Device for removing iron from high-purity hafnium tetrachloride

Abstract

The application discloses a device for preparing high-purity hafnium tetrachloride and removing iron, relates to the technical field of hafnium tetrachloride purification, and comprises a mixing treatment device, the mixing treatment device comprises a first outer shell, a stirring device is arranged below the first outer shell, an inert gas filling pipe is arranged on the left side of the stirring device and at the bottom of the first outer shell, a first electromagnetic control valve is arranged on the inert gas filling pipe, a first discharge pipe is arranged on the right side of the stirring device and at the bottom of the first outer shell, a second electromagnetic control valve is arranged on the first discharge pipe, and a first check valve is arranged below the second electromagnetic control valve and on the first discharge pipe. The raw materials are stirred by the stirring device, inert gas is filled upwards from the bottom of the first outer shell through the inert gas filling pipe, air can be better discharged, the inert gas adopts a gas with a relative molecular mass greater than that of air, for example, argon, and air is discharged to the outside through the exhaust valve.

Description

Technical Field

[0001] This invention relates to the field of hafnium tetrachloride purification technology, specifically to an iron removal device for preparing high-purity hafnium tetrachloride. Background Technology

[0002] High-purity hafnium tetrachloride is an important hafnium compound, widely used in the semiconductor industry, especially in the production of integrated circuits and microelectronic devices. It is also widely used in materials science, electronic devices, and high-temperature alloys.

[0003] Iron removal is a crucial step in the preparation of hafnium tetrachloride, as the presence of iron affects its purity and performance. Current technologies employ acid leaching, solvent extraction, and high-temperature reduction methods to remove iron impurities from hafnium tetrachloride. The conversion of low-purity hafnium tetrachloride containing impurities to high-purity hafnium tetrachloride requires multiple processes. During this conversion, iron must be converted into ionic compounds, which are then extracted from the mixture using an extractant. High-purity hafnium tetrachloride is obtained only after precipitation and reduction. Current technologies lack integrated, multi-functional, and continuously processing hafnium tetrachloride iron removal devices, failing to efficiently remove iron impurities and thus hindering the improvement of hafnium tetrachloride purity. Therefore, a highly efficient iron removal and purification device for hafnium tetrachloride is needed. Summary of the Invention

[0004] The purpose of this invention is to provide an iron removal device for preparing high-purity hafnium tetrachloride, so as to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] A device for preparing high-purity hafnium tetrachloride and removing iron includes a mixing and processing device, an acid-base balancing device below the mixing and processing device, an extraction device below the acid-base balancing device, a precipitation and drying device below the extraction device, a belt conveyor device to the right of the precipitation and drying device, and a calcining furnace to the right of the belt conveyor device.

[0007] The mixing and processing device includes a first outer shell. A stirring device is disposed below the first outer shell. An inert gas injection pipe is disposed to the left of the stirring device at the bottom of the first outer shell, and a first electromagnetic control valve is disposed on the inert gas injection pipe. A first discharge pipe is disposed to the right of the stirring device at the bottom of the first outer shell, and a second electromagnetic control valve is disposed on the first discharge pipe. A first check valve is disposed below the second electromagnetic control valve on the first discharge pipe. A gas extraction pipe is disposed at the top left of the first outer shell, and a drying chamber is disposed on the gas extraction pipe. A third electromagnetic control valve is disposed to the right of the drying chamber on the gas extraction pipe. A distilled water filling pipe is provided on the top front side of the housing, and a fourth electromagnetic control valve is provided on the distilled water filling pipe. An air intake pipe is provided on the top right side of the first housing, and a fifth electromagnetic control valve is provided on the air intake pipe. A first cover plate is provided on the top of the first housing, and an exhaust valve is provided on the first cover plate. A first paramagnetic oxygen sensor is provided on the exhaust valve. A concentrated hydrochloric acid filling pipe is provided to the left of the exhaust valve, and a sixth electromagnetic control valve is provided on the concentrated hydrochloric acid filling pipe. A vacuum degree detection sensor is provided to the left of the concentrated hydrochloric acid filling pipe. A raw material inlet pipe is provided to the left of the vacuum degree detection sensor, and a seventh electromagnetic control valve is provided on the raw material inlet pipe.

[0008] As a further embodiment of the present invention: the stirring device includes a first geared motor, a first stirring rod is fixedly mounted on the output shaft of the first geared motor, a guide fluid is rotatably mounted on the bottom of the first stirring rod through a bearing, and a guide cone is fixedly mounted on the top of the first stirring rod.

[0009] As a further embodiment of the present invention: the acid-base balance device includes a second outer shell, a stirring device is provided at the bottom of the second outer shell, a second cover plate is provided above the second outer shell, an alkaline solution injection pipe is fixedly provided on the second cover plate, an eighth electromagnetic control valve is provided on the alkaline solution injection pipe, a first peristaltic pump is provided at the outlet of the alkaline solution injection pipe, a pH detector is provided at the bottom of the second outer shell, a second discharge pipe is provided below the second outer shell, a second one-way valve is provided on the second discharge pipe, and a ninth electromagnetic control valve is provided below the second one-way valve on the second discharge pipe.

[0010] As a further embodiment of the present invention: the extraction device includes a third outer shell, a stirring device is provided below the third outer shell, a third cover plate is provided above the third outer shell, an extractant addition tube is fixedly provided on the third cover plate, a tenth electromagnetic control valve is fixedly provided on the extractant addition tube, a second peristaltic pump is provided at the outlet of the extractant addition tube, a third discharge pipe is provided below the third outer shell, a third one-way valve is provided on the third discharge pipe, a three-way electromagnetic valve is provided at the outlet of the third discharge pipe, and a first extraction discharge pipe and a second extraction discharge pipe are respectively provided on the three-way electromagnetic valve.

[0011] As a further embodiment of the present invention: the precipitation drying device includes a fourth outer shell, a first vent pipe is provided below the fourth outer shell, a fourth one-way valve is provided on the first vent pipe, an eleventh electromagnetic control valve is provided below the fourth one-way valve on the first vent pipe, a Venturi dryer is provided at the air inlet of the first vent pipe, a drain pipe is provided on one side of the first vent pipe below the fourth outer shell, a twelfth electromagnetic control valve is provided on the drain pipe, a stepped through hole is opened on the side wall of the fourth outer shell, a sealing door is slidably provided in the stepped through hole, a first electric push rod that cooperates with the sealing door is embedded in the side plate of the fourth outer shell, a fourth cover plate is provided on the fourth outer shell, and a square through hole is opened on the fourth cover plate. Limiting blocks are fixedly installed on both sides, and a movable seat is slidably installed between the two limiting blocks. A second electric push rod that cooperates with the movable seat is installed on the outside of the limiting blocks. A second reduction motor is fixedly installed on the movable seat, and the output shaft of the second reduction motor passes through the movable seat. A second stirring rod is fixedly installed on the output shaft of the second reduction motor. A lifting filter device is installed between the two limiting blocks on the fourth cover plate. The outlet of the second extraction outlet pipe is connected to the fourth cover plate. A precipitation solution injection pipe is installed on the fourth cover plate. A thirteenth electromagnetic control valve is installed on the precipitation solution injection pipe. A third peristaltic pump is installed at the inlet of the precipitation solution injection pipe. A cleaning injection pipe is installed on the fourth cover plate. A fourteenth electromagnetic control valve is installed on the cleaning injection pipe.

[0012] As a further embodiment of the present invention: a limiting block is fixedly provided on the inner side of the stepped through hole on the inner wall of the fourth outer shell.

[0013] As a further embodiment of the present invention: the lifting filter device includes two slide rails, on which sliding blocks are slidably mounted via sliders, and rotating blocks are rotatably mounted between adjacent sliding blocks. A bracket is provided inside the fourth outer shell below the slide rails, and rotating seats are fixedly provided on both sides of the upper end face of the bracket. A third electric push rod is provided between the rotating block and the rotating seat, and a filter mechanism is provided below the bracket.

[0014] As a further embodiment of the present invention: the filter mechanism includes a filter body and a telescopic block. A rotating shaft is fixedly provided on both sides of the filter body. A limiting groove that cooperates with the rotating shaft is provided on the inner wall of the fourth outer shell. A flow guiding arc block is provided on one side of the filter body. A sliding column is fixedly provided at both ends of the telescopic block. A telescopic block and a sliding column are slidably provided below the flow guiding arc block and the filter body. A spring that cooperates with the sliding column is provided inside the filter body.

[0015] As a further embodiment of the present invention: the calcining furnace includes a furnace body, a hatch is rotatably mounted on the front side of the furnace body via a hinge, a first air inlet pipe is provided at the bottom left side of the furnace body, a fifteenth electromagnetic control valve is fixedly installed on the first air inlet pipe, a feeding pipe is provided above the furnace body, a sixteenth electromagnetic control valve is installed on the feeding pipe, a collection hopper is provided at the feeding inlet of the feeding pipe, a material adding pipe is provided on one side of the feeding pipe, a seventeenth electromagnetic control valve is installed on the material adding pipe, a second air outlet pipe is provided on one side of the material adding pipe, and an eighteenth electromagnetic control valve is installed on the second air outlet pipe.

[0016] As a further embodiment of the present invention: a second paramagnetic oxygen sensor is provided on the second exhaust pipe below the eighteenth electromagnetic control valve.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] The raw materials are stirred by a stirring device, and inert gas is added from the bottom of the first outer shell upwards through an inert gas injection pipe to better expel air. The inert gas used is argon, which has a relative molecular mass greater than that of air. Air is discharged from the exhaust valve. The first paramagnetic oxygen sensor located on the exhaust valve detects the oxygen content of the discharged gas. When there is no oxygen, the first outer shell is filled with inert gas. The gas extraction pipe extracts the inert gas from the first outer shell after the reaction is completed. The vacuum degree detection sensor monitors the gas pressure in the first outer shell. The drying chamber dries the inert gas, which facilitates the reuse of the inert gas and achieves the purpose of environmental protection and cost saving.

[0019] The alkaline solution is precisely added into the second outer shell by the first peristaltic pump, the stirring device stirs the solution in the second outer shell, and the pH meter monitors the acidity and alkalinity of the solution until the solution shows a neutral solution, which facilitates the subsequent extraction operation of the solution.

[0020] The extractant is precisely added to the third shell by the second peristaltic pump, and the stirring device plays a role in uniform stirring and mixing, so that the extractant can efficiently extract the solution. The three-way solenoid valve divides the solution after extraction and separation, which facilitates the subsequent precipitation treatment of hafnium oxychloride.

[0021] The extracted hafnium oxychloride solution is fed into the fourth shell through the second extraction outlet pipe. The third peristaltic pump adds the precipitate solution into the fourth shell, causing the hafnium oxychloride to be converted into precipitate. The waste liquid is discharged from the drain pipe. The cleaning and filling pipe cleans the precipitate. The Venturi dryer dries the precipitate. The lifting and filtering device lifts the precipitate for easy conveying to the belt conveyor, thereby improving the operating efficiency of the device.

[0022] The combination of telescopic blocks, sliding columns, springs, and filter screen bodies allows the filter screen mechanism to fit tightly against the inner wall of the fourth outer shell, preventing the spillage of sediment and facilitating the feeding of sediment to the belt conveyor. The collection hopper collects solids from the belt conveyor and then feeds them into the furnace, facilitating high-temperature treatment of the collected solids. The material addition pipe delivers reducing agent to the furnace, facilitating the production of high-purity hafnium tetrachloride. Attached Figure Description

[0023] Figure 1 This is a three-dimensional structural diagram of the present invention.

[0024] Figure 2 This is a three-dimensional structural schematic diagram of the mixing and processing device in this invention.

[0025] Figure 3 This is a front view schematic diagram of the mixing and processing device in this invention.

[0026] Figure 4 This is a partial cross-sectional three-dimensional structural schematic diagram of the mixing and processing device in this invention.

[0027] Figure 5 This is a three-dimensional structural diagram of the stirring device in this invention.

[0028] Figure 6 This is a three-dimensional structural diagram of the acid-base balance device in this invention.

[0029] Figure 7 This is a three-dimensional structural diagram of the extraction device in this invention.

[0030] Figure 8 This is a three-dimensional structural diagram of the precipitation drying device in this invention.

[0031] Figure 9 This is a schematic diagram of the main structure of the precipitation drying device in this invention.

[0032] Figure 10 This is an exploded view of the precipitation drying device in this invention.

[0033] Figure 11 This is a three-dimensional structural diagram of the lifting and filtering device in this invention.

[0034] Figure 12This is an exploded view of the filter mechanism in this invention.

[0035] Figure 13 This is a three-dimensional structural diagram of the calcining furnace in this invention.

[0036] Figure reference numerals: 1. Mixing and processing device; 11. First outer shell; 12. Stirring device; 1201. First geared motor; 1202. First stirring rod; 1203. Guide fluid; 1204. Guide cone; 13. Inert gas injection pipe; 14. First electromagnetic control valve; 15. First discharge pipe; 16. First check valve; 17. Second electromagnetic control valve; 18. Gas extraction pipe; 19. Drying oven; 110. Third electromagnetic control valve; 111. Distilled water injection pipe; 112. Fourth electromagnetic control valve; 113. Air inlet pipe; 114. Fifth electromagnetic control valve; 115. First cover plate; 116. Exhaust valve; 117. First paramagnetic oxygen sensor; 118. Concentrated hydrochloric acid injection pipe; 119. 1. Sixth electromagnetic control valve; 120. Vacuum degree detection sensor; 121. Raw material inlet pipe; 122. Seventh electromagnetic control valve; 2. Acid-base balance device; 21. Second outer shell; 22. Second cover plate; 23. Alkaline solution injection pipe; 24. Eighth electromagnetic control valve; 25. First peristaltic pump; 26. pH meter; 27. Second discharge pipe; 28. Second check valve; 29. ​​Ninth electromagnetic control valve; 3. Extraction device; 31. Third outer shell; 33. Third cover plate; 34. Extractant addition pipe; 35. Tenth electromagnetic control valve; 36. Second peristaltic pump; 37. Third discharge pipe; 38. Third check valve; 39. Three-way solenoid valve; 310. First extraction discharge pipe; 311. Second extraction discharge pipe 4. Precipitation drying device; 41. Fourth outer casing; 42. First exhaust pipe; 43. Eleventh solenoid control valve; 44. Fourth check valve; 45. Venturi dryer; 46. Drain pipe; 47. Twelfth solenoid control valve; 48. Stepped through hole; 49. Limiting block; 410. Limiting groove; 411. First electric push rod; 412. Sealing door; 414. Fourth cover plate; 415. Square through hole; 416. Limiting fixing block; 417. Moving seat; 418. Second electric push rod; 419. Second geared motor; 420. Second stirring rod; 421. Precipitation solution filling pipe; 422. Thirteenth solenoid control valve; 423. Third peristaltic pump; 424. Cleaning filling pipe; 425. Fourteenth solenoid control valve. 5. Control valve; 6. Belt conveyor; 7. Calcining furnace; 8. Furnace body; 9. Door; 10. First air inlet pipe; 11. Fifteenth electromagnetic control valve; 12. Collection hopper; 13. Feeding pipe; 14. Sixteenth electromagnetic control valve; 15. Material adding pipe; 16. Seventeenth electromagnetic control valve; 17. Second air outlet pipe; 18. Eighteenth electromagnetic control valve; 19. Second paramagnetic oxygen sensor; 20. Lifting filter device; 21. Slide rail; 22. Sliding block; 33. Rotating block; 44. Third electric push rod; 55. Rotating seat; 66. Support; 77. Filter screen mechanism; 771. Filter screen body; 772. Rotating shaft; 773. Guide arc block; 774. Telescopic block; 775. Sliding column; 776. Spring. Detailed Implementation

[0037] The following embodiments will describe the present invention in detail with reference to the accompanying drawings. In the drawings or description, similar or identical parts are referred to by the same reference numerals, and in practical applications, the shape, thickness, or height of each component may be enlarged or reduced. The embodiments listed in this invention are merely illustrative and not intended to limit the scope of the invention. Any obvious modifications or changes made to this invention do not depart from the spirit and scope of the invention. Example

[0038] Please see Figures 1-13 In this embodiment of the invention, a device for preparing high-purity hafnium tetrachloride and removing iron includes a mixing treatment device 1, an acid-base balancing device 2 below the mixing treatment device 1, an extraction device 3 below the acid-base balancing device 2, a precipitation drying device 4 below the extraction device 3, a belt conveyor device 5 to the right of the precipitation drying device 4, and a calcining furnace 6 to the right of the belt conveyor device 5.

[0039] The mixing and processing device 1 includes a first outer shell 11. A stirring device 12 is disposed below the first outer shell 11. An inert gas injection pipe 13 is disposed on the left side of the stirring device 12 at the bottom of the first outer shell 11, and a first electromagnetic control valve 14 is disposed on the inert gas injection pipe 13. A first discharge pipe 15 is disposed on the right side of the stirring device 12 at the bottom of the first outer shell 11, and a second electromagnetic control valve 17 is disposed on the first discharge pipe 15. A first check valve 16 is disposed below the second electromagnetic control valve 17 on the first discharge pipe 15. A first one-way valve 16 is disposed on the top left side of the first outer shell 11. A gas extraction pipe 18 is provided, and a drying chamber 19 is installed on the gas extraction pipe 18. A third electromagnetic control valve 110 is installed on the right side of the drying chamber 19 on the gas extraction pipe 18. A distilled water filling pipe 111 is provided on the top front side of the first outer casing 11, and a fourth electromagnetic control valve 112 is installed on the distilled water filling pipe 111. An air intake pipe 113 is provided on the top right side of the first outer casing 11, and a fifth electromagnetic control valve 114 is installed on the air intake pipe 113. A first cover plate 115 is provided on the top of the first outer casing 11, and an exhaust valve 116 is installed on the first cover plate 115. The exhaust valve 116 is equipped with a first paramagnetic oxygen sensor 117. A concentrated hydrochloric acid filling pipe 118 is located to the left of the exhaust valve 116. A sixth electromagnetic control valve 119 is installed on the concentrated hydrochloric acid filling pipe 118. A vacuum degree detection sensor 120 is located to the left of the concentrated hydrochloric acid filling pipe 118. A raw material inlet pipe 121 is located to the left of the vacuum degree detection sensor 120. A seventh electromagnetic control valve 122 is installed on the raw material inlet pipe 121. The raw material is stirred by the stirring device 12, and inert gas is injected from the bottom of the first outer casing 11 upwards through the inert gas filling pipe 13, which can better... Air is discharged, and the inert gas used is one with a relative molecular mass greater than that of air, such as argon. The air is discharged from the exhaust valve 116. The first paramagnetic oxygen sensor 117 located on the exhaust valve 116 detects the oxygen content of the discharged gas. When there is no oxygen, the first outer shell 11 is filled with inert gas. The gas extraction pipe 18 extracts the inert gas from the first outer shell 11 after the reaction is completed. The vacuum degree detection sensor 120 monitors the gas pressure inside the first outer shell 11. The drying chamber 19 dries the inert gas, which facilitates the reuse of the inert gas and achieves the purpose of environmental protection and cost saving.

[0040] The stirring device 12 includes a first reduction motor 1201, a first stirring rod 1202 is fixedly mounted on the output shaft of the first reduction motor 1201, a guide fluid 1203 is rotatably mounted on the bottom of the first stirring rod 1202 through a bearing, and a guide cone 1204 is fixedly mounted on the top of the first stirring rod 1202.

[0041] The acid-base balancing device 2 includes a second outer shell 21. A stirring device 12 is installed at the bottom of the second outer shell 21. A second cover plate 22 is installed above the second outer shell 21. An alkaline solution injection pipe 23 is fixedly installed on the second cover plate 22. An eighth electromagnetic control valve 24 is installed on the alkaline solution injection pipe 23. A first peristaltic pump 25 is installed at the outlet of the alkaline solution injection pipe 23. A pH meter 26 is installed at the bottom of the second outer shell 21. A second discharge pipe 27 is installed below the second outer shell 21. A second one-way valve 28 is installed on the second discharge pipe 27. A ninth electromagnetic control valve 29 is installed below the second one-way valve 28 on the second discharge pipe 27. The alkaline solution is precisely injected into the second outer shell 21 by the first peristaltic pump 25. The stirring device 12 stirs the solution in the second outer shell 21. The pH meter 26 monitors the acid-base value of the solution until the solution shows a neutral solution, which facilitates the subsequent extraction operation of the solution.

[0042] The extraction device 3 includes a third outer shell 31, a stirring device 12 below the third outer shell 31, a third cover plate 33 above the third outer shell 31, an extractant addition tube 34 fixedly mounted on the third cover plate 33, a tenth electromagnetic control valve 35 fixedly mounted on the extractant addition tube 34, a second peristaltic pump 36 at the outlet of the extractant addition tube 34, a third discharge tube 37 below the third outer shell 31, a third one-way valve 38 mounted on the third discharge tube 37, and a three-way solenoid valve 39 at the outlet of the third discharge tube 37. A first extraction discharge tube 310 and a second extraction discharge tube 311 are respectively mounted on the three-way solenoid valve 39. The second peristaltic pump 36 precisely adds the extractant into the third outer shell 31, the stirring device 12 uniformly mixes the solution, enabling efficient extraction of the solution by the extractant, and the three-way solenoid valve 39 separates the extracted solution after stratification, facilitating subsequent precipitation of hafnium oxychloride.

[0043] The precipitation drying device 4 includes a fourth outer shell 41. A first vent pipe 42 is disposed below the fourth outer shell 41. A fourth one-way valve 44 is disposed on the first vent pipe 42. An eleventh electromagnetic control valve 43 is disposed below the fourth one-way valve 44 on the first vent pipe 42. A Venturi dryer 45 is disposed at the air inlet of the first vent pipe 42. A drain pipe 46 is disposed on one side of the first vent pipe 42 below the fourth outer shell 41. A twelfth electromagnetic control valve 47 is disposed on the drain pipe 46. A stepped through hole 48 is formed on the side wall of the fourth outer shell 41. The inner side of the stepped through hole 48 is... A limiting block 49 is fixedly installed on the inner wall of the fourth outer shell 41. A sealing door 412 is slidably installed in the stepped through hole 48. A first electric push rod 411 that cooperates with the sealing door 412 is embedded in the side plate of the fourth outer shell 41. A fourth cover plate 414 is provided on the fourth outer shell 41. A square through hole 415 is opened on the fourth cover plate 414. Limiting blocks 416 are fixedly installed on both sides of the square through hole 415. A movable seat 417 is slidably installed between the two limiting blocks 416. A second electric push rod 418 that cooperates with the movable seat 417 is provided on the outside of the limiting blocks 416. A second reduction motor 419 is fixedly mounted on the movable seat 417, and the output shaft of the second reduction motor 419 passes through the movable seat 417. A second stirring rod 420 is fixedly mounted on the output shaft of the second reduction motor 419. A lifting filter device 7 is installed between two limiting and fixing blocks 416 on the fourth cover plate 414. The outlet of the second extraction outlet pipe 311 is connected to the fourth cover plate 414. A precipitation solution injection pipe 421 is installed on the fourth cover plate 414. A thirteenth electromagnetic control valve 422 is installed on the precipitation solution injection pipe 421. A third peristaltic pump 42 is installed at the inlet of the precipitation solution injection pipe 421. 3. A cleaning and filling pipe 424 is provided on the fourth cover plate 414. A fourteenth electromagnetic control valve 425 is provided on the cleaning and filling pipe 424. The extracted hafnium oxychloride solution is fed into the fourth outer shell 41 through the second extraction discharge pipe 311. The third peristaltic pump 423 adds the precipitate solution into the fourth outer shell 41, so that hafnium oxychloride is converted into precipitate. The waste liquid is discharged from the drain pipe 46. The cleaning and filling pipe 424 cleans the precipitate. The Venturi dryer 45 dries the precipitate. The lifting filter device 7 lifts the precipitate for easy conveying to the belt conveyor device 5, thereby improving the operating efficiency of the device.

[0044] The lifting filter device 7 includes two slide rails 71, on which sliding blocks 72 are slidably mounted via sliders. A rotating block 73 is rotatably mounted between adjacent sliding blocks 72. A bracket 76 is provided inside the fourth outer shell 41 below the slide rails 71. Rotating seats 75 are fixedly provided on both sides of the upper surface of the bracket 76. A third electric push rod 74 is provided between the rotating block 73 and the rotating seat 75. A filter screen mechanism 77 is provided below the bracket 76.

[0045] The filter mechanism 77 includes a filter body 771 and a telescopic block 774. A rotating shaft 772 is fixedly installed on both sides of the filter body 771. A limiting groove 410 that cooperates with the rotating shaft 772 is provided on the inner wall of the fourth outer shell 41. A flow-guiding arc block 773 is provided on one side of the filter body 771. Sliding columns 775 are fixedly installed at both ends of the telescopic block 774. The telescopic block 774 and sliding columns 775 are slidably installed below the flow-guiding arc block 773 and slidably mounted with the filter body 771. A spring 776 that cooperates with the sliding column 775 is installed inside the filter body 771. Through the cooperation of the telescopic block 774, sliding column 775, spring 776, and filter body 771, the filter mechanism 77 can fit tightly against the inner wall of the fourth outer shell 41, preventing the sediment from spilling and facilitating the feeding of the sediment to the belt conveyor 5.

[0046] The calcining furnace 6 includes a furnace body 61. A hatch 62 is hinged and rotatably mounted on the front side of the furnace body 61. A first air inlet pipe 63 is located at the bottom left side of the furnace body 61. A fifteenth electromagnetic control valve 64 is fixedly mounted on the first air inlet pipe 63. A feeding pipe 66 is located above the furnace body 61. A sixteenth electromagnetic control valve 67 is mounted on the feeding pipe 66. A collection hopper 65 is located at the feed inlet of the feeding pipe 66. A material adding pipe 68 is located on one side of the feeding pipe 66. A tenth electromagnetic control valve 67 is mounted on the material adding pipe 68. The seventh electromagnetic control valve 69 has a second vent pipe 610 on one side of the material adding pipe 68. The eighteenth electromagnetic control valve 611 is installed on the second vent pipe 610. A second paramagnetic oxygen sensor 612 is installed on the second vent pipe 610 below the eighteenth electromagnetic control valve 611. Solids on the belt conveyor 5 are collected by the collection hopper 65 and then fed into the furnace body 61 to facilitate high-temperature treatment of the collected solids. The material adding pipe 68 delivers a reducing agent to the furnace body 61 to facilitate the production of high-purity hafnium tetrachloride.

[0047] In operation, low-purity hafnium tetrachloride is supplied to the first outer casing 11 via the raw material inlet pipe 121. The first electromagnetic control valve 14 and exhaust valve 116 are opened to supply inert gas to the first outer casing 11. The oxygen content in the exhaust gas is monitored by the first paramagnetic oxygen sensor 117. If the exhaust gas contains no oxygen, the first outer casing 11 is filled with inert gas. Then, the first electromagnetic control valve 14 and exhaust valve 116 are closed, and the fourth electromagnetic control valve 112 is opened to supply distilled water to the first outer casing 11 via the distilled water supply pipe 111. The stirring device 12 is then activated, causing the low-purity hafnium tetrachloride to undergo a hydrolysis reaction with the distilled water, converting the hafnium tetrachloride into hafnium hydroxide. The gas is then discharged from the first outer casing 11 via the gas extraction pipe 18. Gas is extracted and dried in drying chamber 19 for subsequent reuse of inert gas. Vacuum sensor 120 monitors the pressure change inside the first outer shell 11. After the gas in the first outer shell 11 is completely extracted, the fifth electromagnetic control valve 114 is opened to allow air to enter the first outer shell 11. When the vacuum sensor 120 detects no pressure change, the fifth electromagnetic control valve 114 is closed and the sixth electromagnetic control valve 119 is opened, allowing concentrated hydrochloric acid to be added into the first outer shell 11 through the concentrated hydrochloric acid injection pipe 118, converting hafnium hydroxide and iron into hafnium chloride oxychloride, ferric chloride, and ferrous chloride. After the reaction is complete, the fifth electromagnetic control valve 114 and the second electromagnetic control valve 17 are opened, allowing the mixed solution to flow through the first discharge pipe. 15. Feed the material into the second outer shell 21, then open the eighth electromagnetic control valve 24, start the first peristaltic pump 25 and the stirring device 12 to deliver the alkaline solution into the second outer shell 21. The pH meter 26 monitors the change in the acid-base value of the solution until the acid-base value of the solution reaches the set target. Then, close the stirring device 12, the eighth electromagnetic control valve 24 and the first peristaltic pump 25, then open the ninth electromagnetic control valve 29 to feed the adjusted solution into the third outer shell 31. Then, open the tenth electromagnetic control valve 35, start the stirring device 12 and the second peristaltic pump 36 to add the extractant into the third outer shell 31. After extraction is completed, open the three-way solenoid valve 39 to allow the extract containing hafnium oxychloride to be fed from the second extraction outlet pipe 311 to the fourth outer shell 21. Inside the outer casing 41, the thirteenth electromagnetic control valve 422 is opened, and the third peristaltic pump 423 pumps a precipitant, such as ammonia, into the fourth outer casing 41. The second reduction motor 419 is started, causing hafnium oxychloride to precipitate to the bottom of the fourth outer casing 41. After the precipitation reaction is complete, the second electric push rod 418 and the third electric push rod 74 are started, causing the filter screen mechanism 77 and the moving seat 417 to rise, filtering the precipitate above the filter screen mechanism 77. Then, the twelfth electromagnetic control valve 47 is opened, allowing the solution to be discharged from the drain pipe 46. The fourteenth electromagnetic control valve 425 is opened, allowing the cleaning agent to clean the precipitate. After cleaning, the Venturi dryer 45 and the eleventh electromagnetic control valve 43 are opened, allowing hot air to dry the precipitate.Then, the third electric push rods 74 located on both sides of the second stirring rod 420 are controlled respectively, so that the filter screen mechanism 77 and the limiting block 49 form an angle. Under the elastic force of the spring 776, the telescopic block 774 is made to fit against the inner wall of the fourth outer shell 41 to prevent the sediment from spilling. The first electric push rod 411 is activated to open the sealing door 412. The third electric push rod 74, which is away from the sealing door 412, is controlled to move up and down, so that the filter screen body 771 fluctuates, thereby feeding the sediment onto the belt conveyor device 5 and then into the collection hopper 65. The sixteenth electromagnetic control valve 67 is opened to let the sediment fall into the collection hopper 65. Inside furnace 61, calcination furnace 6 is started to calcine the precipitate at high temperature, converting it into hafnium oxide. Then, nitrogen is injected into furnace 61 through the first inlet pipe 63, and the eighteenth electromagnetic control valve 611 is opened. The second paramagnetic oxygen sensor 612 monitors the exhaust gas. When the exhaust gas contains no oxygen, furnace 61 is filled with nitrogen. Then, a reducing agent, such as carbon powder, is added into furnace 61 through material addition pipe 68, and chlorine is added through the first inlet pipe 63. Under high temperature, hafnium oxide is converted into high-purity hafnium tetrachloride, thus completing the purification and iron removal operation of hafnium tetrachloride.

[0048] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0049] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An iron removal apparatus for preparing high-purity hafnium tetrachloride, comprising a mixing and processing device (1), characterized in that, An acid-base balance device (2) is provided below the mixing and processing device (1), an extraction device (3) is provided below the acid-base balance device (2), a precipitation and drying device (4) is provided below the extraction device (3), a belt conveyor device (5) is provided on the right side of the precipitation and drying device (4), and a calcining furnace (6) is provided on the right side of the belt conveyor device (5). The mixing and processing device (1) includes a first outer shell (11), a stirring device (12) is provided below the first outer shell (11), an inert gas injection pipe (13) is provided on the left side of the stirring device (12) at the bottom of the first outer shell (11), a first electromagnetic control valve (14) is provided on the inert gas injection pipe (13), a first discharge pipe (15) is provided on the right side of the stirring device (12) at the bottom of the first outer shell (11), a second electromagnetic control valve (17) is provided on the first discharge pipe (15), a first check valve (16) is provided below the second electromagnetic control valve (17) on the first discharge pipe (15), a gas extraction pipe (18) is provided on the top left side of the first outer shell (11), a drying chamber (19) is provided on the gas extraction pipe (18), a third electromagnetic control valve (110) is provided on the right side of the drying chamber (19) on the gas extraction pipe (18), and a third electromagnetic control valve (110) is provided on the right side of the drying chamber (19) on the gas extraction pipe (18). A distilled water filling pipe (111) is provided, and a fourth electromagnetic control valve (112) is provided on the distilled water filling pipe (111). An air intake pipe (113) is provided on the top right side of the first outer casing (11), and a fifth electromagnetic control valve (114) is provided on the air intake pipe (113). A first cover plate (115) is provided on the top of the first outer casing (11), and an exhaust valve (116) is provided on the first cover plate (115). A first paramagnetic oxygen sensor (117) is provided. A concentrated hydrochloric acid injection pipe (118) is provided on the left side of the exhaust valve (116). A sixth electromagnetic control valve (119) is provided on the concentrated hydrochloric acid injection pipe (118). A vacuum degree detection sensor (120) is provided on the left side of the concentrated hydrochloric acid injection pipe (118). A raw material inlet pipe (121) is provided on the left side of the vacuum degree detection sensor (120). A seventh electromagnetic control valve (122) is provided on the raw material inlet pipe (121).

2. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 1, characterized in that, The stirring device (12) includes a first geared motor (1201), a first stirring rod (1202) is fixedly mounted on the output shaft of the first geared motor (1201), a guide fluid (1203) is rotatably mounted on the bottom of the first stirring rod (1202) through a bearing, and a guide cone (1204) is fixedly mounted on the top of the first stirring rod (1202).

3. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 2, characterized in that, The acid-base balance device (2) includes a second outer shell (21), a stirring device (12) is provided at the bottom of the second outer shell (21), a second cover plate (22) is provided above the second outer shell (21), an alkaline solution injection pipe (23) is fixedly provided on the second cover plate (22), an eighth electromagnetic control valve (24) is provided on the alkaline solution injection pipe (23), a first peristaltic pump (25) is provided at the outlet of the alkaline solution injection pipe (23), a pH detector (26) is provided at the bottom of the second outer shell (21), a second discharge pipe (27) is provided below the second outer shell (21), a second one-way valve (28) is provided on the second discharge pipe (27), and a ninth electromagnetic control valve (29) is provided below the second one-way valve (28) on the second discharge pipe (27).

4. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to any one of claims 1-3, characterized in that, The extraction device (3) includes a third outer shell (31), a stirring device (12) is provided below the third outer shell (31), a third cover plate (33) is provided above the third outer shell (31), an extractant addition tube (34) is fixedly provided on the third cover plate (33), a tenth electromagnetic control valve (35) is fixedly provided on the extractant addition tube (34), a second peristaltic pump (36) is provided at the outlet of the extractant addition tube (34), a third discharge pipe (37) is provided below the third outer shell (31), a third one-way valve (38) is provided on the third discharge pipe (37), a three-way solenoid valve (39) is provided at the outlet of the third discharge pipe (37), and a first extraction discharge pipe (310) and a second extraction discharge pipe (311) are respectively provided on the three-way solenoid valve (39).

5. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 4, characterized in that, The precipitation drying device (4) includes a fourth outer shell (41), a first vent pipe (42) is provided below the fourth outer shell (41), a fourth one-way valve (44) is provided on the first vent pipe (42), an eleventh electromagnetic control valve (43) is provided below the fourth one-way valve (44) on the first vent pipe (42), a Venturi dryer (45) is provided at the air inlet of the first vent pipe (42), and a drain pipe (46) is provided on one side of the first vent pipe (42) below the fourth outer shell (41). 6) A twelfth electromagnetic control valve (47) is provided on the upper part. A stepped through hole (48) is opened on the side wall of the fourth outer shell (41). A sealing door (412) is slidably arranged in the stepped through hole (48). A first electric push rod (411) that cooperates with the sealing door (412) is embedded in the side plate of the fourth outer shell (41). A fourth cover plate (414) is provided on the fourth outer shell (41). A square through hole (415) is opened on the fourth cover plate (414). Limiting blocks are fixedly arranged on both sides of the square through hole (415). (416), a movable seat (417) is slidably arranged between the two limiting and fixing blocks (416). A second electric push rod (418) that cooperates with the movable seat (417) is arranged on the outside of the limiting and fixing blocks (416). A second reduction motor (419) is fixedly arranged on the movable seat (417) and the output shaft of the second reduction motor (419) passes through the movable seat (417). A second stirring rod (420) is fixedly arranged on the output shaft of the second reduction motor (419). A fourth cover plate (414) is located between the two limiting and fixing blocks (416). A lifting filter device (7) is provided. The outlet of the second extraction outlet pipe (311) is connected to the fourth cover plate (414). The fourth cover plate (414) is provided with a precipitation solution injection pipe (421). The precipitation solution injection pipe (421) is provided with a thirteenth electromagnetic control valve (422). The inlet of the precipitation solution injection pipe (421) is provided with a third peristaltic pump (423). The fourth cover plate (414) is provided with a cleaning injection pipe (424). The cleaning injection pipe (424) is provided with a fourteenth electromagnetic control valve (425).

6. The iron removal apparatus for preparing high-purity hafnium tetrachloride according to claim 5, characterized in that, A limiting block (49) is fixedly installed on the inner wall of the fourth outer shell (41) on the inner side of the stepped through hole (48).

7. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 5, characterized in that, The lifting filter device (7) includes two slide rails (71), and sliding blocks (72) are slidably mounted on the slide rails (71) via sliders. A rotating block (73) is rotatably mounted between adjacent sliding blocks (72). A bracket (76) is provided inside the fourth outer shell (41) below the slide rails (71). Rotating seats (75) are fixedly provided on both sides of the upper end face of the bracket (76). A third electric push rod (74) is provided between the rotating block (73) and the rotating seat (75). A filter screen mechanism (77) is provided below the bracket (76).

8. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 7, characterized in that, The filter mechanism (77) includes a filter body (771) and a telescopic block (774). A rotating shaft (772) is fixedly provided on both sides of the filter body (771). A limiting groove (410) that cooperates with the rotating shaft (772) is provided on the inner wall of the fourth outer shell (41). A flow guiding arc block (773) is provided on one side of the filter body (771). A sliding column (775) is fixedly provided at both ends of the telescopic block (774). The telescopic block (774) and the sliding column (775) are slidably provided below the flow guiding arc block (773) and the filter body (771). A spring (776) that cooperates with the sliding column (775) is provided inside the filter body (771).

9. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 8, characterized in that, The calcining furnace (6) includes a furnace body (61). A hatch (62) is mounted on the front side of the furnace body (61) via a hinge. A first air inlet pipe (63) is provided at the bottom left side of the furnace body (61). A fifteenth electromagnetic control valve (64) is fixedly installed on the first air inlet pipe (63). A feeding pipe (66) is provided above the furnace body (61). A sixteenth electromagnetic control valve (67) is provided on the feeding pipe (66). A collection hopper (65) is provided at the inlet of the feeding pipe (66). A material adding pipe (68) is provided on one side of the feeding pipe (66). A seventeenth electromagnetic control valve (69) is provided on the material adding pipe (68). A second air outlet pipe (610) is provided on one side of the material adding pipe (68). An eighteenth electromagnetic control valve (611) is provided on the second air outlet pipe (610).

10. The apparatus for preparing high-purity hafnium tetrachloride and removing iron according to claim 9, characterized in that, A second paramagnetic oxygen sensor (612) is provided on the second exhaust pipe (610) below the eighteenth electromagnetic control valve (611).

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