CN114684854A - Preparation method of nano vanadium trioxide - Google Patents
Preparation method of nano vanadium trioxide Download PDFInfo
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- CN114684854A CN114684854A CN202210325692.1A CN202210325692A CN114684854A CN 114684854 A CN114684854 A CN 114684854A CN 202210325692 A CN202210325692 A CN 202210325692A CN 114684854 A CN114684854 A CN 114684854A
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- C—CHEMISTRY; METALLURGY
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention particularly relates to a preparation method of nano vanadium trioxide, belonging to the technical field of phase change materials, and the method comprises the following steps: mixing a vanadium source and an organic acid to obtain a mixture; drying the mixture to obtain a precursor; calcining the precursor to obtain nano vanadium trioxide; the method has the characteristics of low raw material cost, simple equipment, short preparation period, easiness in mass preparation, environmental friendliness and good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of phase-change materials, and particularly relates to a preparation method of nano vanadium trioxide.
Background
Vanadium trioxide is a phase-change material, and the resistivity, the absorptivity, the reflectivity and the like of the vanadium trioxide are greatly changed after phase change. Due to the characteristics, the catalyst is widely applied to the fields of temperature sensors, catalysts, novel electronic components and the like. With the rapid progress of science and technology, the application of vanadium trioxide is wider and wider, and the market demand is huge.
However, the preparation of vanadium trioxide is still in the laboratory stage at present, mainly because 1, the manufacturing cost is high; 2. vanadium is a multi-valence oxide, and the difficulty in preparing pure-valence vanadium oxide is high. In conclusion, the preparation method of the nano vanadium trioxide powder is complex, the cost is high, and the industrial production is difficult to realize. And the vanadium trioxide powder prepared by the existing preparation method is thick and uneven in particle, and cannot reach the nano level easily. For example, Chinese patent application CN 112811467A V2O3A method for preparing nanoparticles. The scheme is as follows: firstly, dissolving a vanadium source and a sulfur source in absolute ethyl alcohol, uniformly stirring at room temperature, carrying out solvent thermal reaction to obtain a vanadium sulfide precursor, washing the product, and freeze-drying; then calcining the vanadium sulfide precursor in a tube furnace under inert atmosphere, and grinding to obtain V2O3And (3) nanoparticles. Because the sulfur source used in the experimental scheme is a toxic substance and the dosage is large, the generated waste is difficult to treat; the experimental steps are too complex, and the experimental period is long; high cost, and greatly limit the nanometer V2O3Industrial production of (5).
Disclosure of Invention
The application aims to provide a preparation method of nano vanadium trioxide, which aims to solve the problem that the raw materials for preparing the vanadium trioxide at present have toxicity.
The embodiment of the invention provides a preparation method of nano vanadium trioxide, which comprises the following steps:
mixing a vanadium source and an organic acid to obtain a mixture;
drying the mixture to obtain a precursor;
calcining the precursor to obtain nano vanadium trioxide;
wherein the vanadium source and the organic acid are both solids, and the mixing is dry mixing.
Optionally, the vanadium source includes at least one of vanadium dioxide, vanadium pentoxide, and ammonium metavanadate.
Optionally, the solid organic acid comprises at least one of citric acid, tartaric acid and oxalic acid.
Optionally, the molar ratio of the vanadium source to the organic acid is 1: 0.2-6.
Optionally, the drying the mixture to obtain a precursor specifically includes:
and drying the mixture to enable the mixture to reach a set humidity, so as to obtain the precursor.
Optionally, the drying temperature is 40-100 ℃, and the drying time is 1-8 h.
Optionally, the calcining the precursor to obtain nano vanadium trioxide specifically includes:
and calcining the precursor to enable the precursor to react to obtain the nano vanadium trioxide.
Optionally, the calcining temperature is 200-800 ℃, and the calcining time is 0.5-3 h.
Optionally, the calcining atmosphere is nitrogen, argon, a mixed gas of nitrogen and oxygen or a mixed gas of argon and oxygen; the gas flow rate of the calcining atmosphere is 10mL/min-200 mL/min.
Optionally, the particle size of the nano vanadium trioxide is 20nm-1000 nm.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
according to the preparation method of the nano vanadium trioxide, provided by the embodiment of the invention, the precursor is obtained through dry mixing and drying, and then the nano powder of the vanadium trioxide is obtained through a calcining method, so that all the used raw materials are nontoxic, the problem that the raw materials for preparing the vanadium trioxide at present have toxicity is solved, and further, the preparation method of the nano vanadium trioxide has a good industrial application prospect.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow chart of a method provided by an embodiment of the present invention;
FIG. 2 is an X-ray diffraction pattern of the precursor provided in example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the product provided in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of a product provided in example 1 of the present invention;
fig. 5 is a scanning electron microscope image of a product provided in embodiment 2 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
according to a typical embodiment of the present invention, there is provided a method for preparing nano vanadium trioxide, the method comprising:
s1, mixing a vanadium source and an organic acid to obtain a mixture;
in some embodiments, the source of vanadium may be selected from at least one of vanadium dioxide, vanadium pentoxide, ammonium metavanadate.
In some embodiments, the organic acid is a solid organic acid, which may be selected from at least one of citric acid, tartaric acid, oxalic acid.
In some embodiments, the molar ratio of the vanadium source and the organic acid is 1: 0.2-6.
Controlling the molar ratio of the vanadium source to the organic acid to be 1: 0.2 to 6, and if the ratio is too large, it is difficult to reduce the high valence vanadium; if the ratio is too small, the reduction may be excessive, and the economic efficiency may be low.
Specifically, weighing a mixture of 1: (0.2-6) adding raw materials in a proper proportion into a beaker, and stirring for 5-20 minutes by using a glass rod to basically and uniformly mix the raw materials to obtain a mixture.
S2, heating and drying the mixture to obtain a precursor;
in some embodiments, the temperature of the heat drying is 40 ℃ to 100 ℃, and the temperature of the heat drying is 1 to 8 hours.
The temperature of the oven and the reaction time directly influence the reaction degree, and in the application, the temperature of heating and drying is controlled to be 40 DEG C
The temperature is 100 ℃ below zero for 1 to 8 hours.
Specifically, the obtained mixture is placed into an oven with the temperature of 40-100 ℃, and is kept for 1-8 hours until a sample is dried, so that the precursor can be obtained.
And S3, calcining the precursor to obtain the nano vanadium trioxide.
In some embodiments, the temperature of the calcination is from 200 ℃ to 800 ℃ and the time of the calcination is from 0.5h to 3 h.
The applicant has found that the calcination temperature and time affect the purity and particle size of the product, so that the calcination temperature is controlled in the range of 200 ℃ to 800 ℃ for 0.5h to 3h in the present application.
In some embodiments, the atmosphere of calcination is a flowing atmosphere, and the atmosphere of calcination is nitrogen, argon, or a mixture thereof with oxygen. The applicant found that: the gas concentration directly affects the reaction system, so in the present application, the gas concentration of the atmosphere is controlled to be 10mL/min-200 mL/min.
Specifically, the precursor is calcined for 0.5-3 hours at 200-800 ℃ in a flowing atmosphere of a specific gas, the gas type and concentration are cooled to room temperature, and a final product is obtained.
The method obtains the precursor by a dry mixing method, then obtains the vanadium trioxide nano powder by a one-step calcining method, has the characteristics of high product purity, good crystallinity and small particles, has the characteristics of low raw material cost, simple equipment, short preparation period, easiness in mass preparation and environmental friendliness, and has good industrial application prospect.
According to another exemplary embodiment of the present invention, a nano vanadium trioxide is provided, wherein the nano vanadium trioxide is prepared by the method for preparing nano vanadium trioxide.
In some embodiments, the nano vanadium trioxide has a particle size of 20nm to 1000 nm.
The preparation method of nano vanadium trioxide of the present application will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 8.303g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 60 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 1 hour at 500 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Example 2
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 16.606g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 80 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (200ml/min) to be calcined for 2 hours at 800 ℃, and the temperature is cooled to room temperature, thus obtaining a relatively pure vanadium trioxide powder sample.
Example 3
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 12.606g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 60 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 1 hour at 500 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Example 4
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 37.818g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 60 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 1 hour at 500 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Example 5
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 8.303g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 40 ℃, keeping for 8 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 3 hours at 200 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Example 6
A method for preparing nano vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 8.303g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 100 ℃, keeping for 1 hour, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 0.5 hour at 800 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Comparative example 1
A preparation method of vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 8.303g of oxalic acid dihydrate were weighed into a beaker, and stirred with a glass rod for 10 minutes to mix them uniformly. And (3) putting the beaker into an oven at 60 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 1 hour at 1000 ℃, and the temperature is cooled to room temperature, thus obtaining the nano vanadium trioxide powder sample.
Comparative example 2
A preparation method of vanadium trioxide comprises the following steps:
5.849g of ammonium metavanadate and 8.303g of oxalic acid dihydrate were weighed out and added to a beaker, and stirred with a glass rod for 10 minutes to be mixed uniformly. And (3) putting the beaker into an oven at 60 ℃, keeping for 5 hours, completely drying the reactant, and taking out to obtain the precursor. Then, the precursor is put into a tube furnace with flowing nitrogen atmosphere (50ml/min) to be calcined for 1 hour at the temperature of 150 ℃, and the temperature is cooled to the room temperature, thus obtaining the nano vanadium trioxide powder sample.
Experimental example:
the vanadium trioxide obtained in examples 1 to 6 and comparative examples 1 to 2 were examined and the results are shown in the following table.
As can be seen from the table above, the powder obtained in 6 examples has smaller particle size and higher purity, wherein the effect of example 1 is best, the particle size is 50nm-200nm, and the purity reaches 99%. As can be seen from comparison of the comparative example and the examples, when the calcination temperature is out of the range claimed in the present application, the resulting powder has a coarse particle size or a low purity.
Detailed description of the drawings 2-5:
as shown in fig. 2, which is an X-ray diffraction pattern of the precursor in example 1, the precursor was amorphous and had no significant diffraction peak.
FIG. 3 shows the X-ray diffraction pattern of the product of example 1, which is comparable to V of JCDPS No. 84-03172O3The matching proves that the prepared product is vanadium trioxide.
As shown in FIG. 4, which is a scanning electron micrograph of the sample of example 1, it can be seen that the product is highly dispersed spherical particles of 50 to 100 nm.
As shown in fig. 5, which is a scanning electron micrograph of the sample in example 2, the sample particles become larger with an increase in temperature, and sintering occurs to some extent, as compared with example 1, and the overall effect of the powder is good.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) the method provided by the embodiment of the invention obtains the precursor by a dry mixing method, obtains the vanadium trioxide nano powder by a one-step calcining method, and has the advantages of high product purity, good crystallinity and small particles;
(2) the method provided by the embodiment of the invention has the characteristics of low raw material cost, simple equipment, short preparation period, easiness in mass preparation, greenness and environmental friendliness, and has a good industrial application prospect.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of nano vanadium trioxide is characterized by comprising the following steps:
mixing a vanadium source and an organic acid to obtain a mixture;
drying the mixture to obtain a precursor;
calcining the precursor to obtain nano vanadium trioxide;
wherein the vanadium source and the organic acid are both solids, and the mixing is dry mixing.
2. The method for preparing nano vanadium trioxide according to claim 1, wherein the vanadium source comprises at least one of vanadium dioxide, vanadium pentoxide and ammonium metavanadate.
3. The method for preparing nano vanadium trioxide according to claim 1, wherein the solid organic acid comprises at least one of citric acid, tartaric acid and oxalic acid.
4. The method for preparing nano vanadium trioxide according to claim 1, wherein the molar ratio of the vanadium source to the organic acid is 1: 0.2-6.
5. The method for preparing nano vanadium trioxide according to claim 1, wherein the drying of the mixture to obtain a precursor specifically comprises:
and drying the mixture to enable the mixture to reach a set humidity, so as to obtain the precursor.
6. The method for preparing nano vanadium trioxide according to claim 1 or 5, characterized in that the drying temperature is 40-100 ℃, and the drying time is 1-8 h.
7. The method for preparing nano vanadium trioxide according to claim 1, wherein the step of calcining the precursor to obtain nano vanadium trioxide specifically comprises:
and calcining the precursor to enable the precursor to react to obtain the nano vanadium trioxide.
8. The method for preparing nano vanadium trioxide according to claim 1 or 7, characterized in that the calcining temperature is 200-800 ℃ and the calcining time is 0.5-3 h.
9. The method for preparing nano vanadium trioxide according to claim 1, wherein the calcining atmosphere is nitrogen, argon, a mixed gas of nitrogen and oxygen or a mixed gas of argon and oxygen; the gas flow rate of the calcining atmosphere is 10mL/min-200 mL/min.
10. The method for preparing nano vanadium trioxide according to claim 1, wherein the nano vanadium trioxide has a particle size of 20nm to 1000 nm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107662946A (en) * | 2017-08-11 | 2018-02-06 | 攀枝花学院 | The preparation method of vanadium trioxide |
| CN108726572A (en) * | 2018-06-01 | 2018-11-02 | 南昌大学 | A kind of preparation method of mixed vanadium dioxide nano powder |
| CN109336176A (en) * | 2018-11-23 | 2019-02-15 | 江苏集萃工业过程模拟与优化研究所有限公司 | A kind of method that solid phase method largely prepares rutile phase hypovanadic oxide nano-powder |
| CN110857222A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of vanadium trioxide powder |
| CN112320848A (en) * | 2020-11-12 | 2021-02-05 | 齐鲁工业大学 | Preparation method of vanadium trioxide porous particles |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107662946A (en) * | 2017-08-11 | 2018-02-06 | 攀枝花学院 | The preparation method of vanadium trioxide |
| CN108726572A (en) * | 2018-06-01 | 2018-11-02 | 南昌大学 | A kind of preparation method of mixed vanadium dioxide nano powder |
| CN110857222A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of vanadium trioxide powder |
| CN109336176A (en) * | 2018-11-23 | 2019-02-15 | 江苏集萃工业过程模拟与优化研究所有限公司 | A kind of method that solid phase method largely prepares rutile phase hypovanadic oxide nano-powder |
| CN112320848A (en) * | 2020-11-12 | 2021-02-05 | 齐鲁工业大学 | Preparation method of vanadium trioxide porous particles |
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