Preparation device and method of high-purity cerium peroxide

Abstract

The application relates to the field of chemical product production, and discloses a preparation device and a preparation method of high-purity cerium per sulfate, which comprise an outer barrel, an inner barrel, the outer barrel is a closed barrel-shaped structure, the upper cover and the lower cover of the barrel-shaped structure can be opened, the inner barrel is arranged in the outer barrel, the shape of the inner barrel is a cylindrical pipe, the inner wall of the inner barrel is provided with a barrel bottom, the barrel bottom and the inner barrel form a raw material reaction cavity, a rotating shaft is arranged at the center of the barrel bottom, the upper end of the rotating shaft extends to the outer side of the upper cover and is connected with a motor, the rotating shaft side wall of the inner barrel is provided with stirring blades arranged at equal angles, the shape of the stirring blades is a curved triangle, the lower edge of the stirring blades is in contact with the upper surface of the barrel bottom, the inner barrel is connected with the outer barrel through supporting rods, and the cerium oxide can be gradually added into the raw material reaction cavity to react with dilute sulfuric acid; the closed reaction reduces the possibility of impurities entering, and the quality of the high-purity cerium per sulfate is ensured.

Description

An apparatus and method for preparing high-purity cerium-containing sulfuric acid Technical Field

[0001] This invention relates to the field of chemical product manufacturing, and in particular to an apparatus and method for preparing high-purity cerium sulfate. Background Technology

[0002] Cerium sulfate is soluble in water and reacts with water to decompose into basic salts. It is soluble in dilute sulfuric acid and turns light pink in water. It has strong oxidizing properties and is used as an oxidizing agent in analytical chemistry and industry. It is also used in the manufacture of waterproofing agents and antifungal agents.

[0003] The existing process for producing cerium sulfate is as follows: cerium carbonate is calcined to obtain cerium oxide with a large specific surface area; the cerium oxide is then reacted with dilute sulfuric acid under heating conditions to obtain a clear and soluble cerium sulfate solution; the solution is then concentrated, cooled, separated into solid and liquid phases, dried, and pulverized to obtain high-purity cerium sulfate; however, the dilute sulfuric acid needs to be added to the cerium oxide while stirring, which increases the possibility of impurities entering and affects the quality of the high-purity cerium sulfate. Summary of the Invention

[0004] The purpose of this invention is to provide an apparatus and method for preparing high-purity cerium-rich sulfuric acid, thereby solving the problem of impurities entering during the chemical reaction mentioned in the background art.

[0005] The technical solution adopted in this invention is as follows: A device for preparing high-purity cerium-containing sulfuric acid includes an outer barrel and an inner barrel. The outer barrel is a closed barrel-shaped structure, with both the upper and lower lids being openable, and sealing rings are provided on their connecting surfaces. The outer barrel is cylindrical in shape. An inner barrel is installed inside the outer barrel, positioned at the center of the outer barrel, with a gap between the inner barrel and the upper lid of the outer barrel. The inner barrel is cylindrical in shape, and a bottom is installed on its inner wall. The bottom and the inner barrel form a raw material reaction chamber. A rotating shaft is connected to the center of the bottom via a sealed bearing. The shaft is arranged vertically upwards, with its upper end extending to the outside of the upper cover. The shaft is driven by a motor, which is fixedly connected to the upper cover. The shaft and the upper cover are connected by a sealed bearing. Four stirring blades are fixedly attached to the side wall of the shaft in the inner barrel at equal angles. The stirring blades are curved triangles, and their lower edges are in contact with the upper surface of the barrel bottom. The inner barrel and the outer barrel are connected by four support rods, which are arranged at 90-degree intervals. The support rods are L-shaped, with the horizontal section fixed to the inner wall of the outer barrel and the vertical section fixed to the upper edge of the inner barrel.

[0006] A method for preparing high-purity cerium-containing sulfuric acid includes the following steps: (1) calcining cerium carbonate as a raw material to obtain a specific surface area greater than 110 m². 2 / g of cerium oxide; (2) dilute sulfuric acid in the above preparation device, mix dilute sulfuric acid and react with cerium oxide to obtain cerium sulfate slurry, separate cerium sulfate from solid and liquid, and dry cerium sulfate; (3) pulverize to obtain high-purity cerium sulfate.

[0007] The beneficial effects of this invention are as follows: This application allows cerium oxide to be gradually added to the raw material reaction chamber to react with dilute sulfuric acid. The closed reaction reduces the possibility of impurities entering and ensures the quality of high-purity sulfuric acid with high cerium content. Attached Figure Description

[0008] Figure 1 is a schematic diagram of the front cross-sectional structure of the present invention.

[0009] Figure 2 is a schematic diagram of the front cross-sectional structure of the hot cavity plate.

[0010] Figure 3 is a schematic diagram of the front cross-sectional structure of the vacuum tube.

[0011] Figure 4 is a three-dimensional structural diagram of the feed pipe and the liquid inlet pipe.

[0012] Figure 5 is a schematic diagram of the front cross-sectional structure of the limiting rod.

[0013] Figure 6 is a three-dimensional structural diagram of the column and frame.

[0014] Figure 7 is a schematic diagram of the main cross-sectional structure of the material collection trough.

[0015] Figure 8 is a schematic diagram of the main cross-sectional structure of the filter pores.

[0016] Figure 9 is a schematic diagram of the main cross-sectional structure of the filter cloth.

[0017] Figure 10 is a schematic diagram of the main cross-sectional structure of the liquid storage tank.

[0018] Figure 11 is a schematic diagram of the main structure of the upper rotating shaft of the lower cover.

[0019] Figure 12 is a side view sectional view of the traction rod.

[0020] Figure 13 is a side view cross-sectional diagram of the compression spring inside the groove.

[0021] Figure 14 is a schematic diagram of the front cross-sectional structure of the guide plate.

[0022] Figure 15 is a three-dimensional structural diagram of the guide plate.

[0023] Figure 16 is a schematic diagram of the main cross-sectional structure of the storage tank.

[0024] Figure 17 is a schematic diagram of the front cross-sectional structure of the scraper.

[0025] Figure 18 is a schematic diagram of the front cross-sectional structure of the positioning rod and the anti-rotation rod.

[0026] Figure 19 is a schematic diagram of the side cross-sectional structure when the second side plate is flipped down.

[0027] In the diagram: 1. Outer barrel; 2. Inner barrel; 3. Top cover; 4. Bottom cover; 5. Barrel bottom; 6. Raw material reaction chamber; 7. Rotating shaft; 8. Motor; 9. Stirring blade; 10. Support rod; 11. Heating chamber plate; 12. Conveying pipe; 13. Steam generator; 14. Vacuum pipe; 15. Gas pipe; 16. Negative pressure pump; 17. Feed pipe; 18. First valve; 19. Liquid inlet pipe; 20. Second valve; 21. Nut; 22. Limiting rod; 23. Sliding sleeve; 24. Crossbar; 25. Boom; 26. Column; 27. Hydraulic cylinder; 28. Frame; 29. ​​Addition... 30. Rib; 31. Collection trough; 32. First side plate; 33. Second side plate; 34. Third side plate; 35. Guide plate; 36. Filter holes; 37. Filter cloth; 38. Liquid storage tank; 39. Drain pipe; 40. Third valve; 41. Hanging lug; 42. Traction rod; 43. Support rod; 44. Rib plate; 45. Slide groove; 46. Compression spring; 47. Guide plate; 48. Through groove; 49. Baffle; 50. Storage trough; 51. Discharge port; 52. Material gate; 53. Fixing plate; 54. Scraper; 55. Positioning rod; 56. Anti-rotation rod. Detailed Implementation

[0028] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0029] In the description of this invention, it should be understood that the terms "center," "length," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0030] Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first," "second," or "third" may explicitly or implicitly include one or more of that feature.

[0031] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0032] Example 1

[0033] As shown in Figure 1, a device for preparing high-purity cerium-containing sulfuric acid includes an outer barrel 1 and an inner barrel 2. The outer barrel 1 is a closed barrel-shaped structure, with both the upper cover 3 and the lower cover 4 being openable, or alternatively, with the upper cover 3 and the lower cover 4 being openable, and sealing rings provided on their connecting surfaces. The outer barrel 1 is cylindrical in shape, but can be replaced with other shapes besides cylinder, such as rectangles. The inner barrel 2 is installed inside the outer barrel 1, with its installation position at the center of the outer barrel 1, and a gap is left between the inner barrel 2 and the upper cover 3 of the outer barrel 1. The inner barrel 2 is cylindrical in shape, and a barrel bottom 5 is installed on the inner wall of the inner barrel 2. The barrel bottom 5 is cylindrical in shape, and the barrel bottom 5 and the inner barrel 2 form a raw material reaction chamber 6. A rotating shaft 7 is connected to the center of the barrel bottom 5 through a sealed bearing. The rotating shaft 7 is arranged vertically upward, with its upper end extending to the outside of the upper cover 3. The rotating shaft 7 is driven by a motor 8, and the motor 8 is connected to the upper cover 3. The inner barrel 2 is fixedly connected to the outer barrel 1 via a sealed bearing. Four stirring blades 9 are fixedly attached to the side wall of the rotating shaft 7 at equal angles. The stirring blades 9 are curved triangles and, in addition to their stirring function, can push the raw material from the inside out. The lower edge of the stirring blades 9 contacts the upper surface of the barrel bottom 5. The inner barrel 2 is connected to the outer barrel 1 via support rods 10. There are four support rods 10, spaced 90 degrees apart. The support rods 10 are L-shaped, with the horizontal section fixed to the inner wall of the outer barrel 1 and the vertical section fixed to the upper edge of the inner barrel 2. During the stirring process, the rotating shaft 7 is rotated by the motor 8, causing the stirring blades 9 to stir the dilute sulfuric acid in the raw material reaction chamber 6. At this time, cerium oxide can be gradually added to the raw material reaction chamber 6 for reaction. The closed reaction reduces the possibility of impurities entering, ensuring the high-purity cerium sulfuric acid.

[0034] As shown in Figure 2, as an optimization of the embodiment, a heating plate 11 is welded to the inner wall of the outer barrel 1. The heating plate 11 has a U-shaped rotating cross-section, or the heating plate 11 can be set in a serpentine shape, so that an annular heating surface is formed inside the outer barrel 1. The heating plate 11 is connected to a steam generator 13 through an inlet and outlet conveying pipe 12. The model of the steam generator 13 is RY-RJ-0.2. Steam is injected into the heating plate 11 through the steam generator 13, which can provide heating conditions for the dilution of sulfuric acid, for the reaction of dilute sulfuric acid with cerium oxide, and for the drying of high-cerium sulfuric acid.

[0035] As shown in Figure 3, as an optimization of the embodiment, a vacuum tube 14 is fixedly connected to the side wall of the outer barrel 1. The vacuum tube 14 is connected to a negative pressure pump 16 through a gas pipe 15. The negative pressure pump 16 is model gm-0.33a. The negative pressure pump 16 draws the inner wall of the outer barrel 1 into a negative pressure, which can provide vacuum conditions for the reaction process of cerium sulfate and for the solid-liquid separation process of cerium sulfate.

[0036] As shown in Figure 4, as an optimization of the embodiment, a feed pipe 17 is fixedly connected to the side wall of the outer barrel 1, and a first valve 18 is installed on the side wall of the feed pipe 17. The outlet end of the feed pipe 17 is located above the raw material reaction chamber 6 of the inner barrel 2, and the inlet end of the feed pipe 17 can be connected to the feeder of wy-22. A liquid inlet pipe 19 is fixedly connected to the side wall of the outer barrel 1, and a second valve 20 is installed on the side wall of the liquid inlet pipe 19. The outlet end of the liquid inlet pipe 19 is located above the raw material reaction chamber 6 of the inner barrel 2. By setting the liquid inlet pipe 19 and the feed pipe 17, the upper cover 3 can be added without opening, which is convenient and reduces the introduction of impurities during the feeding process.

[0037] Example 2

[0038] As shown in Figure 5, unlike Embodiment 1, the inner wall of the inner tub 2 is smooth, and the bottom of the tub 5 is slidably connected to the inner wall, with a sealing ring provided on the connection surface. To prevent the bottom of the tub 5 from rotating with the shaft 7, two nuts 21 are fixed to the bottom surface of the bottom of the tub 5, respectively arranged on both sides of the shaft 7. Vertically downward-arranged limiting rods 22 are screwed onto the nuts 21. The limiting rods 22 are cylindrical in shape, and their height is less than the height of the inner tub 2. The sides of the limiting rods 22... The wall is slidably connected with a sliding sleeve 23. A crossbar 24 is welded to the side wall of the sliding sleeve 23. The crossbar 24 can also connect two limiting rods 22. The two ends of the crossbar 24 are fixed to the lower edge of the inner barrel 2 by bolts. The length of the crossbar 24 is less than the diameter of the inner barrel 2. Since the length of the rotating shaft 7 is fixed, the descending barrel bottom 5 is prevented from squeezing the crossbar 24 and causing damage. By setting the crossbar 24 and the vertical rod, the barrel bottom 5 can be prevented from rotating with the rotating shaft 7, and the vertical displacement of the barrel bottom 5 is not affected.

[0039] As shown in Figure 6, as an optimization of the embodiment, a lifting arm 25 is installed on the top cover 3 of the outer barrel 1. The connecting surface of the lifting arm 25 is located in the middle of the outer barrel 1 to ensure uniform force distribution. The other end of the lifting arm 25 is slidably connected to a column 26, with the sliding direction being up and down. A hydraulic cylinder 27 is fixedly connected to the inner side of the column 26. The piston end of the hydraulic cylinder 27 is used to lift the lifting arm 25 to cause displacement. The lower end of the column 26 is connected to a frame 28, and a reinforcing rib 29 is provided at the angle between the column 26 and the frame 28. The frame 28 is fixedly connected to the side wall of the outer barrel 1. The opening and closing of the top cover 3 of the outer barrel 1 can be controlled by the hydraulic cylinder 27. As the top cover 3 of the outer barrel 1 moves upward, it can drive the bottom 5 of the barrel to move upward synchronously, so that the product (cerium sulfate) in the raw material reaction chamber 6 is pushed out, making discharge convenient. The bottom 5 of the barrel can prevent the product from sticking to the wall, and the stirring blades 9 can scrape off all the product, thus improving the usage effect.

[0040] Example 3

[0041] As shown in Figure 7, unlike Embodiment 2, the outer side of the inner barrel 2 is fixedly connected to a collection trough 30. The collection trough 30 includes a first side plate 31, a second side plate 32, and a third side plate 33. The first side plate 31 is a rigid plate, such as polypropylene, and is shaped as a downward-sloping ring, which can be replaced by a horizontal ring. The free end of the second side plate 32 is fixedly connected to a second side plate 32, which is also a rigid plate, such as polypropylene, and is shaped as an upward-sloping ring. The free end of the second side plate 32 is fixedly connected to a third side plate 33, which is also a rigid plate, such as polypropylene, and is shaped as a vertically upward-sloping ring. The upper edge of the third side plate 33 is flush with or exceeds the upper edge of the inner barrel 2. The collection trough 30 can collect the pushed-out products.

[0042] As shown in Figure 10, as an optimization of the embodiment, a guide plate 34 is fixedly connected to the bottom surface of the first side plate 31 of the collection tank 30. The guide plate 34 is a rigid plate, such as polypropylene, and is shaped as a vertical downward ring to guide the flow downward. As shown in Figure 8, a filter hole 35 is provided on the end face of the first side plate 31. Preferably, the filter hole 35 is located at the lowest point of the first side plate 31. Through the vacuum action of the negative pressure pump 16, the excess sulfuric acid in the cerium sulfate is filtered out, thereby realizing the solid-liquid separation of cerium sulfate.

[0043] As shown in Figure 9, as an optimization of the embodiment, the upper surface of the first side plate 31 is wrapped with filter cloth 36, which covers the filter holes 35. The filter cloth 36 can be made of PP polypropylene and is made of long strips wound into a ring. By setting the filter cloth 36, the filter holes 35 can be prevented from being blocked, thus ensuring the continuous production of the device.

[0044] Example 4

[0045] As shown in Figure 10, unlike Embodiment 3, the lower cover 4 of the outer barrel 1 is connected to a rotating shaft 7 via a sealed bearing. The rotating shaft 7 is arranged vertically downwards, with its lower end extending to the outside of the lower cover 4. The rotating shaft 7 is driven by a motor 8, which is fixedly connected to the lower cover 4. A liquid storage tank 37 is connected to the side wall of the rotating shaft 7 in the inner barrel 2 via a sealed bearing. The liquid storage tank 37 is cylindrical, and the projected area of ​​the upper opening of the liquid storage tank 37 is larger than the projected area of ​​the guide plate 34. The upper edge of the liquid storage tank 37 and the lower edge of the guide plate 34 are staggered to ensure that the filtered sulfuric acid enters the liquid storage tank 37. A drain pipe 38 is fixedly connected to the side wall of the liquid storage tank 37. The drain pipe 38 is located at a lower position, and a third valve 39 is installed on the side wall of the drain pipe 38. After the lower cover 4 is lowered, the third valve 39 can be opened to discharge the filtered sulfuric acid.

[0046] As shown in Figure 11, as an optimization of the embodiment, a lifting arm 25 is installed on the lower cover 4 of the outer barrel 1. The connecting surface of the lifting arm 25 is located in the middle of the outer barrel 1 to ensure uniform force distribution. The other end of the lifting arm 25 is slidably connected to the column 26. A hydraulic cylinder 27 is fixedly connected to the inner side of the column 26. The piston end of the hydraulic cylinder 27 is used to lift the lifting arm 25 to cause displacement. The opening and closing of the lower cover 4 of the outer barrel 1 can be controlled by the hydraulic cylinder 27. As the lower cover 4 of the outer barrel 1 moves down, it can drive the liquid storage tank 37 to move down synchronously, which facilitates the discharge of filtered sulfuric acid.

[0047] Example 5

[0048] As shown in Figure 12, unlike Embodiment 4, the second side plate 32 is made of a soft board, such as fluororubber or perfluororubber, which has high chemical stability and is resistant to strong oxidizing inorganic acids such as nitric acid and concentrated sulfuric acid; allowing the collection tank 30 to undergo bending deformation; the side wall of the third side plate 33 is connected to a traction rod 41 via a hanging lug 40, using a rotating connection; there are two traction rods 41, which are rectangular in shape and are respectively arranged at the quadrant points of the third side plate 33; the lower end of the traction rod 41 is fixedly connected to a support rod 42, which is horizontally arranged, and its free end is fixedly connected to the side wall of the storage tank 37; To improve the stability of the support, a rib plate 43 is fixed at the clamping position of the support rod 42 and the traction rod 41; by improving the material of the second side plate 32, the collection tank 30 not only has the function of storing materials, but also the function of unloading materials; as shown in Figure 19, after the solid-liquid separation of cerium sulfate is completed, the lower cover 4 of the outer barrel 1 moves downward, and then the storage tank 37 begins to move downward, causing the traction rod 41 to drive the third side plate 33 to move downward, and the second side plate 32 undergoes downward bending deformation, and the solid cerium sulfate in the collection tank 30 is discharged, while the bent second side plate 32 can block the opening of the storage tank 37 to prevent cerium sulfate from entering the storage tank 37.

[0049] As shown in Figure 13, as an optimization of the embodiment, the vertical section of the traction rod 41 is provided with a groove 44. The cross-sectional shape of the groove 44 is T-shaped, and the stroke length is 1-2 times the length of the third side plate 33. If it is too long, it will affect the load-bearing effect. The hanging ear 40 slides in the groove 44. A compression spring 45 is provided in the groove 44. The compression spring 45 is located below the hanging ear 40 in an elastic connection. By providing the compression spring 45, the third side plate 33 generates a restoring elastic force. As the cerium sulfate gradually falls, the compression spring 45 loses weight in sections, producing a vibration effect. The vibration can reduce the amount of cerium sulfate adhering to the wall during unloading.

[0050] As shown in Figure 14, as an optimization of the embodiment, in the first case, a guide plate 46 is fixedly connected to the inner wall of the outer barrel 1. The guide plate 46 is located between the hot chamber plate 11 and the support rod 10. The guide plate 46 is a rigid plate, such as polypropylene, and is shaped as a vertically downward L-shaped ring, which plays a role in guiding the flow downward. The projected area of ​​the opening of the guide plate 46 is larger than the projected area of ​​the liquid storage tank 37, and the lower edge of the guide plate 46 and the upper edge of the liquid storage tank 37 are staggered to ensure that cerium sulfate enters the storage tank 50, while preventing cerium sulfate from entering the liquid storage tank 37.

[0051] As shown in Figure 15, as an optimization of the embodiment, in the second embodiment, a guide plate 47 is fixedly connected to the bottom surface of the upper cover 3 of the outer barrel 1. The guide plate 47 is a rigid plate, such as polypropylene, and is shaped as a vertical downward ring to guide the flow downward. The projected area of ​​the opening of the guide plate 47 is larger than the projected area of ​​the storage tank 37, and the lower edge of the guide plate 46 is staggered with the upper edge of the storage tank 37 to ensure that cerium sulfate enters the storage tank 50 while preventing cerium sulfate from entering the storage tank 37. To avoid structural interference, a through groove 48 is opened on the side wall of the guide plate 47. The through groove 48 is U-shaped with the opening facing downward to prevent structural interference between the guide plate 47 and the support rod 10. To prevent cerium sulfate from flowing out of the through groove 48, a baffle 49 is hung on the side wall of the support rod 10. The outer side of the baffle 49 is attached to the inner wall of the guide plate 47 to close the through groove 48 and ensure the flow direction of cerium sulfate.

[0052] Example 6

[0053] As shown in Figure 16, unlike Embodiment 5, the side wall of the rotating shaft 7 located in the inner barrel 2 is connected to a storage tank 50 via a sealed bearing. The storage tank 50 is located below the liquid storage tank 37. The storage tank 50 is cylindrical in shape. The projected area of ​​the upper opening of the storage tank 50 is larger than the projected area of ​​the guide plate 46 or the guide plate 47. The upper edge of the storage tank 50 is close to the lower edge of the guide plate 46 or the guide plate 47, ensuring that the discharged cerium sulfate enters the storage tank 50. A discharge port 51 is fixedly connected to the side wall of the storage tank 50. A material gate 52 is detachably installed on the discharge port 51. After the lower cover 4 is lowered, the material gate 52 can be opened to discharge the cerium sulfate.

[0054] Example 7

[0055] As shown in Figure 17, unlike Embodiment 6, a fixing plate 53 is fixedly connected to the side wall of the rotating shaft 7. The fixing plate 53 is located inside the liquid storage tank 37 and the material storage tank 50, and the fixing plate 53 is arranged horizontally. A scraper 54 is connected to the bottom surface of the fixing plate 53 by bolts. The scraper 54 is made of soft board, such as fluororubber or perfluororubber. The scraper 54 is L-shaped and elastically contacts the inner wall of the liquid storage tank 37 and the material storage tank 50. After the lower cover 4 of the outer barrel 1 moves down, the motor 8 drives the rotating shaft 7 to rotate. The rotating shaft 7 drives the scraper 54 to rotate, which can push out the sulfuric acid in the liquid storage tank 37 and the cerium sulfate in the material storage tank 50.

[0056] As shown in Figure 18, as an optimization of the embodiment, a positioning rod 55 is fixedly connected to the outer wall of the liquid storage tank 37, and a positioning rod 55 is fixedly connected to the outer wall of the material storage tank 50. The positioning rods 55 are arranged horizontally, and the upper and lower positioning rods 55 are on the same vertical plane. An anti-rotation rod 56 is slidably connected to the side wall of the positioning rod 55. The anti-rotation rod 56 is arranged vertically downward and fixed to the lower cover 4 of the outer barrel 1 by bolts. By setting the positioning rod 55 and the anti-rotation rod 56, the liquid storage tank 37 and the material storage tank 50 can be prevented from rotating with the rotating shaft 7, thus ensuring the discharge process of sulfuric acid and cerium sulfate.

[0057] As an optimization of the embodiment, the rotating shaft 7 of the storage tank 50 is not equipped with a fixing rod and a scraper 54. In this way, the storage tank 50 can collect cerium sulfate and provide heating conditions for drying to produce block cerium sulfate, which further enriches the function of the device.

[0058] This application further proposes a method for preparing high-purity cerium-containing sulfuric acid, comprising the following steps: (1) calcining cerium carbonate as a raw material to obtain a specific surface area greater than 110 m². 2 / g of cerium oxide; (2) dilute sulfuric acid in the above preparation device, mix dilute sulfuric acid and react with cerium oxide to obtain cerium sulfate slurry, separate cerium sulfate from solid and liquid, and dry cerium sulfate; (3) pulverize to obtain high-purity cerium sulfate.

[0059] The calcination temperature in step (1) is 300℃; the concentration of dilute sulfuric acid in step (2) is 50%, the mass ratio of cerium oxide to dilute sulfuric acid is 1:1.3, the reaction heating temperature of dilute sulfuric acid and cerium oxide is 110℃ (heat loss occurs due to air-to-air heat exchange), and the vacuum degree is 0.1MPa; the drying temperature of high-cerium sulfuric acid is 150℃; the total amount of high-purity sulfuric acid and high-cerium rare earth obtained in step (3) is 60%.

[0060] At normal pressure, the temperature of steam is 100℃. The temperature of steam depends on the pressure. When the pressure is between 0.1-5 MPa, the temperature of steam can reach 110-250℃.

[0061] Although the present invention has been described in detail with reference to the foregoing examples, those skilled in the art can still make and modify the technical solutions described in the foregoing embodiments, or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A device for preparing high-purity cerium-rich sulfuric acid, comprising an outer barrel (1) and an inner barrel (2), characterized in that... The outer barrel (1) is a closed barrel-shaped structure, and the upper cover (3) and lower cover (4) of the barrel-shaped structure can be opened; an inner barrel (2) is provided inside the outer barrel (1); the inner barrel (2) is cylindrical in shape, and the inner wall of the inner barrel (2) is provided with a barrel bottom (5), which together with the inner barrel (2) forms a raw material reaction chamber (6); a first rotating shaft is provided at the center of the barrel bottom (5), and the upper end of the first rotating shaft extends to the outside of the upper cover (3) and is connected to a motor (8); a stirring blade (9) is provided on the side wall of the first rotating shaft in the inner barrel (2), and the stirring blade (9) is curved triangular in shape, and the stirring blade ( 9) The lower edge contacts the upper surface of the bottom of the bucket (5); the inner bucket (2) and the outer bucket (1) are connected by a support rod (10); the side wall of the outer bucket (1) is provided with a vacuum tube (14), and the vacuum tube (14) is connected to a negative pressure pump (16) through an air pipe (15); the inner wall of the inner bucket (2) is a smooth surface, and the bottom of the bucket (5) is slidably connected to the inner wall; the bottom surface of the bottom of the bucket (5) is provided with a vertically downwardly arranged limiting rod (22); the side wall of the limiting rod (22) is slidably connected with a crossbar (24), and the two ends of the crossbar (24) are fixed to the lower edge of the inner bucket (2); The outer barrel (1) has a first lifting arm on its upper cover (3), and a column (26) is slidably connected to the other end of the first lifting arm; a first hydraulic cylinder is provided on the inner side of the column (26), with the piston end of the first hydraulic cylinder facing upward, and the first hydraulic cylinder is used to lift the first lifting arm to cause displacement; a frame (28) is connected to the lower end of the column (26); the frame (28) is fixedly connected to the side wall of the outer barrel (1); a material collection trough (30) is provided on the outer side of the inner barrel (2), and the material collection trough (30) includes a first side plate (31), a second side plate (32), and a third side plate (33), the shape of the first side plate (31) is... The first side plate (31) is shaped as a downward-sloping ring; the upper edge of the first side plate (31) is connected to the outer wall of the inner barrel (2); the free end of the first side plate (31) is provided with a second side plate (32); the shape of the second side plate (32) is a downward-sloping ring; the free end of the second side plate (32) is provided with a third side plate (33); the shape of the third side plate (33) is a vertically upward-sloping ring; the upper edge of the third side plate (33) is flush with or exceeds the upper edge of the inner barrel (2); a filter hole (35) is provided on the end face of the first side plate (31); a filter cloth (36) covering the filter hole (35) is wrapped around the upper surface of the first side plate (31).

2. The apparatus for preparing high-purity cerium sulfate according to claim 1, characterized in that... The inner wall of the outer barrel (1) is provided with a hot cavity plate (11), so that an annular heating surface is formed inside the outer barrel (1); the hot cavity plate (11) is connected to a steam generator (13) through a conveying pipe (12).

3. The apparatus for preparing high-purity cerium-rich sulfuric acid according to claim 1, characterized in that... The outer barrel (1) has a feed pipe (17) on its side wall, and a first valve (18) on its side wall. The outlet end of the feed pipe (17) is located above the raw material reaction chamber (6) of the inner barrel (2). The outer barrel (1) has a liquid inlet pipe (19) on its side wall, and a second valve (20) on its side wall. The outlet end of the liquid inlet pipe (19) is located above the raw material reaction chamber (6) of the inner barrel (2).

4. The apparatus for preparing high-purity cerium-rich sulfuric acid according to claim 1, characterized in that... The material of the second side plate (32) is fluororubber or perfluororubber, which makes the collection tank (30) easy to bend and deform to discharge solid cerium sulfate; the side wall of the third side plate (33) is connected to the traction rod (41) by the hanging ear (40); the lower end of the traction rod (41) is provided with a support rod (42), and the free end of the support rod (42) is fixed to the side wall of the storage tank (37); the vertical section of the traction rod (41) is provided with a sliding groove (44), and the hanging ear (40) slides in the sliding groove (44); a compression spring (45) is provided in the sliding groove (44), and the compression spring (45) is located below the hanging ear (40) in an elastic connection manner.

5. The apparatus for preparing high-purity cerium sulfate according to claim 4, characterized in that... A second rotating shaft is provided at the center of the lower cover (4) of the outer barrel (1), and the lower end of the second rotating shaft extends to the outside of the lower cover (4) and is connected to a motor (8); a storage tank (37) for collecting the discharge from the filter holes (35) is provided on the side wall of the second rotating shaft inside the outer barrel (1); a drain pipe (38) is provided on the side wall of the storage tank (37), and a third valve (39) is provided on the side wall of the drain pipe (38); a storage material for collecting solid cerium sulfate is provided on the side wall of the second rotating shaft inside the outer barrel (1). The storage tank (50) is located below the liquid storage tank (37); the side wall of the storage tank (50) is provided with a discharge port (51), and a material gate (52) is detachably installed on the discharge port (51); the lower cover (4) of the outer barrel (1) is provided with a second boom, and the other end of the second boom is slidably connected to the column (26); the inner side of the column (26) is provided with a second hydraulic cylinder, the piston end of the second hydraulic cylinder is downward, and the second hydraulic cylinder is used to lift the second boom to cause displacement.

6. The apparatus for preparing high-purity cerium sulfate according to claim 5, characterized in that... The second rotating shaft has a fixing plate (53) on its side wall, which is located inside the liquid storage tank (37) and the material storage tank (50). The bottom surface of the fixing plate (53) is provided with a scraper (54), which is in elastic contact with the inner wall of the liquid storage tank (37) and the material storage tank (50). The outer side wall of the liquid storage tank (37) is provided with a positioning rod (55), and the outer side wall of the material storage tank (50) is provided with a positioning rod (55), and the upper and lower positioning rods (55) are on the same vertical plane. The side walls of the upper and lower positioning rods (55) are slidably connected with an anti-rotation rod (56), which is located on the lower cover (4) of the outer barrel (1).

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