A method for preparing crude vanadium metal

Abstract

This invention relates to a method for preparing crude vanadium metal, comprising: step a) weighing V₂O₅, metallic Al, and CaO according to a preset mass ratio to obtain raw materials; step b) placing the raw materials in a reactor to trigger an aluminothermic reaction to obtain a reaction product; and step c) cooling the reaction product for 20–50 minutes, removing the furnace shell and its packing material, and waiting for the reaction product to cool to 400–1000°C before immersing it in water and further cooling it to 200°C to obtain crude vanadium metal. The method described in this invention improves the crushing performance of crude vanadium metal, making it easier to crush and process, and resulting in a lower impurity content, which is beneficial for improving the precision of subsequent preparation of refined vanadium metal.

Description

Technical Field

[0001] This invention relates to the field of iron and steel metallurgy, and specifically to a method for preparing crude vanadium. Background Technology

[0002] Vanadium, as a rare metal, has good plasticity, corrosion resistance and excellent high temperature strength, and is widely used in aerospace, steel, energy, chemical, pharmaceutical, nuclear power and other fields.

[0003] The preparation of metallic vanadium generally begins with the use of techniques such as calcothermic reduction, magnesothermic reduction, vacuum carbothermic reduction, or aluminothermic reduction to obtain crude vanadium containing certain impurities. This crude vanadium is then purified and refined using methods such as molten salt electrolysis and electron beam refining to obtain high-purity metallic vanadium. The crushing properties of the crude vanadium have a significant impact on the refining process, and current methods for preparing crude vanadium do not adequately meet the requirements for crude vanadium refining.

[0004] Therefore, existing technologies still need improvement. Summary of the Invention

[0005] In view of the shortcomings of the prior art, the present invention mainly provides a method for preparing crude vanadium metal, which can effectively improve the crushing performance of the prepared crude vanadium metal.

[0006] Specifically, the present invention provides a method for preparing crude vanadium metal, comprising:

[0007] Step a: Weigh V2O5, metallic Al and CaO according to a preset mass ratio to obtain the raw materials for preparation;

[0008] Step b: Place the raw materials in the reactor to trigger the aluminothermic reaction and obtain the reaction products;

[0009] Step c: After cooling the reaction product for 20-50 minutes, remove the furnace shell and its packing material. Wait for the reaction product to cool to 400-1000°C, then immerse it in water and continue cooling to 200°C to obtain crude vanadium metal.

[0010] In some embodiments, step a includes:

[0011] V2O5, metallic Al, and CaO were weighed in a mass ratio of 1:0.445–0.470:0.386–0.425 to obtain the raw materials for preparation.

[0012] In some embodiments, step b includes:

[0013] The raw materials are placed in a container and mixed for 5–30 minutes. After mixing, the mixture is placed in a graphite crucible, and the aluminothermic reaction is triggered by igniting an igniter to obtain the reaction products.

[0014] In some embodiments, the purity of V2O5 is not less than 99.5%, wherein the Fe content is not greater than 0.01%, the Si content is not greater than 0.01%, and the Cr content is not greater than 0.01%.

[0015] In some embodiments, the purity of metallic Al is not less than 99.7%, wherein the Fe content is not greater than 0.005% and the Si content is not greater than 0.005%.

[0016] In some embodiments, the purity of CaO is not less than 9.5%, wherein the Fe content is not greater than 0.1%, the Si content is not greater than 0.1%, and the C content is not greater than 0.1%.

[0017] In some embodiments, the particle size of V2O5 is no greater than 3 mm.

[0018] In some embodiments, the weighing weight of V2O5 ranges from 30 kg to 50 kg.

[0019] In some embodiments, the particle size of metallic Al ranges from 1 mm to 3 mm.

[0020] In some embodiments, the particle size of CaO is no greater than 80 mesh.

[0021] The beneficial effects of this invention are as follows: The method for preparing crude vanadium metal provided by this invention improves the cooling method in the process of preparing crude vanadium metal. After the raw material for preparing crude vanadium metal undergoes an aluminothermic reaction, the product is first cooled with the furnace for 20-50 minutes. The furnace shell and its filler are removed, and the furnace is dismantled when the slag surface temperature cools to 400-1000℃. The obtained crude vanadium metal is then cooled by immersion in water to below 200℃ before being removed. This improves the crushing performance of the crude vanadium metal, making it easier to crush and process. The crude vanadium metal also has a low impurity content, which is beneficial for improving the precision of subsequent preparation of refined vanadium metal. Attached Figure Description

[0022] Figure 1 A flowchart of a method for preparing crude vanadium metal provided by an embodiment of the present invention is shown. Detailed Implementation

[0023] It should be understood that the embodiments of the invention shown in the exemplary embodiments are merely illustrative. Although only a few embodiments have been described in detail in this invention, those skilled in the art will readily recognize that various modifications are possible without substantially departing from the teachings of the invention. Accordingly, all such modifications should be included within the scope of the invention. Other substitutions, modifications, variations, and deletions can be made to the design, operating conditions, and parameters of the following exemplary embodiments without departing from the spirit of the invention.

[0024] According to the present invention, a method for preparing crude vanadium metal is provided, such as... Figure 1 As shown, it includes:

[0025] Step a: Weigh V2O5, metallic Al and CaO according to a preset mass ratio to obtain the raw materials for preparation;

[0026] Step b: Place the raw materials in the reactor to trigger the aluminothermic reaction and obtain the reaction products;

[0027] Step c: After cooling the reaction product for 20-50 minutes, remove the furnace shell and its packing material. Wait for the reaction product to cool to 400-1000°C, then immerse it in water and continue cooling to 200°C to obtain crude vanadium metal.

[0028] By improving the cooling method in the preparation of crude vanadium, the product after the aluminothermic reaction of the raw material for preparing crude vanadium is first cooled with the furnace for 20-50 minutes. The furnace shell and its filler are then removed, and the furnace is dismantled when the slag surface temperature cools to 400-1000℃. The obtained crude vanadium is then cooled by immersion in water to below 200℃ before being removed. This improves the crushing performance of the crude vanadium and is beneficial for improving the precision of subsequent preparation of refined vanadium.

[0029] According to several embodiments of the present invention, step a includes:

[0030] V2O5, metallic Al, and CaO were weighed in a mass ratio of 1:0.445–0.470:0.386–0.425 to obtain the raw materials for preparation.

[0031] According to several embodiments of the present invention, step b includes:

[0032] The raw materials are placed in a container and mixed for 5–30 minutes. After mixing, the mixture is placed in a graphite crucible, and the aluminothermic reaction is triggered by igniting an igniter to obtain the reaction products.

[0033] According to several embodiments of the present invention, the purity of V2O5 is not less than 99.5%, wherein the Fe content is not greater than 0.01%, the Si content is not greater than 0.01%, and the Cr content is not greater than 0.01%.

[0034] According to several embodiments of the present invention, the purity of metallic Al is not less than 99.7%, wherein the Fe content is not greater than 0.005% and the Si content is not greater than 0.005%.

[0035] According to several embodiments of the present invention, the purity of CaO is not less than 9.5%, wherein the Fe content is not greater than 0.1%, the Si content is not greater than 0.1%, and the C content is not greater than 0.1%.

[0036] According to several embodiments of the present invention, the particle size of V2O5 is no greater than 3 mm.

[0037] According to several embodiments of the present invention, the weighing weight range of V2O5 is 30kg to 50kg.

[0038] According to several embodiments of the present invention, the particle size of metallic Al ranges from 1 mm to 3 mm.

[0039] According to several embodiments of the present invention, the particle size of CaO is no greater than 80 mesh.

[0040] In one embodiment of the present invention, a method for preparing crude vanadium metal includes the following steps:

[0041] (1) Weigh high-purity V2O5, high-purity metallic Al and high-purity CaO at a mass ratio of 1:0.445~0.470:0.386~0.425;

[0042] (2) Put the weighed materials into the material tank for mixing. The mixing time is 5 to 30 minutes.

[0043] (3) The mixed materials are loaded into a graphite crucible and the aluminothermic reaction is triggered by igniting the igniter at the top.

[0044] (4) After cooling in the furnace for 20-50 minutes, remove the furnace shell and packing material;

[0045] (5) Dismantle the furnace when the slag surface temperature has cooled to 400-1000℃;

[0046] (6) Immerse the obtained crude vanadium metal in water and cool it to below 200°C before taking it out.

[0047] In another embodiment of the present invention, the purity of V2O5 is ≥99.5%, wherein the content of Fe is ≤0.01%, the content of Si is ≤0.01%, and the content of Cr is ≤0.01%; the purity of Al is ≥99.7%, wherein the content of Fe is ≤0.005%, and the content of Si is ≤0.005%; the purity of CaO is ≥99%, the purity of Fe is ≤0.1%, the purity of Si is ≤0.1%, and the purity of C is ≤0.1%. This results in a low impurity content in the prepared crude vanadium metal, which is beneficial for the next step of refining the crude vanadium metal.

[0048] In another embodiment of the present invention, the amount of high-purity V2O5 added is controlled between 30 kg and 50 kg, the particle size of the high-purity V2O5 is ≤3 mm, the particle size of the high-purity metallic Al is in the range of 1 mm to 3 mm, and the particle size of the high-purity CaO is ≤80 mesh. This can effectively control the intensity of the aluminothermic reduction reaction while ensuring good slag-metal separation.

[0049] The prepared crude vanadium metal has a V content ranging from 91.5% to 93.5%, an Al content ranging from 0.4% to 0.7%, an Fe content ≤0.02%, a Si content ≤0.02%, a Cr content ≤0.015%, and a C content ≤0.02%.

[0050] The following are several embodiments of a method for preparing crude vanadium metal based on the present invention. By improving the cooling process, the crushing performance of the prepared crude vanadium metal is improved, and the impurity content in the prepared crude vanadium metal is reduced, which is beneficial for the subsequent preparation of refined vanadium metal.

[0051] Example 1

[0052] Weigh 30 kg of high-purity V2O5 (particle size ≤ 2 mm, purity 99.5%, of which Fe is 0.008%, Si is 0.009%, and Cr is 0.005%), 13.797 kg of high-purity metallic Al (2 mm to 3 mm, purity 99.7%, of which Fe is 0.004% and Si is 0.004%), and 11.608 kg of high-purity CaO (particle size 80 to 120 mesh, purity 99.1%, Fe is 0.08%, Si is 0.07%, and C is 0.1%) and put them into a material tank and mix for 18 minutes. Then, put the mixed material into a graphite crucible and trigger the aluminothermic reaction by igniting the igniter in the upper part. After cooling the furnace for 20 minutes, remove the furnace shell and the packing material. When the slag surface temperature cools to 900 to 1000°C, dismantle the furnace. Immerse the crude vanadium metal obtained from dismantling the furnace in water and cool it to below 100°C before taking it out. The resulting crude vanadium metal is easily broken, containing 91.9% V, 0.53% Al, 0.018% Fe, 0.017% Si, 0.014% Cr, and 0.015% C.

[0053] Example 2

[0054] Weigh 40 kg of high-purity V2O5 (particle size ≤3 mm, purity 99.6%, of which Fe is 0.009%, Si is 0.007%, and Cr is 0.008%), 18.791 kg of high-purity metallic Al (1 mm to 2 mm, purity 99.9%, of which Fe is 0.003% and Si is 0.002%), and 16.848 kg of high-purity CaO (particle size 120 to 160 mesh, purity 99.2%, Fe is 0.07%, Si is 0.09%, and C is 0.09%) and put them into a material tank and mix for 5 minutes. Then, put the mixed material into a graphite crucible and trigger the aluminothermic reaction by igniting the igniter in the upper part. After cooling the furnace for 50 minutes, remove the furnace shell and the packing material. When the slag surface temperature cools to 400 to 500°C, dismantle the furnace. Immerse the crude vanadium metal obtained from dismantling the furnace in water and cool it to below 200°C before taking it out. The obtained crude vanadium metal is easily broken, with a V content of 92.8%, an Al content of 0.68%, an Fe content of 0.017%, a Si content of 0.018%, a Cr content of 0.016%, and a C content of 0.013%.

[0055] Example 3

[0056] Weigh 50 kg of high-purity V2O5 (particle size ≤ 2 mm, purity 99.7%, of which Fe is 0.006%, Si is 0.008%, and Cr is 0.006%), 22.253 kg of high-purity metallic Al (1 mm to 2 mm, purity 99.8%, of which Fe is 0.004% and Si is 0.003%), and 21.215 kg of high-purity CaO (particle size 80 to 120 mesh, purity 99%, Fe is 0.09%, Si is 0.1%, and C is 0.08%) and put them into a material tank and mix for 30 minutes. Then, put the mixed material into a graphite crucible and trigger the aluminothermic reaction by igniting the igniter in the upper part. After cooling with the furnace for 25 minutes, remove the furnace shell and the packing material. When the slag surface temperature cools to 600 to 700°C, dismantle the furnace. Immerse the crude vanadium metal obtained from dismantling the furnace in water and cool it to below 50°C before taking it out. The resulting crude vanadium metal is easily broken, containing 93.4% V, 0.42% Al, 0.015% Fe, 0.016% Si, 0.012% Cr, and 0.011% C.

[0057] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of the present invention. Any modifications or equivalent substitutions made to the present invention without departing from the spirit and scope thereof should be covered within the protection scope of the claims of the present invention.

Claims

1. A method for preparing crude vanadium metal, characterized in that, include: Step a: Weigh V2O5, metallic Al and CaO according to a preset mass ratio to obtain the preparation raw materials, wherein the V2O5, metallic Al and CaO are weighed in a mass ratio of 1:0.445~0.470:0.386~0.425; Step b: Place the raw material in a reactor to trigger an aluminothermic reaction and obtain the reaction product; Step c: After cooling the reaction product for 20-50 minutes, remove the furnace shell and its packing material from the reactor. Wait for the reaction product to cool to 400-1000°C, then immerse it in water and continue cooling to 200°C to obtain crude vanadium metal. The purity of the V2O5 is not less than 99.5%, and the Fe content is not greater than 0.01%, the Si content is not greater than 0.01%, and the Cr content is not greater than 0.01%. The purity of the metal Al is not less than 99.7%, wherein the Fe content is not greater than 0.005% and the Si content is not greater than 0.005%. The purity of the CaO is not less than 9.5%, wherein the Fe content is not greater than 0.1%, the Si content is not greater than 0.1%, and the C content is not greater than 0.1%.

2. The method for preparing crude vanadium metal according to claim 1, characterized in that, Step b includes: The raw materials are placed in a container and mixed for 5-30 minutes. After mixing, the mixture is placed in a graphite crucible, and the aluminothermic reaction is triggered by igniting an igniter to obtain the reaction products.

3. The method for preparing crude vanadium metal according to claim 1, characterized in that, The particle size of the V2O5 is no greater than 3 mm.

4. The method for preparing crude vanadium metal according to claim 1, characterized in that, The weighing weight range of the V2O5 is 30kg to 50kg.

5. The method for preparing crude vanadium metal according to claim 1, characterized in that, The particle size of the metallic Al ranges from 1 mm to 3 mm.

6. The method for preparing crude vanadium metal according to claim 1, characterized in that, The particle size of the CaO is no greater than 80 mesh.

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