Device and method for preparing micro-nano cerium oxide by ultrasonic and microwave synergistic method

Abstract

The present invention discloses a device and method for preparing micro-nano cerium oxide by ultrasonic-microwave cooperation, belonging to the field of nano-material preparation, including: The housing includes an ultrasonic atomization chamber and a microwave heating chamber that are independent of each other. A feeding device is arranged at the top of the housing, and the feeding device is communicated with the ultrasonic atomization chamber. An ultrasonic switch and a microwave switch are arranged on the side wall of the housing. The ultrasonic switch is electrically connected to the ultrasonic device in the ultrasonic atomization chamber, and the microwave switch is electrically connected to the microwave device on the side wall of the microwave heating chamber; The heating channel penetrates through the microwave heating chamber, the inlet of the heating channel is arranged in the ultrasonic atomization chamber, and the outlet of the heating channel is communicated with the particle collection tank; The elastic sheet is arranged in the ultrasonic atomization chamber, and the elastic sheet is inclined below the feeding device to bounce the feed into the heating channel. The present invention makes the reaction solution fully atomized and uniformly heated by cooperating ultrasonic and microwave, thereby preparing cerium oxide powder with good dispersion, small and uniform particle size.

Description

Technical Field

[0001] The present invention belongs to the field of preparation of nanomaterials, and particularly relates to an apparatus and method for co-preparing micro-nano cerium oxide by ultrasound and microwave. Background Art

[0002] Cerium oxide is an important industrial resource and even a strategic resource, which has the advantages of low price, non-toxicity and stable chemical properties, and plays a key role in the development of emerging industries. At present, it has been widely used in fields such as chemical mechanical polishing, fuel cells, and biomedicine. When cerium oxide particles reach the nanoscale, they will have quantum size effect, interface effect, small size effect, etc., and have new advantages in physical properties such as electricity, magnetism, and light. At present, the preparation methods of cerium oxide mainly include solid-phase method, liquid-phase method and gas-phase method. The solid-phase method prepares products through solid-solid reaction at high temperature, but the solid-phase method is easy to mix impurities, resulting in low product purity and large particle size distribution. The liquid-phase method mainly includes precipitation method, sol-gel method and microemulsion method, etc. Among them, the precipitation method is easy to cause agglomeration, the sol-gel method has a complex preparation process, and a large amount of acid or alkali is required in the production process, which is easy to cause environmental pollution. The microemulsion method has a high cost, and the gas-phase method also has high requirements for reaction condition control, expensive equipment and low output. To sum up, the current methods such as gas-phase method, solid-phase method and liquid-phase method for preparing cerium oxide all have certain defects, which will limit the industrial production and popularization and application of nano-cerium oxide to a certain extent. Therefore, how to provide a micro-nano cerium oxide preparation technology with convenient preparation and good economy is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0003] In view of this, the present invention provides an apparatus and method for co-preparing micro-nano cerium oxide by ultrasound and microwave, which can fully atomize the reaction solution and uniformly heat it, and is easy to prepare ultrafine cerium oxide powder with good dispersion, small and uniform particle size.

[0004] On the one hand, in order to achieve the above object, the present invention adopts the following technical scheme:

[0005] An apparatus for co-preparing micro-nano cerium oxide by ultrasound and microwave, comprising:

[0006] A housing, the housing includes an ultrasonic atomization chamber and a microwave heating chamber that are independent of each other. A feeding device is provided at the top of the housing, and the feeding device is communicated with the ultrasonic atomization chamber. An ultrasonic switch and a microwave switch are provided on the side wall of the housing. The ultrasonic switch is electrically connected to an ultrasonic device in the ultrasonic atomization chamber, and the microwave switch is electrically connected to a microwave device on the side wall of the microwave heating chamber;

[0007] A heating channel that penetrates through the microwave heating cavity. The inlet of the heating channel is arranged in the ultrasonic atomization cavity, and the outlet of the heating channel is communicated with a particle collection tank;

[0008] A shrapnel is arranged in the ultrasonic atomization cavity, and the shrapnel is obliquely arranged below the feeding device to bounce the feed into the heating channel.

[0009] Preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a touch screen display, which is arranged on the side wall of the housing. Both the ultrasonic device and the microwave device are electrically connected to the touch screen display.

[0010] Preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a gas phase channel, which is arranged on the housing. The outlet of the gas phase channel is communicated with the ultrasonic atomization cavity, and the outlet of the gas phase channel faces the inlet of the heating channel.

[0011] Preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a handle and a universal ball. The universal ball is rotationally connected to the housing. One end of the universal ball is fixedly connected to the handle, and the other end of the universal ball is connected to the shrapnel to adjust the inclination angle of the shrapnel.

[0012] Preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a gas phase outlet, which is arranged above the outlet of the heating channel.

[0013] Preferably, the feeding device includes a hopper and a dropper. The hopper and the dropper are communicated, and the dropper is arranged directly above the shrapnel.

[0014] Preferably, a partition is arranged between the ultrasonic atomization cavity and the microwave heating cavity. A vibration damping layer is arranged on the side of the partition close to the ultrasonic atomization cavity, and a heat insulation layer is arranged on the side of the partition close to the microwave heating cavity.

[0015] On the other hand, the present invention provides a method for co-preparing micro-nano cerium oxide by ultrasonic and microwave, including the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave as described above. The preparation method specifically includes:

[0016] S10: Turn on the ultrasonic switch and the microwave switch, and check the vibration frequency of the shrapnel and the temperature of the microwave heating cavity;

[0017] S20: After the vibration frequency of the shrapnel and the temperature of the microwave heating cavity are confirmed to meet the preset requirements, pour the cerium chloride solution into the feeding device;

[0018] S30: The droplets of the cerium chloride solution fall onto the shrapnel, form a water mist flow and bounce into the heating channel, and then introduce air or pure oxygen into the heating channel;

[0019] S40: Collect the reaction solid product through the particle collection tank, and turn off the ultrasonic switch and the microwave switch after the reaction is complete.

[0020] The beneficial effects of the present invention are as follows: By using ultrasonic waves to drive the elastic sheet to vibrate, the liquid surface bulges under the action of directional pressure, resulting in cavitation in the surrounding liquid surface, atomizing the liquid in the ultrasonic atomization chamber into small molecule aerosols, and through microwaves, the polar molecules and charged particles in the microwave heating chamber will repeatedly turn with the change of the electric field direction, move violently and collide with each other to generate friction, thereby generating a large amount of heat. The cerium chloride solution is fully atomized in the ultrasonic atomization chamber and can be uniformly heated, thereby preparing ultrafine cerium oxide powder with good dispersion, small and uniform particle size. The additional aspects and advantages of the present invention will be partially given in the following description and will become obvious from the following description. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only the embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained according to the provided drawings.

[0022] Figure 1 is the overall structural schematic diagram of the device for ultrasonic and microwave collaborative preparation of micro-nano cerium oxide of the present invention;

[0023] Figure 2 is the side view of the housing of the present invention.

[0024] 1. Handle; 2. Hopper; 3. Dropper; 4. Gas phase channel; 5. Ultrasonic atomization chamber; 6. Universal ball; 7. Elastic sheet; 8. Heating channel; 9. Microwave heating chamber; 10. Microwave device; 11. Gas phase outlet; 12. Particle collection tank; 13. Touch screen display; 14. Ultrasonic switch; 15. Microwave switch. SPECIFIC EMBODIMENTS

[0025] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0026] On the one hand, referring to the attached Figure 1-2 , the present invention discloses a device for ultrasonic and microwave collaborative preparation of micro-nano cerium oxide, including:

[0027] A housing, the housing includes an independent ultrasonic atomization chamber 5 and a microwave heating chamber 9. A feeding device is provided at the top of the housing, and the feeding device is in communication with the ultrasonic atomization chamber 5. An ultrasonic switch 14 and a microwave switch 15 are provided on the side wall of the housing. The ultrasonic switch 14 is electrically connected to the ultrasonic device in the ultrasonic atomization chamber 5, and the microwave switch 15 is electrically connected to the microwave device 10 on the side wall of the microwave heating chamber 9; the ultrasonic switch 14 is used to control the start and stop of the ultrasonic device, and the microwave switch 15 is used to control the start and stop of the microwave device 10. Preferably, the ultrasonic device includes an ultrasonic generator and an ultrasonic transducer. Ultrasonic atomization uses the directional pressure of ultrasonic waves to make the liquid surface bulge, resulting in cavitation in the surrounding liquid surface, atomizing the liquid into small molecule aerosols. Compared with heating atomization, it saves about 90% of energy and has higher economy. Preferably, the microwave device 10 includes a waveguide and a magnetron. The microwave and the magnetron are arranged on the side of the microwave heating chamber 9 body. Preferably, the power of the magnetron is between 0.5 and 1.5 kW, and the microwave frequency is 300 MHz to 300 GHz, corresponding to electromagnetic waves with wavelengths from 1 m to 1 mm. When using microwave to heat cerium chloride solution, there are a large number of water molecules which are polar molecules in the aqueous solution, and there are also a large number of charged ions including chloride ions and cerium ions in the solution. Under the action of microwave, the polar molecules and charged particles will repeatedly turn with the change of the electric field direction, move violently and collide with each other to generate friction, thus generating a large amount of heat. Microwave heating of cerium chloride solution has high efficiency, is easy to control, and is more environmentally friendly.

[0028] A heating channel 8, the heating channel 8 penetrates through the microwave heating chamber 9. The inlet of the heating channel 8 is arranged in the ultrasonic atomization chamber 5, and the outlet of the heating channel 8 is in communication with the particle collection tank 12; the heating channel 8 is made of glass material to facilitate microwave heating of cerium chloride solution. The outlet of the heating channel 8 preferably opens downward, and the particle collection tank 12 preferably adopts a cylindrical structure to facilitate the collection of the solid reaction products falling freely.

[0029] A shrapnel 7, the shrapnel 7 is arranged in the ultrasonic atomization chamber 5, and the shrapnel 7 is inclined below the feeding device to bounce the feed into the heating channel 8; the shrapnel 7 vibrates with the vibration of the ultrasonic wave, so as to disperse the cerium chloride solution while bouncing the cerium chloride solution into the heating channel 8, forming a natural and floating water mist flow.

[0030] In this embodiment, preferably, the equipment for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a touch screen display 13. The touch screen display 13 is arranged on the side wall of the housing. Both the ultrasonic device and the microwave device 10 are electrically connected to the touch screen display 13, and the power of the ultrasonic device and the microwave device 10 is controlled through the touch screen display 13, so as to make the preparation of cerium oxide solid reach the best efficiency.

[0031] In this embodiment, preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a gas phase channel 4. The gas phase channel 4 is arranged on the housing. The outlet of the gas phase channel 4 is communicated with the ultrasonic atomization chamber 5, and the outlet of the gas phase channel 4 faces the inlet of the heating channel 8. Preferably, the center of the heating channel 8 coincides with the center of the gas phase channel 4. Preferably, the diameter of the heating channel 8 is at least twice the diameter of the gas phase channel 4, and the gas phase channel 4 and the heating channel 8 are coaxially arranged. The inlet of the gas phase channel 4 is preferably provided with a blower or an oxygen cylinder to pump air or pure oxygen into the gas phase channel 4, so as to provide oxygen for the chemical reaction. At the same time, the pumped air or pure oxygen can also blow the cerium chloride droplets scattered by the elastic sheet 7 into the heating channel 8.

[0032] In this embodiment, preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a handle 1 and a universal ball 6. The universal ball 6 is rotatably connected to the housing. One end of the universal ball 6 is fixedly connected to the handle 1, and the other end of the universal ball 6 is connected to the elastic sheet 7 to adjust the inclination angle of the elastic sheet 7. Preferably, the inclination angle of the elastic sheet 7 is 30°-60°. By fixing the handle 1, the universal ball 6 and the elastic sheet 7 are fixed. Preferably, the universal ball 6 is embedded in the inner wall of the ultrasonic atomization chamber 5. By pressing down or lifting the handle 1, the angle of the elastic sheet 7 swings. The inclination angle of the elastic sheet 7 is determined according to the ultrasonic vibration frequency, so that the dripping cerium chloride solution can accurately enter the heating channel 8.

[0033] In this embodiment, preferably, the device for co-preparing micro-nano cerium oxide by ultrasonic and microwave also includes a gas phase outlet 11. The gas phase outlet 11 is arranged above the outlet of the heating channel 8. After the chemical reaction is completed, certain gas impurities will be formed. Preferably, the gas phase outlet 11 is communicated with an exhaust gas collection tank. The gas impurities are collected by the exhaust gas collection tank to prevent air pollution and facilitate the treatment of gas impurities in the later stage.

[0034] In this embodiment, preferably, the feeding device includes a hopper 2 and a dropper 3. The hopper 2 and the dropper 3 are communicated. The dropper 3 is arranged directly above the elastic sheet 7. Preferably, the diameter of the dropper 3 is less than 1 mm to control the falling rate of the cerium chloride solution and prevent the adjacent droplets from colliding due to too fast dripping, which affects the effect of entering the heating channel 8.

[0035] In this embodiment, preferably, a partition is arranged between the ultrasonic atomization chamber 5 and the microwave heating chamber 9. A vibration damping layer is arranged on the side of the partition close to the ultrasonic atomization chamber 5, and a heat insulation layer is arranged on the side of the partition close to the microwave heating chamber 9. Through the arrangement of the vibration damping layer and the heat insulation layer, the mutual influence between the ultrasonic atomization chamber 5 and the microwave heating chamber 9 is weakened, and the partition is also beneficial to the installation and fixation of the heating channel 8.

[0036] On the other hand, the present invention provides a method for preparing micro-nano cerium oxide in a coordinated manner using ultrasound and microwaves, including the above-mentioned device for preparing micro-nano cerium oxide in a coordinated manner using ultrasound and microwaves. The preparation method specifically comprises:

[0037] S10: Turn on the ultrasonic switch 14 and the microwave switch 15, check the vibration frequency of the shrapnel 7 and the temperature of the microwave heating cavity 9; press down or lift the handle 1 to achieve the angular swing of the shrapnel 7, adjust the shrapnel 7 to the calculated inclination angle and then fix the handle 1, thereby fixing the shrapnel 7 so that the droplets can bounce into the heating channel 8. After the ultrasonic switch 14 is turned on, the universal ball 6 embedded in the inner wall of the ultrasonic atomization cavity 5 drives the shrapnel 7 to start ultrasonic vibration along with the ultrasonic vibration cavity, and the microwave heating cavity 9 and the heating channel 8 are preheated to the specified temperature.

[0038] S20: After the vibration frequency of the shrapnel 7 and the temperature of the microwave heating cavity 9 are confirmed to meet the preset requirements, the cerium chloride solution is poured into the feeding device; the hopper 2 stores the solution, and the stored solution slowly enters the dropper 3.

[0039] S30: Droplets of cerium chloride solution fall onto the shrapnel 7, forming a water mist flow that bounces into the heating channel 8, and then air or pure oxygen is introduced into the heating channel 8; the dropper 3 is placed directly above the shrapnel 7, and the cerium chloride solution drips drop by drop onto the shrapnel 7, and under the ultrasonic vibration and elastic action of the shrapnel 7, it turns into a naturally flowing water mist flow that enters the heating channel 8, and air or pure oxygen is introduced into the heating channel 8 through the gas phase channel 4. The air or pure oxygen pumped into the gas phase channel 4 simultaneously drives the water mist flow toward the heating channel 8, and the cerium chloride water mist flow and oxygen react chemically in the heating channel 8 to form gaseous impurities and solid cerium oxide particles.

[0040] S40: The solid reaction product is collected through the particle collection tank 12, and the ultrasonic switch 14 and the microwave switch 15 are turned off after the reaction is complete; the solid cerium oxide particles fall into the particle collection tank 12 under the action of their own gravity to complete the collection, and the gas impurities formed by the chemical reaction are moved to the bottom of the heating channel 8 and discharged through the gas phase outlet 11 under the blowing of air or pure oxygen introduced into the gas phase channel 4. After the reaction is completed, the ultrasonic and microwave switches are turned off to complete the preparation.

[0041] The present invention realizes the dynamic and continuous operation of atomization and pyrolysis reaction with variable ultrasonic amplitude and variable microwave power by coordinating ultrasound and microwave, so that the reaction solution is fully atomized and evenly heated, and ultrafine cerium oxide powder with good dispersibility, small and uniform particle size is easily prepared.

[0042] The foregoing description of the disclosed embodiments enables those skilled in the art to practice or use the present invention. Various modifications to the embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An apparatus for preparing micro-nano cerium oxide by ultrasonic-microwave synergism, characterized in that, Comprising: A housing, the housing includes an independent ultrasonic atomization chamber and a microwave heating chamber, a feeding device is provided at the top of the housing, the feeding device is communicated with the ultrasonic atomization chamber, an ultrasonic switch and a microwave switch are provided on the side wall of the housing, the ultrasonic switch is electrically connected to an ultrasonic device in the ultrasonic atomization chamber, and the microwave switch is electrically connected to a microwave device on the side wall of the microwave heating chamber; A heating channel, the heating channel penetrates through the microwave heating chamber, an inlet of the heating channel is arranged in the ultrasonic atomization chamber, and an outlet of the heating channel is communicated with a particle collection tank; A shrapnel, the shrapnel is arranged in the ultrasonic atomization chamber, and the shrapnel is obliquely arranged below the feeding device to bounce the feed into the heating channel; It further includes a gas phase channel, the gas phase channel is arranged on the housing, an outlet of the gas phase channel is communicated with the ultrasonic atomization chamber, and the outlet of the gas phase channel faces the inlet of the heating channel; It further includes a handle and a universal ball, the universal ball is rotationally connected to the housing, one end of the universal ball is fixedly connected to the handle, and the other end of the universal ball is connected to the shrapnel to adjust the inclination angle of the shrapnel; It further includes a gas phase outlet, the gas phase outlet is arranged above the outlet of the heating channel; the feeding device includes a hopper and a dropper, the hopper is communicated with the dropper, and the dropper is arranged directly above the shrapnel; A partition is arranged between the ultrasonic atomization chamber and the microwave heating chamber, a vibration damping layer is arranged on one side of the partition close to the ultrasonic atomization chamber, and a heat insulation layer is arranged on one side of the partition close to the microwave heating chamber.

2. The device for preparing micro-nano cerium oxide by ultrasonic-microwave synergism according to claim 1, characterized in that, It further includes a touch screen display, the touch screen display is arranged on the side wall of the housing, and both the ultrasonic device and the microwave device are electrically connected to the touch screen display.

3. A method for preparing micro-nano cerium oxide by ultrasonic and microwave synergistically, characterized in that: Comprising an apparatus for co-preparing micro-nano cerium oxide by ultrasonic and microwave as described in any one of claims 1-2, the preparation method specifically includes: S10: Turn on the ultrasonic switch and the microwave switch, and check the vibration frequency of the shrapnel and the temperature of the microwave heating chamber; S20: After the vibration frequency of the shrapnel and the temperature of the microwave heating chamber are confirmed to meet the preset requirements, pour the cerium chloride solution into the feeding device; S30: The droplets of the cerium chloride solution fall on the shrapnel, form a water mist flow and bounce into the heating channel, and then introduce air or pure oxygen into the heating channel; S40: Collect the reaction solid product through the particle collection tank, and turn off the ultrasonic switch and the microwave switch after the reaction is complete.

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