafnium solid compound. During the dissolution process, the mixing and synergistic module 6 is used to stir the compound (after the sealing door 2 is opened to place the zirconium-hafnium solid compound in the reaction barrel 9, the sealing door 2 is closed, and the solvent is injected into the reaction barrel 9 through the transport pipe 5, and the hydraulic rod 1 601 is started, and the hydraulic rod 1 601 drives the fixed box 602 to descend, so that the main shaft 608 descends into the reaction barrel 9, and the motor 1 609 is started, and the motor 1 609 drives the main shaft 608 to rotate, so that the cross bar 1 610 connected to the main shaft 608 rotates, and the secondary shaft 611 on the cross bar 1 610 drives the cross bar 2 614 to rotate through the meshing of the gear 612 and the inner gear ring 613, so that the stirring rod 616 on the vertical rod 615 stirs the mixture in the reaction barrel 9); Step 2: Add the extractant, stir for a period of time, let it stand, and after the solution is separated, use the extraction module 7 to extract the upper layer of the solution (after adding the extractant to extract and separate the hafnium compound, start the hydraulic rod 1 601, so that the hydraulic rod 1 601 lifts the main shaft 608 from the reaction barrel 9 and separates it, inject sulfuric acid solution into the reaction barrel 9, start the motor 2 624, the motor 2 624 drives the rotating rod 622 to rotate, start the hydraulic rod 2 623, and the output end of the hydraulic rod 2 623 is extended, so that the motor 2 624 connected to the hydraulic rod 2 623 drives the rotating rod 622 to rotate, and start the hydraulic rod 2 623. The push rod 620 squeezes the containing groove 619 and rotates in the connecting platform 606, so that the solution in the reaction barrel 9 is continuously shaken. After the device adds the extractant to extract the hafnium compound, the motor 3 703 is started, and the motor 3 703 drives the screw rod 702 to rotate, so that the movable block 705 on the screw rod 702 drives the extraction tube 706 to move downward on the fixed frame 701, so that one end of the extraction tube 706 contacts the upper layer of the organic solvent containing the hafnium compound and extracts it, so that only the lower layer of the inorganic solvent containing the zirconium compound exists in the reaction barrel 9).

[0032] Step 3: add sulfuric acid solution to the remaining solution in the reaction barrel 9 through the delivery pipe 5, stir the reaction barrel 9, and then let it stand to allow the solution to crystallize and precipitate. During the whole process, use the waste gas treatment module 8 to absorb and wash the waste gas generated in the equipment (add sulfuric acid solution to the remaining solution in the reaction barrel 9 through the delivery pipe 5, start the hydraulic rod 1 601, so that the hydraulic rod 1 601 lifts the main shaft 608 from the reaction barrel 9 and separates it, inject sulfuric acid solution into the reaction barrel 9, start the motor 2 624, the motor 2 624 drives the rotating rod 622 to rotate, start the hydraulic rod 2 623, and the output end of the hydraulic rod 2 623 is extended, so that the output end connected to the hydraulic rod 2 623 is connected to the main shaft 608. Motor 2 624 drives push rod 620 to squeeze receiving groove 619 and rotate in connecting platform 606, so that the solution in reaction barrel 9 is continuously shaken. During the whole separation process, the air pump 806 is kept in the open state. Air pump 806 drives gas collecting box 805 to collect harmful substances such as hydrogen sulfide and hydrocyanic acid extracted from the bottom of the device by air intake frame 801 into gas collecting box 805 through air guide pipe 804, and transports them to activated carbon tank 808 through collecting pipe 807. After the activated carbon in activated carbon tank 808 absorbs hydrogen sulfide, it is transported to alkaline washing box 810 through transfer pipe 809, so that the alkaline solution in alkaline washing box 810 can clean and absorb hydrocyanic acid).

[0033] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A zirconium-hafnium solution crystallization separation device, comprising a housing (1), characterized in that: The upper side of the box body (1) is fixedly connected to a top cover (4), and a mixing efficiency enhancement module (6) is arranged below the top cover (4). The mixing efficiency enhancement module (6) is located inside the box body (1), and a reaction barrel (9) is arranged inside the box body (1). The mixing efficiency enhancement module (6) comprises a connecting platform (606), a receiving groove (619) is provided at the bottom of the connecting platform (606), a push rod (620) is slidably connected in the receiving groove (619), a connecting rod (621) is fixedly connected to the bottom of the push rod (620), and a second motor (624) is fixedly connected to the inner wall of the bottom of the box body (1), and an output end of the second motor (624) is connected to a rotating rod (622) via a coupling, and a portion of the rotating rod (622) close to the connecting rod (621) is connected to the rotating rod (622). A circular groove is provided on the side, a hydraulic rod 2 (623) is fixedly connected to the inner wall of the circular groove, the output end of the hydraulic rod 2 (623) is fixedly connected to the side opposite to the connecting rod (621), the box body (1) is provided with an exhaust gas treatment module (8), the exhaust gas treatment module (8) is located outside the reaction barrel (9), and the box body (1) is provided with an extraction module (7), a notch is provided on one side of the box body (1), a sealing door (2) is connected to the inner wall of one side of the notch through a hinge, an observation window (3) is provided on the sealing door (2), and two symmetrical circular holes are provided on the side of the box body (1) close to the sealing door (2), a delivery pipe (5) is fixedly connected in each of the circular holes, and the two delivery pipes (5) are connected to the side opposite to the reaction barrel (9) through a flange.

2. The zirconium-hafnium solution crystallization separation equipment according to claim 1, characterized in that: The bottom of the top cover (4) is fixedly connected to a hydraulic rod 1 (601), the output end of the hydraulic rod 1 (601) is fixedly connected to a fixing box (602), the top inner wall of the fixing box (602) is fixedly connected to a motor 1 (609), and a fine hole is opened at the bottom of the fixing box (602), and a main shaft (608) is movably connected in the fine hole, the upper side of the main shaft (608) is connected to the output end of the motor 1 (609) via a coupling, the main shaft (608) is located inside the reaction barrel (9), and the outside of the main shaft (608) is fixedly connected to two symmetrical cross bars 1 (610).

3. The zirconium-hafnium solution crystallization separation device according to claim 2, characterized in that: Two symmetrical secondary shafts (611) are movably connected to opposite sides of the two crossbars (610); the exteriors of the two secondary shafts (611) are fixedly connected to gears (612); the gears (612) are located above the crossbar (610); the exterior of the fixed box (602) is fixedly connected to a shielding cover (603); the inner wall of the shielding cover (603) is fixedly connected to an inner gear ring (613); and the two gears (612) are meshed with the inner gear ring (613).

4. The zirconium-hafnium solution crystallization separation device according to claim 3, characterized in that: The exterior of the secondary shaft (611) is fixedly connected to two symmetrical second cross bars (614), each of which is located between the two first cross bars (610), and the opposite sides of the two second cross bars (614) located on the same side are fixedly connected to two symmetrical vertical bars (615), and the exterior of the vertical bars (615) is fixedly connected to a plurality of stirring bars (616) distributed at equal distances.

5. The zirconium-hafnium solution crystallization separation device according to claim 4, characterized in that: The inner wall of the box body (1) is fixedly connected to a mounting frame (604), the mounting frame (604) is located outside the reaction barrel (9), the inner wall of the mounting frame (604) is fixedly connected to a plurality of springs (605) distributed at equal intervals around the circumference, one end of the spring (605) away from the mounting frame (604) is fixedly connected to the outside of the reaction barrel (9), and the inner wall of the box body (1) is fixedly connected to a support plate (607), the support plate (607) is located below the reaction barrel (9) and outside the connecting platform (606), an annular groove (617) is provided on the upper side of the support plate (607), and the bottom of the reaction barrel (9) is fixedly connected to a plurality of spherical rollers (618) distributed at equal intervals around the circumference, the outside of the spherical rollers (618) are in contact with the bottom inner wall of the annular groove (617).

6. The zirconium-hafnium solution crystallization separation device according to claim 5, characterized in that: The extraction module (7) comprises a fixed frame (701), the fixed frame (701) being fixedly connected to a side opposite to the inner wall of the box body (1), a hole groove being provided on the fixed frame (701), a screw rod (702) being movably connected in the hole groove, an isolation cover (704) being fixedly connected to the upper side of the fixed frame (701), a motor three (703) being fixedly connected to the top inner wall of the isolation cover (704), an output end of the motor three (703) being connected to the upper side of the screw rod (702) via a coupling, and a movable block (705) being arranged outside the screw rod (702), and the outer portion of the movable block (705) being slidably connected to the inner wall of the fixed frame (701).

7. The zirconium-hafnium solution crystallization separation device according to claim 6, characterized in that: The movable block (705) is provided with a circular notch, an extraction tube (706) is fixedly connected in the circular notch, one end of the extraction tube (706) away from the movable block (705) is located inside the reaction barrel (9), one end of the extraction tube (706) close to the movable block (705) is fixedly connected to a hose (707), one end of the hose (707) away from the extraction tube (706) is fixedly connected to a discharge tube (708), and a circular hole is provided on the inner wall of one side of the box body (1) close to the fixed frame (701), and the inner wall of the circular hole is fixedly connected to the outside of the discharge tube (708).

8. The zirconium-hafnium solution crystallization separation device according to claim 7, characterized in that: The exhaust gas treatment module (8) comprises two symmetrical air intake frames (801), the bottoms of the two air intake frames (801) are fixedly connected to the upper side of the support plate (607), the air intake frames (801) are provided with slots, the inner walls of the slots are fixedly connected to filter screens (802), and the top cover (4) is provided with two symmetrical circular openings, the circular openings are fixedly connected to air supply pipes (803), the upper sides of the air intake frames (801) are provided with holes, the inner walls of the two holes are respectively fixedly connected to the outside of the two air supply pipes (803), the ends of the two air supply pipes (803) away from the air intake frames (801) are fixedly connected to air guide pipes (804), and the ends of the two air guide pipes (804) away from the air supply pipes (803) are fixedly connected to the same air collecting box (805).

9. The zirconium-hafnium solution crystallization separation device according to claim 8, characterized in that: An air pump (806) is fixedly connected to the upper side of the air collecting box (805); an input end of the air pump (806) is connected to the outside of the air collecting box (805) via a conduit; an output end of the air pump (806) is connected to a collecting pipe (807) via a round pipe; an end of the collecting pipe (807) away from the air pump (806) is fixedly connected to an activated carbon canister (808); an end of the activated carbon canister (808) away from the collecting pipe (807) is fixedly connected to a transfer pipe (809); an end of the transfer pipe (809) away from the activated carbon canister (808) is externally provided with an alkaline gas washing box (810); and the bottom of the alkaline gas washing box (810) is fixedly connected to the upper side of the top cover (4).

10. A method for crystallizing and separating a zirconium-hafnium solution, using the device for crystallizing and separating a zirconium-hafnium solution according to claim 9, characterized in that: The steps include: Step 1: After the zirconium-hafnium solid compound is placed in a reaction barrel (9), a solvent is transported into the reaction barrel (9) through a transport pipe (5) to dissolve the zirconium-hafnium solid compound. During the dissolution process, the solvent is stirred using a mixing and synergistic module (6); Step 2: Add the extractant, stir for a period of time, let it stand, and after the solution is separated into layers, use the extraction module (7) to extract the upper layer of solution. Step 3: add sulfuric acid solution to the remaining solution in the reaction barrel (9) through the delivery pipe (5), stir the reaction barrel (9), and then let it stand to allow the solution to crystallize and precipitate. During the whole process, use the waste gas treatment module (8) to absorb and wash the waste gas generated in the equipment.

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