Preparation method of flaky vanadium pentoxide

Abstract

The invention relates to a preparation method of flaky vanadium pentoxide, and relates to the technical field of flaky vanadium pentoxide preparation.The preparation method comprises the steps that combustion heat of converter gas and combustion-supporting gas is adopted for melting a vanadium material, and the material obtained after melting is subjected to sheet casting to obtain flaky vanadium pentoxide; wherein the combustion heat temperature is controlled to be a first temperature zone and a second temperature zone in the flowing direction of the vanadium material in the melting process; the temperature of the first temperature zone is lower than that of the second temperature zone. According to the preparation method provided by the invention, by adopting specific combustion gas configuration, stable and efficient operation of vanadium material melting is realized, efficient preparation of the flaky vanadium pentoxide is facilitated, the yield of the prepared flaky vanadium pentoxide is greater than or equal to 98.85%, and the content of V2O5 in the flaky vanadium pentoxide is greater than or equal to 98.52%.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of flaky vanadium pentoxide, and in particular to a method for preparing flaky vanadium pentoxide. Background Art

[0002] At present, vanadium pentoxide is widely used in metallurgy, chemical industry and other industries, mainly for smelting ferrovanadium and as an alloy additive, while the production of flake vanadium pentoxide is usually carried out in a melting furnace.

[0003] For example, CN111592041A discloses a melting furnace and a method for smelting vanadium pentoxide using the same, which belongs to the field of metallurgical technology. In order to make up for the shortcomings of the existing process, the present invention provides a method for smelting vanadium pentoxide using a melting furnace, comprising: adding vanadium-containing materials into the melting furnace through a feeding port, and piling them into two oblique triangular material piles leading to a discharge port; first controlling the temperature to 300-550°C for drying and dehydration; then controlling the temperature to 550-650°C for deamination and dehydration; and finally controlling the temperature to 676-800°C for vanadium oxidation and melting, and the molten material is discharged immediately after melting.

[0004] CN115218639A discloses a method for intelligently producing vanadium tablets based on an expert control system, and belongs to the technical field of vanadium production. The method for producing vanadium tablets provided by the present invention comprises the following steps: S1, the raw material ammonium polyvanadate is discharged into a flash drier for drying, and a feed amount closed-loop control system is provided to achieve stable feed amount of the flash evaporation system; S2, the dried ammonium polyvanadate is discharged into a calcining furnace for calcination, decomposition, and deamination to form a powdery material, and multiple negative pressure detection transmitters are installed; S3, the material is added into a melting furnace for melting, and cooled and crystallized to obtain a flaky vanadium pentoxide product, and multiple negative pressure detection transmitters are installed; the negative pressure detection transmitter detects the negative pressure of each process in real time, and a temperature transmitter is installed in the furnace of the melting furnace to detect the furnace temperature of the melting furnace in real time; based on fuzzy control theory, an expert control system is constructed using collected signals.

[0005] CN206203905U discloses a device for melting vanadium pentoxide by an electric furnace method, comprising a melting furnace, which is cylindrical and is provided with a melting pool and three ridges evenly distributed on the inner wall of the melting furnace, wherein the ridges are columnar, the busbars of which are parallel to the central axis of the melting furnace, and the ridges all protrude toward the center of the melting furnace; one end of the ridge is fixedly connected to the base of the melting furnace, and the other end is flush with the top of the melting furnace; the Y-shaped area surrounded by the melting furnace and the ridges is the melting pool; a plurality of columnar graphite electrodes are provided in the melting pool between the two ridges; a discharge hole is provided at the lower part of the melting furnace, and a discharge switch is provided on the discharge hole.

[0006] However, the current use of a melting furnace to prepare flake vanadium pentoxide still has problems such as poor combustion heat supply, unstable combustion, and uneven temperature field distribution during the process, resulting in poor product yield and recovery rate. Summary of the invention

[0007] In view of the problems existing in the prior art, the purpose of the present invention is to provide a method for preparing flake vanadium pentoxide to solve the problems of poor combustion heat supply, unstable combustion and uneven temperature field distribution during the preparation of flake vanadium pentoxide in a melting furnace, resulting in poor product yield and recovery rate.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] The present invention provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0010] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0011] Wherein, during the melting, the combustion heat temperature is controlled to be in a first temperature zone and a second temperature zone along the flow direction of the vanadium material; and the temperature of the first temperature zone is less than the temperature of the second temperature.

[0012] The preparation method provided by the present invention realizes stable and efficient melting of vanadium material by adopting a specific combustion gas configuration, which is beneficial to the efficient preparation of flaky vanadium pentoxide. The yield of the prepared flaky vanadium pentoxide is ≥98.85%, and the content of V2O5 in the flaky vanadium pentoxide is ≥98.52%.

[0013] As a preferred technical solution of the present invention, the flow ratio of the converter gas and the combustion-supporting gas is (4.5-5.5):1.

[0014] As a preferred technical solution of the present invention, the combustion-supporting gas includes oxygen.

[0015] As a preferred technical solution of the present invention, the vanadium material includes ammonium polyvanadate.

[0016] Preferably, the feeding rate of the vanadium material is 2-2.5 t / h.

[0017] As a preferred technical solution of the present invention, the temperature of the first temperature zone is 500-600°C.

[0018] As a preferred technical solution of the present invention, the temperature of the second temperature zone is 680-800°C.

[0019] As a preferred technical solution of the present invention, the residence time of the vanadium material in the first temperature zone is 2-3 minutes.

[0020] As a preferred technical solution of the present invention, the residence time of the vanadium material in the second temperature zone is 3-5 minutes.

[0021] As a preferred technical solution of the present invention, the melting is assisted by ultrasonic treatment.

[0022] As a preferred technical solution of the present invention, the power of the ultrasonic generator in the ultrasonic treatment is 800-1200w and the frequency is 15-30kHz.

[0023] Compared with the prior art solutions, the present invention has the following beneficial effects:

[0024] (1) The preparation method provided by the present invention significantly improves the uniformity of the temperature field during the melting process by adopting a specific combustion field configuration and cooperating with a specific ultrasonic process, thereby achieving efficient preparation of flake vanadium pentoxide. The yield of the prepared flake vanadium pentoxide is ≥98.85%, and the content of V2O5 in the flake vanadium pentoxide is ≥98.52%.

[0025] (2) In the preparation method provided by the present invention, the safety factor of the combustion process is improved by adopting a specific configuration of converter gas and combustion-supporting gas, and accurate gas control and combustion ratio are achieved to realize safe, automated and digital applications. This is an industry first and of great significance. DETAILED DESCRIPTION

[0026] To better illustrate the present invention and facilitate understanding of the technical solution of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0027] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0028] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0029] Wherein, during the melting, the combustion heat temperature is controlled to be in a first temperature zone and a second temperature zone along the flow direction of the vanadium material; and the temperature of the first temperature zone is less than the temperature of the second temperature.

[0030] In the present invention, the converter gas may be replaced by other combustible gases that meet the composition of the converter gas, such as replacing the converter gas by mixing multiple gases.

[0031] Specifically, the flow ratio of the converter gas and the combustion-supporting gas is (4.5-5.5):1, for example, it can be 4.5:1, 4.6:1, 4.7:1, 4.8:1, 4.9:1, 5:1, 5.1:1, 5.2:1, 5.3:1, 5.4:1 or 5.5:1, but is not limited to the listed values, and other values ​​not listed in this range also meet the requirements.

[0032] Specifically, the combustion-supporting gas includes oxygen.

[0033] Specifically, the vanadium material includes ammonium polyvanadate;

[0034] Specifically, the feeding rate of the vanadium material is 2-2.5 t / h, for example, 2 t / h, 2.1 t / h, 2.2 t / h, 2.3 t / h, 2.4 t / h or 2.5 t / h.

[0035] Specifically, the temperature in the first temperature zone is 500-600°C, for example, it can be 500°C, 510°C, 520°C, 530°C, 540°C, 550°C, 560°C, 570°C, 580°C, 590°C or 600°C, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0036] Specifically, the temperature in the second temperature zone is 680-800°C, for example, it can be 680°C, 690°C, 700°C, 710°C, 720°C, 730°C, 740°C, 750°C, 760°C, 770°C, 780°C, 790°C or 800°C, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0037] In the present invention, the temperature selection of the first temperature zone and the second temperature zone may be to select a single point value temperature within a limited temperature range, or to select a certain temperature range within the limited range to set the corresponding temperature zone.

[0038] Specifically, the residence time of the vanadium material in the first temperature zone is 2-3 min, for example, it can be 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min or 25 min, but is not limited to the listed values, and other values ​​not listed in the range also meet the requirements.

[0039] Specifically, the residence time of the vanadium material in the second temperature zone is 3-5 min, for example, it can be 30 min, 31 min, 32 min, 33 min, 34 min, 35 min, 36 min, 37 min, 38 min, 39 min, 40 min, 41 min, 42 min, 43 min, 44 min or 45 min, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0040] Specifically, the melting is assisted by ultrasonic treatment.

[0041] Specifically, the power of the generator in the ultrasonic treatment is 800-1200w, and the frequency is 15-30kHz.

[0042] In the present invention, the power of the generator in the ultrasonic treatment is 800-1200W, for example, it can be 800W, 850W, 900W, 950W, 1000W, 1050W, 1100W, 1150W or 1200W, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0043] In the present invention, the frequency of the generator in the ultrasonic treatment is 15-30kHz, for example, it can be 15kHz, 16kHz, 17kHz, 18kHz, 19kHz, 20kHz, 21kHz, 22kHz, 23kHz, 24kHz, 25kHz, 26kHz, 27kHz, 28kHz, 29kHz or 30kHz, but is not limited to the listed values, and other unlisted values ​​within this range also meet the requirements.

[0044] Further, in order to illustrate the excellent output effect that can be achieved by the method for preparing flaky vanadium pentoxide provided by the present invention, an actual example is used for exemplary description, as follows:

[0045] The volume percentage composition of the converter gas used in the following embodiments is: 41% carbon monoxide, 16% carbon dioxide, 0.8% oxygen, and the rest is nitrogen.

[0046] Example 1

[0047] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0048] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0049] The flow ratio of the converter gas to the combustion-supporting gas is 5:1; the combustion-supporting gas is oxygen;

[0050] The vanadium material is ammonium polyvanadate;

[0051] The combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material during the melting; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 550°C; the temperature of the second temperature zone is 700°C; the residence time of the vanadium material in the first temperature zone is 2.5 minutes; the residence time of the vanadium material in the second temperature zone is 4 minutes;

[0052] The melting is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 900w and the frequency is 20kHz.

[0053] Example 2

[0054] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0055] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0056] The flow ratio of the converter gas to the combustion-supporting gas is 5.2:1; the combustion-supporting gas is oxygen;

[0057] The vanadium material is ammonium polyvanadate;

[0058] The combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material during the melting; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 560°C; the temperature of the second temperature zone is 720°C; the residence time of the vanadium material in the first temperature zone is 2.4 minutes; the residence time of the vanadium material in the second temperature zone is 4.5 minutes;

[0059] The melting is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 1000w and the frequency is 25kHz.

[0060] Example 3

[0061] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0062] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0063] The flow ratio of the converter gas to the combustion-supporting gas is 4.6:1; the combustion-supporting gas is oxygen;

[0064] The vanadium material is ammonium polyvanadate;

[0065] The combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material during the melting; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 580°C; the temperature of the second temperature zone is 760°C; the residence time of the vanadium material in the first temperature zone is 2.2 minutes; the residence time of the vanadium material in the second temperature zone is 4 minutes;

[0066] The melting process is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 850w and the frequency is 27kHz.

[0067] Example 4

[0068] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0069] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0070] The flow ratio of the converter gas to the combustion-supporting gas is 4.8:1; the combustion-supporting gas is oxygen;

[0071] The vanadium material is ammonium polyvanadate;

[0072] The combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material during the melting; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 520°C; the temperature of the second temperature zone is 740°C; the residence time of the vanadium material in the first temperature zone is 2.6 minutes; the residence time of the vanadium material in the second temperature zone is 3.5 minutes;

[0073] The melting is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 1100w and the frequency is 18kHz.

[0074] Example 5

[0075] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0076] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0077] The flow ratio of the converter gas to the combustion-supporting gas is 4.5:1; the combustion-supporting gas is oxygen;

[0078] The vanadium material is ammonium polyvanadate;

[0079] The combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material during the melting; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 500°C; the temperature of the second temperature zone is 680°C; the residence time of the vanadium material in the first temperature zone is 3 minutes; the residence time of the vanadium material in the second temperature zone is 5 minutes;

[0080] The melting is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 800w and the frequency is 30kHz.

[0081] Example 6

[0082] This embodiment provides a method for preparing flaky vanadium pentoxide, the preparation method comprising:

[0083] The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide;

[0084] The flow ratio of the converter gas to the combustion-supporting gas is 5.5:1; the combustion-supporting gas is oxygen;

[0085] The vanadium material is ammonium polyvanadate;

[0086] During the melting, the combustion heat temperature is controlled to be a first temperature zone and a second temperature zone along the flow direction of the vanadium material; the temperature of the first temperature zone is less than the temperature of the second temperature; the temperature of the first temperature zone is 600°C; the temperature of the second temperature zone is 800°C; the residence time of the vanadium material in the first temperature zone is 2 minutes; the residence time of the vanadium material in the second temperature zone is 3 minutes;

[0087] The melting is assisted by ultrasonic treatment; the power of the ultrasonic generator in the ultrasonic treatment is 1200w and the frequency is 15kHz.

[0088] Comparative Example 1

[0089] The only difference from Example 1 is that the flow ratio of converter gas to combustion-supporting gas is 2:1.

[0090] Comparative Example 2

[0091] The only difference from Example 1 is that the flow ratio of converter gas to combustion-supporting gas is 6:1.

[0092] Comparative Example 3

[0093] The only difference from Example 1 is that the melting is not subjected to ultrasonic treatment.

[0094] The yield index and purity index of the flake vanadium pentoxide obtained in the examples and comparative examples were statistically calculated. The yield was calculated based on the vanadium content in the raw material and the product. See Table 1 for details.

[0095] Table 1

[0096] Yield <![CDATA[Content of V2O5 in flaky vanadium pentoxide]]> Example 1 98.99％ 99.12％ Example 2 99.32％ 98.66％ Example 3 99.23％ 98.89％ Example 4 99.21％ 99.26％ Example 5 98.86％ 98.64％ Example 6 98.94％ 99.22％ Comparative Example 1 86.54％ 75.35％ Comparative Example 2 85.62％ 84.36％ Comparative Example 3 83.64％ 82.32％

[0097] As can be seen from Table 1, the preparation method provided by the present invention, by adopting a specific combustion gas configuration, realizes stable and efficient melting of vanadium material, which is beneficial to the efficient preparation of flake vanadium pentoxide. The yield of the prepared flake vanadium pentoxide is ≥98.85%, and the content of V2O5 in the flake vanadium pentoxide is ≥98.52%.

[0098] It is stated that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the components selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0099] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0100] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0101] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A method for preparing flaky vanadium pentoxide, characterized in that: The preparation method comprises: The vanadium material is melted by using the combustion heat of converter gas and combustion-supporting gas, and the melted material is cast into flake vanadium pentoxide; Wherein, during the melting, the combustion heat temperature is controlled to be in a first temperature zone and a second temperature zone along the flow direction of the vanadium material; and the temperature of the first temperature zone is less than the temperature of the second temperature.

2. The preparation method according to claim 1, characterized in that The flow ratio of the converter gas to the combustion-supporting gas is (4.5-5.5):

1.

3. The preparation method according to claim 1 or 2, characterized in that: The combustion-supporting gas includes oxygen.

4. The preparation method according to any one of claims 1 to 3, characterized in that: The vanadium material includes ammonium polyvanadate; Preferably, the feeding rate of the vanadium material is 2-2.5 t / h.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The temperature of the first temperature zone is 500-600°C.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The temperature of the second temperature zone is 680-800°C.

7. The preparation method according to any one of claims 1 to 6, characterized in that: The residence time of the vanadium material in the first temperature zone is 2-3 minutes.

8. The preparation method according to any one of claims 1 to 7, characterized in that: The residence time of the vanadium material in the second temperature zone is 3-5 minutes.

9. The preparation method according to any one of claims 1 to 8, characterized in that: The melting is assisted by ultrasonic treatment.

10. The preparation method according to claim 9, characterized in that: The power of the ultrasonic generator in the ultrasonic treatment is 800-1200w and the frequency is 15-30kHz.