Device for synthesizing nano rare earth carbonate through continuous precipitation
By designing a continuous precipitation and synthesizing nano rare earth carbonate device, using multi-stage precipitation kettles and ultrasonic and microwave technologies, the problems of rare earth nanooxide particles are easily agglomerated and poor dispersible, and the continuous production and performance improvement of rare earth carbonate is achieved.
Patent Information
- Application Number
- CN202421342489.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-13
- Publication Date
- 2025-05-02
- Estimated Expiration
- 2034-06-13
AI Technical Summary
In the prior art, rare earth nanooxide particles are prone to agglomeration, have poor dispersion, and it is difficult to achieve continuous production of nano rare earth carbonate.
A continuous precipitation synthetic nano rare earth carbonate device is designed. By setting up a multi-stage precipitation kettle and connecting it in series with overflow tubes, an ultrasonic generator and a microwave controller, the sufficient reaction of rare earth materials and effective control of particle size are achieved.
The yield of rare earth materials is improved, the subsequent wastewater treatment volume is reduced, and rare earth carbonates with small particle size, good dispersion and large specific surface area are obtained, achieving continuous production of rare earth carbonates.
Smart Images
Figure CN222816350U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of rare earth metallurgy and materials, and more specifically, to a device for continuously precipitating and synthesizing nano rare earth carbonate. Background Art
[0002] Rare earth elements have unique 4f sublayer electronic structures and special optical, electrical, and magnetic properties. Rare earths play an important role in the field of high-tech and are known as a "treasure trove of new materials." Rare earth nanomaterials have small size effects, quantum effects, high specific surface area, surface effects, and interface effects. They have extremely strong optical, electrical, and magnetic properties, superconductivity, and high chemical activity, which greatly improves the performance and function of materials, maximizes the excellent performance of rare earth materials, and further expands their applications in traditional materials and new high-tech manufacturing fields.
[0003] There are many methods for preparing rare earth nanomaterials, such as precipitation method, hydrothermal method, gel-sol method, alkoxide method, etc. The precipitation method is the most widely used method for synthesizing ultrafine powder materials and is also the easiest method to achieve industrial large-scale production. Nano rare earth oxide particles prepared by conventional precipitation method are easy to agglomerate and have poor dispersibility.
[0004] Therefore, a device for continuously precipitating and synthesizing nano rare earth carbonate is needed to solve the problems in the prior art. Utility Model Content
[0005] The utility model aims to provide a device for continuously precipitating and synthesizing nano rare earth carbonates to solve the problems existing in the prior art. A plurality of precipitation kettles are arranged, and the plurality of precipitation kettles are connected in series through overflow pipes to form a multi-stage precipitation kettle, so that the precipitation effect is better. An ultrasonic generator and a microwave controller are arranged on the precipitation kettle, so that the rare earth material in the precipitation kettle can be better heated and the reaction of the rare earth material can be accelerated.
[0006] To achieve the above-mentioned purpose, the utility model provides the following scheme: The utility model provides a continuous precipitation synthesis device for nano rare earth carbonate, comprising: a plurality of precipitation kettles, the plurality of precipitation kettles are connected by overflow pipes, and the plurality of precipitation kettles form a multi-stage reaction mechanism; an ultrasonic generator, the ultrasonic generator is an ultrasonic vibration rod, and the ultrasonic vibration rod is arranged in the precipitation kettle; a microwave controller, the microwave controller is arranged in the precipitation kettle; the microwave controller comprises a magnetron and a thermocouple, the magnetron is arranged on the outer wall of the precipitation kettle, and the thermocouple is arranged inside the precipitation kettle.
[0007] Furthermore, one end of the overflow pipe is connected to the overflow port at the top of the precipitation tank, and the other end is connected to the feed port at the bottom of another precipitation tank.
[0008] Furthermore, it also includes a stirring member, which includes a stirring shaft and a stirring paddle. The stirring paddle is arranged below the stirring shaft, and the top of the stirring shaft is connected to the motor.
[0009] Furthermore, a pH meter is provided in the precipitation kettle.
[0010] Furthermore, a discharge port is provided at the bottom of the precipitation kettle.
[0011] The utility model discloses the following technical effects:
[0012] Multiple precipitation kettles are connected in series through an overflow pipe, so that the unreacted rare earth material in the precipitation kettle enters the next-level precipitation kettle for further precipitation, which is convenient for the rare earth material to fully react, improves the yield of the rare earth material, and reduces the subsequent wastewater treatment volume; an ultrasonic generator and a microwave controller are arranged on the precipitation kettle, and the internal heating of microwaves and the cavitation effect of ultrasonic waves are utilized to promote the formation of crystal nuclei while inhibiting the growth of grains, so that rare earth carbonates with small particle size, good dispersibility and large specific surface area can be obtained, which can accelerate the reaction speed and improve the rare earth yield. BRIEF DESCRIPTION OF THE DRAWINGS
[0013] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0014] Figure 1 It is a schematic diagram of the overall structure of the utility model;
[0015] Among them, 1. stirring shaft; 2. stirring paddle; 3. precipitation kettle; 4. ultrasonic vibration rod; 5. magnetron; 6. thermocouple; 7. discharge port; 8. overflow pipe; 9. pH meter. DETAILED DESCRIPTION
[0016] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0017] In order to make the above-mentioned purposes, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.
[0018] like Figure 1As shown, the utility model provides a continuous precipitation synthesis device for nano rare earth carbonate, comprising: a plurality of precipitation tanks 3, which are connected by overflow pipes 8 and form a multi-stage reaction mechanism; an ultrasonic generator, which is arranged in the precipitation tank 3; and a microwave controller, which is arranged in the precipitation tank 3.
[0019] The number of precipitation tanks 3 is determined according to the number of stages of the process configuration. The number of precipitation tanks 3 is determined according to the concentration of the rare earth liquid and the precipitant, and the particle size of the rare earth carbonate. The smaller the particle size of the rare earth carbonate, the lower the concentration of the precipitant, the more stages of precipitation tanks 3, and the smaller the particle size of the rare earth carbonate.
[0020] An overflow outlet is provided on one side of the top of the precipitation kettle 3, and an overflow inlet is provided on one side of the bottom. One end of the overflow pipe 8 is connected to the overflow outlet at the top of the precipitation kettle 3, and the other end is connected to the overflow inlet at the bottom of the next-stage precipitation kettle 3. The two-stage precipitation kettles 3 are connected through the overflow pipe 8, so that the overflow outlet on the top side wall of the precipitation kettle 3 is connected to the lower side wall of the next-stage precipitation kettle 3, so that the unreacted rare earth material in the current-stage precipitation kettle 3 enters the next-stage precipitation kettle 3 for continued precipitation, avoiding waste of rare earth materials due to insufficient reaction, and also reducing the amount of wastewater treated in the later stage.
[0021] A discharge port 7 is provided below the precipitation kettle 3 , and the rare earth material that has reacted sufficiently is discharged from the precipitation kettle 3 through the discharge port 7 . A valve is provided at the discharge port 7 to facilitate control of the discharge port 7 .
[0022] The outer wall of the precipitation kettle 3 is provided with a heat-insulating material, which can prevent the temperature in the precipitation kettle 3 from radiating outwards, ensure the temperature in the precipitation kettle 3 is stable, and facilitate the rare earth material in the precipitation kettle 3 to fully react.
[0023] The ultrasonic generator includes an ultrasonic vibrator, which is arranged in the precipitation kettle 3, and has a power of 1000W to 30000W and a frequency of 20KHz. In the present embodiment, the ultrasonic vibrator 4 has a power of 10000W and a frequency of 20KHz. Ultrasonic waves are introduced into the liquid phase precipitation method, and a large number of tiny bubbles are generated due to the "cavitation effect" of ultrasonic waves. The bubbles burst in an instant, generating a high temperature of 7000 to 19000K and a high pressure of more than 500atm, which provide energy for the formation of crystal nuclei, thereby promoting the crystallization and growth of crystal nuclei. At the same time, the mechanical stirring effect generated by ultrasonic waves during the reaction process hinders the growth and agglomeration of crystal nuclei. Under the interaction of multiple effects, the purpose of fast reaction speed and promoting solution dispersion is achieved.
[0024] The microwave controller includes a magnetron 5 and a thermocouple 6. The number and power of the magnetron 5 are determined according to the output of rare earth carbonate and process conditions. The power of the magnetron 5 is 800W or 1000W, and the frequency is 2450MHz. In this embodiment, four magnetrons 5 are provided, and two are arranged in a group on both sides of the outer wall of the precipitation tank 3. The power of the magnetron 5 is 1000W, and the frequency is 2450MHz. The thermocouple 6 is arranged inside the precipitation tank 3 to monitor the temperature in the precipitation tank 3.
[0025] Microwave heating is different from traditional heating methods. Under the action of microwave energy, the molecules of the material vibrate at ultra-high frequencies, which not only generates heat and causes the temperature to rise, but also increases the collision of the materials, strengthens the reaction, shortens the reaction time, and reduces energy consumption. Microwave heating avoids the "cold center" of conventional heating, does not produce temperature gradients, and the crystal nucleation and growth are relatively stable, greatly reducing the generation of powder agglomeration.
[0026] The stirring member includes a stirring shaft 1 and a stirring paddle 2. The top of the stirring shaft 1 is connected to the output end of the motor, and the bottom is connected to the stirring paddle 2. The stirring paddle 2 is located on the top of the precipitation tank 3 and is used to stir the rare earth material to accelerate the reaction rate of the rare earth material.
[0027] A pH meter 9 is also provided in the precipitation kettle 3 for real-time monitoring of the pH value in the precipitation kettle 3. A flow meter is also provided at the feed inlet of the precipitation kettle 3 for calculating the amount of rare earth material put in.
[0028] The device is also provided with a control system, which adopts a centralized control method and is provided with a control panel, so that each stage of the precipitation tank 3 can be controlled separately, and the temperature in the precipitation tank 3 can be controlled according to different processes.
[0029] In this embodiment, a plurality of precipitation kettles 3 are connected in series to form a multi-stage reaction mechanism, and microwave "internal heating" and ultrasonic "cavitation" are performed in the precipitation kettle 3 to accelerate the reaction rate of the rare earth material. The rare earth material after sufficient reaction forms a suspension and is discharged from the discharge port 7. The unreacted rare earth clear liquid is located at the top of the precipitation kettle 3, enters the overflow pipe 8 from the overflow outlet and then flows into the bottom of the next-stage precipitation kettle 3, and is stirred, microwave "internal heating" and ultrasonic "cavitation" are performed in the next-stage precipitation kettle 3 to react again, thereby improving the rare earth yield, realizing continuous precipitation synthesis of nano rare earth carbonate, and solving the problem that nano rare earth carbonate cannot be continuously produced in the current industry.
[0030] The "internal heating" of microwaves and the "cavitation effect" of ultrasound in this device promote the formation of crystal nuclei while inhibiting the growth of grains, thereby obtaining rare earth carbonates with small particle size, good dispersibility and large specific surface area.
[0031] The setting of this device is reasonable. Mechanical stirring, ultrasonic generator and microwave generator are reasonably applied to the material at the same time, which accelerates the reaction, reduces the reaction conditions, shortens the reaction time, and obtains rare earth carbonate with uniform particle size distribution and no agglomeration. The produced rare earth carbonate has the characteristics of high efficiency and continuity, realizing the continuous production of rare earth carbonate. By controlling the temperature, time, microwave power and ultrasonic power through the equipment, nanometer-level rare earth carbonate can be continuously obtained.
[0032] In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.
[0033] The embodiments described above are only descriptions of the preferred methods of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should fall within the protection scope determined by the claims of the present invention.
Claims
1. A device for continuous precipitation synthesis of nano rare earth carbonate, characterized in that: include: A plurality of precipitation tanks (3), wherein the plurality of precipitation tanks (3) are connected via overflow pipes (8), and the plurality of precipitation tanks (3) form a multi-stage reaction mechanism; An ultrasonic generator, wherein the ultrasonic generator is an ultrasonic vibration rod (4), and the ultrasonic vibration rod (4) is arranged in the precipitation kettle (3); A microwave controller, wherein the microwave controller is arranged in the precipitation kettle (3); The microwave controller comprises a magnetron (5) and a thermocouple (6); the magnetron (5) is arranged on the outer wall of the precipitation kettle (3); and the thermocouple (6) is arranged inside the precipitation kettle (3).
2. The continuous precipitation synthesis nano rare earth carbonate device according to claim 1 is characterized in that: One end of the overflow pipe (8) is connected to the overflow port at the top of the precipitation tank (3), and the other end is connected to the feed port at the bottom of another precipitation tank (3).
3. The continuous precipitation synthesis nano rare earth carbonate device according to claim 1 is characterized in that: It also comprises a stirring member, which comprises a stirring shaft (1) and a stirring paddle (2), wherein the stirring paddle (2) is arranged below the stirring shaft (1), and the top of the stirring shaft (1) is connected to a motor.
4. The continuous precipitation synthesis nano rare earth carbonate device according to claim 1 is characterized in that: A pH meter (9) is provided in the precipitation kettle (3).
5. The continuous precipitation synthesis nano rare earth carbonate device according to claim 1 is characterized in that: The bottom of the precipitation kettle (3) is provided with a discharge port (7).