A method for separating tantalum and niobium by high-energy floatation

Abstract

This invention discloses a high-energy flotation separation and purification method for tantalum and niobium. It processes the impure tantalum and niobium oil phase obtained from acid leaching and pulp extraction of tantalum and niobium raw materials into clean tantalum and niobium solutions for the preparation of high-purity tantalum and niobium products. First, the impure tantalum and niobium oil phase is subjected to 1-3 stages of high-energy flotation washing, followed by 1-2 stages of high-energy flotation co-extraction of the washing liquid and the residual extract to obtain a tantalum and niobium-rich oil phase, achieving the reuse of tantalum and niobium in the washing liquid and residual extract. Next, the tantalum and niobium-rich oil phase is subjected to 1-3 stages of high-energy flotation reverse niobium removal, followed by 1-2 stages of high-energy flotation extraction of the reverse niobium aqueous phase to obtain a tantalum-rich oil phase and a clean niobium solution, achieving the reuse of tantalum in the reverse niobium aqueous phase. Finally, the tantalum-rich oil phase is subjected to 1-3 stages of high-energy flotation reverse tantalum removal to obtain a clean tantalum solution. This invention has advantages such as a short overall process, good tantalum and niobium separation effect, high tantalum and niobium purification efficiency, low reagent loss, and high resource recovery rate, making it suitable for industrial application.

Description

Technical Field

[0001] This invention relates to a method for wet separation and impurity removal of tantalum and niobium, belonging to the technical field of tantalum and niobium resource extraction metallurgy and chemical preparation. Background Technology

[0002] Tantalum, niobium and their compounds possess excellent properties such as high melting point, high density, high temperature resistance, corrosion resistance, wear resistance, superconductivity and high strength. They are widely used in steel, electronics, aerospace, low temperature superconductivity and nuclear industry and are indispensable key raw materials for modern cutting-edge industries.

[0003] Tantalum and niobium are elements in the same group with similar properties, and they often exist as associated minerals in nature. Tantalum and niobium resources are very rare. my country's niobium reserves are approximately 116,500 tons, and its tantalum reserves are 39,800 tons, mainly distributed in provinces such as Jiangxi, Xinjiang, Guangxi, Hunan, Sichuan, and Inner Mongolia. After enrichment through physicochemical methods, high-grade tantalum and niobium concentrates can be obtained from tantalum and niobium ore.

[0004] Hydrometallurgical processes (water-based metallurgy) are the mainstream method for extracting tantalum and niobium from industrial tantalum and niobium concentrates. They mainly consist of acid leaching of tantalum and niobium ore, enrichment-separation-purification of tantalum and niobium in solution, and refining with high-purity tantalum and niobium chemicals. Among these, the enrichment-separation-purification of tantalum and niobium in solution is the most complex part of the tantalum and niobium metallurgical process, including slurry extraction (~10 stages), impurity elution and supernatant extraction (15~30 stages), reverse niobium extraction (15~30 stages), and reverse tantalum extraction (10~30 stages). The cumulative number of extraction and reverse extraction stages can reach hundreds, resulting in significant efficiency losses, energy losses, organic reagent losses, and increased wastewater treatment load. Therefore, developing a new, short-process method for the separation and purification of tantalum and niobium in the hydrometallurgical system is of great significance for the green and low-carbon transformation and upgrading of the tantalum and niobium industry. Summary of the Invention

[0005] This invention provides a method for high-energy flotation separation and purification of tantalum and niobium. The method processes the impure tantalum and niobium oil phase obtained from acid leaching and pulp extraction of tantalum and niobium raw materials into clean tantalum and niobium solutions for the preparation of high-purity tantalum and niobium products. The main process is as follows: First, the impure tantalum and niobium oil phase is subjected to 1-3 stages of high-energy flotation washing, and the washing solution is subjected to 1-2 stages of high-energy flotation co-extraction to obtain a tantalum- and niobium-rich oil phase, achieving the reuse of tantalum and niobium in the washing solution; then, the tantalum- and niobium-rich oil phase is subjected to 1-3 stages of high-energy flotation reverse niobium removal, and the reverse niobium aqueous phase is subjected to 1-2 stages of high-energy flotation tantalum extraction to obtain a tantalum-rich oil phase and a clean niobium solution, achieving the reuse of tantalum in the reverse niobium aqueous phase; finally, the tantalum-rich oil phase is subjected to 1-3 stages of high-energy flotation reverse tantalum removal to obtain a clean tantalum solution. The new method utilizes high-energy flotation to reduce the unit operations required for tantalum-niobium separation and purification to less than 10 stages, while also taking into account the recovery of low-concentration tantalum-niobium from the raffinate, impurity removal solution, and back-extraction solution. Compared with existing processes, it is expected to increase production efficiency by 5 to 8 times and tantalum-niobium recovery rate by 2 to 5%.

[0006] This invention discloses a high-energy flotation method for separating and purifying tantalum and niobium, one of the core technologies of which is high-energy flotation. High-energy flotation involves mixing a loaded metal oil phase or blank extractant with CO2 and an amphiphilic solvent under pressure to create a high-energy oil phase containing dissolved CO2. This oil phase is then introduced into an acidic or neutral aqueous phase through a porous medium, forming high-kinetic-energy micro / nano airborne oil droplets and oil films. In washing, anti-niobium, and anti-tantalum systems, metal ions are released from bottom to top and aggregate on the aqueous phase surface to form a low-loaded metal oil layer. In co-extraction and tantalum extraction systems, metal ions are captured from bottom to top and aggregate on the aqueous phase surface to form a high-loaded metal oil layer.

[0007] The high-energy oil phase is introduced into the aqueous phase under high pressure, possessing high initial kinetic energy. Furthermore, the dissolved CO2 within it rapidly expands and depressurizes in the low-pressure aqueous phase, causing the adhering oil phase to break down into airborne nano-oil droplets or expand into airborne nano-oil films. These micro / nano airborne oil droplets and films are small in size, uniformly dispersed, have high initial buoyancy, and rapid interface renewal. This ensures that processes such as washing, co-extraction, anti-niobium, tantalum extraction, and anti-tantalum possess advantages such as high concentration gradient driving force, large reaction interface area, and ultra-short interphase mass transfer pathways, thereby significantly improving the efficiency of tantalum-niobium separation and purification.

[0008] This invention discloses a method for high-energy flotation separation and purification of tantalum and niobium. Before carrying out the separation and purification operations, the oil phase needs to be pressurized and energized. Specifically, 5-9.5 parts by mass of the loaded metal oil phase or blank extractant and 0.5-5 parts by mass of the amphiphilic solvent are stirred and mixed under CO2 pressure of 1-5 MPa and temperature of -10-40°C to obtain a high-energy oil phase with a dissolved CO2 molar percentage of 4-20%. The loaded metal oil phase includes at least one of impure tantalum and niobium oil phase, tantalum- and niobium-rich oil phase, and tantalum-rich oil phase. The blank extractant is one or more of ketones, alcohols, and amines. The amphiphilic solvent is specifically one or more of toluene, butanol, pentanol, butanone, pentanone, and hexane. These amphiphilic solvents are all hydrophobic, can effectively dissolve CO2, and are miscible with the loaded metal oil phase or blank extractant. High pressure and amphiphilic solvents can simultaneously enhance the solubility of CO2 in the oil phase and ensure that they adhere to each other in the aqueous phase, thereby enabling the oil phase to complete dispersion, diffusion and surface aggregation with gas as a carrier.

[0009] This invention discloses a high-energy flotation method for the separation and purification of tantalum and niobium. The micro / nano-sized gaseous oil droplets and oil films are formed by the expansion and decompression of dissolved CO2 in a high-energy oil phase, resulting in oil droplets adhering to CO2 bubbles and oil films coating CO2 bubbles. The CO2 bubble diameter does not exceed 800 μm, the oil film thickness does not exceed 300 nm, and the oil droplet diameter does not exceed 500 nm. Typically, during flotation, bubbles gradually expand from less than 100 nm to several hundred micrometers. Simultaneously, the oil phase expands and renews on its surface, and the size of the oil droplets and oil films perpendicular to the bubble surface gradually decreases. These effects lead to compression of the oil-water interface layer thickness, shortening of the diffusion path within the oil phase, and intense turbulence / turbulent mass transfer at the oil-water interface. Therefore, the capture or release rate of tantalum, niobium, and impurity ions is significantly improved. Only 1-3 stages of washing, co-extraction, anti-niobium, tantalum extraction, and anti-tantalum are required to achieve efficient separation and impurity removal of tantalum and niobium.

[0010] When pressurizing and energizing the oil phase, the preferred CO2 pressure is 3.0–4.5 MPa.

[0011] When pressurizing and energizing the oil phase, the preferred temperature is 10–35°C, but room temperature can also be used in this invention.

[0012] As a preferred option, after pressurizing and energizing the oil phase, a high-energy oil phase with a dissolved CO2 content of 8-18% is obtained.

[0013] The porous medium is preferably at least one of polytetrafluoroethylene, polyethylene, polypropylene, and mullite, and the pore size of the porous medium is 0.1–500 μm. Of course, other porous media can also be used in this invention.

[0014] This invention discloses a method for high-energy flotation separation and purification of tantalum and niobium. The impurity-containing tantalum and niobium oil phase is obtained by leaching tantalum and niobium ore or tantalum and niobium alloy waste with a mixed acid of sulfuric acid and hydrofluoric acid, followed by extraction with methyl isobutyl ketone, sec-octanol, or acetamide slurry. The tantalum concentration is 10–80 g / L and the niobium concentration is 50–250 g / L. The aqueous phase acid concentrations in the washing, co-extraction, reverse niobium extraction, tantalum extraction, and reverse tantalum extraction processes are respectively: 3–4.5 mol / L sulfuric acid, 6–8 mol / L hydrofluoric acid mixed with 3.5–5 mol / L sulfuric acid, 0.5–0.8 mol / L sulfuric acid, 0.6–1.0 mol / L sulfuric acid, and 0–0.5 mol / L sulfuric acid. The oil-water phase volume ratio in the washing, reverse niobium extraction, and reverse tantalum extraction processes is (1–4):1, with less water phase used than in conventional reverse extraction methods. The oil-water phase volume ratio in the co-extraction and tantalum extraction processes is (0.25–1):1, with less oil phase used than in conventional forward extraction methods.

[0015] This invention discloses a method for high-energy flotation separation and purification of tantalum and niobium, wherein the niobium content in the clean tantalum solution is less than 0.1 g / L, and the tantalum content in the clean niobium solution is less than 0.1 g / L; the clean tantalum solution and the clean niobium solution are used to prepare 3-6N pure potassium fluorocarbonate, tantalum oxide, and niobium oxide.

[0016] This invention prepares a high-energy oil phase containing dissolved CO2 by mixing a loaded metal oil phase or blank extractant with CO2 and an amphiphilic solvent under appropriate pressure. This high-energy oil phase is then introduced into an acidic or neutral aqueous phase through a porous medium to form high-kinetic-energy micro-nano gas-carrying oil droplets and oil films. Utilizing the characteristics of small size, uniform dispersion, high initial flotation velocity, and rapid interface renewal, this invention ensures that the washing, co-extraction, anti-niobium, tantalum extraction, and anti-tantalum processes have advantages such as high concentration gradient driving force, large reaction interface area, and ultra-short interphase mass transfer path, significantly improving the efficiency of tantalum and niobium separation and purification. Attached Figure Description

[0017] Figure 1 This is a process flow diagram of the present invention. Detailed Implementation

[0018] The present invention will be further explained and illustrated below with reference to the embodiments. The scope of protection of the claims of the present invention is not limited by the following embodiments.

[0019] Example 1

[0020] Using an oil phase containing 52 g / L tantalum, 110 g / L niobium, 1.8 g / L tungsten, and 1.6 g / L antimony obtained by methyl isobutyl ketone pulp extraction as the target, a two-stage high-energy flotation washing process was first performed on it with 4.0 mol / L sulfuric acid at an oil-water volume ratio of 2:1 to obtain a tantalum- and niobium-rich oil phase. The washing solution was then adjusted to a mixture of 6.0 mol / L hydrofluoric acid and 4.0 mol / L sulfuric acid at an oil-water volume ratio of 0.5:1 for a first-stage high-energy flotation. The process involves co-extraction to recover tantalum and niobium from the washing solution; then, a two-stage high-energy flotation process is performed on the tantalum- and niobium-rich oil phase using 0.7 mol / L sulfuric acid at an oil-to-water volume ratio of 2:1 to obtain a tantalum-rich oil phase. The niobium-reducing aqueous phase is then adjusted to a 0.75 mol / L sulfuric acid solution and subjected to a first-stage high-energy flotation extraction of tantalum at an oil-to-water volume ratio of 0.5:1 to obtain a clean niobium solution. Finally, a two-stage high-energy flotation process is performed on the tantalum-rich oil phase using pure water at an oil-to-water ratio of 2:1 to obtain a clean tantalum solution.

[0021] In the processes of high-energy flotation washing, high-energy flotation co-extraction, high-energy flotation anti-niobium, high-energy flotation extraction of tantalum, and high-energy flotation anti-tantalum, the oil phase components are first adjusted and mixed in a high-pressure reactor at 8 parts by mass of loaded metal (tantalum, niobium, or other impurities) methyl isobutyl ketone or blank methyl isobutyl ketone, 1 part by mass of pentanone, and 1 part by mass of toluene. The CO2 pressure in the reactor is controlled at 3.8–4.2 MPa, the temperature at 15–20 °C, and the stirring time at 20 min. This yields a high-energy oil phase with a dissolved CO2 content of 10–15%. Subsequently, the high-energy oil phase is introduced into the aqueous phase through a polyethylene medium with an average pore size of 1 μm to form high-kinetic-energy gas-carried nano-oil droplets or nano-oil films, thereby completing the separation and purification of tantalum and niobium.

[0022] Following the above method, after two stages of high-energy flotation washing, the tungsten content in the oil phase containing impurities (tantalum and niobium) was 0.15 g / L and the antimony content was 0.22 g / L, with an oil phase loss of 0.5%. After one stage of high-energy flotation co-extraction, the tantalum and niobium content in the aqueous phase was reduced to below 0.05 g / L, with an oil phase loss of 0.3%, and the tantalum and niobium recoveries were 98.1% and 98.3%, respectively. After two stages of high-energy flotation reverse niobium removal, the oil... The niobium content in the aqueous phase was reduced to 0.03 g / L, with an oil phase loss of 0.5%. After a first-stage high-energy flotation extraction of tantalum in the anti-niobium aqueous phase, the niobium content in the clean niobium solution was 202 g / L, the tantalum content was 0.04 g / L, the oil phase loss was 0.3%, and the tantalum recovery rate reached 97.7%. After a second-stage high-energy flotation anti-tantalum extraction of the tantalum-rich oil phase, the tantalum content in the clean tantalum solution was 96 g / L, the niobium content was 0.03 g / L, and the oil phase loss was 0.3%. This operation is far more efficient and produces a much higher purity product than existing technologies.

[0023] Example 2

[0024] Using an oil phase containing 40 g / L tantalum, 102 g / L niobium, 2.2 g / L tungsten, and 2.0 g / L antimony obtained by octanol pulp extraction as the target, a two-stage high-energy flotation washing process was first performed on it with 3.8 mol / L sulfuric acid at an oil-water volume ratio of 2:1 to obtain a tantalum- and niobium-rich oil phase. The washing solution was then adjusted to a mixture of 7.0 mol / L hydrofluoric acid and 3.5 mol / L sulfuric acid at an oil-water volume ratio of 0.5:1 for a first-stage high-energy flotation process. Co-extraction was performed to recover tantalum and niobium from the washing solution. Then, tantalum- and niobium-rich oil phases were subjected to two-stage high-energy flotation reverse niobium extraction using 0.75 mol / L sulfuric acid at an oil-to-water volume ratio of 2:1 to obtain tantalum-rich oil phases. The reverse niobium aqueous phase was then adjusted to 0.8 mol / L sulfuric acid solution and subjected to one-stage high-energy flotation tantalum extraction using an oil-to-water volume ratio of 0.5:1 to obtain clean niobium solution. Finally, tantalum-rich oil phases were subjected to two-stage high-energy flotation reverse niobium extraction using pure water at an oil-to-water ratio of 2:1 to obtain clean tantalum solution.

[0025] In the processes of high-energy flotation washing, high-energy flotation co-extraction, high-energy flotation anti-niobium, high-energy flotation extraction of tantalum, and high-energy flotation anti-tantalum, the oil phase components are first adjusted and mixed in a high-pressure reactor at 8 parts by mass of loaded metal (tantalum, niobium, or other impurities) 2-octanol or blank 2-octanol, 1 part by mass of pentanol, and 1 part by mass of toluene. The CO2 pressure in the reactor is controlled at 4.0-4.4 MPa, the temperature at 15-20℃, and the stirring time at 20 min. This yields a high-energy oil phase with a dissolved CO2 content of 12-16%. Subsequently, the high-energy oil phase is introduced into the aqueous phase through a polyethylene medium with an average pore size of 1 μm to form high-kinetic-energy gas-carried nano-oil droplets or nano-oil films, thereby completing the separation and purification of tantalum and niobium.

[0026] Following the above method, after two stages of high-energy flotation washing, the tungsten content in the oil phase containing impurities (tantalum and niobium) was 0.18 g / L, the antimony content was 0.2 g / L, and the oil phase loss was 0.5%. After one stage of high-energy flotation co-extraction, the tantalum and niobium content in the aqueous phase decreased to 0.06 g / L, the oil phase loss was 0.3%, and the tantalum and niobium recovery rates were 97.3% and 97.5%, respectively. After two stages of high-energy flotation anti-niobium treatment, the tantalum and niobium content in the oil phase decreased further. The niobium content was reduced to below 0.05 g / L, with an oil phase loss of 0.5%. After a first-stage high-energy flotation extraction of tantalum from the anti-niobium aqueous phase, the clean niobium solution contained 196 g / L of niobium and 0.05 g / L of tantalum, with an oil phase loss of 0.3% and a tantalum recovery rate of 97.1%. After a second-stage high-energy flotation anti-tantalum extraction of the tantalum-rich oil phase, the clean tantalum solution contained 76 g / L of tantalum and 0.04 g / L of niobium, with an oil phase loss of 0.3%. This process is far more efficient and produces a much higher purity product than existing technologies.

[0027] Example 3

[0028] Using the same impure tantalum-niobium oil phase as in Example 2, one additional unit operation was added to each of the high-energy flotation washing, high-energy flotation co-extraction, high-energy flotation anti-niobium, high-energy flotation tantalum extraction, and high-energy flotation anti-tantalum processes, and the preparation method of the high-energy oil phase was also the same as in Example 2.

[0029] Following the above method, after three stages of high-energy flotation washing, the tungsten content in the oil phase containing impurities (tantalum and niobium) was 0.07 g / L and the antimony content was 0.09 g / L, with an oil phase loss of 0.74%. After two stages of high-energy flotation co-extraction, the tantalum and niobium content in the aqueous phase decreased to 0.01 g / L, with an oil phase loss of 0.52%, and the tantalum and niobium recoveries were 98.9% and 99.2%, respectively. After three stages of high-energy flotation anti-niobium treatment, the tantalum and niobium content in the oil phase decreased further. The niobium content was reduced to below 0.01 g / L, with an oil phase loss of 0.76%. After two stages of high-energy flotation tantalum extraction, the niobium content in the clean niobium solution was 195 g / L, the tantalum content was 0.01 g / L, the oil phase loss was 0.45%, and the tantalum recovery rate reached 99.0%. After three stages of high-energy flotation tantalum extraction, the tantalum content in the clean tantalum solution was 77 g / L, the niobium content was 0.01 g / L, and the oil phase loss was 0.47%.

[0030] It is evident that adding one high-energy flotation unit operation to each separation and purification step can further improve the separation efficiency of tantalum and niobium, the recovery rate of tantalum and niobium, and the cleanliness of the tantalum / niobium solution, providing high-quality raw materials for the preparation of ultrapure tantalum and niobium products. This operation is far more efficient than existing technologies, and the purity of the product is also significantly higher.

[0031] Comparative Example 1

[0032] Using the same impurity-containing tantalum-niobium oil phase as in Example 1, and 4.0 mol / L sulfuric acid as the detergent, the impurities were eluted using a conventional oil-water countercurrent method at an oil-water volume ratio of 2:1. The results are shown in Table 1.

[0033] Table 1 Results of conventional multi-stage washing of oil phase containing impurities such as tantalum and niobium.

[0034]

[0035] As shown in Table 1, after 10 stages of washing, the tungsten impurity content in the oil phase was 0.6 g / L, the antimony impurity content was 0.8 g / L, and the oil phase loss rate was 1.2%. All of these indicators were significantly worse than those of the 2-stage high-energy flotation washing under the same conditions.

[0036] Comparative Example 2

[0037] Using the tantalum-niobium-rich oil phase from Example 2 as the object, and 0.75 mol / L sulfuric acid as the anti-niobium agent, niobium cascade back-extraction was performed using conventional back-extraction methods at an oil-water volume ratio of 2:1. The results are shown in Table 2.

[0038] Table 2 Results of conventional multi-stage anti-niobium reaction in tantalum- and niobium-rich oil phases

[0039]

[0040] As shown in Table 2, after 10 stages of back-extraction, the residual niobium content in the oil phase still reached 6.0 g / L, and the oil phase loss rate was 1.0%. All of these indicators were significantly worse than those of the 2-stage high-energy flotation niobium back-extraction under the same conditions.

[0041] Comparative Example 3

[0042] Using the anti-niobium aqueous phase from Example 2 as an example, the sulfuric acid concentration in the aqueous phase was adjusted to 0.8 mol / L, and tantalum was extracted using 2-octanol as the extractant at an oil-water volume ratio of 0.5:1 using conventional cascade extraction. The tantalum content in the resulting clean niobium solution is shown in Table 3.

[0043] Table 3 Results of conventional multi-stage extraction of tantalum in aqueous phase with anti-niobium properties

[0044]

[0045] As shown in Table 3, after 8 stages of back-extraction, the residual tantalum content in the oil phase still reached 0.6 g / L, and the tantalum recovery rate was 94.4%, which was significantly worse than that of the tantalum extracted by the first stage of high-energy flotation under the same conditions.

[0046] Comparative Example 4

[0047] Using the same raw materials as in Example 1, during the high-energy flotation washing process, 100% of the impurity-containing tantalum-niobium oil phase was directly placed in a high-pressure reactor with a CO2 pressure of 0.5-0.7 MPa and a temperature of 15-20°C and stirred for 20 minutes. Only an oil phase with a dissolved CO2 content of 2-3% was obtained. Subsequently, the oil phase was introduced into a 4.0 mol / L sulfuric acid solution through a polyethylene medium with an average pore size of 1 μm, and a two-stage flotation washing was performed at an oil-water volume ratio of 2:1. Analysis of the oil phase composition showed that the residual amount of tungsten impurities in the oil phase was 0.5 g / L and the residual amount of antimony impurities was 0.65 g / L, indicating poor impurity elution effect.

Claims

1. A process for high energy levitation separation and purification of tantalum and niobium, characterized by: Using an impure tantalum-niobium oil phase as the target, a tantalum-niobium-rich oil phase is obtained by performing 1-3 stages of high-energy flotation washing on the impure tantalum-niobium-rich oil phase and 1-2 stages of high-energy flotation co-extraction on the washing solution and the residual mineral extract, thus realizing the reuse of tantalum and niobium in the washing solution. Then, a tantalum-rich oil phase and a clean niobium solution are obtained by performing 1-3 stages of high-energy flotation reverse niobium on the tantalum-rich oil phase and 1-2 stages of high-energy flotation extraction on the reverse niobium aqueous phase, thus realizing the reuse of tantalum in the reverse niobium aqueous phase. Finally, a clean tantalum solution is obtained by performing 1-3 stages of high-energy flotation reverse tantalum on the tantalum-rich oil phase. The high-energy flotation process involves mixing a loaded metal oil phase or blank extractant with CO2 and an amphiphilic solvent, then pressurizing and energizing it to create a high-energy oil phase containing dissolved CO2. This high-energy oil phase is then introduced into an acidic or neutral aqueous phase through a porous medium, forming high-kinetic-energy micro / nano airborne oil droplets and oil films. In washing, anti-niobium, and anti-tantalum systems, metal ions are released from bottom to top and aggregate on the aqueous phase surface to form a low-loaded metal oil layer. In co-extraction and tantalum extraction systems, metal ions are captured from bottom to top and aggregate on the aqueous phase surface to form a high-loaded metal oil layer. The aforementioned pressurized energization refers to mixing 5-9.5 parts by mass of a loaded metal oil phase or blank extractant with 0.5-5 parts by mass of an amphiphilic solvent under conditions of CO2 pressure of 1-5 MPa and temperature of -10-40℃ to obtain a high-energy oil phase with a dissolved CO2 molar percentage of 4-20%. The loaded metal oil phase includes an impure tantalum-niobium oil phase, a tantalum-niobium rich oil phase, and a tantalum rich oil phase; the blank extractant is one or more of ketones, alcohols, and amines; the amphiphilic solvent is a solvent that is both CO2-friendly and compatible with the loaded metal oil phase or the blank extractant, specifically one or more of toluene, butanol, pentanol, butanone, pentanone, and hexane.

2. The method for high energy floatation separation and purification of tantalum and niobium according to claim 1, characterized in that: The impure tantalum-niobium oil phase is the tantalum-niobium oil phase obtained by acid leaching and pulp extraction of tantalum-niobium raw materials.

3. The method for high-energy flotation separation and purification of tantalum and niobium according to claim 1, characterized in that: The micro-nano airborne oil droplets and oil films are formed by the expansion of dissolved CO2 in a high-energy oil phase due to pressure release, with oil droplets adhering to CO2 bubbles and oil films covering CO2 bubbles. The diameter of the CO2 bubbles does not exceed 800 μm, the thickness of the oil film does not exceed 300 nm, and the diameter of the oil droplets does not exceed 500 nm.

4. The method for high-energy flotation separation and purification of tantalum and niobium according to claim 1, characterized in that: The impurity-containing tantalum-niobium oil phase is obtained by leaching tantalum-niobium raw materials with a mixed acid of sulfuric acid and hydrofluoric acid, followed by extraction with methyl isobutyl ketone, 2-octanol, or acetamide slurry, wherein the tantalum concentration is 10~80 g / L and the niobium concentration is 50~250 g / L.

5. The method for high-energy flotation separation and purification of tantalum and niobium according to claim 1, characterized in that: The aqueous phase acid concentrations during the washing, co-extraction, anti-niobium, tantalum extraction, and anti-tantalum processes are respectively: 3~4.5 mol / L sulfuric acid, 6~8 mol / L hydrofluoric acid mixed with 3.5~5 mol / L sulfuric acid, 0.5~0.8 mol / L sulfuric acid, 0.6~1.0 mol / L sulfuric acid, and 0~0.5 mol / L sulfuric acid; the oil phase-water phase volume ratio during the washing, anti-niobium, and anti-tantalum processes is (1~4):1; and the oil phase-water phase volume ratio during the co-extraction and tantalum extraction processes is (0.25~1):

1.

6. The method for high-energy flotation separation and purification of tantalum and niobium according to claim 1, characterized in that: The clean tantalum solution contains less than 0.1 g / L of niobium, and the clean niobium solution contains less than 0.1 g / L of tantalum. The clean tantalum solution and the clean niobium solution are used to prepare 3-6 N pure potassium fluorocarbonate, tantalum oxide and niobium oxide.

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