CN110465257B - Nanoparticle swirl flame atomization doping synthesis system and synthesis method thereof - Google Patents
Nanoparticle swirl flame atomization doping synthesis system and synthesis method thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B01J2219/00049—Controlling or regulating processes
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- B01J2219/00157—Controlling the temperature by means of a burner
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
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Abstract
The invention discloses a nanoparticle rotational flow flame atomization doping synthesis system and a synthesis method thereof. The system comprises a flame cavity, a dilution cooling cavity, a cyclone impact atomizer and a combined burner. The combined burner comprises a cyclone burner and a gas guide block, and is arranged around the cyclone impact atomizer and forms gas-liquid combined combustion. The air guide block is provided with an air flow channel group comprising a primary air channel and a fuel air channel. The cyclone burner comprises a plurality of cyclone combustion modules which are close to each other to form a concentric ring shape, and air inlet channels which are arranged in one-to-one correspondence with the air flow channels and are communicated with the cyclone. Primary air and fuel gas enter the cyclone burner through adjacent air flow channels to form cyclone air flow, and the fuel gas is ignited to form cyclone flame. And atomizing the metal precursor solution by a cyclone impact atomizer, and then enabling the atomized metal precursor solution to enter a cyclone flame for combustion to generate a nanoparticle flow. The nanoparticle stream is diluted and cooled to complete collection. The invention has the advantages of high nanoparticle generation yield, good effect and the like.
Description
Technical Field
The invention relates to a nanoparticle rotational flow flame atomization doping synthesis system and a synthesis method thereof, in particular to an atomic-level multielement doping nanoparticle rotational flow flame atomization doping synthesis system and a synthesis method thereof, and belongs to the technical field of nanomaterial synthesis.
Background
Modern nanometer technology is important to the fields of medicine, catalysis, electronics and materials, and nanometer particles have unique performance advantages in many fields due to the characteristics of small particle size, large specific surface area and the like. At present, nano particles are mainly synthesized by flame synthesis method, chemical vapor deposition method, sol-gel method, liquid phase precipitation method, hydrothermal method, plasma spraying method and the like. Compared with other methods, the flame synthesis method has the advantages of easy realization of scale, no liquid phase pollutant, small particle size of nano particles, easy doping and the like.
The swirl flame is easy to stabilize, low in emission and wide in regulation range, and can be widely applied to industries such as gas combustion. The invention patent of applying the rotational flow stagnation flame to the field of flame synthesis, namely a system and a method for synthesizing nano particles by using the rotational flow stagnation flame (CN 33464064A), has the characteristics of simple structure of a burner, small particle size, uniformity, high purity and the like. The system is directed to the precise synthesis of a single precursor and a single species of nanoparticle. With the further development of flame synthesis technology, another invention patent refers to an atomized flame nano particle synthesis system (CN 204445881U) based on multi-cyclone reinforced mixing, which is suitable for small and medium-volume production aiming at low-volatility liquid phase precursors, can realize mass production aiming at high-volatility gas phase precursors, and realizes the industrial amplification of flame synthesis technology to a certain extent.
Disclosure of Invention
The invention aims to provide a nanoparticle cyclone flame atomization doping synthesis system and a synthesis method thereof, wherein a cyclone burner is selected to form stable cyclone duty flame, precursors are sprayed in a direct atomization mode to form a gas-liquid combined combustion mode, the flame directly participates in a particle synthesis reaction process, and the yield of the nanoparticle synthesized by the flame is greatly improved by matching with a corresponding particle collection method, so that the industrial amplification of nanoparticle synthesis can be realized. Meanwhile, on the basis of realizing the synthesis of the atomic-level multi-element doped nano particles, the precise control of particle size, morphology and crystal orientation is further realized.
The invention is realized by the following technical scheme:
a nano-particle cyclone flame atomization doping synthesis system comprises a flame cavity, a dilution cooling cavity, a cyclone impact atomizer, a combined combustor and a product collecting device.
The swirl impact atomizer is arranged at the center of the combined burner, and the combined burner is arranged at the bottom of the flame cavity around the swirl impact atomizer.
The combined burner comprises a cyclone burner and a gas flow guide block which is arranged around the cyclone burner, and the cyclone burner is in a concentric ring shape, so that the cyclone impact atomizer, the cyclone burner and the gas flow guide block are arranged in a concentric circle from inside to outside; the air guide block is provided with at least one group of radially-communicated air flow channel groups, each group of air flow channel groups comprises two air flow channels which are uniformly arranged in a circumference manner, one air flow channel is used as a primary air channel, and the other air flow channel is used as a fuel air channel and is respectively used for introducing primary air and fuel air.
The dilution cooling chamber is disposed at the top of the flame chamber. The inlet end of the product collecting device is arranged in the dilution cooling cavity.
The swirl impingement atomizer is provided with an atomizing gas inlet and a precursor liquid inlet.
In the above technical scheme, the top of the flame cavity is provided with the necking baffle plate which is obliquely arranged, so that the flame cavity is gradually reduced to the dilution cooling cavity and a shrinkage nozzle is formed in the dilution cooling cavity; the product collection device inlet end is located above the converging spout.
In the above technical scheme, the dilution cooling cavity is also provided with a tertiary air pipe, an outlet of the tertiary air pipe is arranged in the dilution cooling cavity, and the outlet of the tertiary air pipe corresponds to the inlet of the product collecting device in height.
In the technical scheme, the relative height h of the central axis of the inlet of the product collecting device and the shrinkage nozzle is 3-5 cm.
In the technical scheme, the necking baffle adopts a hollow structure and is provided with a secondary air inlet; the inner wall surface of the necking baffle is provided with a plurality of air holes for introducing secondary air.
In the above technical scheme, the cyclone burner comprises at least two cyclone combustion modules, the cyclone combustion modules are close to each other and can form concentric circular rings to surround the cyclone impact atomizer, a cyclone air inlet channel is formed between every two adjacent cyclone combustion modules, the cyclone air inlet channels are in one-to-one correspondence with the airflow channels and are communicated with each other, and the number of the cyclone combustion modules is consistent with the number of the cyclone air inlet channels and the number of the airflow channels.
In the above technical scheme, the airflow channel group is provided with more than two groups, the primary air channel and the fuel gas channel are correspondingly and respectively provided with more than two groups, and the primary air channel and the fuel gas channel are circumferentially and uniformly distributed and sequentially arranged at intervals.
In the above technical solution, three to five groups of the airflow channel groups are provided, and six to ten swirl combustion modules are correspondingly provided; the cyclone combustion modules are approximately triangular arc-shaped cyclone blocks and are close to each other to form concentric rings, and a cyclone air inlet channel is formed between two adjacent cyclone combustion modules and communicated with the airflow channels in a one-to-one correspondence mode.
In the above technical scheme, the gas flow guiding block adopts a cylindrical hollow regular polygon structure, the number of sides of the regular polygon structure corresponds to the number of the airflow channels, and each side block is provided with one airflow channel.
A nanoparticle rotational flow flame atomization doping synthesis method comprises the following steps:
enabling primary air and fuel gas to respectively pass through a primary air channel and a fuel gas channel of the airflow channel group, entering a cyclone burner under the flow guide of the gas flow guide block to form cyclone airflow, and enabling the fuel gas to be ignited to form stable cyclone duty flame;
introducing a metal precursor solution and atomizing gas into a cyclone impact atomizer through a precursor liquid inlet and an atomizing gas inlet respectively, so that the precursor solution is atomized into metal precursor droplets with the particle size smaller than or equal to 30 mu m by the atomizing gas, and the particle size of the droplets can be adjusted through the relative heights of a precursor liquid outlet and an atomizing gas outlet;
the metal precursor microdrops enter stable rotational flow duty flame, are ignited by the rotational flow duty flame, and are combusted to synthesize nano particles; the nano particles form a high-temperature nano particle flow along with the ascending of the combustion flue gas;
the high-temperature nano particle flow enters the dilution cooling cavity from the flame cavity, is cooled and diluted under the action of high-speed gas, and is simultaneously pumped by the product collecting device and is introduced into the product collecting device for collection.
As a further optimized technical scheme, tertiary air is sprayed into the dilution cooling cavity through the tertiary air pipe at the speed of 100-150 m/s, a venturi effect is formed on the upper part of a shrinkage nozzle of a shrinkage baffle at the top of the flame cavity, and a pressure difference is generated so that high-temperature nano particle flow is introduced into the dilution cooling cavity and is collected by a product collecting device.
In the technical scheme, the airflow channel group is provided with more than two groups, the primary air channel and the fuel gas channel are correspondingly and respectively provided with more than two groups, and the primary air channel and the fuel gas channel are circumferentially uniformly distributed and sequentially arranged at intervals; the number of the cyclone combustion modules is set according to the number of the airflow channel groups, and each airflow channel group comprises two airflow channels; the cyclone combustion modules are close to each other and can form concentric rings to surround the cyclone impact atomizer, cyclone air inlet channels are formed between the wall surfaces of two adjacent cyclone combustion modules, and the cyclone air inlet channels are communicated with the air flow channels in a one-to-one correspondence manner; the method further comprises the steps of:
the primary air is uniformly distributed to more than two primary air channels, and the fuel gas is uniformly distributed to more than two fuel gas channels, so that the primary air and the fuel gas are sequentially and alternately distributed from the gas guide blocks to enter the cyclone air inlet channel between the wall surfaces of the cyclone combustion module, enter the center of the burner and are mixed in a cyclone manner in the inner circumference of the cyclone combustion module to form cyclone airflow, and the fuel gas in the cyclone airflow is ignited to form stable cyclone duty flame;
introducing a metal precursor solution and atomizing gas into a cyclone impact atomizer through a precursor liquid inlet and an atomizing gas inlet respectively, so that the precursor solution is atomized into metal precursor droplets with the particle size smaller than or equal to 30 mu m by the atomizing gas, and the particle size of the droplets can be adjusted through the relative heights of a precursor liquid outlet and an atomizing gas outlet;
the metal precursor microdrops enter stable rotational flow duty flame, are ignited by the rotational flow duty flame, and are combusted to synthesize nano particles; the nanoparticles travel upward with the combustion flue gas to form a high temperature nanoparticle stream.
In the above technical scheme, the method further comprises preparation of a metal precursor solution, wherein the preparation of the metal precursor solution comprises the following steps:
selecting and weighing a proper amount of metal nitrate as a metal precursor according to the concentration of metal ions being less than or equal to 0.5 mol/L, wherein the metal comprises any one or a mixture of more of magnesium, aluminum, yttrium, nickel, cobalt and manganese;
selecting and measuring a proper amount of organic additive and organic fuel to make the volume ratio of the organic additive to the organic fuel be 1 (4-9); the organic additive comprises 2-ethylhexanoic acid and naphthenic acid, and the organic fuel comprises ethanol, butanol or xylene;
uniformly mixing metal nitrate with organic additive and organic fuel to obtain the metal precursor solution
The invention has the following advantages and beneficial effects: (1) the swirl gas burner generates swirl flame, and can burn together with atomized precursor liquid drops through the outer expansion plate, so that the ignition and stable combustion effects are achieved on the combustion of the atomized precursor liquid drops. (2) The flame directly participates in the particle synthesis reaction process, and the control degree of the flame synthesis reaction is further improved by combining a gas-liquid combined combustion mode.
(3) The particle composition of the metal oxide can be regulated and controlled by changing the types and the proportions of the metal nitrate in the liquid phase precursor, and the atomic-level doping can be realized. (4) By utilizing the dissolubility of the metal nitrate, under the modification effect of the organic additive, a large number of metal oxide particles are synthesized by directly atomizing the precursor for combustion, and the particle size distribution and the crystal phase of the nanometer are precisely controlled by combining an advanced combustion technology. (5) The liquid phase precursor is fed in large amount and is fed continuously, so that the yield of the nano particles is greatly improved. (6) The necking baffle cooperates with high-speed air flow generated by the air supply pump to generate a Venturi effect to introduce the nanoparticle flow into the collecting pipeline, and the high-temperature nanoparticle flow is diluted and cooled, so that the collecting quality and efficiency are greatly improved. (7) The necking baffle is hollow, the inner wall is provided with a plurality of air holes, and secondary air forms a layer of air film on the surface of the baffle, so that the deposition of particles on the baffle can be effectively avoided.
Drawings
FIG. 1 is a schematic diagram of a nanoparticle swirling flame atomizing doping synthesis system according to the present invention.
Fig. 2 is a schematic view of a combined burner and swirl impingement atomizer arrangement in accordance with the present invention.
FIG. 3 is a schematic view of a combined burner with circular gas guide blocks and two gas flow channels according to the present invention.
Fig. 4 is a schematic structural diagram of a combined burner when the gas guide block is in a circular ring shape and the gas flow channel groups are four groups.
Fig. 5 is a schematic view of a combined burner structure when the outer surface of the gas guiding block in fig. 4 is a regular polygon.
Fig. 6 is an XRD pattern when the nanoparticle product according to the present invention is YAP.
Fig. 7 is a TEM image of the product of fig. 6.
FIG. 8 is a TEM image of YAP as a product doped with different proportions of Yb element.
In the figure: 1-flame chamber; 2-diluting the cooling chamber; 3-necking baffle plates; 4-a combined burner; 41-swirl burners; 42-gas diversion block; 43-lower cover plate; 44-upper cover plate; 45-bolt holes; 46-an outer expansion plate; 5-a cyclone impact atomizer; 51-an atomizing gas inlet; 52-precursor liquid inlet; 6-connecting means; 7-a set of air flow channels; 8-a secondary air inlet; 9-tertiary air pipes; 10-a product collection device.
Detailed Description
The following describes the embodiments and working processes of the present invention with reference to the accompanying drawings.
The terms of upper, lower, left, right, front, rear, and the like in the present application are established based on the positional relationship shown in the drawings. The drawings are different, and the corresponding positional relationship may be changed, so that the scope of protection cannot be understood.
As shown in fig. 1, a nanoparticle swirl flame atomization doping synthesis system comprises a flame cavity 1, a dilution cooling cavity 2, a swirl impingement atomizer 5, a combined burner 4 and a product collection device 10.
The dilution cooling cavity 2 is arranged at the top of the flame cavity 1, and the top of the flame cavity 1 is provided with a necking baffle 3 which is obliquely arranged, so that the flame cavity 1 is gradually reduced to the dilution cooling cavity 2 and a shrinkage nozzle is formed in the middle of the dilution cooling cavity.
The product collection device 10 includes a product collection chamber and a drainage pump, and a filter bag or a filter membrane is provided in the product collection chamber to collect the product. The inlet end of the product collection chamber is located in the dilution cooling chamber 2 above and adjacent to the converging nozzle. The dilution cooling chamber 2 is further provided with a tertiary air duct 9, the outlet of which is arranged in the dilution cooling chamber 2 and on the opposite side of the same height as the inlet of the product collecting device 10. The relative height h between the central axis of the inlet of the product collecting device 10 and the shrinkage nozzle is 3-5 cm.
As shown in fig. 2, a combination burner 4 and a swirl impingement atomizer 5 are provided at the bottom of the flame chamber 1. And the cyclone impact atomizer 5 is arranged in the center of the combined burner 4, and the combined burner 4 is concentrically arranged around the cyclone impact atomizer 5. The cyclone impact atomizer 5 adopts a double-fluid flow passage structure, the center is a liquid passage, and a gas passage is arranged outside the liquid passage. The gas channel and the liquid channel are provided with an atomizing gas inlet 51 and a precursor liquid inlet 52 for feeding atomizing gas and a metal precursor solution, respectively.
An external expansion plate 46 is arranged between the top of the cyclone impact atomizer 5 and the inner wall of the combined burner 4, so that cyclone flame formed by the inner wall of the combined burner 4 can stably spread and burn in the flame cavity 1, and metal precursor droplets atomized by the cyclone impact atomizer 5 are ignited.
The combined burner 4 comprises a cyclone burner 41 and a gas guide block 42 arranged around the cyclone burner 41, and the cyclone burner 41 is in a concentric ring shape, so that the cyclone impact atomizer 5, the cyclone burner 41 and the gas guide block 42 are arranged in a concentric circle from inside to outside. The air guide block 42 is provided with at least one group of radially-through air flow channel groups 7, each group of air flow channel groups comprises two air flow channels which are uniformly arranged circumferentially, one air flow channel is a primary air channel 71, and the other air flow channel is a fuel air channel 72 which is respectively used for introducing primary air and fuel air. The combined burner 4 is further provided with a lower cover plate 43 and an upper cover plate 44, which can be clamped by the lower cover plate 43 and the upper cover plate 44 in a vertically fixed manner. The connecting device 6 is arranged outside the upper part of the cyclone impact atomizer 5, and the cyclone impact atomizer 5 and the combined burner 4 can be fixedly connected. The lower cover plate 43 and the upper cover plate 44 fix the cyclone burner 41 and the gas guide block 42 as a unit. In the embodiment shown in fig. 2, the gas guiding block 42, the lower cover plate 43 and the upper cover plate 44 are provided with bolt holes 45 penetrating up and down, and the bolt holes are provided with a plurality of groups and can be fixedly connected through bolts.
As shown in fig. 3 to 5, the cyclone burner 41 includes at least two cyclone combustion modules, the cyclone combustion modules are close to each other and can form a concentric ring shape to surround the cyclone impact atomizer 5, and a cyclone air inlet channel is formed between two adjacent cyclone combustion modules, the cyclone air inlet channels are in one-to-one correspondence with the airflow channels, and the number of the cyclone combustion modules is consistent with the number of the cyclone air inlet channels and the number of the airflow channels.
When the airflow channel group 7 is provided with more than two groups, the primary air channel and the fuel gas channel are correspondingly and respectively provided with more than two groups, and the primary air channel 71 and the fuel gas channel 72 are sequentially spaced and are circumferentially and uniformly distributed. At this time, there is a gas distribution device between more than two primary air channels or between two fuel gas channels.
Fig. 3 shows an embodiment in which two sets of gas flow channels are provided, and the gas guiding block 42 is selected from annular ones.
The airflow channel groups 7 are three to five groups, the cyclone combustion modules are correspondingly arranged in six to ten groups, and fig. 4 and 5 are embodiments when the airflow channel groups are four groups. The cyclone combustion modules are approximately triangular arc-shaped cyclone blocks and are close to each other to form concentric rings, and a cyclone air inlet channel is formed between two adjacent cyclone combustion modules.
In fig. 4, the gas guiding block 42 is selected from a ring shape, in fig. 5, the gas guiding block 42 is selected from a cylindrical hollow regular polygon structure, the number of sides of the regular polygon structure is set corresponding to the number of air flow channels, and each side block is provided with an air flow channel.
As an optimized technical scheme, the necking baffle 3 adopts a hollow structure and is provided with a secondary air inlet 8; the inner wall surface of the necking baffle 3 is provided with a plurality of air holes for introducing secondary air, the diameter of each air hole is 1-2 mm, and the direction of outlet air flow is upward along the direction of the inner wall surface. The secondary air is introduced so that the nanoparticle flow does not adhere to the necking baffle 3.
Nanoparticle synthesis mainly includes metal precursor solution preparation, metal precursor solution atomization and swirl flame combustion, and nanoparticle stream collection.
The preparation of the metal precursor solution comprises the following steps:
according to the prepared nano particle target product, selecting corresponding metal nitrate as a metal precursor, wherein the metal comprises any one or a mixture of a plurality of magnesium, aluminum, yttrium, nickel, cobalt or manganese. When preparing the metal doped nano particle material, the metal type and the doping ratio are selected and changed.
Meanwhile, suitable organic fuels are selected according to the metal nitrate types, and the organic fuels comprise ethanol, butanol or xylene. In order to improve the solubility of the metal nitrate in the organic fuel, an organic additive is usually added, and the organic additive is selected from 2-ethylhexanoic acid or naphthenic acid.
And (3) weighing a proper amount of metal nitrate and taking the organic additive and the organic fuel according to the metal ion concentration of less than or equal to 0.5 mol/L and the volume ratio of the organic additive to the organic fuel of 1 (4-9), and uniformly mixing the metal nitrate, the organic additive and the organic fuel to obtain the metal precursor solution. In order to further ensure complete dissolution and even mixing of the metal nitrate, the mixed solution can be prepared under the action of ultrasonic waves.
The primary air is uniformly distributed to more than two primary air channels, and the fuel gas is uniformly distributed to more than two fuel gas channels, so that the primary air and the fuel gas are sequentially and alternately distributed from the gas guide blocks 42 to enter the cyclone air inlet channel between the wall surfaces of the cyclone combustion module, enter the center of the burner and are mixed in a cyclone manner in the inner circumference of the cyclone combustion module to form cyclone airflow, and the fuel gas in the cyclone airflow is ignited to form stable cyclone duty flame.
Then the prepared metal precursor solution is quantitatively and controllably introduced into the cyclone impact atomizer 5 through the precursor liquid inlet 52 by a liquid feeding pump, and simultaneously air is selected as atomizing gas to be also introduced into the cyclone impact atomizer 5 through the atomizing gas inlet 51, and the flow rate of the atomizing gas is regulated by a flowmeter, so that the precursor solution is atomized into metal precursor droplets with the particle size of less than or equal to 30 mu m by the atomizing gas.
The metal precursor microdrops enter stable rotational flow duty flame, are ignited by the rotational flow duty flame, and are combusted to synthesize nano particles; the nanoparticles travel upward with the combustion flue gas to form a high temperature nanoparticle stream.
The high-temperature nano particle flow is guided by a necking baffle 3 at the top of the flame cavity 1 and is sprayed into the dilution cooling cavity 2 from a shrinkage nozzle; and tertiary air is sprayed into the dilution cooling cavity 2 through the tertiary air pipe 9 at a speed of 100-150 m/s, and a venturi effect is formed at the upper part of the shrinkage nozzle, so that high-temperature nanoparticle flow is introduced into the product collecting device 10 for collection.
Embodiment one: swirl flame atomization synthesis of YAP (yttrium aluminate YAlO) 3 ) Nanomaterial for the preparation of a nanoparticle
9.49g of yttrium nitrate hexahydrate and 14.76g of aluminum nitrate nonahydrate are selected and respectively weighed in the preparation of the precursor solution as metal precursors, the metal precursors and the yttrium nitrate hexahydrate are dissolved in 141mL of organic fuel ethanol, 39mL of 2-ethylhexanoic acid is added as an organic additive, and the yttrium ion concentration and the aluminum ion concentration in the mixed solution are 0.15mol/L and 0.25mol/L respectively. The fuel gas adopted by the cyclone burner is methane, the primary air is compressed air, and the flow rates are 3L/min and 30L/min respectively. The cyclone impact atomizer adopts compressed air as atomizing gas, and the flow is 15L/min. The YAP nano particles obtained by burning and collecting the above method have the production rate of more than 100 g/h. BET measurement gave the particles having a specific surface area of 69.78m 2 And/g, the average particle size reaches 14nm. The crystal phase XRD and morphology TEM of YAP nanoparticle products after post-treatment are shown in fig. 6 and 7. The crystal phase peaks of the initial synthesis products were evident, corresponding to YAP particles. The prepared YAP nano-particles are regular spheres in morphology, small in particle size and uniform in distribution.
Further, YAP may be post-treated to obtain YAG (yttrium aluminum garnet Y) 3 Al 5 O 12 ) The XRD pattern of the crystalline phase of the particles is shown in fig. 6.
Embodiment two: rotational flow flame atomization synthesis of Yb element doped YAP nano material
In the preparation of the precursor in the first embodiment, metal nitrate (ytterbium nitrate pentahydrate) corresponding to the doping element Yb is added according to the set doping proportion to prepare the precursor solution, so that the morphology of the synthesized nano particles under different doping proportions is shown in fig. 8. The prepared nano particles are regular spherical in morphology, the particle size distribution is uniform, and the particle size is increased along with the increase of the doping proportion.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. The nanoparticle swirl flame atomization doping synthesis system is characterized by comprising a flame cavity (1), a dilution cooling cavity (2), a swirl impingement atomizer (5), a combined burner (4) and a product collecting device (10);
the swirl impact atomizer (5) is arranged in the center of the combined burner (4), and the combined burner (4) is arranged at the bottom of the flame cavity (1) around the swirl impact atomizer (5);
the combined burner (4) comprises a cyclone burner (41) and a gas guide block (42) arranged around the cyclone burner (41), and the cyclone burner (41) is in a concentric ring shape, so that the cyclone impact atomizer (5), the cyclone burner (41) and the gas guide block (42) are arranged in concentric circles from inside to outside; at least one group of radially-communicated air flow channel groups (7) are arranged on the air guide block (42), each group of air flow channel groups comprises two air flow channels which are uniformly arranged in a circumference manner, one air flow channel is a primary air channel (71), and the other air flow channel is a fuel air channel (72) which is respectively used for introducing primary air and fuel air;
the cyclone burner (41) comprises at least two cyclone combustion modules which are close to each other and can form concentric rings to be arranged around the cyclone impact atomizer (5);
the dilution cooling cavity (2) is arranged at the top of the flame cavity (1), and the inlet end of the product collecting device (10) is arranged in the dilution cooling cavity (2);
the swirl impingement atomizer (5) is provided with an atomizing gas inlet (51) and a precursor liquid inlet (52).
2. The nanoparticle swirl flame atomization doping synthesis system according to claim 1, wherein a necking baffle (3) is arranged at the top of the flame cavity (1) in an inclined manner, so that the flame cavity (1) tapers towards the dilution cooling cavity (2) and forms a contraction nozzle in the dilution cooling cavity (2); the inlet end of the product collection device (10) is located above the constriction nozzle.
3. A nanoparticle swirl flame atomizing and doping synthesis system according to claim 1 or 2, wherein a tertiary air pipe (9) is further arranged in the dilution cooling chamber (2), and the outlet of the tertiary air pipe (9) corresponds to the inlet height of the product collecting device.
4. The nanoparticle swirl flame atomizing and doping synthesis system according to claim 2, wherein the relative height h between the central axis of the inlet of the product collecting device (10) and the shrinkage nozzle is 3-5 cm.
5. The nanoparticle swirl flame atomization doping synthesis system according to claim 2, wherein the necking baffle (3) adopts a hollow structure and is provided with a secondary air inlet (8); the inner wall surface of the necking baffle (3) is provided with a plurality of air holes for introducing secondary air.
6. The nanoparticle swirl flame atomization doping synthesis system according to claim 2, wherein swirl air inlet channels are formed between the swirl combustion modules, the swirl air inlet channels are arranged in one-to-one correspondence and communicated with the airflow channels, and the number of the swirl combustion modules is consistent with the number of the swirl air inlet channels and the number of the airflow channels.
7. The nanoparticle swirl flame atomizing and doping synthesis system according to claim 1 or 6, wherein the airflow channel group (7) is provided with more than two groups, the primary air channel (71) and the fuel gas channel (72) are correspondingly and respectively provided with more than two groups, and the primary air channel (71) and the fuel gas channel (72) are circumferentially and uniformly distributed and sequentially arranged at intervals.
8. The nanoparticle swirl flame atomization doping synthesis system according to claim 7, wherein three to five groups of the airflow channel groups (7) are provided, and six to ten swirl combustion modules are correspondingly provided; the cyclone combustion modules are approximately triangular arc-shaped cyclone blocks and are close to each other to form concentric rings, and a cyclone air inlet channel is formed between two adjacent cyclone combustion modules and communicated with the airflow channels in a one-to-one correspondence mode.
9. The nanoparticle swirl flame atomizing and doping synthesis system as recited in claim 8, wherein the gas guide block (42) is a cylindrical hollow regular polygonal structure, the number of sides of the regular polygonal structure is set corresponding to the number of gas flow channels, and each side block is provided with one gas flow channel.
10. A nanoparticle swirl flame atomized doping synthesis method using a nanoparticle swirl flame atomized doping synthesis system according to claim 1, the method comprising:
the primary air and the fuel gas respectively pass through a primary air channel (71) and a fuel gas channel (72) of the air flow channel group (7), enter the cyclone burner (41) to form cyclone air flow under the flow guide of the air flow guide block (42), and are ignited to form stable cyclone duty flame;
introducing the metal precursor solution and atomizing gas into a cyclone impact atomizer (5) through a precursor liquid inlet (52) and an atomizing gas inlet (51) respectively, so that the precursor solution is atomized into metal precursor droplets with the particle size of less than or equal to 30 mu m by the atomizing gas;
the metal precursor microdrops enter stable rotational flow duty flame, are ignited by the rotational flow duty flame, and are combusted to synthesize nano particles; the nano particles form a high-temperature nano particle flow along with the ascending of the combustion flue gas;
the high-temperature nano particle flow enters the dilution cooling cavity (2) from the flame cavity (1), and is guided into the product collecting device (10) for collection under the suction of the product collecting device (10).
11. The nanoparticle swirl flame atomization doping synthesis method according to claim 10, wherein the airflow channel group (7) is provided with more than two groups, the primary air channel (71) and the fuel gas channel (72) are correspondingly and respectively provided with more than two groups, and the primary air channel (71) and the fuel gas channel (72) are circumferentially and uniformly distributed and sequentially arranged at intervals; the number of the cyclone combustion modules is set according to the number of the airflow channel groups, and each airflow channel group comprises two airflow channels; the cyclone combustion modules are close to each other and can form concentric rings to surround the cyclone impact atomizer (5), cyclone air inlet channels are formed between the wall surfaces of two adjacent cyclone combustion modules, and the cyclone air inlet channels are communicated with the air flow channels in a one-to-one correspondence manner; the method further comprises the steps of:
the primary air is uniformly distributed to more than two primary air channels, and the fuel gas is uniformly distributed to more than two fuel gas channels, so that the primary air and the fuel gas are sequentially and alternately distributed from the gas guide blocks (42) to enter the cyclone air inlet channel between the wall surfaces of the cyclone combustion module, enter the center of the burner and are mixed in a cyclone manner in the inner circumference of the cyclone combustion module to form cyclone airflow, and the fuel gas in the cyclone airflow is ignited to form stable cyclone duty flame;
introducing a metal precursor solution and atomizing gas into a cyclone impact atomizer (5) through a precursor liquid inlet (52) and an atomizing gas inlet (51) respectively, so that the precursor solution is atomized into metal precursor droplets with the particle size smaller than or equal to 30 mu m by the atomizing gas, and the particle size of the droplets can be regulated through the relative heights of a precursor liquid outlet and an atomizing gas outlet;
the metal precursor microdrops enter stable rotational flow duty flame, are ignited by the rotational flow duty flame, and are combusted to synthesize nano particles; the nanoparticles travel upward with the combustion flue gas to form a high temperature nanoparticle stream.
12. The nanoparticle swirl flame atomized doping synthesis method according to claim 10 or 11, further comprising a metal precursor solution preparation comprising:
selecting and weighing a proper amount of metal nitrate as a metal precursor according to the concentration of metal ions being less than or equal to 0.5 mol/L, wherein the metal comprises any one or a mixture of more of magnesium, aluminum, yttrium, nickel, cobalt and manganese;
selecting and measuring a proper amount of organic additive and organic fuel to make the volume ratio of the organic additive to the organic fuel be 1 (4-9); the organic additive comprises 2-ethylhexanoic acid and naphthenic acid, and the organic fuel comprises ethanol, butanol or xylene;
and uniformly mixing the metal nitrate with the organic additive and the organic fuel to obtain the metal precursor solution.
13. The nanoparticle swirl flame atomization doping synthesis method according to claim 10, wherein a necking baffle (3) which is obliquely arranged is arranged at the top of the flame cavity (1), so that the flame cavity (1) tapers towards the dilution cooling cavity (2) and forms a contraction nozzle in the dilution cooling cavity (2); the inlet end of the product collecting device (10) is positioned above the contraction spout; a tertiary air pipe (9) is further arranged in the dilution cooling cavity (2), and the outlet of the tertiary air pipe (9) corresponds to the inlet of the product collecting device in height; the method further comprises the steps of:
the tertiary air is sprayed into the dilution cooling cavity (2) through the tertiary air pipe (9) at the speed of 100-150 m/s, a venturi effect is formed on the upper part of a shrinkage nozzle of a shrinkage baffle plate (3) at the top of the flame cavity (1), and pressure difference is generated so that high-temperature nano particle flow is introduced into the dilution cooling cavity (2) and is collected by a product collecting device (10).
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