CN112707430A - Combustion chamber and method for synthesizing superfine lanthanum oxide powder by combustion - Google Patents
Combustion chamber and method for synthesizing superfine lanthanum oxide powder by combustion Download PDFInfo
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- CN112707430A CN112707430A CN202110033393.6A CN202110033393A CN112707430A CN 112707430 A CN112707430 A CN 112707430A CN 202110033393 A CN202110033393 A CN 202110033393A CN 112707430 A CN112707430 A CN 112707430A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/229—Lanthanum oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the technical field of rare earth oxide powder, and provides a combustion chamber and a method for synthesizing superfine lanthanum oxide powder by combustion. The invention adopts a combustion chamber comprising four atomizing nozzles to synthesize superfine lanthanum oxide powder, wherein a first atomizing nozzle and a third atomizing nozzle are symmetrically distributed, and a second atomizing nozzle and a fourth atomizing nozzle are symmetrically distributed. The method provided by the invention has the advantages of simple process, short flow, easy operation and low cost, and the obtained superfine lanthanum oxide powder has good dispersibility, high purity and uniform particle size.
Description
Technical Field
The invention relates to the technical field of rare earth oxide powder, in particular to a combustion chamber and a method for synthesizing superfine lanthanum oxide powder by combustion.
Background
Lanthanum oxide (La)2O3) The rare earth is one of important products in light rare earth, has good physical and chemical properties, is well applied to the fields of civil, military and commercial science and technology and the like, and is widely applied to the fields of glass, ceramics, catalysts, fluorescent powder, laser, heating bodies, cathode materials, electric contacts and the like at present. Superfine La2O3Due to the characteristics of small-size effect, surface effect, quantum size effect, macroscopic quantum tunneling effect and the like, the powder has different heat, magnetic, electric, light and other sensitive characteristics and surface stability and the like from the traditional powder, shows more excellent physical and chemical properties and has wider application prospect.
At present, the existing methods for producing ultrafine lanthanum oxide powder mainly include a vacuum condensation method, a physical crushing method, a mechanical ball milling method, a precipitation method, a hydrothermal synthesis method, a sol-gel method, a supercritical fluid method, a solvent evaporation method and the like, but the methods for preparing ultrafine lanthanum oxide powder all have the problems of complex preparation process, difficult control and large input cost, and cannot easily obtain ultrafine lanthanum oxide powder with high purity, good dispersibility and uniform particle size. Lanthanum oxide powder D prepared as in conventional oxalate precipitation50The particle size is large and the distribution is wide, wherein the particle size is 2.5-6.0 mu m; the method of ammonium bicarbonate precipitation, ultrasonic uniform precipitation, solid phase synthesis and the like is used for preparing the superfine La2O3Agglomeration is easy to generate in the powder process, so that the particle size is not uniform; the sol-gel method has the defects of slow gel process, large shrinkage during drying, uneven powder granularity and the like.
Disclosure of Invention
In view of the above, the present invention provides a combustion chamber and a method for synthesizing ultra-fine lanthanum oxide powder by combustion. The method provided by the invention has the advantages of simple steps and low cost, and the obtained superfine lanthanum oxide powder has high purity, good dispersibility and uniform granularity.
In order to achieve the above object, the present invention provides the following technical solutions:
the utility model provides a combustion chamber, be provided with first atomizing nozzle, second atomizing nozzle, third atomizing nozzle and fourth atomizing nozzle on the lateral wall of combustion chamber, first atomizing nozzle and third atomizing nozzle are the symmetric distribution as the axle with the perpendicular line of crossing the combustion chamber center, and second atomizing nozzle and fourth atomizing nozzle use the perpendicular line of crossing the combustion chamber center to be the symmetric distribution as the axle.
Preferably, the bottom outlet of the combustion chamber is sequentially connected with a cyclone separator and a cloth bag filter.
The invention also provides a method for synthesizing the superfine lanthanum oxide powder by utilizing the combustion chamber in the scheme, which comprises the following steps:
(1) the flammable solvent is fed into the combustion chamber from the first atomizing nozzle and the third atomizing nozzle under the action of first carrier gas, and the flammable solvent is ignited to be combusted; after the combustible solvent is stably combusted, sending a lanthanum salt solution into the combustion chamber from the second atomizing nozzle and the fourth atomizing nozzle under the action of second carrier gas, and igniting the lanthanum salt to obtain a combustion product; the first carrier gas is combustion-supporting gas, and the second carrier gas is combustion-supporting gas and/or combustible gas;
(2) and (3) carrying out microwave oxidation calcination on the combustion product to obtain superfine lanthanum oxide powder.
Preferably, the solvent of the lanthanum salt solution is a combustible solvent; the concentration of the lanthanum salt solution is 0.1-10 mol/L.
Preferably, the combustion-supporting gas is air and/or oxygen; the combustible gas is hydrogen and/or methane.
Preferably, the flammable solvent includes one or more of methanol, ethanol, acetone and gasoline.
Preferably, the feeding speeds of the first atomizing nozzle and the third atomizing nozzle are independently 10-30 mL/min; the pressure of the first carrier gas is 1-3 atmospheric pressures; the feeding speeds of the second atomizing nozzle and the fourth atomizing nozzle are independently 1-20 mL/min; the pressure of the second carrier gas is 1-3 atmospheres.
Preferably, the combustion products are extracted from the bottom of the combustion chamber under the action of the cyclone separator, filtered by a cloth bag filter and collected.
Preferably, the temperature of the microwave oxidation calcination is 100-300 ℃, and the time is 20-60 min.
Preferably, the particle size of the superfine lanthanum oxide powder is 0.01-1.0 μm.
The invention provides a combustion chamber, wherein four atomizing nozzles are arranged on the side wall of the combustion chamber, wherein a first atomizing nozzle and a third atomizing nozzle are symmetrically distributed by taking a vertical line passing through the center of the combustion chamber as an axis, and a second atomizing nozzle and a fourth atomizing nozzle are symmetrically distributed by taking a vertical line passing through the center of the combustion chamber as an axis. The lanthanum oxide is prepared by adopting the four-nozzle combustion chamber, the preparation steps are simple, the operation is easy, and the lanthanum oxide powder with good dispersity and uniform granularity can be obtained.
The invention provides a method for synthesizing superfine lanthanum oxide powder by combustion in a combustion chamber, which comprises the steps of firstly, conveying a combustible solvent into the combustion chamber from a first atomizing nozzle and a third atomizing nozzle under the action of first carrier gas for ignition, then conveying a lanthanum salt solution into the combustion chamber from a second atomizing nozzle and a fourth atomizing nozzle under the action of second carrier gas for combustion, and then carrying out microwave oxidation and calcination on combustion products to obtain the superfine lanthanum oxide powder. The invention synthesizes lanthanum oxide by utilizing a combustion chamber with four atomizing nozzles, fuel is conveyed into the combustion chamber by adopting a first nozzle and a third nozzle which are symmetrically distributed, the fuel is uniformly distributed in the combustion chamber, the uniform temperature in the combustion chamber can be ensured, and sufficient heat is provided for the combustion of lanthanum salt; in the combustion process, more than 80% of lanthanum salt is combusted to generate lanthanum oxide, and the invention carries out microwave oxidation calcination on the combustion product, can convert the residual small amount of lanthanum salt into lanthanum oxide, and ensures to obtain high-purity superfine lanthanum oxide powder.
The method provided by the invention adopts the combustion chamber comprising four nozzles to synthesize lanthanum oxide by combustion, can effectively improve the rate and the conversion amount of converting lanthanum salt into lanthanum oxide, and has the advantages of simple process, short flow, easy operation and low cost.
Furthermore, the invention adopts the combustible solvent as the solvent of the lanthanum salt solution, and can be used as fuel to be combusted in the combustion chamber while dissolving the lanthanum salt, thereby further improving the intensity of combustion of the lanthanum salt, promoting the conversion of the lanthanum salt into lanthanum oxide and improving the conversion rate of the lanthanum salt in the combustion chamber.
The results of the examples show that the superfine lanthanum oxide powder prepared by the invention has good dispersibility, no agglomeration, purity of 99.8 percent, small particle size distribution and good uniformity.
Drawings
FIG. 1 is a schematic view of the distribution of nozzles on the sidewall of a combustor when the combustor chamber is circular;
FIG. 2 is a schematic view of a combustion chamber;
FIG. 3 is a schematic view of a process for synthesizing ultra-fine lanthanum oxide powder by combustion in an embodiment of the present invention;
FIG. 4 is a diagram showing the morphology of the ultra-fine lanthanum oxide powder obtained in example 1;
FIG. 5 is a particle size distribution diagram of the ultra-fine lanthanum oxide powder obtained in example 1.
Detailed Description
The invention provides a combustion chamber, wherein a first atomizing nozzle, a second atomizing nozzle, a third atomizing nozzle and a fourth atomizing nozzle are arranged on the side wall of the combustion chamber.
In the present invention, the first atomizing nozzle and the third atomizing nozzle are symmetrically distributed about a perpendicular line passing through the center of the combustion chamber, the second atomizing nozzle and the fourth atomizing nozzle are symmetrically distributed about a perpendicular line passing through the center of the combustion chamber, and the first atomizing nozzle to the fourth atomizing nozzle are respectively referred to as a nozzle P1, a nozzle P2, a nozzle P3, and a nozzle P4. In the present invention, the nozzles P1, P2, P3 and P4 are preferably evenly distributed on the side wall of the combustion chamber, i.e., the distances between adjacent nozzles are equal; the nozzle P1, the nozzle P2, the nozzle P3 and the nozzle P4 are preferably arranged at the lower part of the side wall of the combustion chamber, and the spray angle is inclined upwards, and preferably the spray angle is 45 degrees; the shape of the inner cavity of the combustion chamber is not particularly required by the invention, the combustion chamber can be in a shape common in the field, in the specific embodiment of the invention, the inner cavity of the combustion chamber is preferably circular, when the inner cavity of the combustion chamber is circular, the nozzle P1, the nozzle P2, the nozzle P3 and the nozzle P4 are preferably uniformly distributed on the side wall of the combustion chamber, namely, the connecting line of the nozzle P1 and the nozzle P3 is vertical to the connecting line of the nozzle P2 and the nozzle P4, and the specific distribution schematic diagram is shown in FIG. 1. The traditional combustion chamber has only 1 ~ 2 nozzles, and fuel and lanthanum salt solution can only get into from same nozzle, perhaps a nozzle gets into the fuel, and another nozzle gets into the lanthanum salt solution, and the inventor finds that this kind of traditional combustion chamber can't guarantee the evenly distributed of fuel and lanthanum salt solution in the combustion chamber, and appears fuel and reactant supply easily inadequately, and the problem that temperature variation is big in the combustion chamber causes the lanthanum salt burning insufficient, the conversion rate is low. The invention uses the four-nozzle combustion chamber, adopts the fuel and the lanthanum salt solution which are respectively conveyed by the mutually symmetrical nozzles, and the fuel and the lanthanum salt solution can be uniformly distributed in the combustion chamber, so that the combustion is more violent and complete, the temperature in the combustion chamber is higher, the problem of sudden temperature change can not occur, and the lanthanum salt can be more favorably converted into lanthanum oxide.
The present invention does not require any special kind of atomizing nozzle, and a commercially available atomizing nozzle may be installed at a specific position on the sidewall of the combustion chamber.
In the invention, the bottom outlet of the combustion chamber is preferably connected with a cyclone separator and a cloth bag filter in sequence; the airflow effect of the cyclone separator can extract combustion products from the bottom of the combustion chamber, and the extracted combustion products are collected after being filtered by the cloth bag filter. The invention has no special requirements on the specific connection mode of the cyclone separator and the bag filter, and the mode known by the technical personnel in the field can be adopted. In a particular embodiment of the invention, the combustion chamber is schematically configured as shown in fig. 2 (in fig. 2, the two rear atomizing nozzles and the two front atomizing nozzles coincide and are therefore not shown, and in fig. 2, the atomizing nozzles shown are nozzle P1 and nozzle P2).
The invention provides a method for synthesizing superfine lanthanum oxide powder by combustion in a combustion chamber, which comprises the following steps:
(1) the flammable solvent is fed into the combustion chamber from the first atomizing nozzle and the third atomizing nozzle under the action of first carrier gas, and the flammable solvent is ignited to be combusted; after the combustible solvent is stably combusted, sending a lanthanum salt solution into the combustion chamber from the second atomizing nozzle and the fourth atomizing nozzle under the action of second carrier gas, and igniting the lanthanum salt to obtain a combustion product; the first carrier gas is combustion-supporting gas, and the second carrier gas is combustion-supporting gas and/or combustible gas;
(2) and (3) carrying out microwave oxidation calcination on the combustion product to obtain superfine lanthanum oxide powder.
The combustible solvent is fed into the combustion chamber from the first atomizing nozzle and the third atomizing nozzle under the action of the first carrier gas, and the combustible solvent is ignited to be combusted. In the present invention, the flammable solvent preferably includes one or more of methanol, ethanol, acetone, and gasoline; the first carrier gas is preferably air and/or oxygen; the feeding speeds of the first atomizing nozzle and the third atomizing nozzle are preferably 10-30 mL/min independently, more preferably 15-25 mL/min independently, and the feeding speeds of the first atomizing nozzle and the third atomizing nozzle can be the same or different, preferably the same; the first carrier gas preferably has a pressure of 1 to 3 atmospheres, more preferably 1.5 to 2.5 atmospheres.
After the combustible solvent is stably combusted, the lanthanum salt solution is fed into the combustion chamber from the second atomizing nozzle and the fourth atomizing nozzle under the action of the second carrier gas, and the lanthanum salt is ignited to obtain a combustion product. In the specific embodiment of the invention, the flammable solvent is considered to be stable after being combusted in the combustion chamber for 3-5 min; in the invention, the solvent of the lanthanum salt solution is preferably a combustible solvent, the combustible solvent is preferably ethanol and/or acetone, and when the solvent is a mixed solvent of ethanol and acetone, the volume ratio of the ethanol to the acetone in the mixed solvent is not particularly required, and any proportion can be adopted; the solute of the lanthanum salt solution is preferably one or more of lanthanum nitrate, lanthanum chloride and lanthanum sulfate; the concentration of the lanthanum salt solution is preferably 0.1-10 mol/L, and more preferably 1-8 mol/L; the second carrier gas is preferably combustion-supporting gas and/or combustible gas, the combustion-supporting gas is preferably air and/or oxygen, and the combustible gas is preferably hydrogen and/or methane; the feeding speeds of the second atomizing nozzle and the fourth atomizing nozzle are independently 1-20 mL/min, and more preferably 5-15 mL/min; the second carrier gas preferably has a pressure of 1 to 3 atmospheres, more preferably 1.5 to 2.5 atmospheres. In the invention, the lanthanum salt solution preferably enters the combustion chamber under the action of a second carrier gas after the combustible solvent is combusted for 3-5 min.
In the invention, after the combustible solvent is combusted in the combustion chamber, the temperature in the combustion chamber is very high, the combustion-supporting gas is excessive, the lanthanum salt solution is atomized into uniformly dispersed small droplets under the action of the second carrier gas and the atomizing nozzle mist, the small droplets contain the combustion-supporting gas and/or the combustible gas, the solvent of the lanthanum salt solution also plays a role of fuel, and the small droplets are contacted with the combustion-supporting gas in the combustion chamber at high temperature to generate violent combustion reaction, so that the lanthanum salt is converted into lanthanum oxide; in the combustion reaction process, the temperature of the flame reaction zone is about 2000 ℃, the temperature of other areas in the combustion chamber is about 300 ℃, and the atmospheric pressure in the combustion chamber is 0.7-0.9 atmospheric pressure. More than 80% of the lanthanum salt can be converted to lanthanum oxide by combustion.
The combustion products generated in the combustion process are pumped out from the bottom of the combustion chamber under the action of the airflow of the cyclone separator, and are collected together after being filtered by the cloth bag filter.
After obtaining the combustion product, the invention carries out microwave oxidation calcination on the combustion product to obtain the superfine lanthanum oxide powder. In the invention, the temperature of the microwave oxidation calcination is preferably 100-300 ℃, more preferably 150-250 ℃, and the time of the microwave oxidation calcination is preferably 20-60 min, more preferably 30-50 min; the microwave power of the microwave oxidation calcination is preferably 1-2 kW; the microwave oxidation calcination is preferably carried out in a microwave muffle furnace; the invention converts a small amount of unreacted lanthanum salt in the combustion product into lanthanum oxide by microwave oxidation calcination.
In the present invention, the particle size of the ultrafine lanthanum oxide powder is preferably 0.01 to 1.0 μm, more preferably 0.2 to 1.0 μm, and even more preferably 0.4 to 0.8 μm, and the purity is preferably not less than 99.8%. In the embodiment of the invention, by controlling the parameters in the combustion process, the superfine lanthanum oxide powder with different particle sizes can be obtained, specifically, when the feeding speed is high and the concentration of the lanthanum salt solution is high, the superfine lanthanum oxide powder with larger particle size can be obtained, and when the feeding speed is low and the concentration of the lanthanum salt solution is low, the superfine lanthanum oxide powder with smaller particle size can be obtained.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Fig. 3 is a schematic view of a process for synthesizing ultra-fine lanthanum oxide powder by combustion in an embodiment of the present invention, in which a combustible solvent is fed into a combustion chamber from a nozzle P1 and a nozzle P3 for combustion by using a first carrier gas, then a lanthanum salt solution is fed into the combustion chamber from a nozzle P2 and a nozzle P4 for combustion by using a second carrier gas, and after the combustion product is separated, filtered and collected, the combustion product is placed in a microwave muffle furnace for calcination, so as to obtain the ultra-fine lanthanum oxide powder.
Example 1
(1) Adding lanthanum nitrate into ethanol, and stirring at room temperature to obtain a clear lanthanum nitrate solution with the concentration of 5 mol/L;
(2) preparing an ethanol solvent, feeding ethanol into a combustion chamber from nozzles P1 and P3 of the combustion chamber by taking oxygen as carrier gas, wherein the feeding speed is 20mL/min, and igniting to combust the ethanol;
(3) after ethanol burns for 3 minutes, hydrogen is used as carrier gas, the lanthanum nitrate solution prepared in the step (2) is sent into the combustion chamber from nozzles P2 and P4 of the combustion chamber, the feeding rate is 15mL/min, after the lanthanum nitrate solution is ignited, lanthanum oxide is generated by burning, and the air pressure in the combustion chamber is 0.8 atmospheric pressure;
(3) capturing combustion products in the combustion chamber by using a cyclone separator and a cloth bag filter, wherein the content of lanthanum oxide in the combustion products is 92% through detection;
(4) calcining the collected combustion products in a microwave muffle furnace at 200 ℃ for 30min to ensure that all lanthanum nitrate is converted into lanthanum oxide powder; the purity of the obtained superfine lanthanum oxide powder is 99.8%, and the total conversion rate of lanthanum nitrate is 99.9%.
FIG. 4 is a diagram illustrating the morphology of the ultra-fine lanthanum oxide powder obtained in this example; as can be seen from FIG. 4, the lanthanum oxide powder obtained in this example has good dispersibility and no agglomeration.
FIG. 5 is a particle size distribution diagram of the ultra-fine lanthanum oxide powder obtained in the present example; the results in FIG. 5 show that the mean particle size of the ultra-fine lanthanum oxide powder obtained in this example is 0.6 μm, and the particle size distribution is between 0.3 μm and 0.9. mu.m.
Example 2
(1) Adding lanthanum chloride into a mixed solvent of ethanol and acetone, and stirring at room temperature to obtain a clarified lanthanum chloride solution with the concentration of 8 mol/L;
(2) preparing a gasoline solvent, feeding gasoline into a combustion chamber from nozzles P1 and P3 in the combustion chamber by taking oxygen as carrier gas, wherein the feeding rate is 20mL/min, and igniting to combust;
(3) after gasoline burns for 3 minutes, the lanthanum chloride solution prepared in the step (1) is fed into the combustion from nozzles P2 and P4 in a combustion chamber by taking air as carrier gas, the feeding rate is 10mL/min, and after the lanthanum chloride solution is ignited, lanthanum oxide is generated by combustion, and the air pressure in the combustion chamber is 0.7 atmospheric pressure;
(4) capturing combustion products generated in the combustion chamber by using a cyclone separator and a cloth bag filter, wherein the content of lanthanum oxide in the combustion products is 87% through detection;
(5) and calcining the collected combustion products in a microwave muffle furnace at 100 ℃ for 50min to ensure that all the rare earth powder is converted into lanthanum oxide powder. The purity of the obtained superfine lanthanum oxide powder is 99.6%, the average particle size is 0.5 mu m, the particle size distribution is 0.2-0.8 mu m, and the total conversion rate of lanthanum nitrate is 99.8%.
Example 3
(1) Adding lanthanum sulfate into an acetone solvent, and stirring at room temperature to obtain a clear lanthanum sulfate solution, wherein the concentration of rare earth salt is 1 mol/L;
(2) preparing acetone solvent, loading acetone into nozzles P1 and P3 in a combustion chamber by using oxygen at a feeding rate of 20mL/min, and igniting to combust;
(3) after acetone burns for 3 minutes, oxygen is used as carrier gas to send the prepared lanthanum sulfate solution in the step (1) into the combustion chamber from nozzles P2 and P4 of the combustion chamber, the feeding speed is 5mL/min, after the lanthanum sulfate solution is ignited, lanthanum oxide powder is generated by burning, and the air pressure in the combustion chamber is 0.9 atmospheric pressure;
(4) capturing combustion products produced by reaction in the combustion chamber by using a cyclone separator and a cloth bag filter, wherein the content of lanthanum oxide in the combustion products is 94% through detection;
(5) calcining the collected combustion products in a microwave muffle furnace at 150 ℃ for 40min to ensure that all rare earth powder is completely converted into La2O3And (3) powder. The purity of the obtained superfine lanthanum oxide powder is 99.8%, the average particle size is 0.6 mu m, the particle size distribution is 0.3-0.9 mu m, and the total conversion rate of lanthanum nitrate is 99.7%.
The appearance of the superfine lanthanum oxide powder obtained in the examples 2-3 is observed, and the result shows that the superfine lanthanum oxide powder has good dispersibility and no agglomeration phenomenon.
Comparative example
The method is characterized in that a traditional two-nozzle combustion chamber is adopted to prepare the lanthanum oxide powder, other conditions are the same as those in the embodiment 1, only the combustion chamber is changed into the two-nozzle combustion chamber, except that the number of nozzles is different, other structures of the combustion chamber are the same as those in the embodiment 1, fuel and lanthanum nitrate solution enter the combustion chamber from different nozzles under the action of carrier gas, and the feeding speeds of the fuel and the lanthanum nitrate solution are the same as those in the embodiment 1.
Through detection, the content of lanthanum oxide in the combustion products collected in the combustion chamber is 63%;
and (3) carrying out microwave calcination on the collected combustion products, wherein the calcination conditions are the same as those in the example 1, the purity of the obtained lanthanum oxide powder is 96.5%, the average particle size is 1.3 mu m, the particle size distribution is 0.8-1.8 mu m, and the total conversion rate of lanthanum nitrate is 61%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The utility model provides a combustion chamber, its characterized in that, be provided with first atomizing nozzle, second atomizing nozzle, third atomizing nozzle and fourth atomizing nozzle on the lateral wall of combustion chamber, first atomizing nozzle and third atomizing nozzle use the perpendicular line of crossing the combustion chamber center to be the symmetric distribution as the axle, and second atomizing nozzle and fourth atomizing nozzle use the perpendicular line of crossing the combustion chamber center to be the symmetric distribution as the axle.
2. The combustor of claim 1, wherein a cyclone separator and a bag filter are connected to the bottom outlet of the combustor in sequence.
3. A method for synthesizing superfine lanthanum oxide powder by utilizing the combustion of the combustion chamber of claim 1 or 2, which is characterized by comprising the following steps:
(1) the flammable solvent is fed into the combustion chamber from the first atomizing nozzle and the third atomizing nozzle under the action of first carrier gas, and the flammable solvent is ignited to be combusted; after the combustible solvent is stably combusted, sending a lanthanum salt solution into the combustion chamber from the second atomizing nozzle and the fourth atomizing nozzle under the action of second carrier gas, and igniting the lanthanum salt to obtain a combustion product; the first carrier gas is combustion-supporting gas, and the second carrier gas is combustion-supporting gas and/or combustible gas;
(2) and (3) carrying out microwave oxidation calcination on the combustion product to obtain superfine lanthanum oxide powder.
4. The method as claimed in claim 3, wherein the solvent of the lanthanum salt solution is a flammable solvent; the concentration of the lanthanum salt solution is 0.1-10 mol/L.
5. A method according to claim 3, characterized in that said combustion-supporting gas is air and/or oxygen; the combustible gas is hydrogen and/or methane.
6. The method of claim 3, wherein the flammable solvent comprises one or more of methanol, ethanol, acetone, and gasoline.
7. The method according to claim 3 or 6, wherein the feeding speeds of the first and third atomizing nozzles are independently 10 to 30 mL/min; the pressure of the first carrier gas is 1-3 atmospheric pressures; the feeding speeds of the second atomizing nozzle and the fourth atomizing nozzle are independently 1-20 mL/min; the pressure of the second carrier gas is 1-3 atmospheres.
8. A method according to claim 3, wherein the combustion products are drawn from the bottom of the combustion chamber by means of a cyclone, filtered through a bag filter and collected.
9. The method according to claim 3, wherein the temperature of the microwave oxidation calcination is 100 to 300 ℃ and the time is 20 to 60 min.
10. The method according to claim 3, wherein the particle size of the ultrafine lanthanum oxide powder is 0.01 to 1.0 μm.
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|---|---|---|---|---|
| CN113753937A (en) * | 2021-08-27 | 2021-12-07 | 淮南前景新材料有限公司 | Method for preparing micro-nano lanthanum oxide by combustion-calcination |
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| CN114247439A (en) * | 2021-12-02 | 2022-03-29 | 内蒙合成化工研究所 | Rare earth catalytic material for composite solid propellant, preparation and evaluation method and application |
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