Continuous purification device for hafnium chloride processing

By designing a continuous purification device with multiple reaction tanks, continuous circulation of impurity removal, purification and cooling and cooling processes is realized, and the problem of low purification efficiency of existing devices is solved, significantly improving the purification efficiency and process safety of hafnium chloride.

CN222907557UActive Publication Date: 2025-05-27JIANGXI JINGHUI ZIRCONIUM HAFNIUM NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202421850326.9
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-08-01
Publication Date
2025-05-27
Estimated Expiration
2034-08-01

AI Technical Summary

Technical Problem

The existing hafnium chloride purification device is carried out in the same reaction tank at the same time in multiple processes, resulting in an increase in the overall purification time and a decrease in the purification efficiency.

Method used

A continuous purification device including three reaction tanks is designed. Each reaction tank corresponds to a station for decomposition, purification and cooling. The three reaction tanks are continuously circulated through the adjustment components to achieve continuous purification.

Benefits of technology

Through continuous process cycles, the time waiting for the previous process to be completed is removed, the purification efficiency of hafnium tetrachloride is significantly improved, and the reaction tank is prevented from shifting through the limit design of the rubber rod and the retaining ring, and the rapid cooling device improves the cooling efficiency of the reaction tank.

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Abstract

The utility model relates to a hafnium chloride purification device, in particular to a continuous purification device for processing hafnium chloride. A continuous purification device for hafnium chloride processing comprises a base, a heater and the like. Heaters are arranged at the middle part and the rear part of the base, an adjusting assembly is arranged at the right part of the base, three reaction tanks are arranged on the adjusting assembly, square feeding holes are formed in the tops of the three reaction tanks, baffles are connected to the tops of the three reaction tanks in a sliding manner, and the baffles can seal the square feeding holes formed in the adjacent reaction tanks; a telescopic pipe is arranged on the side wall of the condensation tank. The three reaction tanks are arranged and correspond to the impurity removal station, the purification station and the cooling station respectively, the positions of the three reaction tanks can be replaced by rotating the connecting frame, the three working procedures are continuously circulated, the time needed for waiting for the completion of the previous working procedure is omitted, and then continuous purification of hafnium tetrachloride is achieved; the purification efficiency of hafnium tetrachloride is greatly improved.
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Description

Technical Field

[0001] The utility model relates to a hafnium chloride purification device, in particular to a continuous purification device for hafnium chloride processing. Background Art

[0002] Hafnium tetrachloride is a kind of hafnium chloride, which has broad application prospects in the fields of materials science, catalysts, semiconductor industry, etc., and is an important inorganic compound.

[0003] The patent with the publication number CN112624193B discloses a purification method of hafnium tetrachloride, which includes mixing and heating crude hafnium tetrachloride containing impurities and a mixed molten salt. The mixed molten salt includes sodium chloride, potassium chloride and zirconium powder, and the impurities with lower boiling points are volatilized and discharged at 270 - 340°C respectively, and the gaseous hafnium tetrachloride is condensed by opening a condensation trap at 580 - 620°C to obtain hafnium tetrachloride with higher purity. The heating and melting temperature of the reaction tank is reduced to below 300°C, and crude HfCl4 containing impurities and the mixed molten salt are continuously added into the reaction tank, and the above steps are repeated to realize the continuous purification of hafnium tetrachloride. The invention can effectively improve the purification efficiency of hafnium tetrachloride and avoid using flammable and explosive gases for purification operations, thereby improving the safety of the process.

[0004] However, when the above scheme is implemented, multiple processes are carried out in the same reaction tank, and the next process can only be carried out after the previous process is completed. This increases the overall purification time and reduces the purification efficiency. Summary of the Utility Model

[0005] In order to overcome the above-mentioned shortcomings in the prior art, the technical problem of the utility model is: to provide a continuous purification device for hafnium chloride processing.

[0006] The technical implementation scheme of the utility model is: a continuous purification device for hafnium chloride processing, which includes a base, a heater, an adjustment component, a reaction tank, a baffle, a condensation tank and a telescopic pipe. Heaters are arranged in the middle and rear of the base, and an adjustment component is arranged on the right of the base. Three reaction tanks are arranged on the adjustment component. Square feeding ports are opened at the tops of the three reaction tanks. Baffles are slidably connected to the tops of the three reaction tanks, and the baffle can close the square feeding ports arranged on adjacent reaction tanks. A condensation tank is arranged on the left of the base, and a telescopic pipe is arranged on the side wall of the condensation tank. A valve is arranged on the side of the telescopic pipe close to the condensation tank. Valve pipes are arranged on the side walls of the three reaction tanks. When the telescopic pipe extends, it can be connected to the valve pipe. The adjustment component is used to adjust the positions of the three reaction tanks so that the three reaction tanks can be respectively connected to the condensation tank through the valve pipe and the telescopic pipe. It also includes a feeding component, and a feeding component for adding reaction raw materials into the reaction tank is arranged on the adjustment component.

[0007] Optionally, the adjustment component includes a short shaft, a connecting frame, and a placement tray. A short shaft is fixedly connected to the middle of the right part of the base. A connecting frame is rotatably connected to the short shaft. Three placement trays are fixedly connected to the connecting frame at intervals. The three reaction vessels are respectively arranged on the three placement trays.

[0008] Optionally, the feeding component includes an L-shaped bracket, a material frame, a lid, and a sealing plate. An L-shaped bracket is fixedly connected to the top of the short shaft. The end of the L-shaped bracket away from the short shaft is fixedly connected to a material frame. A lid is rotatably connected to the top of the material frame. A sealing plate is slidably connected to the bottom of the material frame.

[0009] Optionally, it further includes a clamping rod. The clamping rod is slidably connected to the sealing plate. Jack holes are formed on all three baffle plates. The clamping rod can be inserted into the jack holes.

[0010] Optionally, it further includes a rubber rod and a snap ring. The rubber rod is arranged on the left part of the base. Snap rings are arranged on the side walls of all three placement trays.

[0011] Optionally, it further includes a recovery box and a sprayer. The recovery box is arranged on the right part of the base. The sprayer is arranged on the side wall of the recovery box.

[0012] Compared with the prior art, the utility model has the following advantages: 1. By arranging three reaction vessels, the three reaction vessels respectively correspond to the workstations of impurity removal, purification, and cooling, and the positions of the three reaction vessels can be changed by rotating the connecting frame, so that the three processes are continuously cycled, eliminating the time required to wait for the completion of the previous process, thereby achieving continuous purification of hafnium tetrachloride and greatly improving the purification efficiency of hafnium tetrachloride.

[0013] 2. By arranging the rubber rod and the snap ring, the position of the placement tray is limited, thereby preventing the reaction vessel from shifting and failing to dock with the telescopic tube.

[0014] 3. By arranging the recovery box and the sprayer, the sprayer sprays the cooling water in the recovery box onto the reaction vessel in the cooling process, thereby achieving rapid cooling of the reaction vessel. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a three-dimensional structural schematic diagram of the utility model.

[0016] Figure 2 It is a three-dimensional structural schematic diagram of the heater, reaction vessel, baffle, etc.

[0017] Figure 3 It is a three-dimensional structural schematic diagram of the material frame, lid, clamping rod, etc.

[0018] Figure 4 It is a three-dimensional structural schematic diagram of the rubber rod, recovery box, sprayer, etc.

[0019] Meanings of the reference numerals in the drawings: 1: base, 2: heater, 3: reaction tank, 4: baffle, 5: condensation tank, 6: telescopic pipe, 7: short shaft, 71: connecting frame, 8: placement tray, 9: L-shaped bracket, 10: material box, 11: lid, 111: sealing plate, 12: clamping rod, 13: snap ring, 14: rubber rod, 15: recycling box, 16: sprayer. Specific embodiments

[0020] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0021] Embodiment: A continuous purification device for hafnium chloride processing, as Figures 1-4 shown, includes a base 1, a heater 2, an adjustment component, a reaction tank 3, a baffle 4, a condensation tank 5, and a telescopic pipe 6. Heaters 2 are provided in the middle and rear parts of the base 1, and an adjustment component is provided on the right part of the base 1. Three reaction tanks 3 are provided on the adjustment component. Square feeding ports are opened at the tops of the three reaction tanks 3. Baffles 4 are slidably connected to the tops of the three reaction tanks 3. The baffle 4 can close the square feeding ports provided on adjacent reaction tanks 3. Stirring motors, exhaust valves, and thermometers are provided at the tops of the three reaction tanks 3. Stirring rods are provided inside the three reaction tanks 3. The stirring motor is used to drive the stirring rod to stir the reaction raw materials in the reaction tank 3. The stirring rod is a common component, so it is not shown additionally in the drawings. The thermometer is used to display the reaction temperature in the reaction tank in real time. A condensation tank 5 is provided on the left part of the base 1. A telescopic pipe 6 is provided on the side wall of the condensation tank 5. A valve is provided on the side of the telescopic pipe 6 close to the condensation tank 5. Valve pipes are provided on the side walls of the three reaction tanks 3. When the telescopic pipe 6 extends, it can be connected to the valve pipe. The adjustment component is used to adjust the positions of the three reaction tanks 3 so that the three reaction tanks 3 can be respectively connected to the condensation tank 5 through the valve pipe and the telescopic pipe 6. It further includes a feeding component, and a feeding component for adding reaction raw materials into the reaction tank 3 is provided on the adjustment component.

[0022] As Figure 2 shown, the adjustment component includes a short shaft 7, a connecting frame 71, and a placement tray 8. A short shaft 7 is fixedly connected to the middle of the right part of the base 1. A connecting frame 71 is rotatably connected to the short shaft 7. Three placement trays 8 are fixedly connected to the connecting frame 71 at intervals. The three reaction tanks 3 are respectively arranged on the three placement trays 8.

[0023] As Figure 3As shown in the figure, the feeding assembly includes an L-shaped bracket 9, a material box 10, a lid 11 and a sealing plate 111. The top of the short shaft 7 is fixedly connected with the L-shaped bracket 9. The end of the L-shaped bracket 9 away from the short shaft 7 is fixedly connected with the material box 10. The top of the material box 10 is rotatably connected with the lid 11, and the bottom of the material box 10 is slidably connected with the sealing plate 111.

[0024] First, open the lid 11, add a sufficient amount of reaction raw materials into the material box 10, then pull out the sealing plate 111 and the baffle 4 respectively. The reaction raw materials in the material box 10 fall into the reaction tank 3. Start the heater 2 at the rear side. The heater 2 heats the reaction tank 3 located on it through the placement plate 8, so that the reaction temperature of the reaction raw materials in the reaction tank 3 reaches 270 - 340 °C. At this time, a part of the impurities volatilize to form gaseous impurity chlorides, and another part of the impurities form impurity alkali metal chloride double salts and dissolve in the reaction tank 3. Open the exhaust valve provided at the top of the reaction tank 3 to discharge the gaseous impurity chlorides from the reaction tank 3. After closing the exhaust valve, rotate the connecting frame 71 counterclockwise by 120 degrees to make the placement plate 8 drive the reaction tank 3 to move to a position close to the condensation tank 5. At this time, start the heater 2 at the front side. Here, the heater 2 heats the reaction tank 3 through the placement plate 8, so that the reaction temperature of the reaction raw materials in the reaction tank 3 reaches 580 - 620 °C. At this time, hafnium tetrachloride volatilizes. Stretch out the telescopic tube 6 and connect it to the valve tube provided on the side wall of the reaction tank 3. Open the valve tube, and at the same time open the valve provided on the telescopic tube 6 to connect the condensation tank 5 with the reaction tank 3. The gaseous hafnium tetrachloride enters the condensation tank 5 through the valve tube and the telescopic tube 6. The condensation tank 5 condenses the gaseous hafnium tetrachloride to obtain purified liquid hafnium tetrachloride and collect it. Since there are three reaction tanks 3, and the three reaction tanks 3 correspond to the workstations of impurity removal, purification and cooling respectively, the time required to wait for the completion of the previous process is removed, achieving the effect of continuous purification processing and greatly improving the purification efficiency of hafnium tetrachloride.

[0025] As Figure 3 shown, it further includes a clamping rod 12. The clamping rod 12 is slidably connected to the sealing plate 111. Jack holes are opened on all three baffles 4, and the clamping rod 12 can be inserted into the jack holes.

[0026] By setting the clamping rod 12, when it is necessary to pull out the baffle 4 and the sealing plate 111, the clamping rod 12 can be inserted downward into the jack hole provided on the sealing plate 111. At this time, the baffle 4 and the sealing plate 111 can be pulled out simultaneously.

[0027] As Figure 4 shown, it further includes a rubber rod 14 and a snap ring 13. The rubber rod 14 is provided at the left part of the base 1, and snap rings 13 are provided on the side walls of all three placement plates 8.

[0028] By setting the rubber rod 14 and the snap ring 13, every time the connecting frame 71 rotates 120 degrees, the snap ring 13 provided on the placement tray 8 close to the condensation tank 5 will have an interference fit with the rubber rod 14, thereby limiting the placement tray 8 and further preventing the reaction tank 3 from shifting and failing to dock with the telescopic tube 6.

[0029] As Figure 1 and Figure 4 shown, it further includes a recovery frame 15 and a sprayer 16. The recovery frame 15 is provided on the right part of the base 1, and the sprayer 16 is provided on the side wall of the recovery frame 15.

[0030] By setting the recovery frame 15 and the sprayer 16, the staff adds cooling water to the recovery frame 15 and starts the sprayer 16. The sprayer 16 pumps the cooling water in the recovery frame 15 upward to the upper part of the adjacent reaction tank 3 and sprays it out, thereby cooling the reaction tank 3 and enabling the reaction tank 3 in a high-temperature state to cool down quickly.

[0031] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes can be made therein without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A continuous purification device for hafnium chloride processing, characterized in that: The invention comprises a base (1), a heater (2), an adjustment component, a reaction tank (3), a baffle (4), a condensation tank (5) and a telescopic tube (6); the middle and rear parts of the base (1) are provided with a heater (2); the right part of the base (1) is provided with an adjustment component; three reaction tanks (3) are provided on the adjustment component; the tops of the three reaction tanks (3) are provided with a square feed opening; the tops of the three reaction tanks (3) are slidably connected with a baffle (4); the baffle (4) can close the square feed opening provided on the adjacent reaction tanks (3); the left part of the base (1) is provided with a A condensation tank (5), a telescopic tube (6) is arranged on the side wall of the condensation tank (5), a valve is arranged on the side of the telescopic tube (6) close to the condensation tank (5), valve tubes are arranged on the side walls of the three reaction tanks (3), and when the telescopic tube (6) is extended, it can be connected to the valve tube, and the adjustment component is used to adjust the positions of the three reaction tanks (3) so that the three reaction tanks (3) can be connected to the condensation tank (5) respectively through the valve tube and the telescopic tube (6), and also includes a feeding component, and the adjustment component is provided with a feeding component for adding reaction raw materials into the reaction tank (3).

2. A continuous purification device for hafnium chloride processing according to claim 1, characterized in that: The adjustment component comprises a short shaft (7), a connecting frame (71) and a placement plate (8); the short shaft (7) is fixedly connected to the middle of the right part of the base (1); the connecting frame (71) is rotatably connected to the short shaft (7); three placement plates (8) are fixedly connected to the connecting frame (71) at intervals; and the three reaction tanks (3) are respectively arranged on the three placement plates (8).

3. A continuous purification device for hafnium chloride processing according to claim 2, characterized in that: The feeding assembly comprises an L-shaped bracket (9), a material frame (10), a cover (11) and a sealing plate (111); the top of the short shaft (7) is fixedly connected to the L-shaped bracket (9); the end of the L-shaped bracket (9) away from the short shaft (7) is fixedly connected to the material frame (10); the top of the material frame (10) is rotatably connected to the cover (11); and the bottom of the material frame (10) is slidably connected to the sealing plate (111).

4. A continuous purification device for hafnium chloride processing according to claim 3, characterized in that: It also includes a clamping rod (12), which is slidably connected to the sealing plate (111), and each of the three baffles (4) is provided with an insertion hole, into which the clamping rod (12) can be inserted.

5. A continuous purification device for hafnium chloride processing according to claim 4, characterized in that: It also includes a rubber rod (14) and a snap ring (13). The left part of the base (1) is provided with the rubber rod (14), and the side walls of the three placement plates (8) are all provided with snap rings (13).

6. A continuous purification device for hafnium chloride processing according to claim 5, characterized in that: It also includes a recovery frame (15) and a sprayer (16). The recovery frame (15) is arranged on the right part of the base (1), and the sprayer (16) is arranged on the side wall of the recovery frame (15).

Citation Information

Patent Citations

  • A method for purifying hafnium tetrachloride

    CN112624193B