Rare earth mixture mixing and roasting process and dispersing and grinding equipment thereof

Abstract

The invention relates to the technical field of dispersing devices, and discloses a rare earth mixture mixing and roasting process and dispersing and grinding equipment thereof.The rare earth mixture mixing and roasting process comprises a dispersing barrel used for dispersing and mixing, a stirring rod is arranged at the axis of the dispersing barrel, and stirring blades used for dispersing and stirring are vertically arrayed on the stirring rod; a discharging port allowing processed raw materials to pass through is formed in the lower portion in the dispersing barrel, at least one partition assembly is arranged in the dispersing barrel and composed of a fixed piece and a rotating piece, the partition assembly is attached to the inner wall of the dispersing barrel and divides the interior of the dispersing barrel into at least two independent spaces, groove holes are formed in the fixed piece and the rotating piece, and the fixed piece fixes the angle. The rotating piece is connected with the stirring rod and is driven by the motor to rotate along with the stirring rod, when the stirring rod rotates, the slotted hole in the fixed piece is blocked by the rotating piece to form a gap with variable size, the gap is in a closed state at a specific rotating angle, and an ultrasonic device is arranged at the bottom in the dispersing barrel and can emit upward ultrasonic waves.

Description

Technical Field

[0001] The invention relates to the technical field of dispersion devices, in particular to a rare earth mixture mixed roasting process and dispersion grinding equipment thereof. Background Art

[0002] The main purpose of the dispersion device of rare earth mixture is to uniformly mix the compounds or mixtures of rare earth elements (such as lanthanide elements and scandium, yttrium, etc.) with other substances (such as solvents, additives, carriers, etc.), and make the rare earth particles reach the desired dispersion state through physical or chemical methods, which helps to improve the performance of rare earth materials, such as luminous efficiency, catalytic activity, magnetic properties, etc. The material is mechanically stirred by the agitator to make the rare earth particles evenly distributed in the medium. There are various types of agitators, such as paddle type, anchor type, turbine type, etc., which can be selected according to the material characteristics and dispersion requirements. The high-speed rotating shearing parts are used to strongly shear the material to break the rare earth particles and evenly disperse them in the medium. This method is suitable for occasions requiring high dispersion. The cavitation effect and microjet effect generated by ultrasound in the medium are used to disperse the rare earth particles non-contactly. Ultrasonic dispersion has the advantages of high efficiency and environmental protection.

[0003] During the mixing process, metal oxides and rare earth elements are prone to agglomeration and precipitation due to their high surface energy, which will have a certain impact on subsequent roasting and lead to a decrease in product quality. Agglomeration is due to the mutual attraction between particles, which causes small particles to aggregate into large particles, while precipitation is due to the gravity that causes the particles with higher density to settle in the mixed system. It is difficult for general dispersion devices to generate sufficient shear force to disperse the agglomerates. At the same time, it is difficult to ensure the uniformity of dispersion and mixing when precipitation occurs, and it is impossible to generate upward water flow to ensure mixing. In order to improve the quality of the product after roasting, it is necessary to make the metal oxides and rare earth elements evenly mixed in the solvent during the dispersion and mixing process. Summary of the invention

[0004] (I) Technical problems to be solved: In view of the deficiencies of the prior art, the present invention provides a rare earth mixture mixed roasting process and a dispersion grinding device thereof, which has the advantage of uniform dispersion and solves the problems of material agglomeration and precipitation.

[0005] (II) Technical solution: To achieve the above-mentioned uniform dispersion purpose, the present invention provides the following technical solution: a rare earth mixture mixed roasting process, step 1, prepare a mixed roasting material, mix an inorganic oxide containing zinc oxide / manganese oxide / titanium oxide and a rare earth mixture containing lanthanum / cerium to form a mixed roasting material; control the mass ratio of rare earth to inorganic oxide in the mixed roasting material to be 3:7. The metal cerium / metal lanthanum is added in the form of an ethanol solution of cerium nitrate / lanthanum nitrate, and the metal zinc, metal manganese / metal titanium are added in the form of powder.

[0006] Step 2: Mechanical dispersion: put the mixed roasted material prepared in step 1 into the feeding port of the dispersion equipment for mechanical dispersion for 20-30 minutes to mix the components evenly to obtain a paste-like mixture.

[0007] Step 3: high-energy dispersion. The paste mixture prepared in step 2 is put into the feeding port of the dispersion equipment for high-energy dispersion. The mixture is dispersed for 40-50 minutes to fully mix the components at the microscopic level to obtain a solid-liquid separation suspension.

[0008] Step 4: Secondary mechanical dispersion: the suspension that has undergone solid-liquid separation in step 3 is again put into the feeding port of the dispersion equipment for mechanical dispersion for 20-30 minutes to fully mix the components to obtain a paste mixture.

[0009] Step 5: Drying: Place the mixture from step 4 in an oven at 120° C. and dry for 24-48 hours to thoroughly dry the paste mixture.

[0010] Step six, tunnel kiln firing, place the block obtained in step five in a crucible and place it on a conveyor, control a certain gap between the crucibles through a fully automatic intelligent arrangement device to form a roasting air duct, and at the same time control the roasting temperature between the crucibles to be consistent, control the roasting buffer temperature to rise from room temperature to 1500°C, and enter the high-temperature roasting zone after 2 hours of heating and firing, the temperature is 1500°C, the high-temperature roasting time is 3 hours, and then enter the cooling zone, the temperature is 1500°C to room temperature, the cooling zone takes 2 hours, and then transferred to the external conveyor belt, waiting to be taken out, the overall temperature control accuracy is ≤5°C.

[0011] Step seven, grinding, grinding the high-temperature mixed doped oxides calcined in step six, first placing the bulk material in a grinding device for initial grinding to disperse it into small particles, and then selecting different fine grinding equipment for secondary fine grinding according to the purpose of the material to achieve the desired particle size value. The particle size range of the material is 200nm-150,000nm.

[0012] A rare earth mixture dispersion and grinding device comprises a dispersion cylinder for dispersion and mixing, a stirring rod is arranged at the axis center of the dispersion cylinder, the stirring rod is driven by a motor, an inlet for pouring raw materials is arranged above the dispersion cylinder, stirring blades for dispersion and stirring are arranged in a vertical array on the stirring rod, a discharge port for passing the processed raw materials is arranged at the lower part of the dispersion cylinder, at least one partition assembly is arranged in the dispersion cylinder, the partition assembly is composed of a fixed plate and a rotating plate, the partition assembly is fitted with the inner wall of the dispersion cylinder and divides the inside of the dispersion cylinder into at least two independent spaces, slots are arranged on the fixed plate and the rotating plate, the fixed plate has a fixed angle, the rotating plate is connected to the stirring rod and rotates with the stirring rod driven by the motor, when the stirring rod rotates, the slots on the fixed plate are blocked by the rotating plate to form a gap of varying size, and the gap is in a closed state at a specific rotation angle, an ultrasonic device is arranged at the bottom of the dispersion cylinder, and the ultrasonic device can emit upward ultrasonic waves.

[0013] The ultrasonic device is arranged in a circular ring shape at the bottom of the dispersion tube.

[0014] A fixing ring is provided on the inner wall of the dispersion cylinder. The setting position of the fixing ring corresponds to the position of the fixing plate in the separation component and is used to fix and support the fixing plate.

[0015] The stirring blade is arranged on the mounting ring. The mounting ring can be driven to rotate by the stirring rod and can be displaced in the vertical direction on the stirring rod. A retaining ring is arranged at the displacement limit distance, and rubber is arranged between the mounting ring and the retaining ring.

[0016] The stirring blade is an axial flow stirring blade.

[0017] A limiting ring is arranged at the center of the bottom of the dispersion cylinder, the bottom end of the stirring rod penetrates into the limiting ring, and rubber is arranged between the bottom end of the stirring rod and the limiting ring.

[0018] The slots on the fixed plate and the rotating plate are circular, and the area occupied by the slots does not exceed 50% of the entire fixed plate and the rotating plate.

[0019] The slots on the fixed plate and the rotating plate are eccentrically slanted and their occupied areas do not exceed 50% of the fixed plate and the rotating plate as a whole. When the rotating plate is driven to rotate by the stirring rod, the gap formed by the overlapping of the fixed plate and the rotating plate moves from outside to inside or from inside to outside in the slots.

[0020] The eccentric oblique strip-shaped slots on the fixed plate and the rotating plate are divided into multiple sections, each section is provided with a gap, and it is ensured that the gaps formed by the fixed plate and the rotating plate can be closed during the rotation process.

[0021] (III) Beneficial effects: Compared with the prior art, the present invention provides a rare earth mixture mixed roasting process and its dispersion and grinding equipment, which have the following beneficial effects: 1. The rare earth mixture mixed roasting process, by adopting a combination of mechanical dispersion, high-energy dispersion and secondary mechanical dispersion, ensures that each component can achieve sufficient mixing uniformity at the macro and micro levels. This multi-level and multi-stage mixing method effectively avoids local concentration unevenness or agglomeration, improves mixing efficiency and mixing quality, and the drying process is carried out at an appropriate temperature and time to ensure that the paste mixture can be thoroughly dried without affecting the performance of the material. The firing process of the tunnel kiln achieves a smooth transition from room temperature to high temperature and uniform heating through precise temperature control and time management, avoiding the adverse effects of temperature fluctuations on the material structure. At the same time, the setting of the roasting slow zone further ensures the temperature stability during the heating process and improves the roasting effect.

[0022] 2. The rare earth mixture dispersion grinding equipment can achieve efficient mixing of raw materials at the macro and micro levels through the rotation of the stirring rod and stirring blades, combined with the action of the ultrasonic device. The shear force and impact force of the stirring blades help to break the agglomeration between the powder particles. The ultrasonic waves emitted by the ultrasonic device can directly act on the raw materials, refine the particles through mechanisms such as cavitation effect and micro jet, increase the specific surface area, and thus improve the activity of the raw materials, which is crucial for the formation of uniform solid solution or composite oxides in the subsequent heat treatment process. The design of the partition component (the coordination of the fixed plate and the rotating plate) not only generates additional shear force to crush the powder during the rotation process, but also refines the material passing through the pores. The opening and closing of the gaps dynamically squeeze and release the raw materials. The opening and closing of the pores of the partition components also indirectly promotes the refinement of the particles. In particular, when the pores are closed, the upward weak water flow increases the instantaneous pressure on the raw materials, which helps to further break the particles and further enhance the mixing effect. The "acoustic streaming effect" of the ultrasound further promotes the movement and dispersion of tiny particles in the liquid, thereby improving the uniformity of the mixture. The ultrasound promotes the upward movement of the raw materials in the dispersion tube, avoids the accumulation of large-volume materials at the bottom, and increases the uniformity of the dispersion. After the high-energy dispersion stage, the mechanical dispersion again can effectively solve the possible solid-liquid separation phenomenon and restore the uniformity of the mixture. This secondary dispersion process not only ensures the full mixing of the components, but also may further refine the particle size and improve the overall quality of the product.

[0023] 3. The rare earth mixture dispersion and grinding equipment is provided with a stirring blade on a mounting ring. The mounting ring can be driven to rotate by the stirring rod and can be displaced in the vertical direction on the stirring rod. A retaining ring is provided at the displacement limit distance. Rubber is provided between the mounting ring and the retaining ring, so that the stirring blade can move with the water flow in the dispersion tube during the stirring process, reduce the wear caused by the impact of the water flow on itself, increase the service life, and reduce the maintenance cost. The stirring blade adopts an axial flow stirring blade. The blade plane of the axial flow stirring blade is arranged at an angle, which can generate strong axial flow and annular flow. By adjusting the inclination angle and number of the blades, the water flow can be guided to form an upward circulating flow and increase the shear force. A limiting ring is provided at the center of the bottom of the dispersion tube, the bottom end of the stirring rod penetrates into the limiting ring, and rubber is provided between the bottom end of the stirring rod and the limiting ring. The limiting ring reduces the deviation of the stirring rod during the working process. At the same time, the rubber is used to absorb the vibration, reduce the vibration transmitted to the equipment, and reduce the damage to the equipment.

[0024] 4. The rare earth mixture dispersion and grinding equipment has slots on the fixed sheet and the rotating sheet in the shape of eccentric oblique strips, and the area occupied by the slots does not exceed 50% of the fixed sheet and the rotating sheet as a whole. When the rotating sheet is driven to rotate by the stirring rod, the gap formed by the overlap of the fixed sheet and the rotating sheet moves from the outside to the inside or from the inside to the outside in the slot. The eccentric oblique strip slots on the fixed sheet and the rotating sheet are divided into multiple sections, each section is provided with a gap, and it is ensured that the gap formed by the fixed sheet and the rotating sheet during the rotation process can be closed. The eccentric oblique strip slot design makes the gap formed by the overlap with the fixed sheet constantly change during the rotation of the rotating sheet. The dynamically changing gap not only increases the shear force on the raw materials, but also breaks the raw material particles more effectively through the friction and extrusion of the slot edge. Especially when the slot moves from the outside to the inside or from the inside to the outside, the raw material particles will be subjected to forces in different directions, making them easier to be broken and refined. The area occupied by the slot does not exceed 50% of the total area of ​​the fixed plate and the rotating plate. This design reduces the possibility of raw material accumulation inside the slot and reduces the risk of blockage. At the same time, since wear on the edge of the slot is inevitable, the segmented design allows the wear to be dispersed in multiple areas, extending the service life of the partition component. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 Schematic diagram of the dispersion device of the present invention.

[0026] Figure 2 It is a schematic diagram of the dispersion tube structure of the present invention.

[0027] Figure 3 It is a schematic cross-sectional view of the dispersion tube of the present invention.

[0028] Figure 4 Detailed illustration of the dispersion tube of the present invention Figure 1 .

[0029] Figure 5 Detailed illustration of the dispersion tube of the present invention Figure 2 .

[0030] Figure 6 This is a schematic diagram of a first embodiment of a partition assembly of the present invention.

[0031] Figure 7 This is a schematic diagram of Embodiment 2 of the partition assembly of the present invention.

[0032] In the figure: 1, dispersion cylinder; 11, stirring rod; 12, partition assembly; 13, stirring blade; 14, ultrasonic device; 15, discharge port; 111, limiting ring; 121, fixing ring; 122, fixing plate; 123, rotating plate; 131, mounting ring; 132, retaining ring. DETAILED DESCRIPTION

[0033] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] See also Figure 1-Figure 2 and Figure 4 The rare earth mixture mixing, dispersing and grinding equipment comprises a dispersing cylinder 1 for dispersing and mixing, a stirring rod 11 is arranged at the axis of the dispersing cylinder 1, the stirring rod 11 is driven by a motor, an inlet for pouring raw materials is arranged above the dispersing cylinder 1, a stirring blade 13 for dispersing and stirring is arranged vertically on the stirring rod 11, a dispersing cylinder 15 for passing the processed raw materials is arranged at the bottom, at least one partition assembly 12 is arranged in the dispersing cylinder 1, the partition assembly 12 is composed of a fixed sheet 122 and a rotating sheet 123, and the partition assembly 12 and the dispersing cylinder 1 is fitted to the inner wall of the dispersion tube 1, and the interior of the dispersion tube 1 is divided into at least two independent spaces. The fixed sheet 122 and the rotating sheet 123 are provided with slots. The fixed sheet 122 has a fixed angle. The rotating sheet 123 is connected to the stirring rod 11. As the stirring rod 11 is driven by the motor to rotate, when the stirring rod 11 rotates, the slots on the fixed sheet 122 are blocked by the rotating sheet 123 to form gaps of varying sizes, and the gaps are closed at a specific rotation angle. An ultrasonic device 14 is provided at the bottom of the dispersion tube 1, and the ultrasonic device 14 can emit upward ultrasonic waves.

[0035] An inorganic oxide containing zinc oxide / manganese oxide / titanium oxide is mixed with a rare earth mixture containing lanthanum / cerium to form a mixed roasting material, and the mass ratio of rare earth to inorganic oxide in the mixed roasting material is controlled to be 3:7, wherein metal cerium / metal lanthanum is added in the form of cerium nitrate / lanthanum nitrate ethanol solution, and metal zinc, metal manganese / metal titanium is added in the form of powder. The raw materials are added into a dispersion cylinder 1 for dispersion and mixing, which helps them to be more evenly distributed among the inorganic oxide powders during the mixing process. This uniform distribution is essential for forming a uniform solid solution or composite oxide in the subsequent heat treatment process. The stirring rod 11 is driven to rotate by a motor, and a stirring blade 13 is provided on the stirring rod 11. The powder and solution in the mixed roasting material are mixed into a uniform paste mixture through the shear force and impact force generated by the rotation of the stirring blade 13 in the raw material. This physical process helps to break the agglomeration between the powder particles and promote the contact and mixing between the components. The mixed paste mixture is put into the dispersion cylinder 1 for high-energy dispersion. The raw materials to be dispersed in the dispersion cylinder 1 can be subjected to high-energy dispersion through the coordinated use of the ultrasonic device 14 and the partition component 12. The separation component 12 is composed of a fixed sheet 122 and a rotating sheet 123. The rotating sheet 123 rotates with the stirring rod 11, while the fixed sheet 122 does not rotate at a fixed angle. The fixed sheet 122 and the rotating sheet 123 are provided with dense pores. As the rotating sheet 123 rotates, when the pores on the rotating sheet 123 and the fixed sheet 122 overlap, a hole for the raw material to pass through is formed. When the pores do not overlap, they are closed to form a partition that cannot pass through. The cooperation of the fixed sheet 122 and the rotating sheet 123 can not only produce a shock to the powder in the pores during the rotation process, but also can effectively prevent the powder from passing through the pores. The shear force is used to break the particles and at the same time, a closure can be formed. When the ultrasonic device 14 at the bottom of the dispersion tube 1 generates an upward ultrasonic wave, the ultrasonic wave can not only act on the raw materials in the dispersion tube 1 to refine the raw materials, but also drive the formation of an upward moving water flow, and generate a weak directional flow in the liquid through the "acoustic streaming effect" of the sound wave. The acoustic streaming effect is a phenomenon in which the liquid is driven to flow due to the local pressure gradient generated by the nonlinear effect and the absorption of the sound wave energy by the liquid when the ultrasonic wave propagates in the liquid. However, the ultrasonic wave cannot form a significant upward water flow and can only move slightly. See Figure 3When the fixed plate 122 and the rotating plate 123 are in a closed state, the weak water flow moving upward will also produce an instantaneous pressure increase on the raw materials in the dispersion tube 1, increase the degree of refinement of the raw materials, and further promote the uniform mixing of the components of the mixture at the microscopic level to obtain a solid-liquid separated suspension. After the high-energy dispersion is completed, the solid-liquid separated suspension is again put into the feeding port of the high-speed dispersion equipment for mechanical dispersion for 20-30 minutes to fully mix the components to obtain a paste mixture. The ultrasonic device 14 is not used for this dispersion. This process may include particle crushing, redistribution and mutual penetration, which is similar to the first mechanical dispersion, but the solid-liquid separation phenomenon that may occur after the high-energy dispersion is mixed again. This step is intended to restore the uniformity of the mixture and may further refine the particle size.

[0036] The ultrasonic device 14 is arranged in a circular shape at the bottom of the dispersion cylinder 1. The annularly distributed ultrasonic device 14 can better transmit ultrasonic waves to any position of the dispersion cylinder 1. At the same time, the raw materials in the dispersion cylinder 1 can evenly absorb the energy generated by the ultrasonic waves, ensuring the uniformity of material refinement and crushing.

[0037] See also Figure 4 A fixing ring 121 is disposed on the inner wall of the dispersion tube 1 . The fixing ring 121 is disposed at a position corresponding to the position of the fixing plate 122 in the partition assembly 12 , and is used to fix and support the fixing plate 122 .

[0038] See also Figure 5 The stirring blade 13 is arranged on a mounting ring 131. The mounting ring 131 can be driven to rotate by the stirring rod 11 and can be displaced in the vertical direction on the stirring rod 11. A retaining ring 132 is arranged at the displacement limit distance. Rubber is arranged between the mounting ring 131 and the retaining ring 132, so that the stirring blade 13 can move with the water flow in the dispersion tube 1 during the stirring process, reduce the wear caused by the impact of the water flow on itself, increase the service life, and reduce the maintenance cost.

[0039] The stirring blade 13 is an axial flow stirring blade, and the blade plane of the axial flow stirring blade is arranged at an angle, which can generate strong axial flow and annular flow. By adjusting the inclination angle and number of the blades, the water flow can be guided to form an upward circulating flow and increase the shear force.

[0040] A limiting ring 111 is provided at the bottom center of the dispersion cylinder 1, and the bottom end of the stirring rod 11 is inserted into the limiting ring 111. Rubber is provided between the bottom end of the stirring rod 11 and the limiting ring 111. The limiting ring 111 reduces the deviation of the stirring rod 11 during operation. At the same time, the rubber is used to absorb vibration, thereby reducing the vibration transmitted to the equipment and reducing damage to the equipment.

[0041] See also Figure 6 The slots on the fixed plate 122 and the rotating plate 123 are circular, and the area occupied by the slots does not exceed 50% of the entire fixed plate 122 and the rotating plate 123.

[0042] Example 2: Please refer to Figure 1-Figure 2 and Figure 4 The rare earth mixture mixing, dispersing and grinding equipment comprises a dispersing cylinder 1 for dispersing and mixing, a stirring rod 11 is arranged at the axis of the dispersing cylinder 1, the stirring rod 11 is driven by a motor, an inlet for pouring raw materials is arranged above the dispersing cylinder 1, a stirring blade 13 for dispersing and stirring is arranged vertically on the stirring rod 11, a dispersing cylinder 15 for passing the processed raw materials is arranged at the bottom, at least one partition assembly 12 is arranged in the dispersing cylinder 1, the partition assembly 12 is composed of a fixed sheet 122 and a rotating sheet 123, and the partition assembly 12 and the dispersing cylinder 1 is fitted to the inner wall of the dispersion tube 1, and the interior of the dispersion tube 1 is divided into at least two independent spaces. The fixed sheet 122 and the rotating sheet 123 are provided with slots. The fixed sheet 122 has a fixed angle. The rotating sheet 123 is connected to the stirring rod 11. As the stirring rod 11 is driven by the motor to rotate, when the stirring rod 11 rotates, the slots on the fixed sheet 122 are blocked by the rotating sheet 123 to form gaps of varying sizes, and the gaps are closed at a specific rotation angle. An ultrasonic device 14 is provided at the bottom of the dispersion tube 1, and the ultrasonic device 14 can emit upward ultrasonic waves.

[0043] An inorganic oxide containing zinc oxide / manganese oxide / titanium oxide is mixed with a rare earth mixture containing lanthanum / cerium to form a mixed roasting material, and the mass ratio of rare earth to inorganic oxide in the mixed roasting material is controlled to be 3:7, wherein metal cerium / metal lanthanum is added in the form of cerium nitrate / lanthanum nitrate ethanol solution, and metal zinc, metal manganese / metal titanium is added in the form of powder. The raw materials are added into a dispersion cylinder 1 for dispersion and mixing, which helps them to be more evenly distributed among the inorganic oxide powders during the mixing process. This uniform distribution is essential for forming a uniform solid solution or composite oxide in the subsequent heat treatment process. The stirring rod 11 is driven to rotate by a motor, and a stirring blade 13 is provided on the stirring rod 11. The powder and solution in the mixed roasting material are mixed into a uniform paste mixture through the shear force and impact force generated by the rotation of the stirring blade 13 in the raw material. This physical process helps to break the agglomeration between the powder particles and promote the contact and mixing between the components. The mixed paste mixture is put into the dispersion cylinder 1 for high-energy dispersion. The raw materials to be dispersed in the dispersion cylinder 1 can be subjected to high-energy dispersion through the coordinated use of the ultrasonic device 14 and the partition component 12. The separation component 12 is composed of a fixed sheet 122 and a rotating sheet 123. The rotating sheet 123 rotates with the stirring rod 11, while the fixed sheet 122 does not rotate at a fixed angle. The fixed sheet 122 and the rotating sheet 123 are provided with dense pores. As the rotating sheet 123 rotates, when the pores on the rotating sheet 123 and the fixed sheet 122 overlap, a hole for the raw material to pass through is formed. When the pores do not overlap, they are closed to form a partition that cannot pass through. The cooperation of the fixed sheet 122 and the rotating sheet 123 can not only produce a shock to the powder in the pores during the rotation process, but also can effectively prevent the powder from passing through the pores. The shear force is used to break the particles and at the same time, a closure can be formed. When the ultrasonic device 14 at the bottom of the dispersion tube 1 generates an upward ultrasonic wave, the ultrasonic wave can not only act on the raw materials in the dispersion tube 1 to refine the raw materials, but also drive the formation of an upward moving water flow, and generate a weak directional flow in the liquid through the "acoustic streaming effect" of the sound wave. The acoustic streaming effect is a phenomenon in which the liquid is driven to flow due to the local pressure gradient generated by the nonlinear effect and the absorption of the sound wave energy by the liquid when the ultrasonic wave propagates in the liquid. However, the ultrasonic wave cannot form a significant upward water flow and can only move slightly. See Figure 3When the fixed plate 122 and the rotating plate 123 are in a closed state, the weak water flow moving upward will also produce an instantaneous pressure increase on the raw materials in the dispersion tube 1, increase the degree of refinement of the raw materials, and further promote the uniform mixing of the components of the mixture at the microscopic level to obtain a solid-liquid separated suspension. After the high-energy dispersion is completed, the solid-liquid separated suspension is again put into the feeding port of the high-speed dispersion equipment for mechanical dispersion for 20-30 minutes to fully mix the components to obtain a paste mixture. The ultrasonic device 14 is not used for this dispersion. This process may include particle crushing, redistribution and mutual penetration, which is similar to the first mechanical dispersion, but the solid-liquid separation phenomenon that may occur after the high-energy dispersion is mixed again. This step is intended to restore the uniformity of the mixture and may further refine the particle size.

[0044] The ultrasonic device 14 is arranged in a circular shape at the bottom of the dispersion cylinder 1. The annularly distributed ultrasonic device 14 can better transmit ultrasonic waves to any position of the dispersion cylinder 1. At the same time, the raw materials in the dispersion cylinder 1 can evenly absorb the energy generated by the ultrasonic waves, ensuring the uniformity of material refinement and crushing.

[0045] See also Figure 4 A fixing ring 121 is disposed on the inner wall of the dispersion tube 1 . The fixing ring 121 is disposed at a position corresponding to the position of the fixing plate 122 in the partition assembly 12 , and is used to fix and support the fixing plate 122 .

[0046] See also Figure 5 The stirring blade 13 is arranged on a mounting ring 131. The mounting ring 131 can be driven to rotate by the stirring rod 11 and can be displaced in the vertical direction on the stirring rod 11. A retaining ring 132 is arranged at the displacement limit distance. Rubber is arranged between the mounting ring 131 and the retaining ring 132, so that the stirring blade 13 can move with the water flow in the dispersion tube 1 during the stirring process, reduce the wear caused by the impact of the water flow on itself, increase the service life, and reduce the maintenance cost.

[0047] The stirring blade 13 is an axial flow stirring blade, and the blade plane of the axial flow stirring blade is arranged at an angle, which can generate strong axial flow and annular flow. By adjusting the inclination angle and number of the blades, the water flow can be guided to form an upward circulating flow and increase the shear force.

[0048] A limiting ring 111 is provided at the bottom center of the dispersion cylinder 1, and the bottom end of the stirring rod 11 is inserted into the limiting ring 111. Rubber is provided between the bottom end of the stirring rod 11 and the limiting ring 111. The limiting ring 111 reduces the deviation of the stirring rod 11 during operation. At the same time, the rubber is used to absorb vibration, thereby reducing the vibration transmitted to the equipment and reducing damage to the equipment.

[0049] See also Figure 7 The slots on the fixed sheet 122 and the rotating sheet 123 are eccentrically inclined strips, and the area occupied does not exceed 50% of the fixed sheet 122 and the rotating sheet 123 as a whole. When the rotating sheet 123 is driven to rotate by the stirring rod 11, the gap formed by the overlapping of the fixed sheet 122 and the rotating sheet 123 moves from the outside to the inside or from the inside to the outside in the slot. The eccentrically inclined strip slots on the fixed sheet 122 and the rotating sheet 123 are divided into multiple sections, each of which is provided with a gap, and it is ensured that the gap formed by the fixed sheet 122 and the rotating sheet 123 during the rotation process can be closed. The eccentrically inclined strip slot design makes it overlap with the fixed sheet 122 during the rotation of the rotating sheet 123. The gap formed is constantly changing. This dynamically changing gap not only increases the shear force on the raw material, but also crushes the raw material particles more effectively through the friction and extrusion of the slot edge. In particular, when the slot moves from the outside to the inside or from the inside to the outside, the raw material particles will be subjected to forces in different directions, making them easier to be crushed and refined. The area occupied by the slot does not exceed 50% of the total area of ​​the fixed plate 122 and the rotating plate 123. This design reduces the possibility of raw material accumulation inside the slot and reduces the risk of blockage. At the same time, since wear on the edge of the slot is inevitable, the segmented design allows the wear to be dispersed in multiple areas, thereby extending the service life of the partition component.

[0050] Working principle: Inorganic oxides containing zinc oxide / manganese oxide / titanium oxide are mixed with rare earth mixtures containing lanthanum / cerium to form a mixed roasting material, and the mass ratio of rare earth to inorganic oxides in the mixed roasting material is controlled to be 3:7, wherein metal cerium / metal lanthanum is added in the form of cerium nitrate / lanthanum nitrate ethanol solution, and metal zinc, metal manganese / metal titanium is added in the form of powder. The raw materials are added into the dispersion cylinder 1 for dispersion and mixing, which helps them to be more evenly distributed among the inorganic oxide powders during the mixing process. This even distribution is essential for forming a uniform solid solution or composite oxide in the subsequent heat treatment process. The stirring rod 11 is driven by a motor to rotate The stirring rod 11 is provided with a stirring blade 13. The shear force and impact force generated by the rotation of the stirring blade 13 in the raw material can mix the powder and solution in the mixed roasting material into a uniform paste mixture. This physical process helps to break the agglomeration between the powder particles and promote the contact and mixing between the components. The mixed paste mixture is put into the dispersion cylinder 1 for high-energy dispersion. The ultrasonic device 14 and the partition component 12 are used in combination to perform high-energy impact on the dispersed raw materials in the dispersion cylinder 1. The partition component 12 is composed of a fixed sheet 122 and a rotating sheet 123. The rotating sheet 123 will rotate with the stirring rod 11. The fixed sheet 122 and the rotating sheet 123 are provided with dense pores. As the rotating sheet 123 rotates, when the pores on the rotating sheet 123 and the fixed sheet 122 overlap, a hole for the raw material to pass through is formed. When the pores do not overlap, they are closed to form a partition that cannot pass through. The cooperation of the fixed sheet 122 and the rotating sheet 123 can not only generate shear force to crush the powder in the pores during the rotation process, but also form a closure. When the ultrasonic device 14 at the bottom of the dispersion cylinder 1 generates an upward ultrasonic wave, the ultrasonic wave can not only act on the raw materials in the dispersion cylinder 1, The raw materials are refined and an upward water flow is formed. A weak directional flow is generated in the liquid through the "acoustic streaming effect" of the sound wave. The acoustic streaming effect is a phenomenon in which the liquid is driven to flow due to the local pressure gradient generated by the nonlinear effect and the absorption of sound wave energy by the liquid when the ultrasonic wave propagates in the liquid. However, the ultrasonic wave cannot form a significant upward water flow and can only move slightly. When the fixed plate 122 and the rotating plate 123 are in a closed state, the weak upward water flow will also increase the instantaneous pressure of the raw materials in the dispersion tube 1, increase the degree of refinement of the raw materials, and further promote the uniform mixing of the components of the mixture at the microscopic level., a suspension with solid-liquid separation is obtained. When the high-energy dispersion is completed, the suspension with solid-liquid separation is put into the feeding port of the high-speed dispersion equipment again for mechanical dispersion. The dispersion lasts for 20-30 minutes to make the components fully mixed and uniform to obtain a paste mixture. This dispersion does not use an ultrasonic device 14. This process may include particle crushing, redistribution and mutual penetration, which is similar to the first mechanical dispersion, but the solid-liquid separation phenomenon that may occur after the high-energy dispersion is re-mixed. This step is intended to restore the uniformity of the mixture and may further refine the particle size. ,

[0051] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0052] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A rare earth mixture mixed roasting process, characterized in that: The calcination process comprises the following steps: step 1, preparing a mixed calcination material, mixing an inorganic oxide containing zinc oxide / manganese oxide / titanium oxide with a rare earth mixture containing lanthanum / cerium to form a mixed calcination material, controlling the mass ratio of rare earth to inorganic oxide in the mixed calcination material to be 3:7, wherein metal cerium / metal lanthanum is added in the form of an ethanol solution of cerium nitrate / lanthanum nitrate, and metal zinc / metal manganese / metal titanium is added in the form of powder; step 2, mechanical dispersion, putting the mixed calcination material prepared in step 1 into the feeding port of a dispersion device for mechanical dispersion, and dispersing 20-30min, so that the various components are evenly mixed to obtain a paste mixture; step three, high-energy dispersion, the mixed paste mixture in step two is put into the feeding port of the dispersion equipment for high-energy dispersion, dispersed for 40-50min, so that the various components are fully mixed at the micro level to obtain a solid-liquid separation suspension; step four, secondary mechanical dispersion, the suspension with solid-liquid separation in step three is put into the feeding port of the dispersion equipment again for mechanical dispersion, dispersed for 20-30min, so that the various components are fully mixed to obtain a paste mixture; Step 5, drying, placing the paste mixture in step 4 in an oven at 120°C for 24-48h, and drying the paste mixture thoroughly; Step 6, tunnel kiln firing, placing the block obtained in step 5 in a crucible and placing it on a conveyor, and controlling a certain gap between each crucible through a fully automatic intelligent arrangement device to form a roasting air duct, while controlling the roasting temperature between each crucible to be consistent, and controlling the roasting buffer temperature to rise from room temperature to 1500°C, and after 2h of heating and firing, entering the high temperature roasting zone, the temperature is 1500°C, and the high temperature The calcination time is 3 hours, and then enters the cooling zone, the temperature drops from 1500°C to room temperature, the cooling zone takes 2 hours, and then is transferred to the external conveyor belt, waiting to be taken out, and the overall temperature control accuracy is ≤5°C; Step seven, grinding, the high-temperature blended doped oxide calcined in step six is ​​ground, first the block material is placed in the grinding equipment for initial crushing and dispersion into small particles, and then different fine grinding equipment is selected according to the purpose of the material for secondary fine grinding to achieve the required particle size value, the particle size range of the material is 200nm-150,000nm.

2. A rare earth mixture dispersing and grinding device for the rare earth mixture mixed roasting process of claim 1, comprising a dispersing cylinder (1) for dispersing and mixing, a stirring rod (11) is arranged at the axis of the dispersing cylinder (1), the stirring rod (11) is driven by a motor, an inlet for pouring raw materials is arranged above the dispersing cylinder (1), stirring blades (13) for dispersing and stirring are arranged in a vertical array on the stirring rod (11), and a discharge port (15) for passing the processed raw materials is arranged at the lower part of the dispersing cylinder (1), characterized in that: At least one partition component (12) is provided in the dispersion cylinder (1). The partition component (12) is composed of a fixed sheet (122) and a rotating sheet (123). The partition component (12) is fitted to the inner wall of the dispersion cylinder (1) and divides the interior of the dispersion cylinder (1) into at least two independent spaces. Slots are provided on the fixed sheet (122) and the rotating sheet (123). The fixed sheet (122) has a fixed angle. The rotating sheet (123) is connected to the stirring rod (11) and rotates with the stirring rod (11) driven by a motor. When the stirring rod (11) rotates, the slot on the fixed sheet (122) is blocked by the rotating sheet (123) to form a gap of varying size, and the gap is in a closed state at a specific rotation angle. An ultrasonic device (14) is provided at the bottom of the dispersion cylinder (1). The ultrasonic device (14) is capable of emitting upward ultrasonic waves.

3. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The ultrasonic device (14) is arranged in a circular ring shape at the bottom of the dispersion cylinder (1).

4. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The inner wall of the dispersion cylinder (1) is provided with a fixing ring (121), the fixing ring (121) being arranged at a position corresponding to the position of a fixing plate (122) in the separation assembly (12), and being used for fixing and supporting the fixing plate (122).

5. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The stirring blade (13) is arranged on a mounting ring (131); the mounting ring (131) can be driven to rotate by the stirring rod (11) and can be displaced in a vertical direction on the stirring rod (11); a retaining ring (132) is arranged at a displacement limit distance; and rubber is arranged between the mounting ring (131) and the retaining ring (132).

6. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The stirring blade (13) is an axial flow stirring blade.

7. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: A limiting ring (111) is provided at the center of the bottom of the dispersion cylinder (1), the bottom end of the stirring rod (11) penetrates into the limiting ring (111), and rubber is provided between the bottom end of the stirring rod (11) and the limiting ring (111).

8. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The slots on the fixed plate (122) and the rotating plate (123) are circular, and the areas occupied by the slots do not exceed 50% of the entire fixed plate (122) and the rotating plate (123).

9. The rare earth mixture dispersion and grinding device according to claim 2, characterized in that: The slots on the fixed plate (122) and the rotating plate (123) are in the shape of eccentric oblique strips, and the area occupied by the slots does not exceed 50% of the entire fixed plate (122) and the rotating plate (123). When the rotating plate (123) is driven to rotate by the stirring rod (11), the gap formed by the overlapping of the fixed plate (122) and the rotating plate (123) moves from the outside to the inside or from the inside to the outside in the slots.

10. The rare earth mixture dispersion and grinding device according to claim 9, characterized in that: The eccentric oblique strip-shaped slots on the fixed plate (122) and the rotating plate (123) are divided into multiple sections, each section is provided with a gap, and it is ensured that the gap formed by the fixed plate (122) and the rotating plate (123) can be closed during the rotation process.

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