CN112107873B - Vertical device and method for preparing superfine powder through spray pyrolysis - Google Patents
Vertical device and method for preparing superfine powder through spray pyrolysis Download PDFInfo
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Abstract
The invention discloses a device and a method for preparing ultrafine powder by vertical spray pyrolysis, wherein the method comprises the following steps: preparing a precursor solution of metal salt; step (b): atomizing the precursor solution into aerosol droplets, and performing microwave irradiation heating to break the aerosol droplets into superfine aerosol droplets; a step (c): the aerosol liquid drops are treated by a vertical tube furnace connected with the lower part to obtain monodisperse aerosol particles, and the monodisperse aerosol particles are mixed with cooling gas 10 at the outlet of the vertical tube furnace and then collected by a filter to obtain monodisperse metal simple substances, alloys or metal oxide ultrafine particles; a step (d): a fan is arranged at the filter to control the flow and the pressure difference; and (c) circularly using the tail gas in the step (c) after environmental protection treatment, cooling, compression and dehydration. The invention reduces the deposition of aerosol liquid drops or powder on equipment and the waste of raw materials, reduces the equipment maintenance frequency, improves the product yield, reduces the explosion risk and improves the safety coefficient.
Description
Technical Field
The invention relates to the field of superfine powder preparation, in particular to a vertical device and a method for preparing superfine powder by spray pyrolysis.
Background
Monodisperse particles refer to a group of particles that are uniform in shape and composition and have a very narrow particle size distribution. The highly monodisperse ultrafine particles have uniform appearance, uniform size and uniform crystal form, and are the premise for developing the basic research and application research of nano materials. The overall performance of the monodisperse particles tends to be consistent, thereby providing convenience for people to research the material performance and having wide application in aspects such as instrument parameter calibration, colloid theory verification and the like. Monodisperse nanoparticles have excellent properties, and currently, the monodisperse nanoparticles have become high-efficiency catalysts for many chemical reactions, such as water decomposition, petroleum cracking, etc., and RuO is dispersed as a catalyst on monodisperse particles of CdS, and water can be decomposed into hydrogen and oxygen by light irradiation, thus making possible application to the manufacture of solar cells. The monodisperse ultrafine particles have great application potential in microscopic researches such as photonic crystals, nano devices, drug loading, gas transmission, separation, catalysis and the like. Various nanostructured materials can be prepared from monodisperse ultra-fine particles by self-assembly techniques.
In the superfine powder preparation process in the prior art, a transverse production line is adopted, namely a tube furnace is parallel to the ground, and the structure has inevitable technical defects, one is that aerosol can be settled in a pipeline due to the action of gravity, so that raw materials are wasted, and the cleaning frequency and the cleaning difficulty of equipment are increased; secondly, if the liquid drops gathered after the aerosol is settled are not timely exploded by the microwave, the liquid drops can flow into the high-temperature dry horizontal tube furnace, and the risk of explosion is caused.
Disclosure of Invention
The invention aims to provide a device and a method for preparing ultrafine powder by vertical spray pyrolysis.
In order to achieve the purpose, the invention adopts the technical scheme that: a vertical device for preparing superfine powder by spray pyrolysis comprises an atomization device, an atomization drying tower and a vertical tube furnace; the atomization device is arranged at the top of the atomization drying tower; the outlet end at the bottom of the atomization drying tower is connected with the inlet end at the top of the vertical tube furnace; the inner wall of the atomization drying tower is provided with not less than 1 microwave magnetron or not less than 1 waveguide tube introduction port; the waveguide tube introduction port is connected with a microwave generator outside the atomization drying tower through a waveguide tube; the outlet end of the vertical tube furnace is sequentially connected with a filter, a tail gas purification device and the inlet end of a tail gas circulating pipeline; a fan is arranged at the inlet end or the outlet end of the filter; the filter is also connected with a product outlet; the outlet end of the tail gas circulating pipeline is connected with a carrier gas pipeline; the tail gas circulating pipeline is also connected with a waste liquid outlet.
The invention also provides a method for preparing the ultrafine powder by vertical spray pyrolysis, which comprises the following steps:
a step (a): dissolving metal salt in a polar solvent to prepare a precursor solution; the metal salt is selected from at least one of nitrate, halogenated salt, hypochlorite, acetate, oxalate or sulfate;
step (b): preparing the precursor solution prepared in the step (a) into aerosol liquid drops through an atomizing device; introducing the aerosol droplets into an atomization drying tower through hot carrier gas at 50-300 ℃, heating through microwave irradiation of a microwave magnetron or a microwave generator, and expanding and crushing the atomized droplets into micron, submicron or nano aerosol droplets;
step (c): the micron, submicron or nano aerosol droplets obtained in the step (b) fall into a vertical tubular furnace which is tightly connected below an atomization drying tower under the action of gravity and carrier gas, are treated at 300-1000 ℃ to obtain monodisperse aerosol particles, are mixed with a large amount of cooling gas at the outlet of the vertical tubular furnace, are rapidly cooled to reduce the original temperature of 300-1000 ℃ to 30-60 ℃, and are collected by a filter to obtain monodisperse metal simple substance, alloy or metal oxide ultrafine particles with the particle size of 10 nm-5 microns; the filter is a ceramic filter or a polymer membrane filter; the cooling gas is air, nitrogen, a mixed gas of hydrogen and nitrogen or a mixed gas of hydrogen and air; the hydrogen volume concentration is <5%;
step (d): controlling flow and filter pressure difference through a fan to perform membrane interception; selectively catalytically reducing nitrogen oxides in the hot tail gas obtained in the step (c) into harmless nitrogen and water through a catalyst and discharging; or absorbing carbon dioxide, oxysulfide, acetic acid, hydrogen chloride and hydrogen sulfide acid gas by alkali liquor, cooling and compressing by a tail gas purification device, removing water, and recycling by a tail gas circulation pipeline.
Further, the total power of the microwave magnetrons in the step (b) is 30W-600kW, the power of each microwave magnetron is equal or unequal, and the spatial arrangement of the microwave magnetrons ensures that the microwave field in the atomizing dryer is uniform.
Further, the inclination angle between the vertical tube furnace and the ground is 60-90 degrees.
Further, the carrier gas is air, nitrogen, a mixed gas of hydrogen and nitrogen, or a mixed gas of hydrogen and air, wherein the volume concentration of hydrogen is less than 5%.
Furthermore, the atomization mode of the atomization device is high-speed centrifugal spray atomization, ultrasonic atomization or high-pressure airflow atomization.
Further, the size of the liquid drop formed after atomization is 500nm-500 μm; the size of the liquid drop formed after microwave crushing is 20nm-50 μm.
Further, the metal salt is at least one of nitrate, halide, hypochlorite, acetate, oxalate or sulfate of Ag, au, cu, pt, pd, fe, co, ni, ti, sn, sb, mo, V, W, mn, ru, zr, ce, zn or Cr metal; the metal salt solution has a weight concentration of 0.01-40% and the solvent is high-purity water.
Further, in the step (c), the residence time of the aerosol liquid drops in the atomization drying tower (2) is 0.1 second-10 minutes, and the residence time of the aerosol liquid drops in the vertical tube furnace (3) is 0.1 second-10 minutes.
Further, the temperature of the cooling gas in the step (c) is-50-40 ℃; the flow ratio of the cooling gas to the hot air flow at the outlet of the vertical tube furnace is 3-100.
According to the device and the method for preparing the ultrafine powder through vertical spray pyrolysis, the movement direction of aerogel liquid drops is optimized through the improvement of the tubular furnace, so that the deposition of aerosol on equipment and the waste of raw materials are reduced, the product yield is improved, the cleaning frequency and the cleaning difficulty of the equipment are reduced, the explosion risk is reduced, and the safety coefficient is improved.
Drawings
FIG. 1 is an SEM photograph of monodisperse iron oxide particles prepared in example 1;
FIG. 2 is an XRD pattern of monodisperse iron oxide particles prepared in example 1;
FIG. 3 is an SEM image of monodisperse silver particles prepared in example 2;
FIG. 4 is an XRD pattern of the monodisperse silver particles obtained in example 2;
FIG. 5 is a DLS plot of monodisperse silver nanoparticles made in example 2;
FIG. 6 is an SEM photograph of monodisperse copper nanoparticles prepared in example 5;
FIG. 7 is an XRD pattern of monodisperse zinc oxide particles prepared in example 6;
FIG. 8 is a schematic structural diagram of the apparatus of the present invention.
In the figure, 1, an atomization device, 2, an atomization drying tower, 3, a vertical tube furnace, 4, a filter, 5, a fan, 6, a tail gas purification device, 7, a tail gas circulation pipeline, 8, a microwave magnetron, 9, carrier gas, 10, cooling gas, 11, a product outlet and 12, a waste liquid outlet.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples.
As shown in fig. 8, a vertical apparatus for preparing ultrafine powder by spray pyrolysis comprises an atomization apparatus 1, an atomization drying tower 2 and a vertical tube furnace 3; the atomization device 1 is arranged at the top of the atomization drying tower 2; the outlet end at the bottom of the atomization drying tower 2 is connected with the inlet end at the top of the vertical tubular furnace 3; the inner wall of the atomization drying tower 2 is provided with not less than 1 microwave magnetron 8 or not less than 1 waveguide tube introduction port; the waveguide tube inlet is connected with a microwave generator outside the atomizing drying tower 2 through a waveguide tube; a fan 5 is arranged at the inlet end or the outlet end of the filter 4; the filter 4 is also connected with a product outlet 11; the outlet end of the tail gas circulating pipeline 7 is connected with a carrier gas 9 pipeline; the tail gas circulating pipeline 6 is also connected with a waste liquid outlet 12.
Example 1
(1) 0.2g of Fe (NO) is weighed out 3 ) 3 (analytically pure) placing in a beaker, adding distilled water to dilute to 0.5%, and mixing uniformly to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 700W;
(3) Opening a nitrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol particles prepared by the centrifugal device to enter an external cylinder, and performing microwave irradiation by a microwave generator for 26s at the preheating temperature of 100 ℃;
(4) The particles after microwave and preheating enter a lower vertical tube furnace 3 (the temperature is set to be 400 ℃) for heat treatment for about 5s;
(5) The heat-treated particles are heat-exchanged with cold air and collected on the filter 4, and the temperature of the filter 4 is maintained at about 80 ℃;
(6) Dispersing the collected particles in an absolute ethanol solution, and testing by SEM and XRD to obtain monodisperse iron oxide particles as shown in figures 1 and 2;
the XRD image shows that the product prepared in the example is ferric oxide, and the SEM image shows that the monodispersity of the product is good.
Example 2
(1) Weighing 0.2g AgNO 3 (analytically pure) placing in a beaker, adding a certain amount of distilled water to dilute to 0.5%, and uniformly mixing to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 700W;
(3) Opening a nitrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol particles prepared by the centrifugal device to enter an external cylinder, performing microwave irradiation in a microwave oven, wherein the irradiation time is about 50s, and the preheating temperature is about 100 ℃;
(4) The particles after microwave and preheating enter a lower vertical tube furnace 3 (the temperature is set to be 400 ℃) for heat treatment for about 5s;
(5) The heat-treated particles exchange heat with cold air and are collected on a filter 4, and the temperature of the filter 4 is maintained at about 80 ℃;
(6) Dispersing the collected particles in an absolute ethanol solution, and testing by SEM, XRD and DLS, the obtained monodisperse ultra-fine silver particles are shown in fig. 3, 4 and 5;
the XRD pattern shows that the product prepared by the embodiment is Ag particles, the SEM pattern shows that the monodispersity of the product is good, and the DLS pattern shows that the particle size of the particles is uniform, and the average particle size is 102nm.
Example 3
(1) 0.5g of Ni (NO) was weighed 3 ) 2 (analytically pure) placing in a beaker, adding a certain amount of distilled water to dilute to 0.5%, and uniformly mixing to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 800W;
(3) Opening a nitrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol liquid drops prepared by the centrifugal device to enter an external cylinder, and performing microwave irradiation by a microwave generator for about 50s at a preheating temperature of about 100 ℃;
(4) The particles after microwave and preheating enter a lower vertical tube furnace 3 (the temperature is set to be 400 ℃) for heat treatment for about 5s;
(5) The heat-treated particles are heat-exchanged with cold air and collected on the filter 4, and the temperature of the filter 4 is maintained at about 80 ℃.
Example 4
(1) 0.5g of Co (NO) is weighed 3 ) 2 (analytically pure) placing in a beaker, adding a certain amount of distilled water to dilute to 0.5%, and uniformly mixing to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 800W;
(3) Opening a nitrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol liquid drops prepared by the centrifugal device to enter an external cylinder, and performing microwave irradiation by a microwave generator for about 50s at a preheating temperature of about 100 ℃;
(4) The particles after microwave and preheating enter a lower vertical tube furnace 3 (the temperature is set to be 400 ℃) for heat treatment for about 5s;
(5) The heat-treated particles are heat-exchanged with cold air and collected on the filter 4, and the temperature of the filter 4 is maintained at about 80 ℃.
Example 5
(1) 0.5g of Cu (NO) was weighed 3 ) 2 (analytically pure) placing in a beaker, adding a certain amount of distilled water to dilute to 0.5%, and uniformly mixing to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 800W;
(3) Opening a hydrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol liquid drops prepared by the centrifugal device to enter an external cylinder, and performing microwave irradiation by a microwave generator for about 50s;
(4) The particles after microwave and preheating treatment enter a lower vertical tube furnace 3 (the temperature is set to be 700 ℃) for heat treatment for about 5s, and the preheating temperature is about 100 ℃;
(5) The heat-treated particles are heat-exchanged with cold air and collected on the filter 4, and the temperature of the filter 4 is maintained at about 80 ℃.
(6) The collected particles were dispersed in an absolute ethanol solution for SEM testing.
Example 6
(1) 0.5g of Zn (NO) is weighed 3 ) 2 (analytically pure) placing in a beaker, adding a certain amount of distilled water to dilute to 0.5%, and uniformly mixing to obtain a solution;
(2) Putting the solution into a container of a centrifugal atomization device 1, and turning on a microwave generator and a drying device to adjust the microwave power to 800W;
(3) Opening a nitrogen steel cylinder, adjusting the rotating speed of a centrifugal device to 20000 revolutions per minute, adjusting the pressure of carrier gas 9 to 20psi, enabling aerosol liquid drops prepared by the centrifugal device to enter an external cylinder, and performing microwave irradiation by a microwave generator for about 50s;
(4) The particles after microwave and preheating action enter a lower vertical tube furnace 3 (the temperature is set to be 700 ℃) for heat treatment for about 5s, and the preheating temperature is about 100 ℃;
(5) The heat-treated particles are heat-exchanged with cold air and collected by the filter 4, and the temperature of the filter 4 is maintained at about 80 ℃.
(6) The collected particles were dispersed in an absolute ethanol solution and tested by XRD.
Claims (7)
1. The method for preparing the ultrafine powder by vertical spray pyrolysis is characterized by using a device which comprises an atomizing device (1), an atomizing and drying tower (2) and a vertical tube furnace (3); the atomization device (1) is arranged at the top of the atomization drying tower (2); the outlet end at the bottom of the atomization drying tower (2) is connected with the inlet end at the top of the vertical tubular furnace (3); the inner wall of the atomization drying tower (2) is provided with not less than 1 microwave magnetron (8) or not less than 1 waveguide tube introduction port; the waveguide tube introduction port is connected with a microwave generator outside the atomization drying tower (2) through a waveguide tube; the outlet end of the vertical tube furnace (3) is sequentially connected with a filter (4), a tail gas purification device (6) and the inlet end of a tail gas circulating pipeline (7); a fan (5) is arranged at the inlet end or the outlet end of the filter (4); the outlet end of the tail gas circulating pipeline (7) is connected with a carrier gas (9) pipeline;
the method comprises the following steps:
step (a): dissolving metal salt in a polar solvent to prepare a precursor solution; the metal salt is selected from at least one of nitrate, halogenated salt, hypochlorite, acetate, oxalate or sulfate;
a step (b): preparing the precursor solution prepared in the step (a) into aerosol liquid drops through an atomizing device (1); introducing the aerosol droplets into an atomization drying tower (2) through hot carrier gas (9) at 50-300 ℃, heating through microwave irradiation of a microwave magnetron (8) or a microwave generator, and expanding and crushing the atomized droplets into micron, submicron or nano aerosol droplets;
a step (c): the micron, submicron or nano aerosol droplets obtained in the step (b) fall into a vertical tubular furnace (3) which is tightly connected below an atomization drying tower (2) under the action of gravity and carrier gas (9), are treated at 300-1000 ℃ to obtain monodisperse aerosol particles, are mixed with a large amount of cooling gas (10) at the outlet of the vertical tubular furnace (3), are rapidly cooled to reduce the original temperature of the aerosol particles from 300-1000 ℃ to 30-60 ℃, and are collected by a filter (4) to obtain monodisperse metal simple substances, alloy or metal oxide ultrafine particles with the particle size of 10 nanometers-5 micrometers; the filter (4) is a ceramic filter or a polymer membrane filter; the cooling gas (10) is air, nitrogen, a mixed gas of hydrogen and nitrogen or a mixed gas of hydrogen and air; the hydrogen volume concentration is <5%; the carrier gas (9) is air, nitrogen, a mixed gas of hydrogen and nitrogen or a mixed gas of hydrogen and air, wherein the volume concentration of hydrogen is less than 5%; the temperature of the cooling gas (10) in the step (c) is-50-40 ℃; the flow ratio of the cooling gas (10) to the hot airflow at the outlet of the vertical tube furnace (3) is 3-100;
step (d): controlling the flow and the pressure difference of the filter (4) through a fan (5) to carry out membrane interception; selectively catalytically reducing nitrogen oxides in the hot tail gas obtained in the step (c) into harmless nitrogen and water through a catalyst and discharging; or absorbing carbon dioxide, oxysulfide, acetic acid, hydrogen chloride and hydrogen sulfide acidic gas by alkali liquor, cooling and compressing by a tail gas purification device (6), removing water, and recycling by a tail gas recycling pipeline (7).
2. The method for preparing ultrafine powder by vertical spray pyrolysis as claimed in claim 1, wherein the total power of the microwave magnetrons (8) in the step (b) is 30W-600kW, the power of each microwave magnetron (8) is equal or unequal, and the spatial arrangement ensures the uniformity of the microwave field in the atomizing dryer.
3. The method for preparing ultrafine powder by vertical spray pyrolysis according to claim 1, wherein the inclination angle between the vertical tube furnace (3) and the ground is 60-90 °.
4. The method for preparing the ultrafine powder by vertical spray pyrolysis according to claim 1 or 2, wherein the atomization mode of the atomization device (1) is high-speed centrifugal spray atomization, ultrasonic atomization or high-pressure airflow atomization.
5. The method for preparing ultrafine powder according to claim 4, wherein the size of the liquid drops formed after atomization is 500nm-500 μm; the size of the liquid drop formed after microwave crushing is 20nm-50 μm.
6. The method for preparing the ultrafine powder through vertical spray pyrolysis according to any one of claims 1 to 3, wherein the metal salt is at least one of nitrate, halide, hypochlorite, acetate, oxalate or sulfate of Ag, au, cu, pt, pd, fe, co, ni, ti, sn, sb, mo, V, W, mn, ru, zr, ce, zn or Cr metal; the metal salt solution has a weight concentration of 0.01-40% and the solvent is high-purity water.
7. The method for preparing ultrafine powder by vertical spray pyrolysis according to claim 6, wherein in the step (c), the residence time of the aerosol droplets in the atomizing and drying tower (2) is 0.1 second to 10 minutes, and the residence time of the aerosol droplets in the vertical tube furnace (3) is 0.1 second to 10 minutes.
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