Method for separating niobium and titanium from each other by electrolysis using soluble anode

Abstract

The application discloses a method for separating metal niobium and titanium by using a soluble anode electrolysis. The method comprises the following steps: mixing metal niobium oxide, metal titanium oxide and graphite according to a set molar ratio to prepare a soluble anode; taking a first graphite electrode as a first cathode to form a first electrolysis system together with the soluble anode and a fused salt electrolyte; setting electrolysis temperature and electrolysis voltage of the first electrolysis system to perform electrolysis; in the electrolysis process, the metal niobium oxide in the soluble anode is converted into niobium ions and is reduced into metal niobium on the surface of the first graphite electrode; taking a second graphite electrode as a second cathode to form a second electrolysis system together with the soluble anode and the fused salt electrolyte; setting electrolysis temperature and electrolysis voltage of the second electrolysis system to perform electrolysis; in the electrolysis process, the metal titanium oxide in the soluble anode is converted into titanium ions and is reduced into metal titanium on the surface of the second graphite electrode.

Description

Technical Field

[0001] This invention belongs to the field of electrochemical metallurgy technology, specifically relating to a method for separating metallic niobium and titanium by electrolysis using a soluble anodic electrode. Background Technology

[0002] With the rapid development of industrial technology, the industrial demand for niobium is constantly increasing. Metallic niobium has excellent ductility, heat resistance, and corrosion resistance, making it an indispensable key metal material in the development of modern high-tech industries. It is widely used in the research and manufacturing of emerging technologies in various fields, such as aerospace, machinery, electronics, and atomic energy.

[0003] The Bayan Obo mining area in my country has proven Nb₂O₅ resources of up to 6.6 million tons, indicating abundant reserves. However, niobium and titanium are widely co-occurring isomorphously in niobium-bearing ore phases. These two elements have similar chemical properties, similar oxide chemical properties, and almost identical ionic radii, making separation of niobium and titanium difficult during beneficiation. Common methods for niobium-titanium separation include precipitation separation, liquid-liquid extraction, and traditional selective smelting reduction. However, liquid-liquid extraction has limitations such as high cost, difficulty in operational control, and low product purity. Traditional selective smelting reduction requires extremely stringent conditions regarding reduction temperature, slag composition, and cooling regime, and it is difficult to achieve high-level separation of niobium and titanium in the Bayan Obo mine to obtain high-purity metals. Furthermore, niobium-titanium carbides easily cause slag viscosity and even splashing, resulting in low niobium and titanium yields. Therefore, there is an urgent need to improve traditional approaches, develop new processes, and find an advanced method for niobium-titanium separation. Summary of the Invention

[0004] In view of this, some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, comprising:

[0005] A soluble anode is prepared by mixing niobium oxide, titanium oxide, and graphite in a predetermined molar ratio.

[0006] The first graphite electrode is used as the first cathode, forming a first electrolysis system with the soluble anode and molten salt electrolyte;

[0007] The electrolysis temperature and voltage of the first electrolysis system are set, and electrolysis is carried out. During the electrolysis process, the metallic niobium oxide in the soluble anode is converted into niobium ions, which are reduced to metallic niobium on the surface of the first graphite electrode.

[0008] The second graphite electrode is used as the second cathode to form a second electrolysis system with the soluble anode and molten salt electrolyte;

[0009] The electrolysis temperature and voltage of the second electrolysis system are set, and electrolysis is carried out. During the electrolysis process, the titanium oxide in the soluble anode is converted into titanium ions, which are reduced to titanium metal on the surface of the second graphite electrode.

[0010] Some embodiments disclose a method for separating metallic niobium and titanium by electrolysis using a soluble anode, wherein a first cathode and a soluble anode are placed in a molten salt electrolyte, and the first electrolysis system is formed to electrolyze and obtain metallic niobium;

[0011] After the first electrolysis system is completed, the first cathode is replaced with the second cathode, and the second electrolysis system is used to obtain metallic titanium.

[0012] Some embodiments disclose a method for electrolytically separating metallic niobium and titanium using a soluble anode, wherein a first graphite electrode, a second graphite electrode, and a soluble anode are simultaneously disposed in a molten salt electrolyte;

[0013] Electrolysis in the first electrolysis system yields metallic niobium;

[0014] After the first electrolysis system is completed, the second electrolysis system is used to obtain metallic titanium.

[0015] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the molar ratio of metallic niobium oxide to graphite is 1:1 to 4.

[0016] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the molar ratio of metallic titanium oxide to graphite is 1:1 to 4.

[0017] Some embodiments disclose a method for electrolytically separating metallic niobium and titanium using a soluble anode, wherein the soluble anode is prepared at a temperature of 800°C to 1400°C.

[0018] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the electrolysis voltage of the first electrolysis system is set in the range of 1.5 to 3.0 V, and the electrolysis temperature of the first electrolysis system is set in the range of 700°C to 900°C.

[0019] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the electrolysis voltage of the second electrolysis system is set in the range of 1.5 to 3.0 V, and the electrolysis temperature of the second electrolysis system is set in the range of 700°C to 900°C.

[0020] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the metallic niobium oxide is NbO, NbO2, Nb2O3, or Nb2O5.

[0021] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the titanium oxide is TiO2 or Ti2O3.

[0022] The method for separating metallic niobium and titanium using soluble anode electrolysis disclosed in this invention utilizes the difference in theoretical decomposition voltages of metallic niobium oxide and metallic titanium oxide in molten salt to control the electrolysis voltage of molten salt electrolysis. This allows niobium ions and titanium ions in the soluble anode to be deposited and separated sequentially. Two cathodes are used, and two electrolysis processes are performed sequentially, yielding metallic niobium and metallic titanium on the surfaces of the two cathodes respectively. No anode sludge is generated, and no impurity removal treatment is required. Molten salt pretreatment can remove as much physical water and crystal water as possible from the molten salt, reducing energy consumption during electrolysis and improving product purity. The method for preparing niobium-titanium alloys using molten salt electrolysis disclosed in this invention has a simple process flow, low equipment requirements, significantly reduces production costs, and the entire process is easy to implement. Attached Figure Description

[0023] Figure 1 Theoretical decomposition voltages of niobium oxide and titanium oxide at different temperatures;

[0024] Figure 2 Example 1: Electrolytic separation of metallic niobium and titanium using soluble anodic electrolysis. Figure 1 ;

[0025] Figure 3 Example 1: Electrolytic separation of metallic niobium and titanium using soluble anodic electrolysis. Figure 2 . Detailed Implementation

[0026] The term "embodiment" used herein, as an example, is not necessarily to be construed as superior to or better than other embodiments. Performance testing in the embodiments of this application, unless otherwise specified, employs conventional testing methods in the art. It should be understood that the terminology used in this application is merely for describing particular implementations and is not intended to limit the scope of this disclosure.

[0027] Unless otherwise stated, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; other experimental methods and technical means not specifically mentioned herein refer to experimental methods and technical means commonly used by one of ordinary skill in the art.

[0028] The terms “basic” and “approximately” used in this document are to describe small fluctuations. For example, they can mean less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. Numerical data presented or expressed in range format in this document are used for convenience and brevity only, and should therefore be flexibly interpreted to include not only the explicitly listed values ​​that define the range, but also all independent values ​​or subranges contained within that range. For example, a numerical range of “1–5%” should be interpreted to include not only the explicitly listed values ​​from 1% to 5%, but also the independent values ​​and subranges within the indicated range. Thus, this numerical range includes independent values ​​such as 2%, 3.5%, and 4%, and subranges such as 1%–3%, 2%–4%, and 3%–5%, etc. This principle also applies to ranges that list only one value. Furthermore, this interpretation applies regardless of the width of the range or the characteristics described.

[0029] In this document, including in the claims, conjunctions such as "comprising," "including," "with," "having," "containing," "involving," and "accommodating" are understood to be open-ended, meaning "including but not limited to." Only the conjunctions "consisting of" and "composed of" are closed conjunctions.

[0030] To better illustrate the content of this application, numerous specific details are provided in the following detailed embodiments. Those skilled in the art should understand that this application can be implemented even without certain specific details. In the embodiments, some methods, means, instruments, and devices well-known to those skilled in the art are not described in detail in order to highlight the main points of this application.

[0031] Without conflict, the technical features disclosed in the embodiments of this application can be combined arbitrarily, and the resulting technical solutions belong to the content disclosed in the embodiments of this application. It should be noted that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer" used in this application indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing technical features and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention unless they conflict with the context. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance unless they conflict with the context.

[0032] In some embodiments, the method for separating metallic niobium and titanium using soluble anodic electrolysis includes:

[0033] A soluble anode is prepared by mixing niobium oxide, titanium oxide, and graphite in a predetermined molar ratio.

[0034] The first graphite electrode is used as the first cathode, forming a first electrolysis system with the soluble anode and molten salt electrolyte;

[0035] The electrolysis temperature and voltage of the first electrolysis system are set, and electrolysis is carried out. During the electrolysis process, the metallic niobium oxide in the soluble anode is converted into niobium ions, which are reduced to metallic niobium on the surface of the first graphite electrode.

[0036] The second graphite electrode is used as the second cathode to form a second electrolysis system with the soluble anode and molten salt electrolyte that have participated in the reaction of the first electrolysis system.

[0037] The electrolysis temperature and voltage of the second electrolysis system are set, and electrolysis is carried out. During the electrolysis process, the titanium oxide in the soluble anode is converted into titanium ions, which are reduced to titanium metal on the surface of the second graphite electrode.

[0038] Typically, the cathode needs to be pretreated before electrolysis. The cathode pretreatment process includes: immersing the first and second graphite electrodes in a 30% nitric acid solution for a certain period of time, then removing and cleaning them; degreasing the cleaned first and second graphite electrodes, then cleaning them with deionized water and anhydrous ethanol; and finally placing them in an oven and drying them at 80℃~150℃ for 12~48h to complete the cathode pretreatment.

[0039] As an optional implementation, the method for separating metallic niobium and titanium using soluble anodic electrolysis includes:

[0040] The first graphite electrode and the soluble anode are placed in the molten salt electrolyte to form the first electrolysis system;

[0041] The electrolysis temperature and voltage of the first electrolysis system are set, and electrolysis is carried out. The entire electrolysis process is carried out in a sealed reactor, and argon gas is continuously introduced into the reactor for atmosphere protection.

[0042] During electrolysis, oxygen ions in the soluble anode combine with carbon to generate carbon monoxide or carbon dioxide, which is then discharged. The metallic niobium oxide in the soluble anode is converted into niobium ions, which dissolve into the molten salt electrolyte and migrate from the molten salt electrolyte to the first graphite electrode, where they are reduced to metallic niobium on the surface of the first graphite electrode.

[0043] After niobium ions are completely reduced on the surface of the first graphite electrode, the first graphite electrode is removed and replaced with a second graphite electrode. The second graphite electrode and the soluble anode form a second electrolysis system in the molten salt electrolyte. Keeping other reaction conditions unchanged, the electrolysis voltage of the second electrolysis system is adjusted to carry out electrolysis. During the electrolysis process, the metallic titanium oxide in the soluble anode is converted into titanium ions. The titanium ions dissolve into the molten salt electrolyte and migrate from the molten salt electrolyte to the second graphite electrode, where they are reduced to metallic titanium on the surface of the second graphite electrode.

[0044] As an optional implementation, the method for separating metallic niobium and titanium using soluble anodic electrolysis includes:

[0045] The first graphite electrode, the second graphite electrode, and the soluble anode are simultaneously placed in the molten salt electrolyte; the entire electrolysis process is carried out in a sealed reactor, and argon gas is continuously introduced into the reactor for atmosphere protection.

[0046] A first graphite electrode and a soluble anode are connected to form a first electrolysis system. The electrolysis temperature and voltage of the first electrolysis system are set, and electrolysis is carried out. During the electrolysis process, oxygen ions in the soluble anode combine with carbon to generate carbon monoxide or carbon dioxide, which is then discharged. The metallic niobium oxide in the soluble anode is converted into niobium ions, which dissolve into the molten salt electrolyte and migrate from the molten salt electrolyte to the first graphite electrode, where they are reduced to metallic niobium on the surface of the first graphite electrode. The second graphite electrode does not participate in the reaction of the first electrolysis system.

[0047] After niobium ions are completely reduced on the surface of the first graphite electrode, the connection between the first graphite electrode and the soluble anode is broken, and the second graphite electrode is connected to the soluble anode to form a second electrolysis system. Keeping other reaction conditions unchanged, the electrolysis voltage of the second electrolysis system is adjusted to carry out electrolysis. During the electrolysis process, the metallic titanium oxide in the soluble anode is converted into titanium ions, which dissolve into the molten salt electrolyte and migrate from the molten salt electrolyte to the second graphite electrode, where they are reduced to metallic titanium on the surface of the second graphite electrode.

[0048] Typically, a first graphite electrode containing metallic niobium and a second graphite electrode containing metallic titanium are cooled under the protection of high-purity argon gas. The first and second graphite electrodes are cleaned with deionized water and anhydrous ethanol. Then, the metallic niobium is separated from the surface of the first graphite electrode and the metallic titanium is separated from the surface of the second graphite electrode by ultrasonic vibration. Finally, the metallic niobium and metallic titanium are cleaned three times with deionized water and anhydrous ethanol and then dried in a vacuum drying oven to obtain high-purity metallic niobium and high-purity metallic titanium.

[0049] Typically, the current-time curve is recorded during the electrolysis process. Generally, the electrolysis progress can be judged by the current-time curve, the rate of electrolysis can be controlled by controlling the magnitude of the current or potential, and the metal deposition can be judged by the change in current density.

[0050] As an optional implementation method, the specific preparation method of the soluble anode includes:

[0051] Weigh out niobium oxide, titanium oxide, and graphite according to the set molar ratio;

[0052] The weighed niobium oxide, titanium oxide and graphite were ground in a ball mill and then pressed into cylinders in a pressing machine.

[0053] The cylinder is placed in a high-temperature reactor and heated to 800℃~1400℃ at 10℃ / min for 6~8h to obtain a soluble anode;

[0054] For soluble anodes prepared by sintering, they are tied to electrode rods to test their conductivity. The multimeter is set to the shortest range, and the red and black probes are connected to the two ends of the soluble anode, respectively. When the multimeter displays a stable current value, the soluble anode is considered to be conductive and can be used for molten salt electrolysis.

[0055] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the molar ratio of metallic niobium oxide to graphite is 1:1 to 4.

[0056] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the molar ratio of metallic titanium oxide to graphite is 1:1 to 4.

[0057] Some embodiments disclose a method for electrolytically separating metallic niobium and titanium using a soluble anode, wherein the soluble anode is prepared at a temperature of 800°C to 1400°C.

[0058] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis. The electrolysis voltage of the first electrolysis system is set in the range of 1.5 to 3.0 V, and the electrolysis temperature of the first electrolysis system is set in the range of 700°C to 900°C. The electrolysis voltage of the second electrolysis system is set in the range of 1.5 to 3.0 V, and the electrolysis temperature of the second electrolysis system is set in the range of 700°C to 900°C.

[0059] As an optional implementation, the electrolysis temperature of both the first and second electrolysis systems is 750°C. The selection of the electrolysis temperature generally considers factors such as the electrochemical window of the molten salt, the intermediate products of the reaction process, the solubility of the molten salt in the reactants and products, the environmental friendliness, volatility, and viscosity of the molten salt. If a solid-state reduction reaction is to occur, the melting points of both the reactants and products should be higher than the operating temperature of the molten salt; if a liquid deposition reaction is to occur, the selected operating temperature of the molten salt should be higher than the melting point of the product.

[0060] This invention utilizes the difference in theoretical decomposition voltages of niobium oxide and titanium oxide in molten salt to control voltage electrolytic separation of niobium and titanium; the theoretical decomposition voltages of niobium oxide and titanium oxide at different reaction temperatures are as follows: Figure 1 As shown, the theoretical decomposition voltages of niobium oxide and titanium oxide decrease linearly with increasing decomposition temperature during the reaction. Calculations show that the theoretical decomposition potential difference between niobium pentoxide and titanium dioxide is 0.47 V. The decomposition potential difference of ions during molten salt electrolysis determines whether niobium-titanium separation can be achieved by controlling the potential. For complete separation of the two ions through potential control, the decomposition potential difference must be greater than 0.30 / n V. The theoretical decomposition potential difference between niobium pentoxide and titanium dioxide relative to the evolved oxygen is 0.47 V, which meets the decomposition potential difference requirement. In this electrode system, niobium ions preferentially precipitate, while titanium ions remain on the soluble anode.

[0061] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the metallic niobium oxide is NbO, NbO2, Nb2O3, or Nb2O5.

[0062] Some embodiments disclose a method for separating metallic niobium and titanium using soluble anodic electrolysis, wherein the titanium oxide is TiO2 or Ti2O3.

[0063] As an optional implementation method, niobium pentoxide is selected as the niobium oxide and titanium dioxide is selected as the titanium oxide. Niobium pentoxide and titanium dioxide have good compatibility, which can reduce raw material costs and reduce environmental pollution.

[0064] In some embodiments, the molten salt electrolyte is sodium chloride-potassium chloride.

[0065] In some embodiments, the molar ratio of sodium chloride to potassium chloride is 0.8 to 1.2:1.

[0066] Molten salt electrolytes typically require a pretreatment process before electrolysis to remove moisture and pre-melt them to reach the molten state required for electrolysis.

[0067] As an optional implementation, the pretreatment process of the molten salt electrolyte includes:

[0068] Place the molten salt in a clean, dry container and dry it in a vacuum environment at a temperature of 100℃~250℃ for 8h~24h.

[0069] Remove the dried molten salt and place it in an electrolytic furnace to heat to 300℃~400℃ and keep it at that temperature for 2~12 hours to ensure that the moisture is completely removed.

[0070] The electrolytic furnace is heated to 900°C to melt sodium chloride and potassium chloride, thus obtaining molten salt.

[0071] High-purity molybdenum rods and graphite rods are used as cathodes and anodes, respectively, and are inserted into molten salt for constant voltage electrolysis. When the current stabilizes, electrolysis is stopped, and molten salt pretreatment is completed.

[0072] In some embodiments, the electrolytic separation process of metallic niobium and titanium is carried out under an inert atmosphere.

[0073] In some implementations, the inert atmosphere includes argon or nitrogen.

[0074] The technical details are further illustrated below with reference to the embodiments.

[0075] Example 1

[0076] The method for separating metallic niobium and titanium using soluble anodic electrolysis disclosed in Example 1 specifically includes:

[0077] Niobium pentoxide and graphite are weighed in a molar ratio of 1:4, and titanium dioxide and graphite are weighed in a molar ratio of 1:1.5.

[0078] Niobium pentoxide, titanium dioxide and graphite were weighed and mixed in a ball mill and then pressed into cylinders using a sample press.

[0079] The cylinder was placed in a high-temperature reactor and sintered at 1200℃ for 6 hours at a rate of 10℃ / min to obtain a soluble anode.

[0080] Sodium chloride-potassium chloride were placed in a clean, dry container and dried in a vacuum environment at 150°C for 8 hours.

[0081] Remove the dried sodium chloride-potassium chloride mixture, place it in an electrolytic furnace, heat it to 300°C and keep it at that temperature for 4 hours, then heat it to 900°C to melt the sodium chloride-potassium chloride mixture.

[0082] High-purity molybdenum rods and graphite rods were used as cathodes and anodes, respectively, and were inserted into sodium chloride-potassium chloride for constant voltage electrolysis. When the current stabilized, it was considered that the water and redox-active impurities in the sodium chloride-potassium chloride had been basically removed, and electrolysis was stopped to complete the molten salt pretreatment.

[0083] The first graphite electrode and the second graphite electrode were immersed in a 30% nitric acid solution for a certain period of time, then removed and cleaned.

[0084] The washed first and second graphite electrodes were degreased, cleaned with deionized water and anhydrous ethanol, and finally placed in an oven to dry at 150°C for 48 hours to complete the pretreatment of the first and second graphite electrodes.

[0085] The electrolytic process for separating metallic niobium and titanium using soluble anodic electrolysis is as follows;

[0086] The soluble anode, the first graphite electrode, and the second graphite electrode were all inserted into the NaCl-KCl molten salt. Figure 2 As shown, the first graphite electrode and the soluble anode are connected to form the first electrolysis system. The electrolysis temperature is set to 750℃ and the electrolysis voltage is set to 1.9V. The electrolysis power supply is connected to start the electrolysis deposition separation.

[0087] The entire electrolysis process is usually carried out in a sealed reactor, with argon gas continuously introduced into the reactor for atmosphere protection. Generally, the electrolysis temperature is higher than the melting point of the electrolyte in order to maintain its molten state. For example, an electrolysis temperature 50°C higher than the melting point of the electrolyte can give the molten salt electrolyte good conductivity and fluidity, which is beneficial to obtaining good electrolysis results.

[0088] During electrolysis, oxygen ions O in the soluble anode 2- It combines with carbon to generate carbon monoxide (CO) or carbon dioxide (CO2) and is discharged. Niobium ions in the soluble anode dissolve into the NaCl-KCl molten salt and migrate from the NaCl-KCl molten salt to the first graphite electrode, where they are reduced to metallic niobium on the surface of the first graphite electrode.

[0089] Based on the current density, after niobium ions are completely deposited on the surface of the first graphite electrode, the first graphite electrode and the soluble anode are disconnected, and the second graphite electrode and the soluble anode are connected to form a second electrolysis system. Figure 3 As shown, the electrolysis voltage was adjusted to 2.4V, and other conditions were kept unchanged. Electrolysis continued, and titanium ions in the soluble anode dissolved into the NaCl-KCl molten salt and migrated from the NaCl-KCl molten salt to the second graphite electrode, where they were reduced to metallic titanium on the surface of the second graphite electrode.

[0090] The first and second graphite electrodes were cooled under the protection of high-purity argon gas. The electrodes were then cleaned with deionized water and anhydrous ethanol. Next, niobium was separated from the surface of the first graphite electrode and titanium from the surface of the second graphite electrode by ultrasonic vibration. Finally, the niobium and titanium were cleaned three times with deionized water and anhydrous ethanol, and then dried in a vacuum drying oven to obtain high-purity niobium and titanium. In this embodiment of the invention, the separation efficiency of niobium and titanium was 99%, and the purity of niobium was 99.99%.

[0091] The method for separating metallic niobium and titanium using soluble anodic electrolysis disclosed in this invention utilizes the difference in theoretical decomposition voltages of metallic niobium oxide and metallic titanium oxide in molten salt to control the electrolysis voltage of molten salt electrolysis. This allows niobium ions and titanium ions in the soluble anode to be deposited and separated sequentially. Two cathodes are used, and two electrolysis processes are performed sequentially, yielding metallic niobium and metallic titanium on the surfaces of the two cathodes respectively. No anode sludge is generated, and no impurity removal treatment is required. Molten salt pretreatment can remove as much physical water and crystal water as possible from the molten salt, reducing energy consumption during electrolysis and improving product purity. The method for preparing niobium-titanium alloys using molten salt electrolysis disclosed in this invention has a simple process flow, low equipment requirements, significantly reduces production costs, and the entire process is easy to implement.

[0092] The technical solutions and technical details disclosed in the embodiments of this invention are merely illustrative of the inventive concept of this invention and do not constitute a limitation on the technical solutions of this invention. Any conventional changes, substitutions, or combinations made to the technical details disclosed in the embodiments of this invention have the same inventive concept as this invention and are within the protection scope of the claims of this invention.

Claims

1. A method for electrolytic separation of niobium and titanium from a metal using a soluble anode, characterized in that, The application relates to a method for preparing metal niobium and metal titanium. The metal niobium oxide, the metal titanium oxide and the graphite are mixed according to a set molar ratio to prepare a soluble anode; the molar ratio of the metal niobium oxide to the graphite is 1:1-4, the molar ratio of the metal titanium oxide to the graphite is 1:1-4, and the preparation temperature of the soluble anode is 800-1400 DEG C; The first graphite electrode is used as a first cathode to form a first electrolysis system with the soluble anode and a molten salt electrolyte; the molten salt electrolyte is sodium chloride-potassium chloride, and the molar ratio of sodium chloride to potassium chloride is 0.8-1.2:1; The electrolysis temperature of the first electrolysis system is set to be 700-900 DEG C, the electrolysis voltage is set to be 1.5-3.0 V, and electrolysis is carried out; in the electrolysis process, the metal niobium oxide in the soluble anode is converted into niobium ions and is reduced into metal niobium on the surface of the first graphite electrode; The second graphite electrode is used as a second cathode to form a second electrolysis system with the soluble anode after participating in the reaction of the first electrolysis system and the molten salt electrolyte; The electrolysis temperature of the second electrolysis system is set to be 700-900 DEG C, the electrolysis voltage is set to be 1.5-3.0 V, and electrolysis is carried out; in the electrolysis process, the metal titanium oxide in the soluble anode is converted into titanium ions and is reduced into metal titanium on the surface of the second graphite electrode.

2. The method for electrolytic separation of niobium and titanium from their alloy by using soluble anode according to claim 1, characterized in that, The first cathode and the soluble anode are arranged in the molten salt electrolyte to form a first electrolysis system for electrolysis, and metal niobium is obtained; After the electrolysis of the first electrolysis system is completed, the first cathode is replaced by the second cathode, and the second electrolysis system is electrolyzed to obtain metal titanium.

3. The method for electrolytic separation of niobium and titanium from their alloy by using soluble anode according to claim 1, characterized in that, The first graphite electrode, the second graphite electrode and the soluble anode are arranged in the molten salt electrolyte at the same time; The first electrolysis system is electrolyzed to obtain metal niobium; After the electrolysis of the first electrolysis system is completed, the second electrolysis system is electrolyzed to obtain metal titanium.

4. The method for electrolytic separation of niobium and titanium from their alloy by using soluble anode according to claim 1, characterized in that, The metal niobium oxide is NbO, NbO2, Nb2O3 or Nb2O5.

5. The method for electrolytic separation of niobium and titanium from their alloy by using soluble anode according to claim 1, characterized in that, The metal titanium oxide is TiO2 or Ti2O3.

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