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CN-121976253-A - Preparation method of vanadium metal

CN121976253ACN 121976253 ACN121976253 ACN 121976253ACN-121976253-A

Abstract

The invention discloses a preparation method of metal vanadium, which comprises the following steps of firstly dehydrating and pre-treating vanadium pentoxide under a vacuum condition, then carrying out electrolytic reduction for 2-4 hours at 600-800 ℃ in NaCl-KCl mixed molten salt by taking the dehydrated vanadium pentoxide as a cathode and graphite as an anode, cooling a product after reaction, separating and washing to obtain the metal vanadium, and finally annealing for 1-3 hours at 900-1000 ℃ in a hydrogen atmosphere for purification. The method reduces vanadium pentoxide at a relatively low temperature (700-800 ℃), shortens the production period, reduces the energy consumption, solves the problems of equipment corrosion and environmental pollution by adopting a non-corrosive molten salt system, and stably prepares the metal vanadium powder with the purity of more than 99.9 percent, single phase and regular morphology through the synergistic effect of molten salt electrolysis and hydrogen annealing, and has high product quality.

Inventors

  • WU JINGHUI
  • LI DONGXIA
  • Han Huaxiong
  • ZHONG XIANG
  • WANG MINJUN

Assignees

  • 宁波创润新材料有限公司

Dates

Publication Date
20260505
Application Date
20251229

Claims (7)

  1. 1. The preparation method of the metal vanadium is characterized by comprising the following steps of: step one, pretreatment, namely dehydrating a vanadium pentoxide raw material under a vacuum condition; secondly, molten salt electrolysis, namely placing the dehydrated vanadium pentoxide into a molten salt electrolysis system as a cathode, taking graphite as an anode, and carrying out electrolytic reduction reaction, wherein the molten salt electrolysis system consists of mixed molten salt consisting of sodium chloride and potassium chloride, the temperature of the electrolytic reduction reaction is controlled to be 600-800 ℃, and the reaction time is 2-4 hours; step three, post-treatment, namely cooling the reaction product to room temperature after the reaction is finished, separating and washing to obtain metal vanadium; and step four, purifying, namely annealing the metal vanadium obtained in the step three in hydrogen atmosphere at 900-1000 ℃ for 1-3 hours to obtain the high-purity metal vanadium.
  2. 2. The method for producing vanadium metal according to claim 1, wherein in the first step, the dehydration treatment is performed at a vacuum degree of 1.0X10 -3 Pa~2.0×10 -3 Pa, a treatment temperature of 700 ℃ to 900 ℃ and a treatment time of 1 to 3 hours.
  3. 3. The method for preparing vanadium metal according to claim 1, wherein in the second step, the molar ratio of sodium chloride to potassium chloride in the mixed molten salt is 1:2-2:1.
  4. 4. The method for producing vanadium metal according to claim 3, wherein the molten salt mixture is dried at 100 ℃ to 120 ℃ for 10 hours or more before use.
  5. 5. The method of claim 1, wherein in the second step, the cathode is a stainless steel rod containing dehydrated vanadium pentoxide.
  6. 6. The method for preparing vanadium metal according to claim 1, further comprising a fifth step of grinding and sieving the annealed vanadium metal to obtain vanadium metal powder with a predetermined particle size.
  7. 7. The method for producing metallic vanadium according to claim 6, wherein the metallic vanadium powder has a purity of 99.9% or more and a particle size of 100 to 200 mesh.

Description

Preparation method of vanadium metal Technical Field The invention relates to the technical field of metal vanadium preparation, in particular to a preparation method of metal vanadium. Background The metal vanadium is used as an important strategic resource and has wide application in various fields such as aerospace, nuclear energy and battery manufacturing. At present, the industry mainly depends on traditional processes such as an aluminothermic process, a silicothermic process, a carbothermic process and the like to prepare vanadium metal, and the processes are usually carried out under severe conditions such as high temperature, high pressure and the like, so that the energy consumption is high, and the problem of serious environmental pollution is also caused. In addition, the obtained product is often limited in purity, complex in phase composition and uneven in particle size distribution, and further application of the product in the field of high-precision tips is restricted. To overcome the limitations described above, researchers have gradually turned their eyes towards electrolytic preparation techniques. The electrolytic method is considered as a potential alternative path because of the advantages of relatively mild reaction conditions, high product purity, single phase, uniform and regular particle morphology and the like. However, the existing electrolytic methods for preparing vanadium metal still face several problems. Firstly, the traditional electrolysis process mostly depends on a strong acid or alkali system as electrolyte, has serious corrosion to equipment and also has the risk of environmental pollution. Secondly, the method has low overall efficiency, the electrolysis process consumes longer time, a special electrolysis device is often required to be configured, and the equipment investment and the production cost are increased intangibly. Although the purity of the vanadium metal obtained by the prior electrolysis technology is superior to that of a part of the traditional method, the further improvement requirement of the purity of the material for high-end application is still not fully met. Therefore, developing an electrolysis process that is environment-friendly, has low equipment requirements, has higher efficiency and can produce vanadium with higher purity is a key problem to be solved in the technical field. Disclosure of Invention The invention aims at overcoming the defects in the prior art and provides a preparation method of metal vanadium. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: The preparation method of the metal vanadium comprises the following steps: step one, pretreatment, namely dehydrating a vanadium pentoxide raw material under a vacuum condition; secondly, molten salt electrolysis, namely placing the dehydrated vanadium pentoxide into a molten salt electrolysis system as a cathode, taking graphite as an anode, and carrying out electrolytic reduction reaction, wherein the molten salt electrolysis system consists of mixed molten salt consisting of sodium chloride and potassium chloride, the temperature of the electrolytic reduction reaction is controlled to be 600-800 ℃, and the reaction time is 2-4 hours; step three, post-treatment, namely cooling the reaction product to room temperature after the reaction is finished, separating and washing to obtain metal vanadium; and step four, purifying, namely annealing the metal vanadium obtained in the step three in hydrogen atmosphere at 900-1000 ℃ for 1-3 hours to obtain the high-purity metal vanadium. Further, in the first step, the vacuum degree of the dehydration treatment is 1.0X10 -3Pa~2.0×10-3 Pa, the treatment temperature is 700 ℃ to 900 ℃ and the treatment time is 1 to 3 hours. In the second step, the molar ratio of sodium chloride to potassium chloride in the mixed molten salt is 1:2-2:1. Further, the mixed molten salt is dried for more than 10 hours at 100-120 ℃ before use. Further, in the second step, the cathode is a stainless steel rod filled with dehydrated vanadium pentoxide. Further, the method further comprises a fifth step of grinding and screening the annealed vanadium metal to obtain vanadium metal powder with a preset particle size. Further, the purity of the metal vanadium powder is more than 99.9%, and the particle size is 100-200 meshes. Compared with the prior art, the invention has the following technical effects: The invention adopts an optimized fused salt electrolysis method, and can reduce the vanadium pentoxide into the metal vanadium in a high efficiency way only in 2-3 hours at a relatively low temperature of 700-800 ℃, thereby greatly shortening the production period and reducing the energy consumption. The preparation method of the metal vanadium uses a non-corrosive molten salt system to replace the traditional strong acid and strong alkali electrolyte, thereby fundamentally solving the problems of equipment corrosion and