CN112239229A - Preparation of spherical VO by ultrasonic atomization method2Method and device for preparing nano powder - Google Patents
Preparation of spherical VO by ultrasonic atomization method2Method and device for preparing nano powder Download PDFInfo
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Abstract
The invention discloses a method for preparing spherical VO by ultrasonic atomization2A method and a device for preparing nano powder relate to the field of preparation of inorganic functional materials, and the technical problem to be solved is to provide a method and a device for preparing vanadium dioxide powder. Dissolving vanadium pentoxide in water to form a vanadium-containing solution with a certain concentration; and atomizing the vanadium-containing solution, fully drying in the atmosphere of inert gas, reducing vanadium pentoxide with reducing gas under the heating condition, reacting to obtain vanadium dioxide powder, and collecting. In order to promote the dissolution of vanadium pentoxide, vanadium pentoxide is added into deionized water, heated and stirred, and then a cosolvent is added. After the vanadium-containing solution is atomized, the vanadium-containing solution firstly enters a first tube furnace for drying, then enters a buffer container, and then enters a second tube furnace for feedingCarrying out reduction reaction, and entering a collection container after the reaction; wherein the buffer container is provided with a reducing gas inlet. The method is suitable for preparing the vanadium dioxide powder with small granularity and high purity.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic functional materials, in particular to a method for preparing spherical VO by an ultrasonic atomization method2A method and apparatus for producing nano-powder.
Background
Spray pyrolysis is a common method for preparing spherical nano powder, belongs to one of high-temperature pyrolysis, and has the biggest advantages that spherical powder particles can be prepared, and the preparation of the nano powder can be continuously carried out. The principle of spray pyrolysis is that liquid is changed into small liquid drops in an ultrasonic atomization mode, the small liquid drops pass through a high-temperature area under the drive of airflow, drying is carried out instantly, and thermal decomposition is carried out, so that a target product is obtained. The size of the liquid drop of the ultrasonic atomization is generally in the submicron range, and it can be considered that the larger the molecular weight of the vanadium-containing substance in the liquid drop is, the more likely the liquid drop is to become powder with smaller particle size when decomposed after being dried under the condition of a certain liquid drop size.
At present, vanadium sources used for preparing vanadium dioxide by a spray thermal decomposition method mainly comprise tetravalent vanadium, mainly comprise vanadyl sulfate, vanadyl oxalate, vanadyl dichloride and the like, the vanadium source molecules are not large, and most prepared powder is more than 100 nm.
The patent with publication number CN 105819508A discloses a method for preparing VO by spray pyrolysis2The method for preparing (M) nano powder and film is characterized by adding ammonium metavanadate into glycol solvent, heating and stirring to finally form uniform and transparent precursor solution with concentration of 0.02-1 mol/L, atomizing the precursor into small droplets by using an atomizer, spraying the small droplets onto a heated substrate by using carrier gas, decomposing the precursor on the substrate, depositing for a period of time, and collecting the product to obtain VO2(M) a powder or a film.
The method comprises the steps of heating and stirring ammonium metavanadate and glycol solution to obtain ethylene glycol vanadyl, reducing pentavalent vanadium into tetravalent vanadyl ions by using ammonia gas decomposed by the ammonium metavanadate, and combining the tetravalent vanadyl ions with glycol to form organic alkoxide of the tetravalent vanadium. In practice, this reaction is very slow and the final concentration formed is often only 0.02mol/L, so that the overall process yield is very low.
Disclosure of Invention
The invention firstly solves the technical problem of providing a method for preparing vanadium dioxide powder with small granularity and high purity.
The technical scheme adopted by the invention for solving the technical problems is as follows: preparation of spherical VO by ultrasonic atomization method2The method for preparing the nano powder comprises the following steps:
s1, dissolving vanadium pentoxide in water to obtain a vanadium-containing solution with the vanadium element concentration of 0.05-0.20 mol/L.
Further, the method comprises the following steps: in step S1, adding vanadium pentoxide into deionized water, heating and stirring; adding cosolvent until vanadium pentoxide is completely dissolved; finally, the vanadium-containing solution is prepared by constant volume.
Specifically, the method comprises the following steps: in step S1, the cosolvent is ammonia.
Specifically, the method comprises the following steps: in step S1, adding vanadium pentoxide into deionized water according to the proportion of 4.55-18.20 g to 1.00L, and stirring for 4-8 h at the water bath temperature of 80-100 ℃; and then ammonia water is added dropwise until vanadium pentoxide is completely dissolved.
S2, atomizing the vanadium-containing solution, fully drying in the atmosphere of inert gas, reducing vanadium pentoxide with reducing gas under the heating condition, reacting to obtain vanadium dioxide powder, and collecting.
Further, the method comprises the following steps: in the step S2, after the vanadium-containing solution is atomized, the vanadium-containing solution enters a first tubular furnace for drying, then enters a buffer container, then enters a second tubular furnace for reduction reaction, and enters a collection container after the reaction; the buffer container is provided with a reducing gas inlet.
Specifically, the method comprises the following steps: in step S2, the inert gas is argon.
Specifically, the method comprises the following steps: in step S2, the reducing gas is H2CO or NH3。
More specifically: in the step S2, firstly, loading the vanadium-containing solution into an atomization container, arranging an ultrasonic atomizer in the atomization container, and continuously introducing argon into the atomization container to empty the atomization container, the first tube furnace, the buffer container and the second tube furnace; secondly, the first tube furnace and the second tube furnace start to heat up, after the temperature rises to respective target temperature, the ultrasonic atomizer is started, and reducing gas is introduced into the buffer container; wherein the ultrasonic frequency of the ultrasonic atomizer is 5MHz, the target temperature of the first tube furnace is 100-200 ℃, the target temperature of the second tube furnace is 500-600 ℃, and the dispersion liquid is filled in the collecting container; and finally, stopping atomizing by the ultrasonic atomizer, stopping the vanadium-containing solution from entering the first tubular furnace, stopping the reducing gas from entering the buffer container, closing the first tubular furnace and the second tubular furnace, finishing heat preservation, continuously introducing argon into the atomizing container, and stopping introducing argon until the first tubular furnace and the second tubular furnace are cooled to room temperature.
The invention also provides a device for implementing the method, and the device is used for preparing the spherical VO by an ultrasonic atomization method2Device of nanometer powder, including atomizing container, first tube furnace, buffer container, second tube furnace and collection container, set up ultrasonic nebulizer and inert gas entry in the atomizing container, atomizing container's export links to each other with the entry of first tube furnace, the export of first tube furnace links to each other with buffer container, buffer container still sets up the reducing gas air inlet, buffer container's exit linkage second tube furnace, the export of second tube furnace passes through below pipe connection to collection container's the liquid level, the dispersion is equipped with in the collection container, collection container still sets up the export.
Further, the method comprises the following steps: the ultrasonic atomizer is arranged at the bottom of the atomizing container, and the dispersion liquid is deionized water, absolute ethyl alcohol or other alcohol organic solvents.
The invention has the beneficial effects that: preparing spherical VO from vanadium pentoxide by ultrasonic atomization method2The method and the device for preparing the nano powder can prepare the vanadium dioxide powder with good crystallinity, uniform granularity and smaller granularity, and can obtain more excellent visible light and infrared transmittance indexes when being applied to an intelligent film. After the vanadium-containing solution is atomized, the vanadium-containing solution is fully dried in the atmosphere of inert gas and then reducedThe vanadium pentoxide is reduced by the aid of the neutral gas under a heating condition, materials are prevented from being stuck to walls during reduction reaction, reaction can be fully carried out, and vanadium dioxide with higher purity is obtained.
The solubility of vanadium pentoxide in water at normal temperature is extremely low, and heating, stirring and adding the cosolvent are both used for accelerating dissolution. After the vanadium-containing solution is atomized, the vanadium-containing solution enters a first tubular furnace for drying, then enters a buffer container, and then enters a second tubular furnace for reduction reaction. The buffer container not only has a buffer function, but also can retain certain moisture, and simultaneously can preheat reducing gas.
Drawings
FIG. 1 shows that the ultrasonic atomization method of the invention prepares spherical VO2Schematic diagram of a device for nano-powder.
FIG. 2 VO prepared by the method of the invention2XRD pattern of powder.
FIG. 3 VO prepared by the method of the present invention2SEM image of powder.
Reference numerals: an atomization container 1, an ultrasonic atomizer 11, an inert gas inlet 12, a first tube furnace 2, a buffer container 3, a reducing gas inlet 31, a second tube furnace 4, a collection container 5 and a dispersion liquid 51.
Detailed Description
The invention is further illustrated by the following figures and examples.
The invention relates to a method for preparing spherical VO by ultrasonic atomization2The device of the nano powder is used for implementing the method subject of the invention. As shown in figure 1, comprises an atomization container 1, a first tube furnace 2, a buffer container 3, a second tube furnace 4 and a collection container 5, wherein an ultrasonic atomizer 11 is arranged in the atomization container 1, and the ultrasonic atomizer 11 is preferably arranged at the bottom of the atomization container 1 and can completely atomize the vanadium-containing solution in the atomization container 1. The atomization vessel 1 is connected to an inert gas inlet 12 for introducing an inert gas, such as argon, into the ultrasonic atomizer 11. A valve is further provided at the inert gas inlet 12 to control the opening and closing of the inert gas inlet 12. The outlet of the atomizing vessel 1 is connected to the inlet of the first tube furnace 2, and the outlet of the atomizing vessel 1 is preferably arranged at the top of the atomizing vessel 1.
The export of first tubular furnace 2 links to each other with buffer container 3, and buffer container 3 sets up reducing gas inlet 31, and reducing gas inlet 31 is used for letting in reducing gas to buffer container 3, and reducing gas inlet 31 sets up control flap, and second tubular furnace 4 is connected to the exit linkage of buffer container 3. The outlet of the second tube furnace 4 is connected to a collecting container 5, the collecting container 5 is filled with the dispersion liquid 51, and the outlet of the second tube furnace 4 is connected to the position below the liquid level of the collecting container 5 through a pipeline and is used for collecting vanadium dioxide generated by the reaction. The collecting container 5 is further provided with an outlet, for example an outlet arranged at the top of the collecting container 5. The dispersion needs to satisfy two conditions: first, the vanadium dioxide produced by the reaction is not dissolved. Secondly, the function of dispersing powder particles can be achieved. Generally, the dispersion liquid is deionized water, absolute ethyl alcohol or other alcohol organic solvents.
The invention relates to a method for preparing spherical VO by ultrasonic atomization2The method for preparing the nano powder comprises the following steps:
s1, dissolving vanadium pentoxide in water to obtain a vanadium-containing solution with the vanadium element concentration of 0.05-0.20 mol/L.
The solubility of vanadium pentoxide in water at normal temperature is extremely low, so that heating and stirring are required, and the dissolution of vanadium pentoxide is accelerated by adding a cosolvent. The proportion of vanadium pentoxide to water is required to be certain. For example, adding vanadium pentoxide into deionized water according to the proportion of 4.55-18.20 g:1.00L, and stirring for 4-8 h at the water bath temperature of 80-100 ℃. The cosolvent is used for promoting the dissolution of vanadium pentoxide, and the cosolvent is added until the vanadium pentoxide is completely dissolved. And (4) considering the loss of water by heating and stirring, and finally, re-metering the volume to obtain the vanadium-containing solution with the target concentration. The co-solvent is chosen so as to avoid the introduction of impurities, for example aqueous ammonia. The cosolvent adopts ammonia water, and has the advantages that firstly, the pH value of the solution is adjusted to be in a slightly alkaline range, and the solubility of vanadium pentoxide is far higher than that of acid and neutral under an alkaline condition. And secondly, the vanadium ions and the ammonium ions have strong binding capacity, and are also beneficial to dissolving vanadium pentoxide according to the precipitation dissolution balance principle. Thirdly, ammonia water is used as a cosolvent, so that impurities cannot be brought in the subsequent thermal reduction decomposition process, if NaOH is used, sodium vanadate can be produced in the subsequent process, and ammonium vanadate can be easily decomposed.
S2, atomizing the vanadium-containing solution, fully drying in the atmosphere of inert gas, reducing vanadium pentoxide with reducing gas under the heating condition, and reacting to obtain vanadium dioxide powder.
Step S2 is described in detail below with reference to the apparatus subject of the present invention and fig. 1.
Firstly, loading a vanadium-containing solution into an atomization container 1, continuously introducing inert gas such as argon into the atomization container 1, and emptying a subsequent path, namely emptying the atomization container 1, a first tube furnace 2, a buffer container 3 and a second tube furnace 4, wherein the introduction time and the flow of the inert gas are subject to the emptying path.
After the inert gas is evacuated, the first tube furnace 2 and the second tube furnace 4 start to be heated to respective target temperatures, the ultrasonic atomizer 11 is started, and the reducing gas is introduced into the buffer container 3 through the reducing gas inlet 31. Wherein the ultrasonic frequency of the ultrasonic atomizer 11 is 5MHz, the target temperature of the first tube furnace 2 is 100-200 ℃, such as 150 ℃, and the target temperature of the second tube furnace 4 is 500-600 ℃, such as 400 ℃. The reducing gas being H2CO or NH3The reaction processes are respectively as follows: v2O5+H2＝2VO2+H2O；3V2O5+2NH3＝6VO2+3H2O+N2；V2O5+CO＝2VO2+CO2. The collecting container 5 is filled with dispersion liquid, and the purpose of collecting the generated vanadium dioxide can be realized.
And finally, when the vanadium-containing solution in the atomization container 1 is completely consumed or needs to be finished in advance, closing the ultrasonic atomizer 11, stopping the vanadium-containing solution from entering the first tubular furnace 2, stopping the reducing gas from entering the buffer container 3, closing the first tubular furnace 2 and the second tubular furnace 4, and finishing heat preservation. And continuously introducing argon into the atomization container 1 until the first tube furnace 2 and the second tube furnace 4 are cooled to room temperature, and stopping introducing the argon.
Example 1
Weighing 4.55g of vanadium pentoxide, adding deionized water to a constant volume of 1.00L, stirring at a water bath temperature of 80 ℃ for 4h, then dropwise adding ammonia water until the vanadium pentoxide is completely dissolved, re-metering the volume of the solution to 1.00L, and filling the solution into an atomization container 1 of the device shown in figure 1. Firstly, continuously introducing argon gas through an inert gas inlet 12 for 30min, continuously introducing argon gas after 30min, starting the first tubular furnace 2 and the second tubular furnace 4, opening the ultrasonic atomizer 11 when the temperature of the first tubular furnace 2 rises to 100 ℃ and the temperature of the second tubular furnace 4 rises to 500 ℃, and simultaneously introducing H into the buffer container 3 through a reducing gas inlet 312A gas. And when the vanadium-containing solution in the atomization container 1 is completely sprayed, closing the reducing gas inlet 31, closing the first tubular furnace 2 and the second tubular furnace 4, finishing heat preservation, continuing introducing argon, stopping introducing argon when the temperatures of the first tubular furnace 2 and the second tubular furnace 4 are reduced to room temperature, and collecting to obtain a vanadium dioxide target product.
FIG. 2 is VO2The XRD pattern of the powder has very high peak intensity, which indicates that the crystallinity of the product is very high, and no other phase is found, indicating that the VO is2Is M phase pure phase. FIG. 3 is VO2The SEM image of the powder shows that the vanadium dioxide powder is 20-50 nm spherical particles.
Example 2
Weighing 10.50g of vanadium pentoxide, adding deionized water to a constant volume of 1.00L, stirring at a water bath temperature of 90 ℃ for 6h, then dropwise adding ammonia water until the vanadium pentoxide is completely dissolved, re-fixing the volume of the solution to a constant volume of 1.00L, and filling the solution into an atomization container 1 of the device shown in figure 1. Firstly, continuously introducing argon gas through an inert gas inlet 12 for 30min, continuously introducing argon gas after 30min, starting the first tubular furnace 2 and the second tubular furnace 4, opening the ultrasonic atomizer 11 when the temperature of the first tubular furnace 2 rises to 150 ℃ and the temperature of the second tubular furnace 4 rises to 550 ℃, and simultaneously introducing NH into the buffer container 3 through a reducing gas inlet 313A gas. And when the vanadium-containing solution in the atomization container 1 is completely sprayed, closing the reducing gas inlet 31, closing the first tubular furnace 2 and the second tubular furnace 4, finishing heat preservation, continuing introducing argon, stopping introducing argon when the temperatures of the first tubular furnace 2 and the second tubular furnace 4 are reduced to room temperature, and collecting to obtain a vanadium dioxide target product.
Example 3
Weighing 18.20g of vanadium pentoxide, adding deionized water to a constant volume of 1.00L, stirring at a water bath temperature of 100 ℃ for 8h, then dropwise adding ammonia water until the vanadium pentoxide is completely dissolved, re-metering the volume of the solution to 1.00L, and filling the solution into an atomization container 1 of the device shown in figure 1. Firstly, continuously introducing argon gas through the inert gas inlet 12 for 30min, continuously introducing argon gas after 30min, starting the first tubular furnace 2 and the second tubular furnace 4, opening the ultrasonic atomizer 11 when the temperature of the first tubular furnace 2 rises to 200 ℃ and the temperature of the second tubular furnace 4 rises to 60 ℃, and simultaneously introducing CO gas into the buffer container 3 through the reducing gas inlet 31. And when the vanadium-containing solution in the atomization container 1 is completely sprayed, closing the reducing gas inlet 31, closing the first tubular furnace 2 and the second tubular furnace 4, finishing heat preservation, continuing introducing argon, stopping introducing argon when the temperatures of the first tubular furnace 2 and the second tubular furnace 4 are reduced to room temperature, and collecting to obtain a vanadium dioxide target product.
Claims (10)
1. Preparation of spherical VO by ultrasonic atomization method2The method for preparing the nano powder is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving vanadium pentoxide in water to prepare a vanadium-containing solution with the vanadium element concentration of 0.05-0.20 mol/L;
s2, atomizing the vanadium-containing solution, fully drying in the atmosphere of inert gas, reducing vanadium pentoxide with reducing gas under the heating condition, reacting to obtain vanadium dioxide powder, and collecting.
2. The method for preparing spherical VO by ultrasonic atomization according to claim 12The method for preparing the nano powder is characterized by comprising the following steps: in step S1, adding vanadium pentoxide into deionized water, heating and stirring; adding cosolvent until vanadium pentoxide is completely dissolved; finally, the vanadium-containing solution is prepared by constant volume.
3. The spherical VO prepared by the ultrasonic atomization method of claim 22The method for preparing the nano powder is characterized by comprising the following steps: in step S1, the cosolvent is ammonia.
4. The method for preparing spherical VO by ultrasonic atomization according to claim 32The method for preparing the nano powder is characterized by comprising the following steps: in step S1, adding vanadium pentoxide into deionized water according to the proportion of 4.55-18.20 g to 1.00L, and stirring for 4-8 h at the water bath temperature of 80-100 ℃; and then ammonia water is added dropwise until vanadium pentoxide is completely dissolved.
5. The method for preparing spherical VO by ultrasonic atomization method as claimed in any claim 1-42The method for preparing the nano powder is characterized by comprising the following steps: in the step S2, after the vanadium-containing solution is atomized, the vanadium-containing solution enters a first tubular furnace (2) for drying, then enters a buffer container (3), then enters a second tubular furnace (4) for reduction reaction, and enters a collection container (5) after the reaction; the buffer container (3) is provided with a reducing gas inlet (31).
6. The spherical VO prepared by the ultrasonic atomization method of claim 52The method for preparing the nano powder is characterized by comprising the following steps: in step S2, the inert gas is argon.
7. The spherical VO prepared by the ultrasonic atomization method of claim 52The method for preparing the nano powder is characterized by comprising the following steps: in step S2, the reducing gas is H2CO or NH3。
8. The spherical VO prepared by the ultrasonic atomization method of claim 52The method for preparing the nano powder is characterized by comprising the following steps: in the step S2, firstly, the vanadium-containing solution is filled into an atomization container (1), an ultrasonic atomizer (11) is arranged in the atomization container (1), and argon is continuously introduced into the atomization container (1) to empty the atomization container (1), the first tubular furnace (2), the buffer container (3) and the second tubular furnace (4); secondly, the first tube furnace (2) and the second tube furnace (4) start to heat up, after the temperature rises to respective target temperature, the ultrasonic atomizer (11) is started, and reducing gas is introduced into the buffer container (3) at the same time; wherein the ultrasonic frequency of the ultrasonic atomizer (11) is 5MHz, and the target temperature of the first tube furnace (2)The temperature is 100-200 ℃, the target temperature of the second tube furnace (4) is 500-600 ℃, and the dispersion liquid is filled in the collecting container (5); and finally, stopping atomizing by the ultrasonic atomizer (11), stopping the vanadium-containing solution from entering the first tubular furnace (2), stopping the reducing gas from entering the buffer container (3), closing the first tubular furnace (2) and the second tubular furnace (4) to finish heat preservation, continuously introducing argon into the atomizing container (1), and stopping introducing argon until the first tubular furnace (2) and the second tubular furnace (4) are cooled to room temperature.
9. Preparation of spherical VO by ultrasonic atomization method2The device of nanometer powder, its characterized in that: the method for implementing any one of the claims 1 to 8, comprising an atomization container (1), a first tube furnace (2), a buffer container (3), a second tube furnace (4) and a collection container (5), wherein an ultrasonic atomizer (11) and an inert gas inlet (12) are arranged in the atomization container (1), an outlet of the atomization container (1) is connected with an inlet of the first tube furnace (2), an outlet of the first tube furnace (2) is connected with the buffer container (3), the buffer container (3) is further provided with a reducing gas inlet (31), an outlet of the buffer container (3) is connected with the second tube furnace (4), an outlet of the second tube furnace (4) is connected below the liquid level of the collection container (5) through a pipeline, a dispersion liquid (51) is filled in the collection container (5), and an outlet is further arranged in the collection container (5).
10. The ultrasonic atomization method for preparing spherical VO according to claim 92The device of nanometer powder, its characterized in that: the ultrasonic atomizer (11) is arranged at the bottom of the atomizing container (1), and the dispersion liquid (51) is deionized water, absolute ethyl alcohol or other alcohol organic solvents.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023082670A1 (en) * | 2021-11-09 | 2023-05-19 | 成都先进金属材料产业技术研究院股份有限公司 | Method for directly preparing vo2 by using vanadium triisopropoxide oxide as vanadium source |
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