CN116005011A - Method for preparing high-purity vanadium metal - Google Patents
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- CN116005011A CN116005011A CN202310078404.1A CN202310078404A CN116005011A CN 116005011 A CN116005011 A CN 116005011A CN 202310078404 A CN202310078404 A CN 202310078404A CN 116005011 A CN116005011 A CN 116005011A
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Abstract
The invention belongs to the technical field of nonferrous metal smelting, and particularly relates to a method for preparing high-purity vanadium metal. When the invention is used for carrying out the thermit reduction reaction, simple substance aluminum is used as a reducing agent, vanadium oxide is reduced into vanadium metal simple substance, the reacted aluminum is oxidized into aluminum oxide, a large amount of heat energy is released to enable various metal simple substances to be melted to form alloy liquid, the aluminum oxide floats on the surface of the obtained alloy liquid, the aluminum oxide is naturally separated from the metal alloy after cooling, and the aluminum oxide is removed to obtain vanadium-aluminum alloy; the calcium compound as a slag former can reduce the primary crystal temperature of aluminum oxide, provide longer impurity floating time and ensure that the purity of the obtained vanadium-aluminum alloy is higher; after the high-purity vanadium-aluminum alloy is obtained, the method extracts the metal vanadium in the vanadium-aluminum alloy in an electrolysis mode, protects the metal vanadium by a protective gas, and has high purity and high recovery rate; the invention utilizes vanadium oxide to smelt vanadium-aluminum alloy, and has low raw material cost.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal smelting, and particularly relates to a method for preparing high-purity vanadium metal.
Background
With the leap development of the scientific and technical level, the requirement of human on new materials is increasingly increased. Vanadium has many excellent physical and chemical properties, so that the use of vanadium is very wide. Vanadium can be applied to steel, and the coarsening temperature of grains is improved by refining the structure and the grains of the steel, so that the strength, the toughness and the wear resistance of the steel are improved; vanadium can also be applied to titanium alloys, which promotes the breakthrough progress of the aerospace industry. Meanwhile, high-purity and high-grade vanadium metal required in high-end fields such as aerospace and the like is in demand.
Chinese patent CN103498060a provides a method for preparing metal vanadium, in which vanadium oxide and aluminum powder are ball-milled and mixed, and then are smelted by ignition, so as to obtain metal vanadium. The method provided by the patent has the advantages of energy conservation and low cost, but vanadium and aluminum can form a metal solid solution, the content of aluminum in the obtained metal vanadium is too high, and the purity of the metal vanadium is low.
Chinese patent CN201580078650.0 provides a method for preparing metal vanadium, in which part of inorganic molten salt in an electrolytic tank is electrolyzed to produce calcium-reduced vanadium compound, and the metal vanadium is prepared. The vanadium metal obtained by the method has the advantage of high purity, but contains interstitial impurity elements such as carbon, hydrogen, oxygen and the like, so that the recovery rate of the vanadium metal is low.
Chinese patent CN111957984a provides a method for preparing metal vanadium powder, mixing vanadium trioxide, ca and CaO, then igniting to react under inert gas, obtaining a reduced material after the reaction, washing the reduced material with water, pickling and vacuum heat treating, thus obtaining the metal vanadium powder. The method provided by the patent has simple equipment and low cost, but is difficult to store in a large amount and reasonably use due to the activity of the metal Ca, and the obtained metal vanadium has a large amount of impurities.
In view of the above, there is no method for preparing high purity vanadium metal with high recovery rate in the art.
Disclosure of Invention
The invention aims to provide a method for preparing high-purity metal vanadium, which has high purity and high recovery rate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing high-purity vanadium metal, which comprises the following steps:
(1) Mixing vanadium oxide, elemental aluminum and calcium compound to carry out aluminothermic reduction reaction to obtain vanadium-aluminum alloy;
(2) Heating and melting chlorine salt to obtain chloridized electrolyte;
(3) Adding the anode and the cathode into the chloridized electrolyte, introducing chlorine, sealing, and then electrolyzing in a protective atmosphere to obtain metal vanadium;
(4) Boiling the metal vanadium in a hydrochloric acid solution to obtain high-purity metal vanadium;
the purity of the high-purity vanadium metal is not less than 99.94wt%;
the time sequence of the step (1) and the step (2) is not required.
Preferably, the vanadium oxide is vanadium pentoxide or vanadium trioxide;
when the vanadium oxide is vanadium pentoxide, the mass ratio of the vanadium oxide to the elemental aluminum is 1.685-1.977:1, and the mass ratio of the elemental aluminum to the calcium is 1:1.142-1.158;
when the vanadium oxide is vanadium trioxide, the mass ratio of the vanadium oxide to the elemental aluminum is 2.137-2.574:1, and the mass ratio of the elemental aluminum to the calcium is 1:0.835-0.974.
Preferably, the calcium compound comprises one or both of calcium fluoride and calcium oxide;
the chloride salt comprises one or two of KCl and LiCl.
Preferably, the chlorine gas has a mass concentration of 5 to 6% in the chlorinated electrolyte.
Preferably, the temperature of the chloridized electrolyte during electrolysis is 650-700 ℃.
Preferably, the temperature of the thermite reduction reaction is 1820-1920 ℃.
Preferably, the boiling time is 1 to 1.5 hours; the concentration of the hydrochloric acid solution is 24.6-25.4 wt%.
Preferably, the power supply for electrolysis is direct current, the voltage is 0.35-3.5V, and the electrolysis time is 2-20 hours.
Preferably, before the anode is added into the chloridized electrolyte, the method further comprises the steps of crushing and shot blasting the vanadium-aluminum alloy in sequence; the grain diameter of the crushed aluminum-vanadium alloy is 10-100 mm.
Preferably, the cathode is a molybdenum rod.
The invention provides a method for preparing high-purity vanadium metal. In the invention, during the thermite reduction reaction, elemental aluminum is used as a reducing agent to reduce vanadium oxide into vanadium metal elemental, the reacted aluminum is oxidized into aluminum oxide, a large amount of heat energy is released to melt various metal elemental substances (including aluminum, vanadium metal, tin, molybdenum, silicon and other impurities) to form alloy liquid, the aluminum oxide floats on the surface of the obtained alloy liquid, the aluminum oxide is naturally separated from the metal alloy after cooling, and the aluminum oxide is removed to obtain vanadium-aluminum alloy; the calcium compound as a slag former can reduce the primary crystal temperature of aluminum oxide, provide longer impurity floating time and ensure that the purity of the obtained vanadium-aluminum alloy is higher; after the high-purity vanadium-aluminum alloy is obtained, the method extracts the metal vanadium in the vanadium-aluminum alloy in an electrolysis mode, and protects the metal vanadium by a protective gas (rare gas), so that the obtained metal vanadium has high purity and high recovery rate; according to the invention, vanadium oxide is utilized to smelt vanadium-aluminum alloy, so that the raw material cost is low; the method has simple steps and convenient operation, and is suitable for industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows an electrolytic apparatus for producing high purity vanadium metal according to the present invention.
Detailed Description
The invention provides a method for preparing high-purity vanadium metal, which comprises the following steps:
(1) Mixing vanadium oxide, elemental aluminum and calcium compound to carry out aluminothermic reduction reaction to obtain vanadium-aluminum alloy;
(2) Heating and melting chlorine salt to obtain chloridized electrolyte;
(3) Adding the anode and the cathode into the chloridized electrolyte, introducing chlorine, sealing, and then electrolyzing in a protective atmosphere to obtain metal vanadium;
(4) Boiling the metal vanadium in a hydrochloric acid solution to obtain high-purity metal vanadium;
the purity of the high-purity vanadium metal is not less than 99.94wt%;
the time sequence of the step (1) and the step (2) is not required.
According to the invention, vanadium oxide, elemental aluminum and calcium compound are mixed for aluminothermic reduction reaction, and the vanadium-aluminum alloy is obtained. In the present invention, the vanadium oxide is preferably vanadium pentoxide or vanadium trioxide; the calcium compound preferably comprises one or both of calcium fluoride and calcium oxide; the purity of the vanadium oxide, elemental aluminum, and calcium compound is preferably greater than 99.00%, more preferably greater than 99.50%; when the vanadium oxide is vanadium pentoxide, the mass ratio of the vanadium oxide to the elemental aluminum is preferably 1.685-1.977:1, more preferably 1.8-1.9:1, and even more preferably 1.83-1.87:1; the mass ratio of the elemental aluminum to the calcium is preferably 1:1.142-1.158, more preferably 1:1.146-1.152, and even more preferably 1:1.148-1.150; when the vanadium oxide is vanadium trioxide, the mass ratio of the vanadium oxide to the elemental aluminum is preferably 2.137-2.574:1, more preferably 2.2-2.5:1, and even more preferably 2.3-2.4:1; the mass ratio of the elemental aluminum to the calcium is preferably 1:0.835-0.974, more preferably 1:0.85-0.93, and even more preferably 1:0.88-0.90.
In the present invention, the temperature of the thermit reduction reaction is preferably 1820 to 1920 ℃, more preferably 1860 to 1900 ℃, and the heat preservation time is preferably 12 to 24 hours, more preferably 16 to 20 hours; the equipment for the thermit reduction reaction is preferably a thermit reduction furnace; the thermite reduction reaction is preferably ignited by using a magnesium belt; preferably cooling the obtained product after the thermite reduction reaction is finished; the cooling is preferably natural cooling; in the invention, after the thermite reduction reaction product is naturally cooled, the aluminum oxide and the metal alloy are naturally divided into an upper layer and a lower layer which are adhered together, and the aluminum oxide is peeled off from the surface; the mass fraction of vanadium in the vanadium-aluminum alloy is preferably 85-98%, more preferably 93%.
The invention heats and melts chlorine salt to obtain chloridized electrolyte. In the present invention, the chloride salt preferably includes one or both of KCl and LiCl; the heating is preferably performed in a crucible; the heating device is preferably a resistance furnace; the heating temperature is preferably 650-700 ℃, more preferably 680 ℃; the temperature of the chloridized electrolyte during electrolysis is preferably 650-700 ℃, more preferably 670-690 ℃; in a specific embodiment of the invention, the chlorine salt is preferably gradually added during the heating and melting process until the depth of the melt reaches 60 to 75%, more preferably 65 to 70%, of the depth of the crucible.
After vanadium-aluminum alloy and a chloridizing electrolyte are obtained, the vanadium-aluminum alloy is used as an anode, the anode and the cathode are added into the chloridizing electrolyte, chlorine is introduced, and the metal vanadium is obtained by electrolysis under a protective atmosphere after sealing. In the present invention, before the anode is added to the chloridized electrolyte, the method preferably further comprises the steps of sequentially crushing and blasting the vanadium-aluminum alloy; the grain diameter of the aluminum-vanadium alloy obtained after crushing is preferably 10-100 mm, more preferably 30-70 mm; the shot blasting equipment is preferably a shot blasting machine; according to the method, the oxide layer and impurities on the surface of the vanadium-aluminum alloy are removed by shot blasting until no macroscopic foreign matters or films exist on the surface of the vanadium-aluminum alloy; the anode and cathode are preferably added to the chlorinated electrolyte in the following manner: putting a vanadium-aluminum alloy into a molybdenum wire mesh barrel, putting the molybdenum wire mesh barrel into a crucible, adding chlorine salt into the crucible, heating and melting, then introducing chlorine gas, inserting a cathode into the obtained chloridized electrolyte, continuously introducing protective atmosphere until the crucible is full, and then sealing; the vanadium-aluminum alloy (anode) is preferably connected with the positive electrode of the power supply through an anode wire; the cathode is preferably connected with the negative electrode of the power supply through a cathode wire; the height of the molybdenum wire net barrel is preferably 50% of the height of the crucible; the cathode is preferably a molybdenum rod; the cathode is preferably inserted at the center of the crucible. According to the invention, the molybdenum wire mesh barrel is used as a container, and the molybdenum rod is used as an electrode, so that the introduction of impurities can be avoided, and the purity of the vanadium metal can be improved.
In the present invention, the mass concentration of the chlorine gas in the chlorinated electrolyte is preferably 5 to 6%, more preferably 5.2 to 5.8%, still more preferably 5.5%; the chlorine is preferably introduced after the chlorine salt is heated and melted until the target concentration is reached; the chlorine gas introducing equipment is preferably a porcelain tube; the protective atmosphere is preferably a rare gas; the rare gas is preferably argon; the sealing device is preferably vacuumized before filling the rare gas; the rare gas filling test method is preferably as follows: an open flame was placed at the exhaust port of the crucible, and if the open flame was extinguished immediately, filling of the rare gas was confirmed. The invention can avoid the contact of ions and air in the electrolytic process to introduce oxygen, nitrogen and other gas elements, thereby improving the purity of the vanadium metal.
In the present invention, the electrolysis power source is preferably a direct current, and the electrolysis voltage is preferably 0.35 to 3.5V, more preferably 0.8 to 3.0V, further preferably 1.4 to 2.2V, and the electrolysis time is preferably 2 to 20 hours, more preferably 8 to 16 hours, further preferably 12 hours; the electrolytic voltage is preferably obtained by voltage regulator regulation; preferably, the obtained electrolysis product is washed and dried after the electrolysis is finished; the drying is preferably drying; at the position ofIn the electrolytic process of the invention, the aluminum in the vanadium-aluminum alloy firstly obtains electrons to become Al 3+ Dissolved in the melt, the metal vanadium is deposited at the lower end of the cathode molybdenum rod.
The electrolytic device used in the electrolysis of the present invention is shown in FIG. 1. As can be seen from FIG. 1, the electrolysis device comprises an anode, a cathode, a molybdenum wire net barrel, a crucible and an electrolyte, has simple equipment composition and low equipment requirement, and can reduce the investment cost of industrial production.
After the metal vanadium is obtained, the metal vanadium is boiled in a hydrochloric acid solution to obtain the high-purity metal vanadium. In the present invention, the concentration of the hydrochloric acid solution is preferably 24.6 to 25.4wt%, more preferably 25wt%; the boiling time is preferably 1 to 1.5 hours, more preferably 1.2 hours; preferably, the obtained product is washed with water after the boiling; the water for washing is preferably clear water.
The following detailed description of the embodiments of the invention is provided in connection with the accompanying drawings and examples to further illustrate the invention, but should not be construed as limiting the scope of the invention.
Example 1
A method for preparing high-purity vanadium metal, which comprises the following steps:
(1) Mixing 75.83kg of vanadium pentoxide, 45.00kg of elemental aluminum and 6.40kg of calcium fluoride uniformly by using a mixer, putting the mixed material into an aluminothermic reduction furnace, igniting by using magnesium strips, reacting the materials into a melt, cooling to obtain vanadium-aluminum alloy, crushing the obtained vanadium-aluminum alloy to a particle size of 10-100 mm, and cleaning by using a shot blasting machine;
(2) Adding the obtained vanadium-aluminum alloy into a molybdenum wire net barrel, placing the molybdenum wire net barrel in the middle of a crucible, and adding the vanadium-aluminum alloy with the height being 50% of the height of the crucible;
(3) Filling KCl into a crucible, feeding electricity to a resistance furnace, heating up, melting the mixture, controlling the furnace temperature to 650 ℃, and gradually adding KCl along with melting of the material until the height of the melt reaches 60% of the depth of the crucible;
(4) Adding chlorine by using a porcelain tube, and stopping chlorine introduction when the concentration reaches 5% after chlorine introduction;
(5) Inserting a cathode molybdenum rod, filling argon into the crucible, sealing the crucible, and starting electrolysis;
(6) Switching on a direct current power supply, shaking a voltage regulator, regulating the direct current voltage to be 0.35V, recording the voltage and the current every half hour for 2 hours, keeping the direct current voltage to be a normal control value, and stopping the furnace when the anode alloy is about to be electrolyzed and consumed;
(7) Taking out the cathode product to obtain metal vanadium, boiling the metal vanadium for 1 hour by using 25wt% of dilute hydrochloric acid, cleaning the metal vanadium by using clear water, and drying the metal vanadium to obtain the high-purity metal vanadium.
Through the steps, 23.96kg of high-purity metal vanadium is obtained, the recovery rate is 93.96%, the appearance of the obtained metal vanadium is clean, and the vanadium content is 99.94% after analysis.
Example 2
(1) Mixing 87.43kg of vanadium pentoxide, 44.24kg of elemental aluminum and 7.00kg of calcium fluoride uniformly by using a mixer, putting the mixed material into an aluminothermic reduction furnace, igniting by using magnesium strips, reacting the materials into a melt, cooling to obtain vanadium-aluminum alloy, crushing the obtained vanadium-aluminum alloy to a particle size of 10-100 mm, and cleaning by using a shot blasting machine;
(2) Adding the obtained vanadium-aluminum alloy into a molybdenum wire net barrel, placing the molybdenum wire net barrel in the middle of a crucible, and adding the vanadium-aluminum alloy with the height being 50% of the height of the crucible;
(3) Filling LiCl into a crucible, and carrying out power transmission and heating by a resistance furnace to melt the mixture, wherein the furnace temperature is controlled to be 700 ℃, and KCl is gradually added along with melting of the mixture until the height of the melt reaches 75% of the depth of the crucible;
(4) Adding chlorine by using a porcelain tube, and stopping chlorine introduction when the concentration reaches 6% after chlorine introduction;
(5) Inserting a cathode molybdenum rod, filling argon into the crucible, sealing the crucible, and starting electrolysis;
(6) Switching on a direct current power supply, shaking a voltage regulator, regulating the direct current voltage to be 3.5V, recording the voltage and the current every half hour for 20 hours, keeping the direct current voltage to be a normal control value, and stopping the furnace when the anode alloy is about to be electrolyzed and consumed;
(7) Taking out the cathode product to obtain metal vanadium, boiling the metal vanadium for 1.5 hours by using 25wt% of dilute hydrochloric acid, cleaning the metal vanadium by using clear water, and drying the metal vanadium to obtain the high-purity metal vanadium.
Through the steps, 27.40kg of high-purity metal vanadium is obtained, the recovery rate is 93.20%, the appearance of the obtained metal vanadium is clean, and the vanadium content is 99.97% after analysis.
Example 3
(1) Mixing 82.97kg of vanadium pentoxide, 44.53kg of elemental aluminum and 6.80kg of calcium fluoride uniformly by using a mixer, putting the mixed material into an aluminothermic reduction furnace, igniting by using magnesium strips, reacting the materials into a melt, cooling to obtain vanadium-aluminum alloy, crushing the obtained vanadium-aluminum alloy to a particle size of 10-100 mm, and cleaning by using a shot blasting machine;
(2) Adding the obtained vanadium-aluminum alloy into a molybdenum wire net barrel, placing the molybdenum wire net barrel in the middle of a crucible, and adding the vanadium-aluminum alloy with the height being 50% of the height of the crucible;
(3) Filling a crucible with a mixture of KCl and LiCl, heating a resistance furnace by power transmission, melting the mixture, controlling the furnace temperature to 680 ℃, and gradually adding the mixture along with melting of the material until the height of the melt reaches 70% of the depth of the crucible;
(4) Adding chlorine by using a porcelain tube, and stopping chlorine introduction when the concentration reaches 5.5% after chlorine introduction;
(5) Inserting a cathode molybdenum rod, filling argon into the crucible, sealing the crucible, and starting electrolysis;
(6) Switching on a direct current power supply, shaking a voltage regulator, regulating the direct current voltage to be 2V, recording the voltage and the current every half hour for 12 hours, keeping the direct current voltage to be a normal control value, and stopping the furnace when the anode alloy is about to be electrolyzed and consumed;
(7) Taking out the cathode product to obtain metal vanadium, boiling the metal vanadium for 1.3 hours by using 25wt% of dilute hydrochloric acid, cleaning the metal vanadium by using clear water, and drying the metal vanadium to obtain the high-purity metal vanadium.
Through the steps, 26.08kg of metal vanadium is obtained, the recovery rate is 93.50%, the appearance of the obtained metal vanadium is clean, and the vanadium content is 99.96% through analysis.
From the above examples, the method for preparing high purity vanadium metal provided by the invention has the advantages of high purity of the high purity vanadium metal of 99.94% or more, high recovery rate of 93.20% or more and low raw material cost.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. A method for preparing high purity vanadium metal, comprising the steps of:
(1) Mixing vanadium oxide, elemental aluminum and calcium compound to carry out aluminothermic reduction reaction to obtain vanadium-aluminum alloy;
(2) Heating and melting chlorine salt to obtain chloridized electrolyte;
(3) Adding the anode and the cathode into the chloridized electrolyte, introducing chlorine, sealing, and then electrolyzing in a protective atmosphere to obtain metal vanadium;
(4) Boiling the metal vanadium in a hydrochloric acid solution to obtain high-purity metal vanadium;
the purity of the high-purity vanadium metal is not less than 99.94wt%;
the time sequence of the step (1) and the step (2) is not required.
2. The method of claim 1, wherein the vanadium oxide is vanadium pentoxide or vanadium trioxide;
when the vanadium oxide is vanadium pentoxide, the mass ratio of the vanadium oxide to the elemental aluminum is 1.685-1.977:1, and the mass ratio of the elemental aluminum to the calcium is 1:1.142-1.158;
when the vanadium oxide is vanadium trioxide, the mass ratio of the vanadium oxide to the elemental aluminum is 2.137-2.574:1, and the mass ratio of the elemental aluminum to the calcium is 1:0.835-0.974.
3. The method of claim 1, wherein the calcium compound comprises one or both of calcium fluoride and calcium oxide;
the chloride salt comprises one or two of KCl and LiCl.
4. The method according to claim 1, wherein the mass concentration of the chlorine gas in the chlorinated electrolyte is 5 to 6%.
5. The method according to claim 1, wherein the temperature at which the chlorinated electrolyte is electrolyzed is 650-700 ℃.
6. The method of claim 1, wherein the thermite reduction reaction is performed at a temperature of 1820 to 1920 ℃.
7. The method according to claim 1, wherein the boiling time is 1 to 1.5 hours; the concentration of the hydrochloric acid solution is 24.6-25.4 wt%.
8. The method of claim 1, wherein the power source for electrolysis is direct current, the voltage is 0.35-3.5V, and the electrolysis time is 2-20 hours.
9. The method of claim 1, further comprising sequentially crushing and blasting the vanadium-aluminum alloy prior to adding the anode to the chlorinated electrolyte; the grain diameter of the crushed aluminum-vanadium alloy is 10-100 mm.
10. The method of claim 1, wherein the cathode is a molybdenum rod.
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