Atomization pyrolytic reaction device for preparing nano material

Abstract

The utility model belongs to the field of nanometer material preparation, and particularly discloses an atomization pyrolytic reaction device for preparing nanometer materials, which comprises an atomization device, a pyrolytic reaction device, a pyrolytic reaction device and a pyrolytic reaction device, the nanometer material reaction solution is atomized in the atomization reaction bin to form aerosol; the Joule thermal micro-channel reaction device comprises a Joule thermal micro-channel reaction tube, a Joule thermoelectric controller and a powder collecting device, the diameter of the Joule thermal micro-channel reaction tube is 100-500 microns, and aerosol enters the Joule thermal micro-channel reaction tube through carrier gas; the Joule thermoelectric controller is used for heating aerosol in the Joule thermal micro-channel reaction tube to obtain a nano-powder material, and the nano-powder material enters a powder collecting device under the driving of carrier gas. The reaction device is high in heating efficiency, good in control effect and capable of rapidly obtaining uniform nanometer materials.

Description

TECHNICAL FIELD

[0001] The utility model belongs to nanometer material preparation field especially relates to a preparation nanometer material's atomization pyrolysis reaction device. BACKGROUND

[0002] Nanomaterials have been widely used in a large number of important fields, such as energy storage, catalysis, and biomedical engineering. Compared with bulk materials, nanomaterials exhibit unique and superior performance. Rapid and scalable preparation of nanomaterials is crucial for realizing a wide range of applications, but there are still challenges.

[0003] Atomization pyrolysis is a technology that atomizes nanomaterial reaction solution into tiny droplets and performs thermal decomposition reaction under high temperature conditions to prepare ultrafine powders, nanomaterials, or functional coatings. Its core is the combination of chemical synthesis and physical atomization, commonly used in material science, chemical industry, and energy fields. In particular, the preparation of battery cathode materials, catalysts, and other materials based on atomization pyrolysis strategy can obtain high-purity, uniform materials suitable for high-performance application scenarios.

[0004] However, current atomization pyrolysis technology usually relies on a tube furnace as a heating element, which can usually only reach a lower temperature range (usually <1500K), resulting in limited product types, and the furnace cavity is relatively large, leading to uneven heating, low heating efficiency, and difficulty in controlling product quality. For example, Chinese Patent No. CN115889760B discloses a device for rapidly preparing carbon nanotube-coated ultrafine high-entropy alloy composite powder, wherein the gas atomization device is an atomic absorption atomizer, the left side of the atomic absorption atomizer is provided with a pipeline connected with the nanomaterial reaction solution, the lower side is provided with a pipeline through which Ar gas passes, and the right side is provided with a gas atomization nozzle connected with the inlet of a high-temperature device. The high-temperature device is a vacuum tube furnace, the right side of which is connected with the inlet of a collection device; the collection device is composed of a container containing filter paper, wherein the filter paper is located at the outlet of the collection device for intercepting the products in the gas flow to achieve the collection effect.

[0005] Therefore, how to achieve uniform and rapid nanomaterial preparation is a problem that needs to be solved in the field. UTILITY MODEL CONTENT

[0006] The technical problem to be solved by the utility model is to overcome the deficiencies and defects mentioned in the above background technology, and to provide an atomization pyrolysis reaction device that can efficiently obtain uniform nanomaterials.

[0007] To solve the above technical problems, the technical solution provided by the utility model is: an atomization pyrolysis reaction device for preparing nanomaterials, comprising:

[0008] The atomization device comprises an atomization reaction bin, an atomizer and a gas feeding device, the atomization reaction bin is used for containing a nano material reaction solution, the atomizer is used for atomizing the nano material reaction solution, and the gas feeding device is communicated with the atomization reaction bin through a gas feeding pipeline to provide carrier gas, and the nano material reaction solution is atomized in the atomization reaction bin to form an aerosol.

[0009] The Joule heat micro-channel reaction device comprises a Joule heat micro-channel reaction tube, a Joule heat electric controller and a powder collecting device, one end of the Joule heat micro-channel reaction tube is communicated with the atomization reaction bin, and the other end is communicated with the powder collecting device; the diameter of the Joule heat micro-channel reaction tube is 100-500 μm, the aerosol enters the Joule heat micro-channel reaction tube through the carrier gas, the Joule heat electric controller heats the aerosol in the Joule heat micro-channel reaction tube to obtain a nano powder material, and the nano powder material enters the powder collecting device under the driving of the carrier gas.

[0010] In an embodiment, the atomizer is an ultrasonic atomization sheet, and the ultrasonic atomization sheet is arranged at the bottom of the atomization reaction bin.

[0011] In an embodiment, the atomization device further comprises a circulating water cooling system, the atomization reaction bin is arranged in the circulating water cooling system, and the circulating water cooling system is used for adjusting the temperature in the atomization reaction bin.

[0012] In an embodiment, the gas feeding device further comprises a flow meter, the flow meter is arranged on the gas feeding pipeline to monitor the gas feeding amount, and the gas feeding pipeline is in plurality to convey different carrier gases.

[0013] In an embodiment, the atomization device further comprises a reaction solution supply device connected with the atomization reaction bin, the reaction solution supply device comprises a peristaltic pump, a liquid storage tank and a magnetic stirrer, the magnetic stirrer is arranged in the liquid storage tank to stir the nano material reaction solution in the liquid storage tank, and the peristaltic pump is arranged between the liquid storage tank and the atomization reaction bin to convey the nano material reaction solution to the atomization reaction bin.

[0014] In an embodiment, the Joule heat micro-channel reaction tube comprises a transition section connected with the atomization reaction bin and a reaction section arranged at the tail end of the transition section, the reaction section is arranged along a horizontal direction, and the Joule heat electric controller is connected with the reaction section to provide an electric current to the reaction section to make the reaction section self-heating.

[0015] In an embodiment, the transition section comprises a first transition section and a second transition section, the first transition section is arranged at the top of the atomization reaction bin and extends along a vertical direction, and the second transition section is connected with the first transition section and extends along a horizontal direction, and the transition section is fixed on a workbench through a support.

[0016] In an embodiment, the Joule heat micro-channel reaction device further comprises a control system, the control system comprising a controller and a control panel, the controller being connected with the Joule heat micro-channel reaction tube and the control panel, and the controller being used for receiving and controlling the operating parameters of the Joule heat micro-channel reaction tube.

[0017] In an embodiment, a tail gas treatment device is further included, which is connected at the tail end of the powder collecting device, and the tail gas treatment device comprises a waste liquid tank and a tail gas treatment liquid contained in the waste liquid tank.

[0018] In an embodiment, the powder collecting device is an electrostatic powder collecting tank, which is used for collecting the nano powder by electrostatic force.

[0019] Compared with the prior art, the beneficial effects of the present application are as follows: in the prior art, the conventional atomization pyrolysis method uses a conventional tube furnace as a heating element, which can only reach a low temperature range (generally below 1500K), and the relatively large furnace cavity leads to uneven heating, resulting in low heating efficiency and uneven product quality. The atomization pyrolysis reaction device for preparing nano materials provided by the present application can uniformly atomize the reaction solution of the nano material reaction by the ultrasonic atomizer, and can bring the reaction solution into the Joule heat micro-channel reaction tube for pyrolysis, so that the heating is more uniform, the pyrolysis temperature range is wider, and the product size is smaller. The size of the nano material particles synthesized by the atomization pyrolysis reaction device of the present application can be adjusted by relevant parameters (such as temperature, precursor concentration, flow rate, atomization frequency, etc.). The atomization pyrolysis reaction device of the present application has high heating capacity and uniform heating effect, and can obtain nano materials with very strict process requirements, such as high-entropy alloy (HEA) and high-entropy oxide (HEO) nano materials. BRIEF DESCRIPTION OF DRAWINGS

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the embodiments or the prior art description will be briefly introduced as follows. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0021] Figure 1 is a structural schematic view of the atomization pyrolysis reaction device for preparing nano materials in an embodiment.

[0022] 100: atomization pyrolysis reaction device for preparing nanomaterial; 10: gas feeding device; 20: atomization device; 21: atomization reaction bin; 22: circulating water cooling system; 23: atomizer; 30: reaction solution supply device; 40: joule heat micro-channel reaction device; 41: joule heat micro-channel reaction tube; 42: joule heat controller; 411: reaction section; 412: transition section; 50: powder collecting device; 60: tail gas treatment device. DETAILED DESCRIPTION

[0023] For the convenience of understanding the present application, the present application will be described more fully below with reference to the accompanying drawings and preferred embodiments. However, the scope of the present application is not limited to the following specific embodiments.

[0024] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of the present application.

[0025] Unless otherwise specifically mentioned, various raw materials, reagents, instruments and equipment used in the present application can be purchased from the market or can be prepared by existing methods.

[0026] As Figure 1As shown, the utility model embodiment provides a preparation nanometer material's atomization pyrolysis reaction device 100, including the atomization device 20 and joule heat microchannel reaction device 40 of intercommunication. Atomization device 20 will nanometer reaction solution even atomization, bring to joule heat microchannel reaction device 40, can realize heated more evenly, pyrolysis temperature range is wider, the effect of product size is smaller. Specifically, atomization device 20 includes atomization reaction bin 21, atomizer 23 and gas supply device 10, more specifically, still including circulating water cooling system 22 and reaction solution supply device 30. Atomization reaction bin 21 is used to hold nanometer material reaction solution, atomizer 23 is used to atomize nanometer material reaction solution, gas supply device 10 is communicated with atomization reaction bin 21 through gas supply pipeline to provide carrier gas, and nanometer material reaction solution forms aerosol after being atomized in atomization reaction bin 21. Joule heat microchannel reaction device 40 includes joule heat microchannel reaction tube 41, joule heat electric controller 42 and powder collecting device 50, and more specifically, still including tail gas collecting device 60. Joule heat microchannel reaction tube one end is communicated with atomization reaction bin, and the other end is communicated with powder collecting device;The diameter of joule heat microchannel reaction tube 41 is 100 μm-500 μm, and preferably 200-400 μm. Adopt micron level diameter, and the diameter is very small, and heating section is prepared from carbon material, and rapidly generates heat by joule heat electric controller 42. When using, aerosol enters joule heat microchannel reaction tube 41 through carrier gas, and nanometer powder material is obtained after joule heat electric controller 42 heats aerosol in joule heat microchannel reaction tube 41, and nanometer powder material is driven by carrier gas and enters powder collecting device 50, and tail gas treatment device 60 handles carrier gas and tail gas generated during reaction process.

[0027] In the above-mentioned atomization pyrolysis reaction device 100 for preparing nanomaterials, the nanomaterial reaction solution is atomized in the atomization device 20 to obtain aerosol, which is transported to the joule heat micro-channel reaction tube 41 by a carrier gas. The diameter of the joule heat micro-channel reaction tube 41 is 100-500 μm, preferably 200-300 μm, which is about 100 times smaller than the size of a conventional tube furnace chamber. Such a compact size can achieve more uniform heating and significantly reduce the residence time. The residence time during the heating process of the atomization pyrolysis reaction device 100 of the present application is only a few tens of milliseconds. The joule heat micro-channel reaction tube 41 is controlled by the joule heat electric controller 42, which provides electric joule heating by applying appropriate current and voltage, and can efficiently achieve a temperature > 2000 K (conversion rate from input power to radiation > 90%). Therefore, the size of the nanomaterial particles synthesized by the atomization pyrolysis reaction device 100 of the present application can be adjusted by controlling relevant parameters (such as temperature, precursor concentration, flow rate, atomization frequency, etc.). The atomization pyrolysis reaction device 100 of the present application has high and uniform heating capacity, and can obtain nanomaterials that are very demanding for the process, such as high-entropy alloy (HEA) and high-entropy oxide (HEO) nanomaterials.

[0028] Specifically, in an embodiment, the atomization pyrolysis reaction device 100 for preparing nanomaterials comprises a gas feeding device 10, an atomization device 20, a reaction solution supply device 30, a joule heat micro-channel reaction device 40, a collection module 50 and a tail gas treatment device 60. More specifically, the atomization device 20 comprises an atomization reaction chamber 21, a circulating water cooling system 22 and an atomizer 23.

[0029] Specifically, in an embodiment, the atomization reaction chamber 21 is used to place the nanomaterial reaction solution to be treated, such as a graphene oxide solution. The atomization reaction chamber 21 can be made of transparent acrylic material, which facilitates real-time observation of the atomization state, or made of corrosion-resistant polytetrafluoroethylene material, which is suitable for various harsh condition samples. The atomization reaction chamber 21 is placed inside the circulating water cooling system 22, which can effectively maintain the temperature of the entire atomization device 20 through water bath during the working process.

[0030] Specifically, in an embodiment, the atomizer 23 is an ultrasonic atomization sheet. By replacing ultrasonic atomization sheets with different frequencies and powers, the size and amount of atomized droplets can be adjusted to meet the adjustment of more reaction conditions and to be suitable for different scale production. At the same time, the ultrasonic atomization sheet is partially placed in the circulating water cooling system 22 and separated from the nanomaterial reaction solution, which can prevent contamination and avoid the problem of dry burning without nanomaterial reaction solution.

[0031] Specifically, in an embodiment, the reaction solution supply device 30 continuously supplies the reaction nanomaterial reaction solution to the atomization reaction chamber 21, so that long-term continuous production can be achieved.

[0032] The gas feeding device 10 supplies the carrier gas to the atomization reaction chamber 21, and brings the atomized mist in the atomization reaction chamber 21 into the Joule heat micro-channel reaction tube 41. Preferably, the gas feeding device 10 includes a gas feeding device and a flow meter, the gas feeding device 10 is in communication with the atomization reaction chamber 21 through a gas feeding pipeline for feeding the carrier gas into the atomization reaction chamber 21, and the flow meter is arranged on the gas feeding pipeline for detecting and controlling the amount of the carrier gas. More preferably, the gas feeding device 10 includes a plurality of gas inlet channels through which a plurality of different carrier gases can be fed and mixed.

[0033] The reaction solution supply device 30 includes a peristaltic pump, a storage tank and a magnetic stirrer (not shown in the figure). The magnetic stirrer is arranged in the storage tank for stirring the nanomaterial reaction solution in the storage tank, and the peristaltic pump is arranged between the storage tank and the atomization reaction chamber for feeding the nanomaterial reaction solution to the atomization reaction chamber. The nanomaterial reaction solution is stored in the storage tank with the magnetic stirrer to ensure the uniformity of the solution during storage, and the peristaltic pump is used to supplement the reaction nanomaterial reaction solution to the atomization reaction chamber 21 to achieve long-term continuous flow synthesis.

[0034] The Joule heat micro-channel reaction device 40 includes a Joule heat micro-channel reaction tube 41 and a Joule heat controller 42. The aerosol passing through the Joule heat micro-channel reaction tube 41 is driven by the carrier gas into the powder collecting device 50, which is an electrostatic powder collecting tank for collecting the nanometer powder by electrostatic force. The tail gas treatment device 60 treats the carrier gas and the tail gas generated during the reaction, which specifically includes a waste liquid tank and a tail gas treatment liquid contained in the waste liquid tank. The treatment liquid can be dilute acid, such as 5% H2SO4. More specifically, the Joule heat micro-channel reaction tube 41 includes a transition section 412 connected with the atomization reaction chamber 21 and a reaction section 411 arranged at the tail end of the transition section 412. The reaction section 411 is arranged along the horizontal direction, and the Joule heat controller 42 is connected with the reaction section 42 for providing current to the reaction section 411 to heat the reaction section 411. Specifically, the transition section 412 is made of quartz, and the reaction section 411 is made of carbon. The transition section 412 includes a first transition section and a second transition section. The first transition section is arranged at the top of the atomization reaction chamber and extends along the vertical direction, and the second transition section is connected with the first transition section and has the same diameter as the first transition section, and extends along the horizontal direction, so as to better control the temperature. The transition section is fixed on the workbench by a support, and the structure is more stable.

[0035] The Joule heat micro-channel reaction device 40 further comprises a control system, which comprises a controller and a control panel, the controller being connected with the Joule heat micro-channel reaction tube 41 and the control panel, and being used for receiving and controlling the operating parameters (including heating temperature, temperature rising rate, etc.) of the Joule heat micro-channel reaction tube 41, so as to realize more accurate control of current and voltage and real-time and accurate control.

[0036] Preferably, in an embodiment, the powder collecting device 50 is made of filter paper or foamed nickel, is connected at the end of the reaction section 411, and has a larger cross-sectional area than the reaction section 411, so that the powder collecting device 50 can accommodate more samples. Meanwhile, the powder collecting device 50 can also be matched with a heating and insulation device, and the commonly used temperature is 90 o C prevents the solvent water vapor from condensing into liquid to block the powder collecting device 50.

[0037] The above-mentioned atomization pyrolysis reaction device 100 for preparing nanomaterials is used for product preparation and processing, and the reaction section 411 of the Joule heat micro-channel reaction device 40 is first heated to a set temperature by the control system 42; then the reaction solution supply device 30 is started to provide the nanomaterial reaction solution to the atomization reaction chamber 21, the atomization piece 23 is started to start atomization, and the gas supply device 10 is started, so that the atomized aerosol enters the constant-temperature Joule heat micro-channel reaction tube 41 for pyrolysis treatment under the action of the carrier gas, then the treated nanometer powder is collected in the nanometer powder collector 50, and the tail gas enters the tail gas treatment device 60 for treatment. Finally, the reaction solution supply device 30, the atomization piece 23 and the gas supply device 10 are stopped, the Joule heat micro-channel reaction device 40 is stopped heating by the control system 42, the nanometer powder collector 50 is removed, the sample is collected, and the product preparation is completed.

[0038] The tail gas treatment device 60 comprises a waste liquid tank and a tail gas treatment liquid contained in the waste liquid tank, collects the reaction generated tail gas and carrier gas, and removes a small amount of uncollected nanometer powder and generated tail gas by the tail gas treatment device 60.

Claims

1. An atomization pyrolysis reaction apparatus for preparing nanomaterials, characterized by, The application relates to a nano-powder preparation device. The device comprises an atomization device, a Joule heat micro-channel reaction device and a tail gas treatment device. The atomization device comprises an atomization reaction tank, an atomizer and a gas feeding device.

2. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The atomization reaction tank is used for containing a nano-material reaction solution.

3. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein the apparatus is characterized by, The atomizer is used for atomizing the nano-material reaction solution.

4. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The gas feeding device is communicated with the atomization reaction tank through a gas feeding pipeline to provide carrier gas.

5. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The atomization reaction tank is communicated with the Joule heat micro-channel reaction tube at one end and communicated with a powder collecting device at the other end.

6. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The Joule heat micro-channel reaction tube has a diameter of 100-500 mu m.

7. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 6, wherein the apparatus is characterized by, The carrier gas enters the Joule heat micro-channel reaction tube to form an aerosol.

8. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The Joule heat micro-channel reaction tube is heated by the Joule heat electric controller to obtain nano-powder material.

9. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The nano-powder material is driven by the carrier gas to enter the powder collecting device.

10. The apparatus for producing nanomaterials by spray pyrolysis reaction according to claim 1, wherein, The atomizer is an ultrasonic atomization sheet arranged at the bottom of the atomization reaction tank. The atomization device further comprises a circulating water cooling system. The atomization reaction tank is arranged in the circulating water cooling system. The circulating water cooling system is used for adjusting the temperature in the atomization reaction tank. The gas feeding device further comprises a flow meter arranged on the gas feeding pipeline to monitor the gas feeding amount. The gas feeding pipeline is provided with a plurality of gas feeding pipelines to feed different carrier gas. The device further comprises a reaction solution supply device connected with the atomization reaction tank. The reaction solution supply device comprises a peristaltic pump, a liquid storage tank and a magnetic stirrer. The magnetic stirrer is arranged in the liquid storage tank to stir the nano-material reaction solution in the liquid storage tank. The peristaltic pump is arranged between the liquid storage tank and the atomization reaction tank to feed the nano-material reaction solution to the atomization reaction tank. The Joule heat micro-channel reaction tube comprises a transition section connected with the atomization reaction tank and a reaction section arranged at the tail end of the transition section. The reaction section is arranged along the horizontal direction. The Joule heat electric controller is connected with the reaction section to provide current to the reaction section to make the reaction section self-heating. The transition section comprises a first transition section arranged at the top of the atomization reaction tank and extending along the vertical direction. The second transition section is connected with the first transition section and extends along the horizontal direction. The transition section is fixed on a workbench through a support. The Joule heat micro-channel reaction device further comprises a control system. The control system comprises a controller and a control panel. The controller is connected with the Joule heat micro-channel reaction tube and the control panel. The controller is used for receiving and controlling the operation parameters of the Joule heat micro-channel reaction tube. The tail gas treatment device is connected at the tail end of the powder collecting device. The tail gas treatment device comprises a waste liquid tank and tail gas treatment liquid contained in the waste liquid tank. The powder collecting device is an electrostatic powder collecting tank. The nano-powder is collected by electrostatic force.

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