CN110205651B - Method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature - Google Patents
Method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature Download PDFInfo
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- CN110205651B CN110205651B CN201910624805.6A CN201910624805A CN110205651B CN 110205651 B CN110205651 B CN 110205651B CN 201910624805 A CN201910624805 A CN 201910624805A CN 110205651 B CN110205651 B CN 110205651B
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
Abstract
The invention provides a method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature, which comprises the following steps: adding vanadium oxide into electrolyte, taking a metal matrix as a cathode and an inert conductive material as an anode, performing electrodeposition at the temperature of 60-100 ℃ and under the voltage of 2.0-4.5V, and taking out a cathode product after the deposition is finished to obtain the metal vanadium, wherein the electrolyte is ionic liquid, and the solubility of the vanadium oxide in the ionic liquid is more than 10 mmol/L. The method can electrochemically reduce vanadium oxide deposition under a low temperature condition to obtain metal vanadium, can obviously shorten the preparation process of the metal vanadium, reduce the production cost and the operation temperature, reduce the corrosion of equipment, improve the current efficiency, and can realize the green production of the metal vanadium.
Description
Technical Field
The invention relates to the field of preparation of vanadium metal, in particular to a method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature.
Background
Vanadium is a rare metal with important strategic significance, and is widely applied to the top fields of steel, battery energy storage, aerospace, nuclear industry and the like due to the characteristics of high melting point, high hardness, good thermal conductivity and the like.
In recent years, the demand of vanadium metal and its alloy is increasing in various countries, and the production process at present can not meet the demand, so the development of vanadium metal extraction process is highly regarded by people. At present, vanadium oxide or vanadium chloride is mainly used as a raw material, and the preparation of the vanadium metal is realized by a metallothermic reduction method (such as calcium, aluminum, magnesium and the like), a hydrogen reduction method or a vacuum carbon reduction method, but the vanadium metal also contains carbon, oxygen, nitrogen, hydrogen and other impurity elements, and can reach the product standard by further purification and refining. In addition, the preparation of metal vanadium by molten salt electrolysis is an emerging extraction process focused by researchers in recent years. However, the molten salt electrolysis method has the problems of long process flow, high production cost, high operation temperature, serious equipment corrosion, difficult separation of impurities and the like, and greatly limits the application of the vanadium metal and the vanadium metal alloy.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, one of the objects of the present invention is to provide a method for preparing vanadium metal by reducing vanadium oxide at a relatively low temperature with low equipment requirement.
In order to achieve the above object, the present invention provides a method for preparing vanadium metal by low-temperature electrochemical reduction of vanadium oxide, which may include the steps of: adding vanadium oxide into electrolyte, taking a metal matrix as a cathode and an inert conductive material as an anode, performing electrodeposition at the temperature of 60-100 ℃ and under the voltage of 2.0-4.5V, and taking out a cathode product after the deposition is finished to obtain the metal vanadium, wherein the electrolyte is ionic liquid.
In an exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the ionic liquid may be one or a combination of two or more of eutectic solvent, imidazole-based ionic liquid and pyridine-based ionic liquid.
In one exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the electrolyte may be an electrolyte capable of dissolving vanadium oxide, and the solubility may be greater than 10 mmol/L. Further, the solubility may be greater than 30 mmol/L.
In an exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the method may further include adding an additive to the electrolyte, wherein the additive is one or a combination of two or more of malonic acid, ascorbic acid or salicylic acid.
In an exemplary embodiment of the method for preparing vanadium metal by low-temperature electrochemical reduction of vanadium oxide according to the present invention, the vanadium oxide may be one or a combination of vanadium pentoxide, vanadium trioxide, vanadium dioxide and vanadium monoxide.
In one exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the vanadium oxide may be in a powder form.
In one exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the cathode product may be a vanadium metal coating or a vanadium metal thin film attached to the surface of the metal substrate.
In an exemplary embodiment of the method for preparing vanadium metal by low-temperature electrochemical reduction of vanadium oxide according to the present invention, the method may further include a step of separating the vanadium metal coating or the vanadium metal thin film from the metal substrate to obtain vanadium metal powder.
In one exemplary embodiment of the method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention, the thickness of the vanadium metal plating layer or the vanadium metal thin film may be 10 μm to 500 μm.
Compared with the prior art, the invention has the beneficial effects that: the method can electrochemically reduce the vanadium oxide at a lower temperature to prepare the metal vanadium, can obviously shorten the preparation process, reduce the production cost and the operation temperature, can reduce the corrosion of equipment, improve the current efficiency, and can realize the green production of the metal vanadium.
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The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows a cyclic voltammogram of vanadium pentoxide reduction in choline chloride-urea according to an exemplary embodiment of the present invention, wherein the dotted line represents the choline chloride-urea electrochemical window and the solid line represents the cyclic voltammogram of vanadium pentoxide on a glassy carbon electrode;
FIG. 2 shows a diagram of a cathode product of an exemplary embodiment of the invention, wherein (a) is a taken cathode metal substrate and (b) is an SEM image of the product metal vanadium.
Detailed Description
Hereinafter, a method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to the present invention will be described in detail with reference to exemplary embodiments.
Fig. 1 shows a cyclic voltammogram of vanadium pentoxide reduction in choline chloride-urea according to an exemplary embodiment of the present invention, wherein the dotted line represents the choline chloride-urea electrochemical window and the solid line represents the cyclic voltammogram of vanadium pentoxide on a glassy carbon electrode. Fig. 2 shows a diagram of a cathode product according to an exemplary embodiment of the present invention, wherein (a) is a cathode taken out and (b) is an SEM image of metallic vanadium.
The invention provides a method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature. In one exemplary embodiment of the method for preparing vanadium metal by low-temperature electrochemical reduction of vanadium oxide according to the present invention, the method may include the steps of:
vanadium oxide is used as a raw material, added into an ionic liquid electrolyte, a metal matrix is used as a cathode, an inert conductive material is used as an anode, a cell voltage of 2.0V-4.5V is applied, and electrodeposition is carried out at the temperature of 60-100 ℃. And after the deposition is finished, taking out a cathode product to obtain a metal vanadium simple substance.
In this embodiment, the vanadium oxide may be one or a mixture of vanadium pentoxide, vanadium trioxide, vanadium dioxide and vanadium monoxide. The vanadium oxide may be in powder or bulk form. Preferably, the vanadium oxide is in a powder form. The powdery vanadium oxide is beneficial to dissolving in the electrolyte, and the preparation time of the metal vanadium can be shortened. Further, the particle size of the vanadium oxide may be 100 μm or less, and of course, the smaller the particle size, the better.
In this embodiment, the electrolyte is an ionic liquid electrolyte. The ionic liquid is a short for room-temperature ionic liquid, and is a molten salt system which is composed of specific cations and anions and is in a liquid state at room temperature or nearly room temperature. Compared with other solvents, the ionic liquid has the excellent physicochemical properties of small volatility, high thermal stability, wide liquid range, wide electrochemical window, capability of dissolving a plurality of organic matters and inorganic matters and the like. The ionic liquid can be used as a solvent to dissolve vanadium oxide, and can provide a completely different reaction environment from the traditional solvent, so that the chemical reaction which occurs in the ionic liquid can obtain completely different results from the traditional chemical reaction. In the aspect of vanadium oxide electrolytic reduction, the ionic liquid has a wider electrochemical window, and metal vanadium and alloy which can be obtained only by electrolysis in high-temperature molten salt can be obtained at room temperature without strong corrosivity like the high-temperature molten salt; meanwhile, the ionic liquid has good conductivity and relatively negative reduction potential, so that the vanadium metal and the alloy can be obtained by electrolysis at room temperature without side reaction.
The electrolyte may be a eutectic solvent, an imidazole ionic liquid, or a pyridine ionic liquid. For the traditional molten salt electrolysis method for preparing the metal vanadium, molten salts such as calcium chloride and the like are used as electrolyte. Fused salts such as calcium chloride and the like have high melting points, and need to be externally applied with high temperature, which causes huge energy consumption and serious equipment corrosion. According to the invention, eutectic solvent, imidazole ionic liquid or pyridine ionic liquid and other ionic liquids are used as electrolyte, so that vanadium metal can be obtained by electrochemical reduction at a lower temperature, and energy consumption can be saved. For the eutectic solvent, the eutectic solvent has low price, is stable to water and air, has low requirements on equipment and has good dissolving capacity on vanadium oxide. For imidazole ionic liquid or pyridine ionic liquid, the electrochemical window cross of the imidazole ionic liquid or pyridine ionic liquid is wide, so that a larger cell voltage can be applied in the electrolytic process, and the reduction speed of vanadium oxide can be accelerated.
In this embodiment, the electrolyte may be an electrolyte capable of dissolving vanadium oxide. In the case of an electrolyte capable of dissolving vanadium oxide, metallic vanadium can be precipitated on the cathode by applying an electric potential. The solubility of the electrolyte capable of dissolving vanadium oxide needs to be more than 10mmol/L, for example, the solubility can be more than 25mmol/L, and for example, the solubility can be 100mmol/L or 56 mmol/L. For electrolytes with low solubility or incapable of dissolving vanadium oxide, the vanadium metal is difficult to deposit on the cathode or even incapable of depositing on the cathode, and may cause the product to contain low-valence vanadium oxide, resulting in impure product. The higher the solubility of the electrolyte is, the higher the concentration of vanadium ions in the solution is, and in the electrodeposition process, the higher the concentration of vanadium ions on the surface of the cathode is, the precipitation potential of the metal vanadium can be shifted positively, and the deposition speed is accelerated. The inventor researches and discovers that when the solubility of vanadium oxide in the ionic liquid is more than 30mmol/L, the vanadium oxide can be better reduced by the temperature and the voltage which are set, and less vanadium oxide impurities are detected in the product. The electrolyte can be choline chloride-urea or choline chloride-malonic acid and the like. For example, as shown in fig. 1, choline chloride-urea has a wider electrochemical window than the reduction potential of vanadium pentoxide. The reduction peaks C1 and C2 can be inferred as the reduction of vanadium pentoxide, and the vanadium in the vanadium pentoxide reaches from 5 to 3 valences and then 0 valences to obtain the metal vanadium. In the figure, a1 represents the oxidation peak, the ordinate represents the current, and the abscissa represents the potential in volts relative to the silver reference electrode.
In this embodiment, the electrolyte may also be an ionic liquid with a large long chain. The large long chain ionic liquid can dissolve vanadium oxide more easily.
In this embodiment, the electrolysis temperature may be 60 to 100 ℃. Setting the electrolysis temperature ensures that the vanadium oxide can be reduced in the electrolyte of the invention. The set temperature is low by 60 ℃, the reduction efficiency is low, the reduction of the vanadium oxide is incomplete, and the product is mixed with low-valence oxides; the set temperature is higher than 100 ℃, which causes decomposition of the electrolyte and increases energy consumption. Further, the electrolysis temperature may be 65 to 95 ℃, further, 72 to 90 ℃, for example, 80 ℃.
In this embodiment, in order to further increase the solubility of the electrolytic solution, increase the electrolytic efficiency and the production efficiency, an additive may be added to the electrolytic solution. The additive may be malonic acid, ascorbic acid, salicylic acid, or the like, thereby improving the solubility of the vanadium oxide in the eutectic solvent and the electrolysis efficiency. Of course, the additive of the present invention is not limited thereto, and any additive can be used which can improve the electrolysis efficiency of vanadium oxide.
In this embodiment, the cell voltage of the electrolysis may be 2.0V to 4.5V. The voltage is set in consideration of the reduction potential of the vanadium ions and the decomposition voltage of the electrolyte. In an actual electrodeposition process, the cell voltage applied must be greater than the voltage required for the reduction of vanadium ions to vanadium metal and must be less than the voltage at which the electrolyte decomposes. The cell voltage may be adjusted according to the raw material and the electrolyte used. For example, a larger cell voltage can be suitably used when vanadium pentoxide is used as a raw material and an ionic liquid having a wider electrochemical window is used as an electrolyte.
In this embodiment, the metal substrate may be a metal substrate such as a copper sheet, a stainless steel sheet, a nickel sheet, or a titanium sheet. The inert conductive material may be a graphite-based electrode, such as a graphite sheet, a graphite rod, a platinum sheet, or the like.
In this embodiment, the cathode product may be a metal vanadium coating or a metal vanadium film attached to the surface of the metal substrate. However, when vanadium metal powder is required, the metal vanadium plating or the metal vanadium thin film needs to be separated from the metal substrate. For example, the material may be scraped directly from the metal substrate with a tool. The thickness of the obtained metal vanadium plating layer or the metal vanadium film can be 10-500 μm, and further can be 10-200 μm. As shown in fig. 2(a), metal vanadium is deposited on the metal base copper by using the metal base copper as a cathode, so as to form a vanadium plating layer. 2(b) is a surface needle and micro-topography graph of the 2(a) vanadium coating, wherein MAG in the graph represents magnification; WD represents the working distance and the objective focal length; det denotes the detector category.
Exemplary embodiments of the present invention will be described in further detail below with reference to specific examples.
Example 1
Adding vanadium pentoxide powder into choline chloride-urea, taking a copper sheet as a cathode and a graphite rod as an anode, and carrying out electrodeposition under the conditions that the temperature is 62 ℃ and the voltage is 2.1V. And after the deposition is finished, taking out a cathode product to obtain the metal vanadium.
Example 2
Adding vanadium trioxide powder into choline chloride-malonic acid, and carrying out electrodeposition by taking a nickel sheet as a cathode and a platinum sheet as an anode under the conditions of a temperature of 98 ℃ and a voltage of 4.3V. And after the deposition is finished, taking out a cathode product to obtain the metal vanadium.
Example 3
Adding vanadium monoxide powder into choline chloride, taking a nickel sheet as a cathode and a platinum sheet as an anode, and carrying out electrodeposition under the conditions of temperature of 78 ℃ and voltage of 3.1V. And after the deposition is finished, taking out a cathode product to obtain the metal vanadium.
In conclusion, the method can electrochemically reduce the vanadium oxide at low temperature to obtain the metal vanadium, can obviously shorten the preparation process, reduce the production cost and the operation temperature, reduce the corrosion of equipment, improve the current efficiency, and can realize the green production of the metal vanadium.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing vanadium metal by low-temperature electrochemical reduction of vanadium oxide is characterized by comprising the following steps:
adding vanadium oxide into electrolyte, taking a metal matrix as a cathode and an inert conductive material as an anode, performing electrodeposition at the temperature of 60-100 ℃ and under the voltage of 2.0-4.5V, and taking out a cathode product after the deposition is finished to obtain metal vanadium, wherein the electrolyte is ionic liquid, the solubility of the vanadium oxide in the ionic liquid is more than 30mmol/L, and the method further comprises adding an additive into the electrolyte, wherein the additive is one or the combination of more than two of malonic acid, ascorbic acid or salicylic acid.
2. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 1, wherein the ionic liquid is one or a combination of more than two of eutectic solvent, imidazole ionic liquid and pyridine ionic liquid.
3. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 1, wherein the vanadium oxide is one or more of vanadium pentoxide, vanadium trioxide, vanadium dioxide and vanadium monoxide.
4. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 1, wherein the vanadium oxide is in a powder form.
5. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 1, wherein the cathode product is a vanadium metal coating or a vanadium metal film attached to the metal substrate.
6. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 5, further comprising the step of separating the vanadium metal coating or vanadium metal film from the metal substrate to obtain vanadium metal powder.
7. The method for preparing vanadium metal by electrochemically reducing vanadium oxide at low temperature according to claim 5, wherein the thickness of the vanadium metal coating or the vanadium metal film is 10 μm to 500 μm.
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| CN115722239B (en) * | 2022-12-07 | 2024-04-09 | 攀钢集团钒钛资源股份有限公司 | Method for preparing vanadium phosphorus oxide catalyst with assistance of eutectic solvent and application of method |
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| CN101649471B (en) * | 2009-09-23 | 2013-06-12 | 攀钢集团研究院有限公司 | Method for producing high purity vanadium metal |
| CN101994128A (en) * | 2010-11-26 | 2011-03-30 | 昆明理工大学 | Method for preparing Al-Ti alloy or plated Al-Ti alloy by low-temperature electrolytic deposition of ionic liquid |
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