Rare earth oxygen storage material preparation device and method based on coprecipitation method
By using the mixing and dropping mechanism of the co-precipitation method preparation device, the problems of precipitant dropping rate and uniformity were solved, the chemical homogeneity and thermal stability of rare earth oxygen storage materials were improved, and their performance in catalytic converters was enhanced.
Patent Information
- Application Number
- CN202511939505.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-22
- Publication Date
- 2026-02-03
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the preparation of rare earth oxygen storage materials, the dropping rate and uniformity of the precipitant have a decisive influence on the material structure and performance, leading to a wider particle size distribution, component segregation, and deterioration of pore structure, which affects the oxygen buffering performance and low-temperature catalytic activity of the catalytic converter.
The preparation apparatus based on co-precipitation method includes a mixing mechanism and a dropping mechanism. By controlling the slow and uniform addition and stirring of the precipitant, the uniformity of the reaction is ensured. The uniform mixing of the precipitant and rare earth salt solution is achieved by using a feeding frame and a discharging mechanism.
This improved the chemical homogeneity and thermal stability of rare earth oxygen storage materials, enhancing their oxygen buffering performance and low-temperature catalytic activity in automotive exhaust catalytic converters.
Smart Images
Figure CN121446431A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of materials preparation technology, specifically to an apparatus and method for preparing rare earth oxygen storage materials based on co-precipitation. Background Technology
[0002] Automotive exhaust purification is a crucial technological means to improve air quality and reduce environmental pollution. With increasingly stringent global environmental regulations, the development of high-efficiency catalytic converters has become a key issue for the automotive industry. Among numerous exhaust purification materials, rare earth oxygen storage materials (OSMs) have become an irreplaceable core component due to their unique properties. Oxygen storage materials mainly refer to cerium-zirconium solid solutions (CexZr1-xO2) with cerium (Ce) as the main component. Their core function lies in facilitating the purification of Ce³⁺ / Ce⁻. 4 The reversible redox reaction of the ⁺ catalytic converter dynamically regulates the oxygen concentration in the exhaust gas. When the engine is in a rich-fuel state, the material releases stored oxygen to participate in the oxidation reactions of CO and HC; under lean-fuel conditions, it absorbs excess oxygen to promote the reduction of NOx. This "oxygen buffering" effect enables the three-way catalytic converter (TWC) to maintain a high-efficiency operating window near the stoichiometric air-fuel ratio (λ=1), increasing the conversion efficiency of harmful gases to over 90%.
[0003] In the small-batch preparation of rare-earth oxygen storage materials using the co-precipitation method in the laboratory, the dropping rate and uniformity of the precipitant have a decisive impact on the structure and properties of the material. If the precipitant is not slowly and uniformly added to the rare-earth salt solution, it will lead to excessive local supersaturation, causing uneven nucleation and rapid growth, resulting in a wider particle size distribution and even the formation of irregular aggregates. This non-uniform precipitation process will destroy the chemical homogeneity of the cerium-zirconium solid solution, causing segregation of the components in the material, thereby reducing its oxygen storage capacity and thermal stability. In addition, an excessively rapid addition rate of the precipitant will also cause drastic fluctuations in the solution pH, causing some metal ions to preferentially precipitate, making it difficult to form an ideal solid solution structure, ultimately leading to a decrease in the specific surface area and deterioration of the pore structure. This structural defect will make the material more prone to sintering during aging, resulting in grain coarsening and a reduction in active sites, which will seriously affect its oxygen buffering performance and low-temperature catalytic activity in automotive exhaust catalytic converters. Summary of the Invention
[0004] To achieve the above objectives, the present invention is implemented through the following technical solution: a rare earth oxygen storage material preparation device based on co-precipitation method, including a precipitation tank and a base fixedly connected to the lower surface of the precipitation tank for maintaining the stability of the device. A drain valve is provided through the bottom end of the outer surface of the precipitation tank. By setting the precipitation tank, it serves as a reaction vessel for containing the rare earth salt solution and the main reaction space of the precipitation product. By setting the drain valve, the precipitation product generated after the precipitation tank has been left to stand is discharged. The mixing mechanism is used to mix and agitate the solution, and a mixing chamber is set on the outer surface of the mixing mechanism. At the same time, a pH detector is set in the inner cavity of the mixing chamber to monitor the pH value of the internal solution in real time. By setting the mixing mechanism as the core stirring component, the solution is thoroughly mixed and agitated. The mixing chamber set on its outer surface constitutes an independent mixing chamber, which can effectively prevent solution splashing. A dripping mechanism is used to slowly and evenly drip the precipitant into a rare earth salt solution. By setting the dripping mechanism as a feeding component, the uniformity of the co-precipitation reaction is ensured by controlling the rotation of the mixing mechanism. The mixing mechanism includes a feeding frame fixedly connected to the inner wall of the mixing tank. A limiting cylinder is rotatably connected to the inner cavity of the feeding frame, and a discharging mechanism is slidably connected to the inner cavity of the limiting cylinder. This discharging mechanism is used to uniformly drip the precipitant into the rare earth salt solution. The discharging mechanism includes a sliding tube slidably connected to the inner cavity of the limiting cylinder, perpendicular to the limiting cylinder. Both ends of the sliding tube are fixedly connected to drain pipes, and a one-way valve penetrates the lower surface of the drain pipe. The feeding frame, a funnel-shaped structure fixedly connected to the inner wall of the mixing tank, has material perforations on its surface. The hole allows the rare earth salt solution to be evenly dispersed in the inner cavity of the mixing tank. By setting a discharge mechanism, the precipitant flowing out of the dripping mechanism can flow evenly and slowly into the interior of the rare earth salt solution. By setting a sliding tube, a vertical up-and-down movement effect can be generated in the inner cavity of the limiting cylinder, so that the precipitant discharged through the drain pipe and the one-way valve can be located at different heights in the inner cavity of the mixing tank, thereby achieving the effect of evenly mixing the precipitant and the rare earth salt solution. By setting a one-way valve, the effect is that only the precipitant inside the drain pipe can be discharged to the outside, while the solution inside the mixing tank will not enter the inner cavity of the drain pipe.
[0005] Preferably, an internal threaded ring is fixedly connected to the opening of the mixing tank, the dripping mechanism is set directly above the mixing tank through the internal threaded ring, a positioning ring is fixedly connected to the inner wall of the sedimentation tank, and a support cylinder is fixedly connected to the lower surface of the mixing tank. The bottom end of the support cylinder is squeezed and adapted to the upper surface of the positioning ring, and the support cylinder is rubbed and adapted to the inner wall of the sedimentation tank.
[0006] Preferably, the material placement frame is funnel-shaped with several material-through holes on its outer surface. A limiting ring is fixedly connected to the inner wall of the material placement frame. A rotating ring is rotatably connected to the inner cavity of the limiting ring. An inner hexagonal box is fixedly connected to the inner ring of the rotating ring. The cross-section of the inner cavity of the inner hexagonal box is hexagonal. A hexagonal ring is slidably connected to the inner cavity of the inner hexagonal box. The hexagonal ring is fixedly connected to the top of the limiting cylinder. A connecting hole is opened on the upper surface of the limiting cylinder. The connecting hole is aligned with the inner ring of the hexagonal ring. A first spring is fixedly connected to the lower surface of the hexagonal ring. The bottom end of the first spring is fixedly connected to the bottom surface of the inner cavity of the inner hexagonal box.
[0007] Preferably, the mixing mechanism further includes a funnel ring, which is fixedly connected to the lower surface of the mixing box. A rolling bearing is fixedly connected to the bottom end of the limiting cylinder. A blocking disc is fixedly connected to the outer ring of the rolling bearing. A sealing ring is fixedly connected to the lower surface of the blocking disc. The sealing ring is squeezed and adapted to the inner wall of the funnel ring.
[0008] Preferably, a limiting block is fixedly connected to the outer side of the sliding tube, a limiting groove is formed on the outer surface of the limiting cylinder, the limiting block is slidably connected to the limiting groove, a telescopic tube passes through the upper surface of the sliding tube, the top end of the telescopic tube is fixedly connected to the top surface of the inner cavity of the limiting cylinder, the telescopic tube is connected to a hexagonal ring, and a second spring is fixedly connected to the lower surface of the sliding tube, the bottom end of the second spring is fixedly connected to the bottom surface of the inner cavity of the limiting cylinder.
[0009] Preferably, an inclined plate is fixedly connected to the upper surface of the drain pipe, a support rod is fixedly connected to the upper surface of the blocking disc, an inclined track ring is fixedly connected to the top of the support rod, the inclined track ring is at an angle of 30 degrees to the ground, and a squeezing rod is fixedly connected to the lower surface of the sliding pipe, the end of the squeezing rod away from the sliding pipe is rubbed against the inner wall of the inclined track ring.
[0010] Preferably, the dripping mechanism includes a top cover, an external threaded ring fixedly connected to the lower surface of the top cover, the external threaded ring being threadedly connected to an internal threaded ring, a first feed pipe being provided on the outer surface of the top cover, a connecting shell penetrating through the axial center of the upper surface of the top cover, a stepper motor fixedly connected to the top of the connecting shell, a rotating rod being mounted on the output end of the stepper motor via a coupling, a first rotating tube fixedly connected to the bottom end of the rotating rod, a connecting rod fixedly connected to the inner wall of the first rotating tube, a second rotating tube fixedly connected to the bottom end of the connecting rod, and a rotating ring rotatably connected between the first rotating tube and the second rotating tube.
[0011] Preferably, a first hexagonal tube is fixedly connected to the upper surface of the hexagonal ring, and a second hexagonal tube is fixedly connected to the bottom end of the second rotating tube, with the second hexagonal tube rubbing against the inner wall of the first hexagonal tube.
[0012] Preferably, a liquid storage tank is fixedly connected to the outer surface of the top cover, a connecting pipe passes through the upper surface of the liquid storage tank, a second feed pipe is fixedly connected to the end of the connecting pipe, the second feed pipe passes through the outer surface of the top cover, a connecting pipe is fixedly connected to the end of the second feed pipe away from the connecting pipe, the connecting pipe passes through the rotating ring, and a liquid inlet pipe passes through the upper surface of the liquid storage tank.
[0013] A method for preparing rare earth oxygen storage materials based on co-precipitation includes the following steps: Step 1: Prepare rare earth salt solution: Dissolve soluble rare earth salts in deionized water to prepare a rare earth salt solution with a concentration of 0.1-1.0 mol / L; Step 2: Prepare the precipitant solution: Dissolve the precipitant in deionized water to prepare a precipitant solution with a concentration of 0.5-2.0 mol / L; Step 3: Co-precipitation reaction: Place the rare earth salt solution in the dropping mechanism, start the dropping mechanism to make the mixing mechanism continuously stir at a speed of 200-500 rpm, and at the same time, slowly add the precipitant solution to the mixing tank at a rate of 1-5 mL / min through the dropping mechanism and the mixing mechanism, and control the reaction temperature to 40-80℃ and the pH value to 8-11. Step 4: Aging treatment: After the addition is completed, continue stirring for 2-6 hours, then let it stand at 60-90℃ for 12-24 hours. After that, wash the aged precipitate with deionized water until neutral, then filter and separate it. Dry the filter cake at 100-120℃ for 12-24 hours, and then calcine it at 400-800℃ for 2-6 hours to obtain rare earth oxygen storage material.
[0014] This invention provides an apparatus and method for preparing rare earth oxygen storage materials based on co-precipitation. It has the following beneficial effects: I. The rare earth oxygen storage material preparation device and method based on co-precipitation method, by setting up a mixing mechanism as the core stirring component for fully mixing the solution, and the mixing box set on its outer surface constitutes an independent mixing chamber, which can effectively prevent solution splashing.
[0015] II. The device and method for preparing rare earth oxygen storage materials based on coprecipitation method, by setting up a dripping mechanism as a feeding component to slowly and uniformly drip the precipitant into the rare earth salt solution, and by controlling the rotation of the mixing mechanism to ensure the uniformity of the coprecipitation reaction.
[0016] III. The rare earth oxygen storage material preparation device and method based on co-precipitation method, by setting a feeding frame, the funnel-shaped structure is fixedly connected to the inner wall of the mixing tank. The material passage holes opened on its surface can make the rare earth salt solution uniformly dispersed in the inner cavity of the mixing tank. By setting a discharge mechanism, the precipitant flowing out of the dripping mechanism can flow evenly and slowly into the interior of the rare earth salt solution. By setting a sliding tube, a vertical up and down effect can be generated in the inner cavity of the limiting cylinder, so that the precipitant discharged through the drain pipe and the one-way valve can be located at different heights in the inner cavity of the mixing tank, further improving the uniform mixing effect of the precipitant and the rare earth salt solution. By setting a one-way valve, the effect is that only the precipitant inside the drain pipe can be discharged to the outside, while the solution inside the mixing tank will not enter the inner cavity of the drain pipe.
[0017] IV. The rare earth oxygen storage material preparation device and method based on co-precipitation method can guide the mixed solution in the mixing chamber by setting a funnel ring, so that the mixed solution inside can flow through the funnel ring into the bottom support cylinder cavity without being blocked. Attached Figure Description
[0018] Figure 1 This is a schematic diagram of the external structure of a rare earth oxygen storage material preparation device based on co-precipitation method according to the present invention. Figure 2 This is a side view of the structure of the dripping mechanism of the present invention detaching from the mixing tank; Figure 3 This is a schematic cross-sectional view of a rare earth oxygen storage material preparation device based on co-precipitation method according to the present invention. Figure 4 This is a schematic diagram of the hybrid mechanism structure of the present invention; Figure 5 This is a schematic cross-sectional view of the hybrid mechanism of the present invention; Figure 6 This is a partial cross-sectional structural diagram of the mixing mechanism of the present invention; Figure 7 This is a schematic diagram of the material discharge mechanism of the present invention; Figure 8 This is a schematic diagram of the dripping mechanism of the present invention; Figure 9 This is a schematic cross-sectional view of the dripping mechanism of the present invention.
[0019] In the diagram: 1. Sedimentation tank; 2. Base; 3. Positioning ring; 4. Support cylinder; 5. Mixing tank; 6. Internal threaded ring; 7. Mixing mechanism; 8. Drip mechanism; 9. Drain valve; 71. Material placement frame; 72. Limiting ring; 73. Rotating ring; 74. Internal hexagonal box; 75. Hexagonal ring; 76. Limiting cylinder; 77. First spring; 78. Discharge mechanism; 79. Funnel ring; 710. First hexagonal tube; 711. Rolling bearing; 712. Blocking disc; 713. Sealing ring; 714. Support rod; 715. Track ring; 781. Sliding tube; 7 82. Telescopic tube; 783. Limiting block; 784. Second spring; 785. Drain pipe; 786. Inclined plate; 787. One-way valve; 788. Extrusion rod; 81. Top cover; 82. External threaded ring; 83. First feed pipe; 84. Connecting shell; 85. Stepper motor; 86. Rotating rod; 87. First rotating tube; 88. Rotating ring; 89. Connecting rod; 810. Second rotating tube; 811. Second hexagonal tube; 812. Second feed pipe; 813. Connecting pipe; 814. Storage tank; 815. Inlet pipe; 816. Connecting pipe. Detailed Implementation
[0020] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention are given for illustrative and descriptive purposes only, and are not intended to be exhaustive or to limit the invention to the forms disclosed. Many modifications and variations will be apparent to those skilled in the art. The embodiments were chosen and described to better illustrate the principles and practical application of the invention, and to enable those skilled in the art to understand the invention and design various embodiments with various modifications suitable for a particular purpose.
[0021] like Figure 1 - Figure 9 As shown, the present invention provides a technical solution: a rare earth oxygen storage material preparation device based on co-precipitation method, including a precipitation tank 1 and a base 2 fixedly connected to the lower surface of the precipitation tank 1 for maintaining the stability of the device. A drain valve 9 is passed through the bottom of the outer surface of the precipitation tank 1. By setting the precipitation tank 1 as a reaction container, it serves as the main reaction space for containing rare earth salt solution and precipitation products. By setting the drain valve 9, the precipitation products generated by the precipitation tank 1 after settling are discharged. During the precipitation process, the support cylinder 4 is detached from the precipitation tank 1 so that the solution inside the precipitation tank 1 is not affected by other factors. The mixing mechanism 7 is used to mix and agitate the solution, and the mixing chamber 5 is set on the outer surface of the mixing mechanism 7. At the same time, a pH detector is set in the inner cavity of the mixing chamber 5 to monitor the pH value of the internal solution in real time. By setting the mixing mechanism 7 as the core stirring component, the solution is fully mixed and agitated. The mixing chamber 5 set on its outer surface constitutes an independent mixing chamber, which can effectively prevent solution splashing. The dripping mechanism 8 is used to slowly and evenly drip the precipitant into the rare earth salt solution. By setting the dripping mechanism 8 as a feeding component, the uniformity of the co-precipitation reaction is ensured by controlling the rotation of the mixing mechanism 7. The mixing mechanism 7 includes a material placement frame 71, which is fixedly connected to the inner wall of the mixing tank 5. A limiting cylinder 76 is rotatably connected to the inner cavity of the material placement frame 71. A discharge mechanism 78 is slidably connected to the inner cavity of the limiting cylinder 76. The discharge mechanism 78 is used to uniformly drip the precipitant into the rare earth salt solution. The discharge mechanism 78 includes a sliding tube 781, which is slidably connected to the inner cavity of the limiting cylinder 76. The sliding tube 781 is perpendicular to the limiting cylinder 76. Both ends of the sliding tube 781 are fixedly connected to a drain pipe 785. A one-way valve 787 passes through the lower surface of the drain pipe 785. By setting the material placement frame 71, this funnel-shaped structure is fixedly connected to the inner wall of the mixing tank 5, and its surface has a permeable opening. The material orifice allows the rare earth salt solution to be evenly dispersed in the inner cavity of the mixing tank 5. By setting the discharge mechanism 78, the precipitant flowing out of the dripping mechanism 8 can flow evenly and slowly into the interior of the rare earth salt solution. By setting the sliding tube 781, it can produce a vertical up-and-down movement effect in the inner cavity of the limiting cylinder 76, thereby allowing the precipitant discharged through the drain pipe 785 and the one-way valve 787 to be located at different heights in the inner cavity of the mixing tank 5, thereby achieving the effect of evenly mixing the precipitant and the rare earth salt solution. By setting the one-way valve 787, it can produce the effect that only the precipitant inside the drain pipe 785 can be discharged to the outside, while the solution inside the mixing tank 5 will not enter the inner cavity of the drain pipe 785.
[0022] An internal threaded ring 6 is fixedly connected to the opening of the mixing tank 5. The dripping mechanism 8 is detachably mounted on the top of the mixing tank 5 via the internal threaded ring 6. A positioning ring 3 is fixedly connected to the inner wall of the sedimentation tank 1. A support cylinder 4 is fixedly connected to the lower surface of the mixing tank 5. The bottom end of the support cylinder 4 is pressed and fitted with the upper surface of the positioning ring 3, and the support cylinder 4 is rubbed and fitted with the inner wall of the sedimentation tank 1. By setting the internal threaded ring 6, the dripping mechanism 8 can be tightly connected to the mixing tank 5 during the reaction, and the residual solution on the inner wall of the mixing tank 5 can be easily cleaned afterward. By setting the positioning ring 3, the support cylinder 4 at the bottom of the mixing tank 5 can be positioned.
[0023] The material placement frame 71 is funnel-shaped with several material passage holes on its outer surface. A limiting ring 72 is fixedly connected to the inner wall of the material placement frame 71. A rotating ring 73 is rotatably connected to the inner cavity of the limiting ring 72. An inner hexagonal box 74 is fixedly connected to the inner ring of the rotating ring 73. The cross-section of the inner cavity of the inner hexagonal box 74 is hexagonal. A hexagonal ring 75 is slidably connected to the inner cavity of the inner hexagonal box 74. The hexagonal ring 75 is fixedly connected to the top of the limiting cylinder 76. A connecting hole is opened on the upper surface of the limiting cylinder 76. The connecting hole is aligned with the inner ring of the hexagonal ring 75. A first spring 77 is fixedly connected to the lower surface of the hexagonal ring 75. The bottom end of 7 is fixedly connected to the bottom surface of the inner cavity of the inner hexagonal box 74. By setting the limiting ring 72, the rotating ring 73 can be limited, allowing the rotating ring 73 to rotate within the cavity of the limiting ring 72, thereby ensuring the stable rotation of the inner hexagonal box 74. By setting the inner hexagonal box 74, the hexagonal ring 75 can move vertically up and down within its inner cavity. Simultaneously, when the hexagonal ring 75 rotates, the pressure between the hexagonal ring 75 and the inner wall of the inner hexagonal box 74 causes the inner hexagonal box 74 and the rotating ring 73 to rotate. By setting the connecting hole, the precipitant in the inner cavity of the hexagonal ring 75 can... The fluid flows into the inner cavity of the limiting cylinder 76 through the connecting hole. By providing a first spring 77, after the hexagonal ring 75 moves downwards and is no longer subjected to downward pressure, the hexagonal ring 75 causes the limiting cylinder 76 to spring back to its original position. The mixing mechanism 7 also includes a funnel ring 79, which is fixedly connected to the lower surface of the mixing box 5. The bottom end of the limiting cylinder 76 is fixedly connected to the inner ring of the rolling bearing 711. A blocking disc 712 is fixedly connected to the outer ring of the rolling bearing 711. A sealing ring 713 is fixedly connected to the lower surface of the blocking disc 712. The sealing ring 713 is pressed and fitted against the inner wall of the funnel ring 79. By providing the funnel ring... 79 can guide the mixed solution in the inner cavity of the mixing tank 5, so that the mixed solution inside can flow through the funnel ring 79 to the inner cavity of the support cylinder 4 at the bottom without being blocked. By setting the rolling bearing 711, the blocking disc 712 and the limiting cylinder 76 can generate stable rotation. Thus, when the blocking disc 712 and the sealing ring 713 block the funnel ring 79, the rotation of the limiting cylinder 76 will not drive the blocking disc 712 and the sealing ring 713 to rotate. By setting the blocking disc 712 and the sealing ring 713, the mixed solution in the inner cavity of the mixing tank 5 will not leak out when it comes into contact with the inside of the funnel ring 79.
[0024] A limiting block 783 is fixedly connected to the outer side of the sliding tube 781. A limiting groove is formed on the outer surface of the limiting cylinder 76, and the limiting block 783 is slidably connected to the limiting groove. A telescopic tube 782 passes through the upper surface of the sliding tube 781. The top end of the telescopic tube 782 is fixedly connected to the top surface of the inner cavity of the limiting cylinder 76. The telescopic tube 782 is connected to the hexagonal ring 75. A second spring 784 is fixedly connected to the lower surface of the sliding tube 781, and the bottom end of the second spring 784 is fixedly connected to the bottom surface of the inner cavity of the limiting cylinder 76. By setting the limiting block 783, when the sliding tube 781 moves up and down in the inner cavity of the limiting cylinder 76, the sliding tube 781 will only move vertically up and down without rotation. By setting the telescopic tube 782, the sliding tube 781 can be connected to the flow hole at the top of the limiting cylinder 76. By setting the second spring 784, when the sliding tube 781 is no longer subjected to downward pressure, the sliding tube 781 is subjected to the second spring. The 784 moves upward due to elastic potential energy. An inclined plate 786 is fixedly connected to the upper surface of the drain pipe 785. A support rod 714 is fixedly connected to the upper surface of the blocking disc 712. An inclined track ring 715 is fixedly connected to the top of the support rod 714. The angle between the inclined track ring 715 and the ground is thirty degrees. A squeezing rod 788 is fixedly connected to the lower surface of the sliding pipe 781. The end of the squeezing rod 788 away from the sliding pipe 781 is rubbed against the inner wall of the inclined track ring 715. By setting the inclined plate 786, when the drain pipe 785 rotates, the inclined plate 786 can rotate in the inner cavity of the mixing box 5, thereby agitating the solution inside. By setting the inclined track ring 715, the squeezing rod 788 can be limited, so that the squeezing rod 788 slides in the inner cavity of the inclined track ring 715 when the sliding pipe 781 rotates. Then, through the cooperation of the second spring 784, the sliding pipe 781 moves up and down.
[0025] The dripping mechanism 8 includes a top cover 81. An external threaded ring 82 is fixedly connected to the lower surface of the top cover 81, and the external threaded ring 82 is threadedly connected to an internal threaded ring 6. A first feed pipe 83 is provided on the outer surface of the top cover 81. A connecting shell 84 passes through the axial center of the upper surface of the top cover 81. A stepper motor 85 is fixedly connected to the top of the connecting shell 84. A rotating rod 86 is mounted on the output end of the stepper motor 85 via a coupling. A first rotating tube 87 is fixedly connected to the bottom end of the rotating rod 86. A connecting rod 89 is fixedly connected to the inner wall of the first rotating tube 87. A second rotating tube 810 is fixedly connected to the bottom end of the connecting rod 89. A rotating joint is rotatably connected between the first rotating tube 87 and the second rotating tube 810. The rotating ring 88, with its external threaded ring 82, can mate with the internal threaded ring 6, thereby connecting the top cover 81 to the mixing tank 5. The rare earth salt solution can be poured into the inner cavity of the mixing tank 5 via the first feed pipe 83. The stepper motor 85, after power is supplied and the switch is turned on, causes the rotating rod 86 to drive the first rotating tube 87 to rotate. The connecting rod 89 allows the first rotating tube 87 to drive the second rotating tube 810 to rotate. A water-permeable hole is located at the connection between the connecting rod 89 and the second rotating tube 810, allowing the precipitant to flow down through the second rotating tube 810. A first hexagonal tube is fixedly connected to the upper surface of the hexagonal ring 75. 710, a second hexagonal tube 811 is fixedly connected to the bottom end of the second rotating tube 810. The second hexagonal tube 811 is frictionally fitted with the inner wall of the first hexagonal tube 710. By setting the first hexagonal tube 710 and the second hexagonal tube 811, when the top cover 81 is installed with the mixing box 5, the second hexagonal tube 811 is inserted into the inner cavity of the first hexagonal tube 710, thereby allowing the precipitant in the inner cavity of the second rotating tube 810 to flow into the inner cavity of the first hexagonal tube 710. At the same time, when the second rotating tube 810 drives the second hexagonal tube 811 to rotate, the second hexagonal tube 811 drives the first hexagonal tube 710 to rotate, causing the first hexagonal tube 710 to drive the hexagonal ring 75. The top cover 81 rotates, and a liquid storage tank 814 is fixedly connected to the outer surface of the top cover 81. A connecting pipe 813 passes through the upper surface of the liquid storage tank 814. A second feed pipe 812 is fixedly connected to the end of the connecting pipe 813. The second feed pipe 812 passes through the outer surface of the top cover 81. A connecting pipe 816 is fixedly connected to the end of the second feed pipe 812 away from the connecting pipe 813. The connecting pipe 816 passes through the rotating ring 88. An inlet pipe 815 passes through the upper surface of the liquid storage tank 814. By setting up the liquid storage tank 814, the precipitant can be stored. By setting up the second feed pipe 812 and the connecting pipe 816, the precipitant in the inner cavity of the liquid storage tank 814 can enter the inner cavity of the rotating ring 88.
[0026] A method for preparing rare earth oxygen storage materials based on co-precipitation includes the following steps: Step 1: Prepare rare earth salt solution: Dissolve soluble rare earth salts in deionized water to prepare a rare earth salt solution with a concentration of 0.1-1.0 mol / L; Step 2: Prepare the precipitant solution: Dissolve the precipitant in deionized water to prepare a precipitant solution with a concentration of 0.5-2.0 mol / L; Step 3: Co-precipitation reaction: Place the rare earth salt solution in the dropping mechanism 8, and start the dropping mechanism 8 to make the mixing mechanism 7 continuously stir at a speed of 200-500 rpm. At the same time, the precipitant solution is slowly added dropwise to the mixing tank 5 at a rate of 1-5 mL / min through the dropping mechanism 8 and the mixing mechanism 7. Control the reaction temperature at 40-80℃ and the pH value at 8-11. After the addition is completed, continue stirring for 2-6 hours. Step 4: Aging treatment: Let the material stand at 60-90℃ for 12-24 hours. Then wash the aged precipitate with deionized water until neutral, then filter and separate it. Dry the filter cake at 100-120℃ for 12-24 hours, and then calcine it at 400-800℃ for 2-6 hours to obtain rare earth oxygen storage material.
[0027] Working principle: During use, the operator prepares the rare earth salt solution and precipitant solution in sequence. Then, the external threaded ring 82 is connected to the internal threaded ring 6, connecting the top cover 81 and the mixing box 5. The prepared rare earth salt solution is then poured into the inner cavity of the mixing box 5 through the first feed pipe 83, ensuring it covers the upper side of the inclined plate 786. The stepper motor 85 is then connected to the power supply and the switch is turned on, causing the rotating rod 86 to drive the first rotating tube 87, connecting rod 89, and second rotating tube 810 to rotate. When the second rotating tube 810 rotates, it causes the second hexagonal tube 811 to drive the first hexagonal tube 710 and hexagonal ring 75 to rotate, ultimately causing the limiting cylinder 76 to drive the sliding tube 781 to rotate. Due to the tension of the second spring 784, the extrusion rod 788 is always in contact with the inner surface of the track ring 715, causing the extrusion rod 788 to slide within the inner cavity of the track ring 715 when the sliding tube 781 rotates, thereby driving the drain pipe 785 to rotate and move upwards. The sliding tube 781 moves up and down, while the telescopic tube 782 is squeezed. When the telescopic tube 782 is stretched, the internal air pressure of the first hexagonal tube 710 decreases, which in turn generates suction in the inner cavity of the second rotating tube 810, which in turn generates suction in the connecting tube 816. This causes the precipitant in the inner cavity of the storage tank 814 to be drawn in and finally discharged from the one-way valve 787 on the lower surface of the drain pipe 785 into the rare earth salt solution inside the mixing tank 5 (it should be noted that the dripping acceleration rate can be adjusted by controlling the speed of the stepper motor 85 to achieve slow dripping of the precipitant). The pH value is also controlled. After the stirring reaction is completed, the stepper motor 85 is stopped and the dripping mechanism 8 is removed. After being freed from downward pressure, the hexagonal ring 75 moves upward under the elastic potential energy of the first spring 77, which causes the blocking disc 712 and the sealing ring 713 to stop squeezing the funnel ring 79. Finally, the solution in the inner cavity of the mixing tank 5 flows into the inner cavity of the sedimentation tank 1, and then it is allowed to stand.
[0028] Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments obtained by those skilled in the art and related fields based on the embodiments of the present invention without inventive effort should fall within the scope of protection of the present invention. Structures, devices, and operating methods not specifically described and explained in the present invention, unless otherwise specified or limited, shall be implemented according to conventional means in the art.
Claims
1. A device for preparing rare earth oxygen storage materials based on co-precipitation method, characterized in that, include: A sedimentation tank (1) and a base (2) fixedly connected to the lower surface of the sedimentation tank (1), wherein a drain valve (9) is passed through the bottom of the outer surface of the sedimentation tank (1). The mixing mechanism (7) is used to mix and agitate the solution, and the mixing tank (5) is disposed on the outer surface of the mixing mechanism (7). A dripping mechanism (8) is used to slowly and evenly drip the precipitant into a rare earth salt solution; The mixing mechanism (7) includes a material placement frame (71), which is fixedly connected to the inner wall of the mixing box (5). A limiting cylinder (76) is rotatably connected to the inner cavity of the material placement frame (71). A discharge mechanism (78) is slidably connected to the inner cavity of the limiting cylinder (76). The discharge mechanism (78) is used to uniformly drip the precipitant into the rare earth salt solution. The discharge mechanism (78) includes a sliding tube (781), which is slidably connected to the inner cavity of the limiting cylinder (76). The sliding tube (781) is perpendicular to the limiting cylinder (76). Both ends of the sliding tube (781) are fixedly connected to a drain pipe (785). A one-way valve (787) passes through the lower surface of the drain pipe (785).
2. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 1, characterized in that: An internal threaded ring (6) is fixedly connected to the opening of the mixing tank (5). The dripping mechanism (8) is set directly above the mixing tank (5) through the internal threaded ring (6). A positioning ring (3) is fixedly connected to the inner wall of the sedimentation tank (1). A support cylinder (4) is fixedly connected to the lower surface of the mixing tank (5). The bottom end of the support cylinder (4) is squeezed and adapted to the upper surface of the positioning ring (3), and the support cylinder (4) is rubbed and adapted to the inner wall of the sedimentation tank (1).
3. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 2, characterized in that: The material placement frame (71) is funnel-shaped with several material passage holes on its outer surface. A limiting ring (72) is fixedly connected to the inner wall of the material placement frame (71). A rotating ring (73) is rotatably connected to the inner cavity of the limiting ring (72). An inner hexagonal box (74) is fixedly connected to the inner ring of the rotating ring (73). The cross-section of the inner cavity of the inner hexagonal box (74) is hexagonal. A hexagonal ring (75) is slidably connected to the inner cavity of the inner hexagonal box (74). The hexagonal ring (75) is fixedly connected to the top of the limiting cylinder (76). A connecting hole is opened on the upper surface of the limiting cylinder (76). The connecting hole is aligned with the inner ring of the hexagonal ring (75). A first spring (77) is fixedly connected to the lower surface of the hexagonal ring (75). The bottom end of the first spring (77) is fixedly connected to the bottom surface of the inner cavity of the inner hexagonal box (74).
4. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 3, characterized in that: The mixing mechanism (7) also includes a funnel ring (79), which is fixedly connected to the lower surface of the mixing box (5). A rolling bearing (711) is fixedly connected to the bottom end of the limiting cylinder (76). A blocking disc (712) is fixedly connected to the outer ring of the rolling bearing (711). A sealing ring (713) is fixedly connected to the lower surface of the blocking disc (712). The sealing ring (713) is squeezed and adapted to the inner wall of the funnel ring (79).
5. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 4, characterized in that: A limiting block (783) is fixedly connected to the outer side of the sliding tube (781). A limiting groove is opened on the outer surface of the limiting cylinder (76). The limiting block (783) is slidably connected to the limiting groove. A telescopic tube (782) passes through the upper surface of the sliding tube (781). The top end of the telescopic tube (782) is fixedly connected to the top surface of the inner cavity of the limiting cylinder (76). The telescopic tube (782) is connected to the hexagonal ring (75). A second spring (784) is fixedly connected to the lower surface of the sliding tube (781). The bottom end of the second spring (784) is fixedly connected to the bottom surface of the inner cavity of the limiting cylinder (76).
6. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 5, characterized in that: An inclined plate (786) is fixedly connected to the upper surface of the drain pipe (785), a support rod (714) is fixedly connected to the upper surface of the blocking disc (712), an inclined track ring (715) is fixedly connected to the top of the support rod (714), the inclined track ring (715) is at an angle of thirty degrees to the ground, and a squeezing rod (788) is fixedly connected to the lower surface of the sliding pipe (781), the end of the squeezing rod (788) away from the sliding pipe (781) is rubbed against the inner wall of the inclined track ring (715).
7. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 6, characterized in that: The dripping mechanism (8) includes a top cover (81), an external threaded ring (82) is fixedly connected to the lower surface of the top cover (81), the external threaded ring (82) is threadedly connected to an internal threaded ring (6), a first feed pipe (83) is provided on the outer surface of the top cover (81), a connecting shell (84) is passed through the axis of the upper surface of the top cover (81), a stepper motor (85) is fixedly connected to the top of the connecting shell (84), a rotating rod (86) is installed at the output end of the stepper motor (85) through a coupling, a first rotating tube (87) is fixedly connected to the bottom end of the rotating rod (86), a connecting rod (89) is fixedly connected to the inner wall of the first rotating tube (87), a second rotating tube (810) is fixedly connected to the bottom end of the connecting rod (89), and a rotating ring (88) is rotatably connected between the first rotating tube (87) and the second rotating tube (810).
8. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 7, characterized in that: The upper surface of the hexagonal ring (75) is fixedly connected to a first hexagonal tube (710), and the bottom end of the second rotating tube (810) is fixedly connected to a second hexagonal tube (811). The second hexagonal tube (811) is frictionally adapted to the inner wall of the first hexagonal tube (710).
9. The rare earth oxygen storage material preparation device based on co-precipitation method according to claim 8, characterized in that: A liquid storage tank (814) is fixedly connected to the outer surface of the top cover (81). A connecting pipe (813) passes through the upper surface of the liquid storage tank (814). A second feed pipe (812) is fixedly connected to the end of the connecting pipe (813). The second feed pipe (812) passes through the outer surface of the top cover (81). A connecting pipe (816) is fixedly connected to the end of the second feed pipe (812) away from the connecting pipe (813). The connecting pipe (816) passes through the rotating ring (88). An inlet pipe (815) passes through the upper surface of the liquid storage tank (814).
10. A rare earth oxygen storage material preparation apparatus based on co-precipitation method according to any one of claims 1-9, and a method for preparing rare earth oxygen storage materials based on co-precipitation method, characterized in that, Includes the following steps: Step 1: Prepare rare earth salt solution: Dissolve soluble rare earth salts in deionized water to prepare a rare earth salt solution with a concentration of 0.1-1.0 mol / L; Step 2: Prepare the precipitant solution: Dissolve the precipitant in deionized water to prepare a precipitant solution with a concentration of 0.5-2.0 mol / L; Step 3: Co-precipitation reaction: Place the rare earth salt solution in the dropping mechanism (8), start the dropping mechanism (8) to make the mixing mechanism (7) continuously stir at a speed of 200-500 rpm, and at the same time, slowly add the precipitant solution to the mixing tank (5) at a rate of 1-5 mL / min through the dropping mechanism (8) and the mixing mechanism (7), control the reaction temperature to 40-80℃, the pH value to 8-11, and continue stirring for 2-6 hours after the addition is completed; Step 4: Aging treatment: Let the material stand at 60-90℃ for 12-24 hours. Then wash the aged precipitate with deionized water until neutral, then filter and separate it. Dry the filter cake at 100-120℃ for 12-24 hours, and then calcine it at 400-800℃ for 2-6 hours to obtain rare earth oxygen storage material.