A rare earth mixture mixed roasting process and dispersion grinding equipment thereof

Through the method of combining multi-stage dispersion and ultrasonic wave, the agglomeration and precipitation problems of rare earth mixture in the mixing process are solved, the uniform dispersion and refinement of rare earth mixture is achieved, and the quality and uniformity of the product after roasting are improved.

CN119332079BActive Publication Date: 2025-09-19XIRUI MATERIAL TECH (HANGZHOU) CO LTD
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Patent Information

Application Number
CN202411529634.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-30
Publication Date
2025-09-19
Estimated Expiration
2044-10-30

AI Technical Summary

Technical Problem

The existing technology is difficult to effectively prevent the agglomeration and precipitation of rare earth mixtures during the mixing process, resulting in a decrease in product quality after roasting and difficulty in ensuring uneven dispersion.

Method used

A multi-stage dispersion method is adopted, including mechanical dispersion, high-energy dispersion and secondary mechanical dispersion, combined with an ultrasonic device and a tunnel kiln firing with precise temperature control. The rare earth mixture is evenly dispersed and refined through the coordination of stirring rods, stirring blades and ultrasonic waves.

Benefits of technology

The rare earth mixture is fully mixed at the macro and micro levels, agglomeration and precipitation are avoided, the quality and uniformity of the product after roasting are improved, and the uniformity and activity during subsequent heat treatment are ensured.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of dispersion devices, and discloses a rare earth mixture mixed roasting process and dispersion grinding equipment thereof, comprising a dispersion cylinder for dispersion and mixing, a stirring rod is provided at the axis of the dispersion cylinder, stirring blades for dispersion and stirring are arranged in a vertical array on the stirring rod, a discharge port for passing processed raw materials is provided at the lower part of the dispersion cylinder, at least one partition assembly is provided in the dispersion cylinder, the partition assembly consists of a fixed plate and a rotating plate, the partition assembly is fitted with the inner wall of the dispersion cylinder and divides the interior of the dispersion cylinder into at least two independent spaces, slots are provided 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 as the stirring rod is driven by a motor, when the stirring rod rotates, the slots on the fixed plate are blocked by the rotating plate to form gaps of varying sizes, and the pores are in a closed state at a specific rotation angle, an ultrasonic device is provided at the bottom of the dispersion cylinder, and the ultrasonic device can emit upward ultrasonic waves.
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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 for rare earth mixtures is to uniformly mix compounds or mixtures of rare earth elements (such as lanthanides and scandium, yttrium, etc.) with other substances (such as solvents, additives, carriers, etc.), and to achieve the desired dispersion state of rare earth particles 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 an 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 properties and dispersion requirements. The high-speed rotating shearing component is used to strongly shear the material, so that the rare earth particles are broken and evenly dispersed 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 perform non-contact dispersion treatment on rare earth particles. 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 action of gravity, which causes the denser particles to settle in the mixed system. General dispersion devices are difficult 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] (1) Technical problems solved: In response to the shortcomings of the existing technology, the present invention provides a rare earth mixture mixed roasting process and dispersion grinding equipment 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, the present invention provides the following technical solution: a rare earth mixture mixed roasting process, comprising: step 1, preparing a mixed roasting material by mixing an inorganic oxide containing zinc oxide / manganese oxide / titanium oxide with a rare earth mixture containing lanthanum / cerium to form a mixed roasting material; the mass ratio of rare earth to inorganic oxide in the mixed roasting material is controlled to be 3:7. The metallic cerium / metallic lanthanum is added in the form of an ethanol solution of cerium nitrate / lanthanum nitrate, and the metallic zinc, manganese, and metallic titanium are added in the form of powders.

[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, and disperse it for 20-30 minutes to mix the components evenly to obtain a paste mixture.

[0007] Step 3: High-energy dispersion: put the paste mixture mixed in step 2 into the feeding port of the dispersion equipment for high-energy dispersion, and disperse it for 40-50 minutes to fully mix the components at the micro 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 6, tunnel kiln firing, place the block obtained in step 5 in a crucible and place it on a conveyor, and use a fully automatic intelligent arrangement device to control the gap between each crucible to form a roasting air duct, while controlling the roasting temperature between each crucible to be consistent, and control the roasting buffer temperature to rise from room temperature to 1500 ° C. After 2 hours of heating and firing, it enters the high-temperature roasting zone with a temperature of 1500 ° C. The high-temperature roasting time is 3 hours, and then enters the cooling zone with a temperature of 1500 ° C. and drops to room temperature. The cooling zone takes 2 hours, and then it is transferred to the external conveyor belt and waits to be taken out. The overall temperature control accuracy is ≤5 ° C.

[0011] Step 7: Grinding: Grind the high-temperature blended doped oxides calcined in step 6. First, place the bulk material in a grinding device for primary grinding to disperse it into small particles. Then, select different fine grinding equipment according to the purpose of the material for secondary fine grinding to achieve the required particle size. The particle size range of the material is 200nm-150,000nm.

[0012] The dispersing mechanism comprises the following steps: first, moving the mixing mechanism and the mixing mechanism being coupled to the mixing mechanism, and second, moving the mixing mechanism being coupled to the mixing mechanism. The dispersing mechanism comprises a mixing mechanism for mixing the mixing mechanism, a mixing mechanism for mixing the mixing mechanism being coupled to the mixing mechanism. The mixing mechanism comprises a mixing mechanism for mixing the mixing mechanism, a mixing mechanism for mixing the mixing mechanism being coupled to the mixing mechanism.

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

[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 assembly 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 provided at the displacement limit distance, and rubber is provided between the mounting ring and the retaining ring.

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

[0017] A limiting ring is provided 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 provided 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 oblique and occupy an area not exceeding 50% of the entire fixed plate and the rotating plate. 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 the outside to the inside or from the inside to the outside in the slot.

[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 a dispersion grinding equipment thereof, 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, 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 realizes 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 buffer zone further ensures 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, and 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 separation component (the combination 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 squeezes and releases the raw materials. The opening and closing of the pores in the separator components also indirectly promotes particle refinement. In particular, when the pores are closed, the upward-moving weak water flow increases the instantaneous pressure on the raw materials, helping to further break up 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 barrel, avoiding the accumulation of large particles at the bottom and increasing the uniformity of the dispersion. After the high-energy dispersion stage, through the second mechanical dispersion, the possible solid-liquid separation phenomenon can be effectively resolved and the uniformity of the mixture can be restored. This secondary dispersion process not only ensures the full mixing of the components, but also has the potential to 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. While being driven to rotate by the stirring rod, the mounting ring can be displaced in the vertical direction on the stirring rod, and 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 cylinder during the stirring process, reducing the wear caused by the impact of the water flow on itself, increasing the service life, and reducing maintenance costs. 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 cylinder. The bottom end of the stirring rod penetrates into the limiting ring. 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 operation. At the same time, the rubber is used to absorb vibration, reduce the vibration transmitted to the equipment, and reduce damage to the equipment.

[0024] 4. The rare earth mixture dispersion and grinding equipment has slots on the fixed plate and the rotating plate in the shape of eccentric oblique strips, and the area occupied does not exceed 50% of the entire fixed plate and the rotating plate. 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 the outside to the inside or from the inside to the outside in the slot. The eccentric oblique strip slots on the fixed plate and the rotating plate are divided into multiple sections, each with a gap between each section, and ensure that the gap formed by the fixed plate and the rotating plate can be closed during the rotation process. The eccentric oblique strip slot design makes the gap formed by the overlapping with the fixed plate constantly change during the rotation of the rotating plate. This dynamically changing gap not only increases the shear force on the raw materials, but also crushes the raw material particles more effectively through the friction and extrusion of the slot edges. In particular, when the slot moves from outside to inside or from inside to outside, the raw material particles will be subjected to forces in different directions, making them easier to crush and refine. 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 materials accumulating inside the slot and reduces the risk of blockage. At the same time, since wear on the slot edges is inevitable, the segmented design allows the wear to be dispersed in multiple areas, extending the service life of the separation components. 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 diagram of the dispersion tube of the present invention Figure 1 .

[0029] Figure 5 Detailed diagram 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 a second embodiment 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 clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts 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 includes a dispersing cylinder 1 for dispersing and mixing, a stirring rod 11 is provided at the axis center of the dispersing cylinder 1, the stirring rod 11 is driven by a motor, a feeding port for pouring raw materials is provided above the dispersing cylinder 1, a stirring blade 13 for dispersing and stirring is arranged vertically on the stirring rod 11, a dispersing cylinder 1 is provided with a discharge port 15 for the processed raw materials to pass through at the bottom, at least one partition assembly 12 is provided in the dispersing cylinder 1, the partition assembly 12 is composed of a fixed plate 122 and a rotating plate 123, and the partition assembly 12 and the dispersing cylinder are connected. 1 is fitted to the inner wall of the dispersion cylinder 1, and the interior of the dispersion cylinder 1 is divided into at least two independent spaces. The fixed plate 122 and the rotating plate 123 are provided with slots. The fixed plate 122 has a fixed angle. The rotating plate 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 plate 122 are blocked by the rotating plate 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 cylinder 1, and the ultrasonic device 14 can emit upward ultrasonic waves.

[0035] An inorganic oxide containing zinc oxide / manganese oxide / titanium oxide and a rare earth mixture containing lanthanum / cerium are mixed 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 an ethanol solution of cerium nitrate / lanthanum nitrate, and metal zinc, metal manganese / metal titanium is added in the form of powder. The raw materials are added to 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 uniform distribution is crucial 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 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 materials 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 conjunction to perform high-energy dispersion on the dispersed raw materials in the dispersion cylinder 1. Impact, the separation component 12 is composed of a fixed piece 122 and a rotating piece 123. The rotating piece 123 rotates with the stirring rod 11, while the fixed piece 122 does not rotate at a fixed angle. There are dense pores on the fixed piece 122 and the rotating piece 123. As the rotating piece 123 rotates, when the pores on the rotating piece 123 and the fixed piece 122 overlap, a hole for the raw material to pass through is formed. When the pores do not overlap, they will close to form a separator that cannot pass through. The cooperation of the fixed piece 122 and the rotating piece 123 can not only produce a strong impact on the powder in the pores during the rotation process, but also can effectively prevent the powder from passing through the pores. The shear force breaks the particles and forms a closure at the same time. When the ultrasonic device 14 at the bottom of the dispersion tube 1 generates an upward ultrasonic wave, the ultrasonic wave not only acts on the raw materials in the dispersion tube 1 to refine the raw materials, but also drives the formation of an upward moving water flow. The "acoustic streaming effect" of the sound wave generates a weak directional flow in the liquid. The acoustic streaming effect is a phenomenon in which 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, thereby driving the liquid to flow. However, the ultrasonic wave cannot form a significant upward water flow and can only cause slight movement. Figure 3When the fixed plate 122 and the rotating plate 123 are in a closed state, the weak upward water flow will also produce an instantaneous pressure increase on the raw materials in the dispersion cylinder 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, so as to obtain a suspension with solid-liquid separation. After the high-energy dispersion is completed, the suspension with solid-liquid separation will be put into the feeding port of the high-speed dispersion equipment again for mechanical dispersion. It will be dispersed for 20-30 minutes to fully mix its components and 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 it is mixed again to address the solid-liquid separation phenomenon that may occur after high-energy dispersion. 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 Figure 4 A fixing ring 121 is provided on the inner wall of the dispersion cylinder 1 . The fixing ring 121 is provided 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 Figure 5 The stirring blade 13 is set on the mounting ring 131. While being driven to rotate by the stirring rod 11, the mounting ring 131 can be displaced in the vertical direction on the stirring rod 11, and a retaining ring 132 is provided at the displacement limit distance. Rubber is provided 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, reducing the wear caused by the impact of the water flow on itself, increasing the service life, and reducing the maintenance cost.

[0039] The stirring blade 13 is 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.

[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, reduce the vibration transmitted to the equipment, and reduce damage to the equipment.

[0041] See Figure 6 The slots on the fixed plate 122 and the rotating plate 123 are circular, and the area occupied by them 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 includes a dispersing cylinder 1 for dispersing and mixing, a stirring rod 11 is provided at the axis center of the dispersing cylinder 1, the stirring rod 11 is driven by a motor, a feeding port for pouring raw materials is provided above the dispersing cylinder 1, a stirring blade 13 for dispersing and stirring is arranged vertically on the stirring rod 11, a dispersing cylinder 1 is provided with a discharge port 15 for the processed raw materials to pass through at the bottom, at least one partition assembly 12 is provided in the dispersing cylinder 1, the partition assembly 12 is composed of a fixed plate 122 and a rotating plate 123, and the partition assembly 12 and the dispersing cylinder are connected. 1 is fitted to the inner wall of the dispersion cylinder 1, and the interior of the dispersion cylinder 1 is divided into at least two independent spaces. The fixed plate 122 and the rotating plate 123 are provided with slots. The fixed plate 122 has a fixed angle. The rotating plate 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 plate 122 are blocked by the rotating plate 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 cylinder 1, and the ultrasonic device 14 can emit upward ultrasonic waves.

[0043] An inorganic oxide containing zinc oxide / manganese oxide / titanium oxide and a rare earth mixture containing lanthanum / cerium are mixed 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 an ethanol solution of cerium nitrate / lanthanum nitrate, and metal zinc, metal manganese / metal titanium is added in the form of powder. The raw materials are added to 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 uniform distribution is crucial 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 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 materials 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 conjunction to perform high-energy dispersion on the dispersed raw materials in the dispersion cylinder 1. Impact, the separation component 12 is composed of a fixed piece 122 and a rotating piece 123. The rotating piece 123 rotates with the stirring rod 11, while the fixed piece 122 does not rotate at a fixed angle. There are dense pores on the fixed piece 122 and the rotating piece 123. As the rotating piece 123 rotates, when the pores on the rotating piece 123 and the fixed piece 122 overlap, a hole for the raw material to pass through is formed. When the pores do not overlap, they will close to form a separator that cannot pass through. The cooperation of the fixed piece 122 and the rotating piece 123 can not only produce a strong impact on the powder in the pores during the rotation process, but also can effectively prevent the powder from passing through the pores. The shear force breaks the particles and forms a closure at the same time. When the ultrasonic device 14 at the bottom of the dispersion tube 1 generates an upward ultrasonic wave, the ultrasonic wave not only acts on the raw materials in the dispersion tube 1 to refine the raw materials, but also drives the formation of an upward moving water flow. The "acoustic streaming effect" of the sound wave generates a weak directional flow in the liquid. The acoustic streaming effect is a phenomenon in which 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, thereby driving the liquid to flow. However, the ultrasonic wave cannot form a significant upward water flow and can only cause slight movement. Figure 3When the fixed plate 122 and the rotating plate 123 are in a closed state, the weak upward water flow will also produce an instantaneous pressure increase on the raw materials in the dispersion cylinder 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, so as to obtain a suspension with solid-liquid separation. After the high-energy dispersion is completed, the suspension with solid-liquid separation will be put into the feeding port of the high-speed dispersion equipment again for mechanical dispersion. It will be dispersed for 20-30 minutes to fully mix its components and 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 it is mixed again to address the solid-liquid separation phenomenon that may occur after high-energy dispersion. 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 Figure 4 A fixing ring 121 is provided on the inner wall of the dispersion cylinder 1 . The fixing ring 121 is provided 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 Figure 5 The stirring blade 13 is set on the mounting ring 131. While being driven to rotate by the stirring rod 11, the mounting ring 131 can be displaced in the vertical direction on the stirring rod 11, and a retaining ring 132 is provided at the displacement limit distance. Rubber is provided 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, reducing the wear caused by the impact of the water flow on itself, increasing the service life, and reducing the maintenance cost.

[0047] The stirring blade 13 is 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.

[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, reduce the vibration transmitted to the equipment, and reduce damage to the equipment.

[0049] See Figure 7 The slots on the fixed piece 122 and the rotating piece 123 are eccentrically oblique strips, and the area occupied does not exceed 50% of the entire fixed piece 122 and the rotating piece 123. When the rotating piece 123 is driven to rotate by the stirring rod 11, the gap formed by the overlapping of the fixed piece 122 and the rotating piece 123 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 piece 122 and the rotating piece 123 are divided into multiple sections, each section is provided with a gap, and it is ensured that the gap formed by the fixed piece 122 and the rotating piece 123 during the rotation process can be closed. The eccentric oblique strip slot design makes it overlap with the fixed piece 122 during the rotation of the rotating piece 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 a rare earth mixture containing lanthanum / cerium to form a mixed roasting material. The mass ratio of rare earth to inorganic oxides in the mixed roasting material is controlled to be 3:7, wherein metallic cerium / metallic lanthanum is added in the form of ethanol solution of cerium nitrate / lanthanum nitrate, and metallic zinc, metallic manganese / metallic titanium is added in the form of powder. The raw materials are added to 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 uniform distribution is crucial for the formation of 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 conjunction with each other to perform high-energy impact on the dispersed raw materials in the dispersion cylinder 1. The partition component 12 is composed of a fixed piece 122 and a rotating piece 123. The rotating piece 123 will rotate with the stirring rod 11. The fixed piece 122 is fixed at a fixed angle and does not rotate. The fixed piece 122 and the rotating piece 123 are provided with dense pores. As the rotating piece 123 rotates, when the pores on the rotating piece 123 and the fixed piece 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 separator that cannot pass through. The cooperation of the fixed piece 122 and the rotating piece 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 upward ultrasonic waves, the ultrasonic waves can not only act on the raw materials in the dispersion cylinder 1, The raw materials are refined and an upward-moving water flow is formed. The "acoustic streaming effect" of the sound wave generates a weak directional flow in the liquid. The acoustic streaming effect is a phenomenon in which the liquid is driven to flow by a local pressure gradient generated by the nonlinear effect and the absorption of sound wave energy by the liquid when ultrasonic waves propagate in the liquid. However, ultrasonic waves 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-moving water flow will also generate an instantaneous pressure increase on the raw materials in the dispersion cylinder 1, thereby increasing the degree of refinement of the raw materials and further promoting the uniform mixing of the various components of the mixture at the microscopic level., obtaining a suspension with solid-liquid separation. After the high-energy dispersion is completed, the suspension with solid-liquid separation is again added to the feed port of the high-speed dispersion equipment for mechanical dispersion. Dispersion is carried out for 20-30 minutes to fully mix the components and obtain a paste-like mixture. This dispersion does not use an ultrasonic device14. This process may include particle breakage, redistribution, and mutual penetration. It is similar to the first mechanical dispersion, but re-mixing is performed to address the solid-liquid separation phenomenon that may occur after high-energy dispersion. This step aims to restore the uniformity of the mixture and may further refine the particle size.

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

[0052] While 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 these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A rare earth mixture mixed roasting process, characterized in that: The roasting process comprises the following steps: Step 1: preparing a mixed calcined material by mixing an inorganic oxide containing zinc oxide / manganese oxide / titanium oxide with a rare earth mixture containing lanthanum / cerium to form a mixed calcined material, wherein the mass ratio of rare earth to inorganic oxide in the mixed calcined material is controlled to be 3:7, wherein the metallic cerium / metallic lanthanum is added in the form of an ethanol solution of cerium nitrate / lanthanum nitrate, and the metallic zinc / metallic manganese / metallic titanium are added in the form of powder; 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; Step 3: High-energy dispersion: put the paste mixture mixed in step 2 into the feeding port of the dispersion equipment for high-energy dispersion, and disperse it for 40-50 minutes to fully mix the components at the micro level to obtain a suspension with solid-liquid separation; 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-like mixture; Step 5: Drying: Place the paste mixture in step 4 in an oven at 120°C for 24-48 hours to thoroughly dry the paste mixture; Step 6, tunnel kiln firing, the block obtained in step 5 is placed in a crucible and placed on a conveyor, and a certain gap is controlled 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. After 2 hours of heating and firing, it enters the high-temperature roasting zone with a temperature of 1500 ° C. The high-temperature roasting time is 3 hours, and then enters the cooling zone with a temperature of 1500 ° C. and drops to room temperature. The cooling zone takes 2 hours, and then it is transferred to the external conveyor belt and waits for removal. The overall temperature control accuracy is ≤5 ° C. Step 7: Grinding: Grind the high-temperature blended doped oxides calcined in step 6. First, place the bulk material in a grinding device for primary grinding to disperse it into small particles. Then, select different fine grinding equipment according to the purpose of the material for secondary fine grinding to achieve the required particle size. The particle size range of the material is 200nm-150,000nm.

Citation Information

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