CN114288942A - Preparation method of spherical vanadium pentoxide particles - Google Patents
Preparation method of spherical vanadium pentoxide particles Download PDFInfo
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- CN114288942A CN114288942A CN202111367143.2A CN202111367143A CN114288942A CN 114288942 A CN114288942 A CN 114288942A CN 202111367143 A CN202111367143 A CN 202111367143A CN 114288942 A CN114288942 A CN 114288942A
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Abstract
The invention relates to the technical field of chemical industry and discloses a preparation method of spherical vanadium pentoxide particles. Adding vanadium pentoxide powder into water to form a suspension, then adding a hydrogen peroxide solution, and stirring to form a vanadium pentoxide solution; (2) carrying out spray drying on the vanadium pentoxide solution obtained in the step (1), and granulating to obtain spherical powder; (3) and (3) roasting the spherical powder obtained in the step (2) to obtain spherical vanadium pentoxide particles. Vanadium pentoxide powder is used as a raw material, and spherical vanadium pentoxide particles with uniform particle size can be formed by performing secondary shape reconstruction on vanadium pentoxide. The method has relatively low requirement on the preparation temperature and simple process flow; the obtained product has high sphericity, and the particle size of the obtained product can be controlled to be 1-2 mu m.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of spherical vanadium pentoxide particles.
Background
V2O5The method has the advantages of large theoretical capacity, high discharge platform, convenient synthesis, low cost and the like, and is widely concerned. However, there are some disadvantages, such as poor structural stability and low electron ion conductivity, so Li is used in the charging and discharging process+Can cause V2O5Collapse of the layered structure, thereby preventingHampering its practical application. The spheroidization of vanadium pentoxide particles can effectively overcome V2O5The above-mentioned disadvantages of the materials. Also, the spherical vanadium pentoxide particles can be used as catalysts, electrochemical devices, antistatic coatings, and active materials for sensors and secondary batteries. Therefore, the spherical vanadium pentoxide particles have great application potential. However, in the prior art, the technology for preparing spherical vanadium pentoxide particles by using vanadium pentoxide powder as a raw material is less, the preparation process is complex, the sphericity is not high, and the particle size is not uniform.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of spherical vanadium pentoxide particles. According to the method, vanadium pentoxide powder is used as a raw material, and spherical vanadium pentoxide particles with uniform particle sizes can be formed by performing secondary shape reconstruction on vanadium pentoxide.
In order to achieve the above object, the present invention provides a method for preparing spherical vanadium pentoxide particles, comprising the steps of:
(1) adding vanadium pentoxide powder into water to form a suspension, then adding a hydrogen peroxide solution, and stirring to form a transparent brick-red vanadium pentoxide solution;
(2) carrying out spray drying on the vanadium pentoxide solution obtained in the step (1), and granulating to obtain spherical powder;
(3) and (3) roasting the spherical powder obtained in the step (2) to obtain spherical vanadium pentoxide particles.
Preferably, in the step (1), the using amount ratio of the vanadium pentoxide powder to the hydrogen peroxide solution is based on the molar ratio of the vanadium pentoxide to the hydrogen peroxide being 1: 7.1-10.8.
Preferably, in the step (1), the concentration of the hydrogen peroxide solution is 5 to 10% by mass.
Preferably, in step (1), the stirring is performed by using a magnetic stirrer.
Preferably, in the step (1), the stirring speed is 300-400 rpm, and the stirring time is 20-30 min.
Preferably, in step (2), the spray drying is fed by a peristaltic pump; preferably, the feeding speed of the spray drying is 200-300 mL/h.
Preferably, in the step (2), the air inlet temperature of the spray drying is 250-300 ℃.
Preferably, in step (3), the calcination is performed in an oxygen or air atmosphere.
Preferably, in the step (3), the roasting temperature is 400-450 ℃, and the roasting time is 4-6 h.
Preferably, in the step (3), the particle size of the obtained spherical vanadium pentoxide particles is 1-2 μm.
The invention has the following beneficial effects: vanadium pentoxide powder is used as a raw material, and spherical vanadium pentoxide particles with uniform particle size can be formed by performing secondary shape reconstruction on vanadium pentoxide. The method has relatively low requirement on the roasting temperature and simple process flow; the obtained product has high sphericity. In a preferred embodiment, 1-2 μm vanadium pentoxide particles with uniform particle size can be prepared by using a 0.7mm nozzle.
Drawings
FIG. 1 is an SEM photograph of vanadium pentoxide particles prepared in example 1;
FIG. 2 is an SEM photograph of vanadium pentoxide particles prepared in example 2;
fig. 3 is an SEM photograph of the vanadium pentoxide particles prepared in comparative example 1.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The preparation method of the spherical vanadium pentoxide particles provided by the invention comprises the following steps:
(1) adding vanadium pentoxide powder into water to form a suspension, then adding a hydrogen peroxide solution, and stirring to form a transparent brick-red vanadium pentoxide solution;
(2) carrying out spray drying on the vanadium pentoxide solution obtained in the step (1), and granulating to obtain spherical powder;
(3) and (3) roasting the spherical powder obtained in the step (2) to obtain spherical vanadium pentoxide particles.
The invention takes vanadium pentoxide powder as raw material, adds hydrogen peroxide solution to dissolve vanadium pentoxide at normal temperature to form clear and transparent brick-red vanadium pentoxide solution, and the vanadium pentoxide reacts with hydrogen peroxide to form complex (V)2[(OH)3O2]-) And carrying out spray drying and granulation to obtain spherical complex powder, and roasting to obtain spherical vanadium pentoxide particles.
In the method of the present invention, in step (1), the usage ratio of the vanadium pentoxide powder to the hydrogen peroxide solution may be based on a molar ratio of vanadium pentoxide to hydrogen peroxide of 1: 7.1-10.8, specifically, the molar ratio of vanadium pentoxide to hydrogen peroxide may be 1:7.1, 1:7.3, 1:7.5, 1:7.8, 1:8, 1:8.2, 1:8.5, 1:8.8, 1:9, 1:9.2, 1:9.5, 1:9.8, 1:10, 1:10.2, 1:10.5, or 1: 9.8. The molar ratio of the vanadium pentoxide to the hydrogen peroxide is controlled within the range, so that the vanadium pentoxide can be fully dissolved without excessively wasting the hydrogen peroxide.
In a specific embodiment, the concentration of the added hydrogen peroxide solution is not particularly required, as long as the molar ratio of vanadium pentoxide to hydrogen peroxide is 1: 7.1-10.8. For example 1:7.1, 1:7.5, 1:7.8, 1:8, 1:8.5, 1:8.8, 1:9, 1:9.5, 1:10, 1:10.5 or 1: 10.8. In a preferred embodiment, in the step (1), the concentration of the hydrogen peroxide solution may be 5 to 10 mass%, for example, 5 mass%, 5.5 mass%, 6 mass%, 6.5 mass%, 7 mass%, 7.5 mass%, 8 mass%, 8.5 mass%, 9 mass%, 9.5 mass%, or 10 mass%.
In the method of the present invention, the stirring may be performed by a stirring means commonly used in the art. In a specific embodiment, in step (1), the stirring may be performed using a magnetic stirrer. The hydrogen peroxide is fully contacted with the vanadium pentoxide by stirring, so that the vanadium pentoxide is quickly and fully dissolved.
In particular embodiments, in step (1), the stirring rate may be 300 to 400 rpm, such as 300 rpm, 320 rpm, 340 rpm, 360 rpm, 380 rpm, or 400 rpm; the stirring time can be 20-30 min, such as 20min, 22min, 24min, 26min, 28min or 30 min.
In the process of the present invention, the feeding manner of the spray drying may be selected conventionally in the art. In a specific embodiment, in step (2), the spray drying may be fed using a peristaltic pump.
In a preferred embodiment, in step (2), the feed rate of the spray drying is 200 to 300mL/h, for example 200mL/h, 210mL/h, 220mL/h, 230mL/h, 240mL/h, 250mL/h, 260mL/h, 270mL/h, 280mL/h, 290mL/h or 300 mL/h.
In a specific embodiment, in the step (2), the air inlet temperature of the spray drying may be 250 to 300 ℃, for example, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃. Controlling the temperature of the air inlet of the spray drying within the range can generate spherical vanadium pentoxide.
In the method of the present invention, in order to obtain pentavalent vanadium (vanadium pentoxide) having strong oxidizing property, in step (3), the calcination is performed in an oxygen or air atmosphere.
In a specific embodiment, in the step (3), the baking temperature is 400 to 450 ℃, for example 400 ℃, 405 ℃, 410 ℃, 415 ℃, 420 ℃, 425 ℃, 430 ℃, 435 ℃, 440 ℃, 445 ℃ or 500 ℃; the roasting time is 4-6 h, such as 4h, 4.5h, 5h, 5.5h or 6 h. In the method of the present invention, the firing temperature and the firing time are controlled within the ranges, and pure phase spherical vanadium pentoxide can be generated.
By adopting the method, spherical vanadium pentoxide particles with uniform particle size can be obtained. In the step (3), the particle size of the obtained spherical vanadium pentoxide particles is 1-2 μm.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
Example 1
Taking 5g of vanadium pentoxide powder, forming a suspension in 100ml of deionized water, then adding a hydrogen peroxide solution with the concentration of 10 mass% according to the molar ratio of the added vanadium pentoxide to the hydrogen peroxide of 1:7.1, stirring the feed liquid by using a magnetic stirrer, wherein the stirring speed is 300 revolutions per minute, the stirring time is 25min, and forming a vanadium pentoxide solution in the deionized water; feeding the material by a peristaltic pump for a spray dryer at the speed of 200mL/h, controlling the temperature of an air inlet at 250 ℃, and blowing the material liquid to obtain spherical powder; and (3) roasting the spherical powder in a muffle furnace at the roasting temperature of 400 ℃ in an air atmosphere for 4h to obtain spherical vanadium pentoxide particles.
As seen from the SEM photograph shown in fig. 1, the vanadium pentoxide particles prepared in example 1 are spherical and have a high sphericity.
Example 2
Taking 5g of vanadium pentoxide powder, forming a suspension in 100ml of deionized water, then adding a 5 mass% hydrogen peroxide solution according to the molar ratio of the added vanadium pentoxide to the hydrogen peroxide of 1:10.8, stirring the solution by using a magnetic stirrer at a stirring speed of 400 revolutions per minute for 20min, and forming a vanadium pentoxide solution in the deionized water; feeding the material by a peristaltic pump for a spray dryer at the speed of 200mL/h, controlling the temperature of an air inlet at 300 ℃, and blowing the material liquid to obtain spherical powder; and (3) roasting the spherical powder in a muffle furnace at the roasting temperature of 450 ℃ in an air atmosphere for 6 hours to obtain spherical vanadium pentoxide particles.
As seen from the SEM photograph shown in fig. 2, the vanadium pentoxide particles prepared in example 2 were spherical and had a high sphericity.
Example 3
Taking 5g of vanadium pentoxide powder, forming a suspension in 100ml of deionized water, and then adding the vanadium pentoxide and hydrogen peroxide in a molar ratio of 1: adding a hydrogen peroxide solution with the concentration of 8 mass percent into the mixture according to the proportion of 7.1, stirring the mixture by using a magnetic stirrer, wherein the stirring speed is 350 revolutions per minute, the stirring time is 30min, and forming a vanadium pentoxide solution in deionized water; feeding the material by a peristaltic pump for a spray dryer at the speed of 300mL/h, controlling the temperature of an air inlet at 300 ℃, and blowing the material liquid to obtain spherical powder; and (3) roasting the spherical powder in a muffle furnace at the roasting temperature of 400 ℃ in an air atmosphere for 6 hours to obtain spherical vanadium pentoxide particles.
Comparative example 1
Taking 5g of vanadium pentoxide powder, forming a suspension in 100ml of deionized water, and then stirring the feed liquid by using a magnetic stirrer, wherein the stirring speed is 350 revolutions per minute, and the stirring time is 30 min; feeding the material by a peristaltic pump for the spray dryer at the speed of 300mL/h, controlling the temperature of an air inlet at 300 ℃, and blowing the material liquid to obtain spherical particles.
As can be seen from FIG. 3, in comparative example 1, no hydrogen peroxide is used for dissolution, and the particles prepared by directly blowing vanadium pentoxide powder are rice-shaped, the sphericity is not high, and the agglomeration phenomenon is serious.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A preparation method of spherical vanadium pentoxide particles is characterized by comprising the following steps:
(1) adding vanadium pentoxide powder into water to form a suspension, then adding a hydrogen peroxide solution, and stirring to form a transparent brick-red vanadium pentoxide solution;
(2) carrying out spray drying on the vanadium pentoxide solution obtained in the step (1), and granulating to obtain spherical powder;
(3) and (3) roasting the spherical powder obtained in the step (2) to obtain spherical vanadium pentoxide particles.
2. The method according to claim 1, wherein in the step (1), the ratio of the vanadium pentoxide powder to the hydrogen peroxide solution is determined by the molar ratio of the vanadium pentoxide to the hydrogen peroxide being 1: 7.1-10.8.
3. The method according to claim 1 or 2, wherein in the step (1), the concentration of the hydrogen peroxide solution is 5 to 10 mass%.
4. The method according to claim 1, wherein in step (1), the stirring is performed using a magnetic stirrer.
5. The method according to claim 1 or 4, wherein in the step (1), the stirring speed is 300-400 rpm, and the stirring time is 20-30 min.
6. The method of claim 1, wherein in step (2), the spray drying is fed using a peristaltic pump; preferably, the feeding speed of the spray drying is 200-300 mL/h.
7. The method according to claim 1, wherein in step (2), the spray-dried air inlet temperature is 250-300 ℃.
8. The method according to claim 1, wherein in step (3), the firing is performed in an oxygen or air atmosphere.
9. The method according to claim 1 or 8, wherein in the step (3), the roasting temperature is 400-450 ℃, and the roasting time is 4-6 h.
10. The method according to claim 1, wherein in the step (3), the obtained spherical vanadium pentoxide particles have a particle size of 1-2 μm.
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