Device and method for efficiently preparing CeO2 by using hydrothermal method

Abstract

The invention discloses a device for efficiently preparing # imgabs0 # by using a hydrothermal method, which comprises a hydrothermal box, a vacuum heating box is arranged on the upper end surface of the hydrothermal box, and a vacuum pump is connected outside the vacuum heating box; the partition layer plate is horizontally fixed in the middle of the interior of the vacuum heating box, and the interior of the vacuum heating box is divided into a main reaction bin and an auxiliary reaction bin from top to bottom by the partition layer plate; the plurality of placing grooves are arranged and are uniformly distributed on the upper end surface of the separation layer plate; the reaction kettles are arranged corresponding to the spring bases, and a prepared mixed solution is stored in each reaction kettle; the circulating liquid pumping unit is arranged at the upper part in the vacuum heating box; the temperature controller is mounted in the side reaction bin, and the liquid pumping end and the liquid discharging end of the circulating liquid pumping unit are both communicated with the temperature controller.

Description

Technical Field

[0001] The present invention belongs to the technical field of rare earth material preparation, and is specifically a method for efficiently preparing rare earth materials by hydrothermal method. Device and method. Background Art

[0002] In recent years, with the rapid development and wide application of new rare earth materials, experimental studies have found that ultrafine powder cerium dioxide has new and excellent properties, and nano cerium dioxide as a coating and additive can improve the oxidation resistance, thermal corrosion, water corrosion and sulfidation properties of high-temperature alloys and stainless steel, and can also be used as a nodular cast iron inoculant; the current experimental preparation method of cerium dioxide is mainly hydrothermal method, that is, in an autoclave, by controlling the temperature and pressure, the cerium salt is hydrolyzed to generate cerium dioxide, and in the hydrothermal preparation, a single experiment can only heat and pressurize the solution in one reactor. If the hydrothermal box heats and reacts the solutions in multiple reactors at the same time, due to certain differences between each solution, the use of a unified heating and pressurizing method is likely to lead to differences in reaction rate and product properties; and each reactor is located in a different position of the hydrothermal box, it is difficult to ensure that the heating and pressurizing conditions of each reactor are completely consistent, resulting in different reaction conditions.

[0003] Therefore, it is necessary to provide a method for efficiently preparing A device and method are provided to solve the problems raised in the above background technology. Summary of the invention

[0004] To achieve the above object, the present invention provides the following technical solution: a method for efficiently preparing A device comprising:

[0005] A water heating box, the upper end surface of which is provided with a vacuum heating box, and the vacuum heating box is externally connected to a vacuum pump for evacuating the interior thereof;

[0006] A partition plate is horizontally fixed in the middle of the vacuum heating box, and the partition plate divides the interior of the vacuum heating box into a main reaction chamber and a secondary reaction chamber, and the main reaction chamber is located above the secondary reaction chamber;

[0007] A plurality of placement grooves are arranged and evenly distributed on the upper end surface of the separation layer plate, and a spring base is installed in each placement groove;

[0008] A reaction kettle, arranged corresponding to each of the spring bases, wherein a pre-prepared mixed solution is stored in each of the reaction kettles;

[0009] A circulating liquid pumping unit is arranged above the interior of the vacuum heating box, each of the circulating liquid pumping units is arranged corresponding to the placement groove, and the circulating liquid pumping unit is vertically facing the reaction kettle and is detachably threaded and sealed to the reaction kettle;

[0010] A temperature controller is installed in the secondary reaction chamber, and the liquid extraction end and the liquid discharge end of the circulating liquid extraction unit are both connected to the temperature controller; after the solution in the reactor is heated and reacted in the main reaction chamber and the first stage of heating is completed, the circulating liquid extraction unit performs a liquid extraction cycle, and the temperature controller dynamically adjusts the heating temperature according to the current temperature of the mixed solution in the reactor, thereby providing heating assistance, so that the mixed solution in each reactor reaches the corresponding expected reaction temperature, so that the mixed solution in the subsequent reactor can be completely reacted in the main reaction chamber.

[0011] Furthermore, preferably, each of the temperature controllers is provided with a temperature sensor, and the temperature sensor is used to monitor the current temperature of the mixed solution in real time.

[0012] Further, preferably, the circulating pumping unit comprises:

[0013] A kettle cover is threadedly connected and assembled with the reactor, a connecting rod is vertically fixed on the upper part of the interior of the vacuum heating box, and the lower end of the connecting rod is fixed to the kettle cover;

[0014] A liquid drain seat is fixed to the upper end of the connecting rod, and two liquid drain channels are symmetrically arranged on the liquid drain seat, and each of the liquid drain channels is connected to a liquid drain pipe;

[0015] A liquid extraction pipe is vertically connected and fixed on the reactor cover, and the lower end of the liquid extraction pipe is deeply inserted into the reactor;

[0016] A rotating tube connected to the upper end of the liquid extraction tube;

[0017] The pump chamber is arranged above the drainage seat, and a liquid guide tube is vertically connected to the bottom of the pump chamber, and is connected to the drainage seat through the liquid guide tube; the other end of the rotating tube is horizontally connected to the side wall of the pump chamber;

[0018] An impeller is rotatably connected in the pump chamber, and a drive shaft is provided above the pump chamber, one end of the drive shaft is connected to the impeller;

[0019] A reflux pipe is arranged on one side of the pump compartment, one end of the reflux pipe is connected to the temperature controller, and the other end of the reflux pipe is vertically connected to the side wall of the liquid extraction pipe;

[0020] The inner tube is co-centeredly arranged in the liquid extraction tube, and the reflux tube is sealed and connected to the inner tube.

[0021] Furthermore, as a preference, the driving shaft drives the impeller to rotate, pumping the mixed solution in the reactor into the pump chamber through the suction pipe, and diverting it into the temperature controller through each discharge pipe. The mixed solution discharged through the temperature controller enters the reflux pipe, and finally flows into the bottom of the reactor through the inner tube.

[0022] Furthermore, preferably, the lower end of the inner tube extends deep into the bottom of the reactor, and the distance between the lower end of the inner tube and the inner wall of the bottom of the reactor is no more than 2 cm.

[0023] Further, preferably, the temperature controller comprises:

[0024] A cylinder, in which a temperature regulator is installed, an annular cavity is arranged on the side wall of the cylinder, two partitions are vertically symmetrically arranged in the annular cavity, the partitions divide the annular cavity into two flow channels, and each drainage pipe in the circulating pumping unit is connected to the flow channel;

[0025] A plurality of liner plates are evenly arranged, each of which is vertically fixed in the flow channel;

[0026] A guide bar is arranged corresponding to each of the lining plates, one end of the guide bar is connected to the lining plate, a bottom support plate is arranged in the flow channel, the cross section of the bottom support plate is an arc-shaped structure, and the other end of the guide bar is fixed to the bottom support plate;

[0027] An upper flow port is provided on the side wall of each of the lining plates at an even number position; and a lower flow port is provided on the side wall of each of the guide bars at an odd number position;

[0028] The external pipe is vertically connected to the outside of each of the flow channels, and a transverse pipe is connected between the external pipes. The reflux pipe in the circulating pumping unit is connected to the transverse pipe.

[0029] Further, as a preference, the guide bar is slidably connected to the liner, and the bottom support plate slides along the axial direction of the cylinder, an outer ring frame is coaxially arranged below the cylinder, a support rod is vertically connected to the outer ring frame, and the upper end of the support rod is connected to the bottom support plate;

[0030] A pneumatic telescopic rod is fixed on the cylinder, and the telescopic end of the pneumatic telescopic rod is connected to the outer ring frame.

[0031] Furthermore, preferably, the outer ring frame adjusts the effective flow area in the flow channel during the up and down sliding adjustment, so that the mixed solution is heat-conducted and temperature-controlled in the temperature controller along a flow trajectory of corresponding length.

[0032] Further, as a preferred method, a method of efficiently preparing method,

[0033] It includes the following steps:

[0034] S1. Selecting relevant raw materials for preparation of cerium nitrate hexahydrate, sodium hydroxide and deionized water, and dissolving the raw materials, wherein the cerium nitrate hexahydrate is dissolved in a predetermined amount of deionized water, and completely stirred and dissolved by a magnetic stirrer to form a transparent solution, and sodium hydroxide is dissolved in a predetermined amount of deionized water to form a sodium hydroxide solution; then slowly adding the sodium hydroxide solution to the transparent solution, and keeping stirring, and adjusting the pH value of the solution;

[0035] S2. The solution is divided into multiple portions and transferred to each reactor, and then the reactors are spirally mounted under the reactor cover in the circulating pumping unit, so that the pumping tube and the inner tube can be immersed in the mixed solution in the reactor, the door of the vacuum heating box is closed and vacuum heating is performed;

[0036] S3. Maintain the reaction temperature of the vacuum heating box at 120°C for 4-6 hours as scheduled, start the circulating liquid extraction unit to allow the mixed solution in each reactor to enter the temperature controller, and obtain the current temperature of the mixed solution by the temperature sensor in each temperature controller; then the temperature controller adjusts the heating power according to the respective temperature data to ensure that the solution temperature in each reactor reaches the expected reaction temperature of the second stage.

[0037] S4. The mixed solution is finally heated to 180°C in the main reaction chamber for 12 hours. After the reaction is completed, the heating device of the vacuum heating box is turned off, the reactor is taken out of the vacuum heating box, and naturally cooled to room temperature.

[0038] S5. The products after the reaction are separated, washed, completely dried, and finally calcined in a combustion furnace.

[0039] Compared with the prior art, the present invention has the following beneficial effects:

[0040] The present invention can simultaneously heat and pressurize the mixed solutions in multiple reactors to improve Preparation efficiency, the main set of circulating pumping unit can circulate the mixed solution in each reactor to the temperature controller, so that the mixed solution can be accurately adjusted by the temperature controller after the first stage of heating, so that the mixed solution in each reactor can reach the expected reaction temperature of the second stage, and then fully heated and pressurized in the main reaction chamber, achieving multiple Simultaneous preparation of samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 It is a structural schematic diagram of the present invention;

[0042] Figure 2 It is a structural schematic diagram of the circulating liquid pumping unit in the present invention;

[0043] Figure 3 It is a schematic cross-sectional structure diagram of the circulating liquid pumping unit in the present invention;

[0044] Figure 4 It is a structural schematic diagram of the temperature controller in the present invention;

[0045] Figure 5 It is a front view of the thermostat in the present invention;

[0046] In the figure: 1. water heating box; 11. vacuum heating box; 12. partition plate; 13. main reaction chamber; 14. auxiliary reaction chamber; 15. spring base; 2. reactor; 3. circulating pumping unit; 31. reactor cover; 32. connecting rod; 33. drain seat; 34. drain pipe; 35. pumping pipe; 36. rotating pipe; 37. pump chamber; 38. liquid guide pipe; 39. impeller; 310. drive shaft; 311. reflux pipe; 312. inner pipe; 4. temperature controller; 41. cylinder; 42. partition; 43. lining plate; 44. guide bar; 45. bottom support plate; 46. upper flow port; 47. lower flow port; 48. external pipe; 5. outer ring frame; 51. support rod; 52. pneumatic telescopic rod. DETAILED DESCRIPTION

[0047] See also Figure 1-Figure 5 In the embodiment of the present invention, a method for efficiently preparing A device comprising:

[0048] The water heating box 1 has a vacuum heating box 11 disposed on its upper end surface, and the vacuum heating box 11 is externally connected to a vacuum pump for evacuating the interior thereof;

[0049] A partition plate 12 is horizontally fixed in the middle of the vacuum heating box 11. The partition plate 12 divides the interior of the vacuum heating box 11 into a main reaction chamber 13 and a secondary reaction chamber 14, and the main reaction chamber 13 is located above the secondary reaction chamber 14.

[0050] There are multiple placement grooves arranged and evenly distributed on the upper end surface of the separation layer plate 12, and a spring base 15 is installed in each placement groove; the spring base 15 can form a bottom support for the reactor 2, which is convenient for the installation and disassembly of the reactor 2;

[0051] A reaction kettle 2 is arranged corresponding to each of the spring bases 15, and a pre-prepared mixed solution is stored in each of the reaction kettles 2; the mixed solution is a mixture of a sodium hydroxide solution and a Ce (III) salt solution, wherein when the raw materials are dissolved, cerium nitrate hexahydrate is first dissolved in an appropriate amount of deionized water, stirred until completely dissolved, to form a transparent Ce (III) salt solution, and then sodium hydroxide is dissolved in an appropriate amount of deionized water, stirred until completely dissolved, to form a sodium hydroxide solution;

[0052] The circulating pumping unit 3 is arranged above the inside of the vacuum heating box 11, each of the circulating pumping units 3 is arranged corresponding to the placement groove, and the circulating pumping unit 3 is vertically facing the reactor 2 and is detachably threaded and sealed to the reactor;

[0053] The temperature controller 4 is installed in the secondary reaction chamber, and the liquid extraction end and the liquid discharge end of the circulating liquid extraction unit 3 are both connected to the temperature controller 4; after the solution in the reactor 2 is heated and reacted in the main reaction chamber 13 and the first stage of heating is completed, the circulating liquid extraction unit 3 performs liquid extraction circulation, and the temperature controller 4 dynamically adjusts the heating temperature according to the current temperature of the mixed solution in the reactor 2, thereby providing heating assistance, so that the mixed solution in each reactor 2 reaches the corresponding expected reaction temperature, so that the mixed solution in the subsequent reactor 2 can be completely reacted in the main reaction chamber 13, so that it can be ensured that the mixed solution in each reactor 2 can reach the expected reaction temperature before the final heating and pressurization, thereby ensuring the preparation stability and consistency of cerium dioxide in each reactor 2, and avoiding differences in the reaction preparation of cerium dioxide.

[0054] In this embodiment, each of the temperature controllers 4 is provided with a temperature sensor (not shown in the figure), and the temperature sensor is used to monitor the current temperature of the mixed solution in real time.

[0055] As a preferred embodiment, the circulating pumping unit 3 includes:

[0056] A kettle cover 31 is threadedly connected and assembled with the reactor 2. A connecting rod 32 is vertically fixed on the upper part of the vacuum heating box 11. The lower end of the connecting rod 32 is fixed to the kettle cover 31.

[0057] A liquid drain seat 33 is fixed to the upper end of the connecting rod 32. Two liquid drain channels are symmetrically arranged on the liquid drain seat 33. Each liquid drain channel is connected to a liquid drain pipe 34.

[0058] A liquid extraction pipe 35 is vertically connected and fixed on the reactor cover 31, and the lower end of the liquid extraction pipe 35 is deeply inserted into the reactor 2;

[0059] A rotating tube 36 connected to the upper end of the liquid extraction tube 35;

[0060] The pump chamber 37 is arranged above the drainage seat 33. A liquid guide tube 38 is vertically connected to the bottom of the pump chamber 37 and is connected to the drainage seat 35 through the liquid guide tube 38. The other end of the rotating tube 36 is horizontally connected to the side wall of the pump chamber 37.

[0061] An impeller 39 is rotatably connected in the pump chamber 37, and a drive shaft 310 is provided above the pump chamber 37, one end of the drive shaft 310 is connected to the impeller 39;

[0062] A reflux pipe 311 is disposed on one side of the pump chamber 37, one end of the reflux pipe 311 is connected to the temperature controller 4, and the other end thereof is vertically connected to the side wall of the liquid extraction pipe 35;

[0063] The inner tube 312 is co-centrically arranged in the liquid extraction tube 35, and the reflux tube 311 is sealed and connected to the inner tube 312, that is, the liquid extraction tube 35 can extract the mixed solution in the reactor and send it into the temperature controller 4, while the inner tube 312 sends the mixed solution back into the reactor, thereby completing the flow cycle.

[0064] In this embodiment, the driving shaft 310 drives the impeller 39 to rotate, pumping the mixed solution in the reactor 2 into the pump chamber 37 through the liquid extraction pipe 35, and diverting it into the temperature controller 4 through each discharge pipe 34. The mixed solution discharged from the temperature controller 4 enters the reflux pipe 311, and finally flows into the bottom of the reactor 2 through the inner pipe 312, thereby achieving complete pumping of the mixed solution in the reactor and ensuring its flow integrity.

[0065] In this embodiment, the lower end of the inner tube 312 penetrates into the bottom of the reactor 2, and the distance between the inner tube 312 and the inner wall of the bottom of the reactor 2 is not more than 2 cm; it should be noted that a solenoid valve is provided on the rotating tube 36. When the mixed solution in the reactor is completely circulated and reaches the expected reaction temperature of the second stage, the solenoid valve can control the rotating tube 36 to close, so that the extraction pipe cannot extract the mixed solution in the reactor, and the impeller 39 can almost completely return the mixed solution entering the temperature controller 4 to the reactor through the reflux pipe 311 during a period of idling. It is necessary to accurately control the idling time of the impeller to avoid damage to the equipment due to excessive idling (the above belongs to the prior art and will not be elaborated).

[0066] In this embodiment, the temperature controller 4 includes:

[0067] The cylinder 4 has a temperature regulator installed inside. The side wall of the cylinder 41 is provided with an annular cavity. Two partitions 42 are vertically symmetrically arranged in the annular cavity. The partitions 42 divide the annular cavity into two flow channels. Each drainage pipe 34 in the circulating pumping unit 3 is connected to the flow channel; that is, the mixed solution in the drainage pipe 34 can enter each flow channel respectively.

[0068] There are multiple lining plates 43 that are evenly arranged, and each lining plate 43 is vertically fixed in the flow channel;

[0069] A guide bar 44 is provided corresponding to each of the lining plates 43, one end of the guide bar 44 is connected to the lining plate 43, a bottom support plate 45 is provided in the flow channel, the cross section of the bottom support plate 45 is an arc-shaped structure, and the other end of the guide bar 44 is fixed to the bottom support plate 45;

[0070] The upper flow ports 46 are provided on the side walls of the lining plates 43 at even-numbered positions, and the lower flow ports 47 are provided on the side walls of the guide bars 44 at odd-numbered positions, so that the mixed solution can form an S-shaped flow track in the flow channel through the upper flow ports 46 and the lower flow ports 47;

[0071] The external pipes 48 are vertically connected to the outside of each of the flow channels. The external pipes 48 are connected with a transverse pipe, and the return pipe 311 in the circulating pumping unit 3 is connected with the transverse pipe.

[0072] As a preferred embodiment, the guide bar 44 is slidably connected to the liner 43, and the bottom support plate 45 slides along the axial direction of the cylinder 41. An outer ring frame 5 is coaxially arranged below the cylinder 41, and a support rod 51 is vertically connected to the outer ring frame 5. The upper end of the support rod is connected to the bottom support plate;

[0073] A pneumatic telescopic rod 52 is fixed on the cylinder 41 , and a telescopic end of the pneumatic telescopic rod 52 is connected to the outer ring frame 5 .

[0074] In this embodiment, the outer ring frame 5 adjusts the effective flow area in the flow channel during the up and down sliding adjustment, so that the mixed solution is heat-conducted and temperature-controlled in the temperature controller 4 with a flow trajectory of corresponding length, which facilitates accurate heating assistance of the mixed solution.

[0075] In this embodiment, a method of efficiently preparing The method comprises the following steps:

[0076] S1. Selecting relevant raw materials for preparation of cerium nitrate hexahydrate, sodium hydroxide and deionized water, and dissolving the raw materials, wherein the cerium nitrate hexahydrate is dissolved in a predetermined amount of deionized water, and completely stirred and dissolved by a magnetic stirrer to form a transparent solution, and sodium hydroxide is dissolved in a predetermined amount of deionized water to form a sodium hydroxide solution; then slowly adding the sodium hydroxide solution to the transparent solution, and keeping stirring, and adjusting the pH value of the solution;

[0077] S2. The solution is divided into multiple portions and transferred to each reactor 2, and then the reactors 2 are respectively screwed under the reactor cover 31 in the circulating pumping unit 3, so that the pumping tube 35 and the inner tube 312 can be immersed in the mixed solution in the reactor 2, and the door of the vacuum heating box 11 is closed and vacuum heating is performed;

[0078] S3. Maintain the reaction temperature of the vacuum heating box 11 at 120°C for 4-6 hours as scheduled, start the circulating liquid extraction unit 3 to allow the mixed solution in each reactor 2 to enter the temperature controller 4, and obtain the current temperature of the mixed solution by the temperature sensor in each temperature controller 4; then the temperature controller 4 adjusts the heating power according to the respective temperature data to ensure that the solution temperature in each reactor 2 reaches the expected reaction temperature of the second stage.

[0079] S4. The mixed solution is finally heated to 180°C in the main reaction chamber 13 for 12 hours. After the reaction is completed, the heating device of the vacuum heating box 11 is turned off, and the reactor 2 is taken out of the vacuum heating box 11 and naturally cooled to room temperature.

[0080] S5. The products after the reaction are separated, washed, completely dried, and finally calcined in a combustion furnace.

[0081] What is described above is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. An efficient preparation method using hydrothermal method The device is characterized in that: It includes: A water heating box (1), the upper end surface of which is provided with a vacuum heating box (11), the vacuum heating box (11) being externally connected to a vacuum pump for evacuating the interior thereof; A partition plate (12) is horizontally fixed at a middle position inside the vacuum heating box (11), the partition plate (12) divides the inside of the vacuum heating box (11) into a main reaction chamber (13) and a secondary reaction chamber (14) from top to bottom, and the main reaction chamber (13) is located above the secondary reaction chamber (14); A plurality of placement grooves are arranged and evenly distributed on the upper end surface of the separation layer plate (12), and a spring base (15) is installed in each of the placement grooves; A reaction kettle (2) is arranged corresponding to each of the spring bases (15), and a pre-prepared mixed solution is stored in each of the plurality of reaction kettles (2); A circulating liquid pumping unit (3) is arranged above the interior of the vacuum heating box (11), each of the circulating liquid pumping units (3) is arranged corresponding to the placement groove, and the circulating liquid pumping unit (3) is vertically facing the reaction kettle (2) and is detachably threaded and sealed to the reaction kettle; A temperature controller (4) is installed in the secondary reaction chamber, and the liquid extraction end and the liquid discharge end of the circulating liquid extraction unit (3) are both connected to the temperature controller (4); after the solution in the reactor (2) is heated and reacted in the main reaction chamber (13) and the first stage of heating is completed, the circulating liquid extraction unit (3) performs liquid extraction circulation, and the temperature controller (4) dynamically adjusts the heating temperature according to the current temperature of the mixed solution in the reactor (2), thereby providing heating assistance, so that the mixed solution in each reactor (2) reaches the corresponding expected reaction temperature, so that the mixed solution in the subsequent reactor (2) can be completely reacted in the main reaction chamber (13).

2. A method for efficiently preparing the product by hydrothermal method according to claim 1 The device is characterized in that: Each of the temperature controllers (4) is provided with a temperature sensor, and the temperature sensor is used to monitor the current temperature of the mixed solution in real time.

3. The method according to claim 1 for efficiently preparing the The device is characterized in that: The circulating pumping unit (3) comprises: A kettle cover (31) is threadedly connected to the reaction kettle (2); a connecting rod (32) is vertically fixed on the upper part of the interior of the vacuum heating box (11); and the lower end of the connecting rod (32) is fixed to the kettle cover (31); A liquid drain seat (33) is fixed to the upper end of the connecting rod (32), and two liquid drain channels are symmetrically arranged on the liquid drain seat (33), and each of the liquid drain channels is connected to a liquid drain pipe (34); A liquid extraction pipe (35) is vertically connected and fixed on the reactor cover (31), and the lower end of the liquid extraction pipe (35) is deeply inserted into the reactor (2); A rotating tube (36) connected to the upper end of the liquid extraction tube (35); The pump chamber (37) is arranged above the liquid drainage seat (33); a liquid guide tube (38) is vertically connected to the bottom of the pump chamber (37) and is connected to the liquid drainage seat (35) through the liquid guide tube (38); the other end of the rotating tube (36) is horizontally connected to the side wall of the pump chamber (37); An impeller (39) is rotatably connected in the pump chamber (37), and a drive shaft (310) is provided above the pump chamber (37), one end of the drive shaft (310) being connected to the impeller (39); A reflux pipe (311) is arranged on one side of the pump chamber (37), one end of the reflux pipe (311) is connected to the temperature controller (4), and the other end of the reflux pipe (311) is vertically connected to the side wall of the liquid extraction pipe (35); The inner tube (312) is co-centrically arranged in the liquid extraction tube (35), and the return tube (311) is sealed and connected to the inner tube (312).

4. A method for efficiently preparing the product by hydrothermal method according to claim 3 The device is characterized in that: The driving shaft (310) drives the impeller (39) to rotate, pumping the mixed solution in the reactor (2) into the pump chamber (37) through the liquid pumping pipe (35), and sending the mixed solution into the temperature controller (4) through the liquid discharge pipes (34). The mixed solution discharged from the temperature controller (4) enters the reflux pipe (311) and finally flows into the bottom of the reactor (2) through the inner pipe (312).

5. The method according to claim 3 for efficiently preparing the The device is characterized in that: The lower end of the inner tube (312) extends deep into the bottom of the reaction kettle (2), and the distance between the lower end of the inner tube (312) and the inner wall of the bottom of the reaction kettle (2) is no more than 2 cm.

6. The method according to claim 1 for efficiently preparing the The device is characterized in that: The temperature controller (4) comprises: A cylinder (41) having a temperature regulator installed therein, an annular cavity being provided on the side wall of the cylinder (41), two partitions (42) being vertically symmetrically arranged in the annular cavity, the partitions (42) dividing the annular cavity into two flow channels, and each of the liquid discharge pipes (34) in the circulating pumping unit (3) being connected to the flow channels; A plurality of lining plates (43) are evenly arranged, and each lining plate (43) is vertically fixed in the flow channel; A guide bar (44) is arranged corresponding to each of the lining plates (43), one end of the guide bar (44) is connected to the lining plate (43), a bottom supporting plate (45) is arranged in the flow channel, the cross section of the bottom supporting plate (45) is an arc-shaped structure, and the other end of the guide bar (44) is fixed to the bottom supporting plate (45); An upper flow port (46) is provided on the side wall of each of the lining plates (43) at an even-numbered position; and a lower flow port (47) is provided on the side wall of each of the guide bars (44) at an odd-numbered position; The external pipes (48) are vertically connected to the outside of each of the flow channels, and a transverse pipe is connected between the external pipes (48), and the return pipe (311) in the circulating pumping unit (3) is connected to the transverse pipe.

7. The method according to claim 6 for efficiently preparing the The device is characterized in that: The guide bar (44) is slidably connected to the lining plate (43), and the bottom support plate (45) slides along the axial direction of the cylinder (41). An outer ring frame (5) is coaxially arranged below the cylinder (41), and a support rod (51) is vertically connected to the outer ring frame (5). The upper end of the support rod (51) is connected to the bottom support plate (45); A pneumatic telescopic rod (52) is fixed to the cylinder (41), and the telescopic end of the pneumatic telescopic rod (52) is connected to the outer ring frame (5).

8. The method according to claim 7 for efficiently preparing the The device is characterized in that: The outer ring frame (5) adjusts the effective flow area in the flow channel by sliding up and down, so that the mixed solution is heat-conducted and temperature-controlled in the temperature controller (4) along a flow track of corresponding length.

9. An efficient preparation method using hydrothermal method A method for efficiently preparing the product by a hydrothermal method as described in any one of claims 1 to 8 The device is characterized in that It includes the following steps: S1. Selecting relevant raw materials for preparation of cerium nitrate hexahydrate, sodium hydroxide and deionized water, and dissolving the raw materials, wherein the cerium nitrate hexahydrate is dissolved in a predetermined amount of deionized water, and completely stirred and dissolved by a magnetic stirrer to form a transparent solution, and at the same time, sodium hydroxide is dissolved in a predetermined amount of deionized water to form a sodium hydroxide solution; Then slowly add sodium hydroxide solution into the transparent solution, keep stirring, and adjust the pH value of the solution; S2. Divide the solution into multiple portions and transfer them to each reactor (2), and then screw the reactors (2) under the reactor cover (31) in the circulating pumping unit (3), so that the pumping tube (35) and the inner tube (312) can be immersed in the mixed solution in the reactor (2), close the door of the vacuum heating box (11) and perform vacuum heating; S3. The reaction temperature of the vacuum heating box (11) is maintained at 120°C for 4-6 hours according to the predetermined time, and the circulating liquid pumping unit (3) is started to allow the mixed solution in each reaction kettle (2) to enter the temperature controller (4), and the temperature sensor in each temperature controller (4) obtains the current temperature of the mixed solution; then the temperature controller (4) adjusts the heating power according to the respective temperature data to ensure that the solution temperature in each reaction kettle (2) reaches the expected reaction temperature of the second stage. S4. The mixed solution is finally heated to 180° C. in the main reaction chamber (13) for 12 hours. After the reaction is completed, the heating device of the vacuum heating box (11) is turned off, and the reactor (2) is taken out of the vacuum heating box (11) and naturally cooled to room temperature. S5. The products after the reaction are separated, washed, completely dried, and finally calcined in a combustion furnace.

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