Method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste

Abstract

The invention belongs to the technical field of recycling of renewable resources, and particularly relates to a method for efficiently recycling niobium and titanium from niobium-titanium superconducting alloy waste. According to the method, after the outer coating layer of the outer niobium-titanium superconducting alloy waste is removed, the mixed chlorinated melt is obtained through direct chlorination, then titanium tetrachloride and niobium chloride are separated through a rectifying tower by means of the property that the boiling point difference of melts such as titanium tetrachloride and niobium chloride in the mixed chlorinated melt is large, and the niobium-titanium superconducting alloy waste is obtained. And then titanium oxide and niobium oxide can be obtained through hydrolysis, drying and dehydration, the titanium and niobium recovery effect is good, and therefore the technical problem that a method for efficiently recovering niobium and titanium is lacked in the prior art is solved.

Description

Technical Field

[0001] The present application belongs to the field of renewable resource recovery technology, and in particular relates to a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste. Background Art

[0002] Niobium-titanium alloy is the most widely used alloy superconducting material. Its superconducting transition temperature is 8~10K. Adding other elements can further improve the superconducting performance. It has broad application prospects in medical imaging equipment such as magnetic resonance imaging scanners, and large scientific equipment such as particle accelerators.

[0003] However, the reserves of niobium in the earth's crust are relatively low, with a content of 0.002% in the earth's crust and a natural reserve of 520wt. The natural reserves of niobium limit the large-scale application of niobium-titanium alloy superconducting materials; the inner layer of niobium-titanium alloy of niobium-titanium superconducting alloy materials is usually manufactured into rods or wires, and a layer of metal copper coating is coated on the surface. Niobium-titanium-copper superconducting alloy materials will generate waste during the manufacturing process and use process, which wastes niobium resources. By researching and developing a simple and rapid method for recovering niobium and titanium from niobium-titanium alloy waste, the recycling of niobium resources can be achieved, which is of great significance for the widespread application of niobium-titanium alloys. Summary of the invention

[0004] In view of this, the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, which is used to solve the technical problem of the lack of a method for efficiently recovering niobium and titanium in the prior art.

[0005] The first aspect of the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, comprising the steps of:

[0006] Step S1, placing niobium-titanium superconducting alloy waste in an acidic solution to remove the coating layer to obtain an inner layer of niobium-titanium alloy;

[0007] Step S2, forming the niobium-titanium alloy into small pieces or powders and mixing them with carbon powder to obtain a chlorination reaction precursor;

[0008] Step S3, placing the chlorination reaction precursor in a chlorination furnace for chlorination to obtain a mixed chlorinated melt;

[0009] Step S4, under a nitrogen atmosphere, sending the mixed chlorinated melt into a distillation tower with a middle layer temperature of 240-250° C. and a top layer temperature of 130-135° C. for separation, collecting the niobium chloride melt in the middle layer of the distillation tower and the titanium tetrachloride melt at the top layer of the distillation tower;

[0010] Step S5, placing the niobium chloride melt and the titanium tetrachloride melt in an acidic aqueous solution for hydrolysis, respectively, to obtain a hydrated niobium oxide precipitate and a hydrated titanium oxide precipitate;

[0011] Step S6: drying and dehydrating the hydrated niobium oxide precipitate and the hydrated titanium oxide precipitate respectively to obtain niobium oxide and titanium oxide.

[0012] Preferably, in step S1, the acidic solution is a nitric acid solution with a concentration of 40-60%.

[0013] Preferably, in step S2, the method of making small pieces is cutting, and the method of making powder is grinding.

[0014] Preferably, in step S2, the mass ratio of the niobium-titanium alloy to the carbon powder is 100:10-30.

[0015] Preferably, in step S3, the temperature of the chlorination reaction is 800-900° C., and the time is 4-12 hours.

[0016] Preferably, in step S4, the bottom temperature of the distillation tower is 280-300°C.

[0017] Preferably, in step S5, the acidic aqueous solution is a hydrochloric acid aqueous solution with a pH of 3.5-4.

[0018] Preferably, in step S5, the niobium chloride melt is placed in an acidic aqueous solution for hydrolysis at a temperature of 20-60° C. for a time of 2-4 hours.

[0019] Preferably, in step S5, the temperature of the titanium chloride melt being placed in the acidic aqueous solution for hydrolysis is 20-40° C. and the time is 2-4 hours.

[0020] Preferably, in step S6, the temperature of the drying and dehydration is 100-120°C.

[0021] In summary, the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, which is used to solve the technical problem of the lack of a method for efficiently recovering niobium and titanium in the prior art. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the specific implementation methods of the present application or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0023] Figure 1 A schematic flow chart of a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in Example 1 of the present application. DETAILED DESCRIPTION

[0024] The present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, which is used to solve the technical problem that there is a lack of a method for efficiently recovering niobium and titanium in the prior art.

[0025] The technical solution of the present application will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present application.

[0026] In view of the defect that there is currently a lack of methods for efficiently recovering niobium and titanium, the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste; the recovery method comprises: firstly placing the niobium-titanium superconducting alloy waste in an acidic solution to remove the coating layer to obtain an inner layer of niobium-titanium alloy; then making the niobium-titanium alloy into small pieces or powders and mixing them with carbon powder to obtain a chlorination reaction precursor; next placing the chlorination reaction precursor in a chlorination furnace for chlorination to obtain a mixed chlorinated melt; then sending the mixed chlorinated melt into a distillation tower with a middle layer temperature of 240-250° C. and a top layer temperature of 130-135° C. for separation, collecting the niobium chloride melt in the middle layer of the distillation tower and the titanium tetrachloride melt at the top layer of the distillation tower; then placing the niobium chloride melt and the titanium tetrachloride melt in an acidic aqueous solution for hydrolysis respectively to obtain a hydrated niobium oxide precipitate and a hydrated titanium oxide precipitate; and drying and dehydrating the hydrated niobium oxide precipitate and the hydrated titanium oxide precipitate respectively to obtain niobium oxide and titanium oxide.

[0027] In the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the outer coating layer of the niobium-titanium superconducting alloy waste is successfully removed by utilizing the mechanism that the copper material of the outer coating layer of the niobium-titanium superconducting alloy waste easily reacts with the acid solution, thereby obtaining the niobium-titanium alloy; and the niobium-titanium alloy is mixed with carbon powder and placed in a chlorination furnace for chlorination. The chlorination used in the present application is a method for directly obtaining a niobium-titanium melt, which can avoid the defects of poor effect of water leaching separation of niobium and titanium and low recovery rate of niobium and titanium after calcination of the traditional niobium-titanium alloy with a strong alkali; and the niobium-titanium alloy is mixed with carbon powder and placed in a chlorination furnace for chlorination. Before fusion, the present application prepares the niobium-titanium alloy into small pieces or powders to increase the surface area of ​​the niobium-titanium alloy, thereby increasing the contact area between the niobium-titanium alloy and the carbon powder and the chlorine gas, promoting the generation of a mixed chlorinated melt such as titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride, which is beneficial to the recovery of titanium and niobium. At the same time, after chlorination to obtain a mixed chlorinated melt, the present application controls the middle layer temperature of the distillation tower to be 240-250°C, the top layer temperature to be 130-135°C, and after introducing a nitrogen atmosphere, the mixed chlorinated melt is sent to the distillation tower for separation. The temperature of the distillation tower is increased from the bottom layer, the middle layer, and the top layer to the top layer. The temperature of the bottom, middle and top layers gradually increases, and the temperature difference between the bottom, middle and top layers can be used to separate substances with different boiling points. The temperature of the middle layer of the distillation tower is 240-250°C, which is slightly lower than the boiling point of niobium chloride, and the temperature of the top layer is 130-135°C, which is slightly lower than the boiling point of titanium tetrachloride. This allows the present application to collect niobium chloride melt and titanium tetrachloride melt in the middle and top layers of the distillation tower, respectively, to achieve the separation of niobium and titanium components. In addition, due to the large difference in boiling points between niobium chloride and titanium tetrachloride, the separated niobium chloride melt and titanium tetrachloride melt have higher purity. Niobium oxide and titanium oxide can be obtained by hydrolyzing niobium chloride melt and titanium tetrachloride melt and then drying them; therefore, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, a niobium-titanium mixed chloride melt is directly obtained by chlorinating the niobium-titanium alloy into small pieces or powders, and the niobium chloride and titanium tetrachloride are effectively separated by utilizing the large difference in boiling points between niobium chloride and titanium tetrachloride, and the niobium and titanium recovery rate and purity are high, which is a method for efficiently recovering niobium and titanium, thereby overcoming the defect of the current lack of a method for efficiently recovering niobium and titanium.

[0028] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the acidic solution is selected from a nitric acid solution, and the concentration is controlled to be 40-60%; the nitric acid solution will react with the copper material of the coating layer at room temperature, but will not react with the niobium-titanium alloy, thereby retaining the niobium-titanium alloy while removing the coating layer, which is beneficial to improving the recovery rate.

[0029] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the method for making the niobium-titanium alloy into small pieces can be cutting, and the method for making it into powder can be grinding. Compared with small pieces, grinding the niobium-titanium alloy into powder is more conducive to the chlorination reaction to generate a niobium-titanium mixed chlorinated melt. However, compared with grinding the niobium-titanium alloy into powder, the process of cutting the niobium-titanium alloy into small pieces is simpler. Therefore, technicians can choose according to actual needs.

[0030] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the ratio of carbon powder to niobium-titanium alloy is controlled to be 100:10-30 in the chlorination reaction to promote the chlorination reaction.

[0031] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the temperature of the chlorination reaction needs to be controlled to be 800-900°C and the time to be 4-12 hours in the chlorination reaction to promote the chlorination reaction to generate a mixed chlorination melt including titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride.

[0032] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, the bottom layer of the distillation tower is the injection position of titanium tetrachloride melt, niobium chloride and a small amount of mixed chlorinated melt such as niobium oxychloride, and the temperature is 280-300°C.

[0033] Preferably, in the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in the present application, during the hydrolysis of niobium chloride melt and titanium chloride melt, the hydrolysis temperature of the niobium chloride melt is slightly higher than the hydrolysis temperature of the titanium chloride melt; the temperature for hydrolysis of the niobium chloride melt is 20-60°C, while the temperature for hydrolysis of the titanium chloride melt is 20-40°C.

[0034] The following will specifically describe a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided by the present application in combination with examples and recovery data of niobium and titanium.

[0035] Example 1

[0036] Embodiment 1 of the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, the method comprising: a step of removing a coating layer, a step of preparing a chlorination reaction precursor, a step of chlorination reaction, a step of separation in a distillation tower, a step of hydrolysis, and a step of drying and dehydration.

[0037] The step of removing the coating layer includes: weighing 30 kg of niobium-titanium superconducting alloy waste and 10 kg of nitric acid solution (50%), and then immersing the niobium-titanium superconducting alloy waste in the nitric acid solution (50%) to remove the coating layer of the outer layer of the niobium-titanium superconducting alloy waste to obtain an inner layer of niobium-titanium alloy, which weighs about 11.31 kg;

[0038] The steps of preparing the chlorination reaction precursor include: cutting the inner layer of niobium-titanium alloy into small pieces, washing and drying the pieces with deionized water, and then mixing the pieces with 1.70 kg of carbon powder in a mass ratio of 100:15 to obtain the chlorination reaction precursor.

[0039] The steps of the chlorination reaction include: placing a chlorination reaction precursor into a chlorination furnace, introducing nitrogen and setting a temperature rise program for the chlorination furnace to replace the air in the chlorination furnace and take away the moisture introduced by the material; after the temperature of the chlorination furnace reaches the set 850°C, the chlorination reaction is carried out for 8 hours, and then the temperature is lowered to 120°C to take out the melt in the chlorination furnace to obtain a mixed chlorination melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride).

[0040] The steps of separation in the distillation tower include: after nitrogen is passed through the distillation equipment in advance to replace the air, the distillation tower temperature rising program is set, the bottom temperature of the distillation tower is set to 280°C, the middle layer temperature of the tower is set to 245°C, and the top temperature of the tower is set to 130°C. After the bottom, middle layer and top of the distillation tower reach the set temperature, the mixed chlorinated melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride) is transferred to the distillation tower. The melt collected in the middle layer of the distillation tower is the separated niobium chloride melt, and the melt collected at the top of the tower is the separated titanium tetrachloride melt. The niobium chloride melt and the titanium tetrachloride melt are stored in transfer tanks and other equipment.

[0041] The hydrolysis step includes: adding titanium tetrachloride melt to dilute hydrochloric acid (pH controlled at 3.5) for hydrolysis, the mass of the dilute hydrochloric acid is three to five times that of titanium tetrachloride, keeping warm at 30°C, stirring for 4 hours, filtering to obtain hydrated titanium oxide precipitate; adding the obtained niobium chloride melt to dilute hydrochloric acid water (pH controlled at 3.5) for hydrolysis, the mass of the dilute hydrochloric acid is four to five times that of niobium chloride, keeping warm at 55°C, stirring for 4 hours, and centrifuging to obtain hydrated niobium oxide precipitate.

[0042] The drying and dehydration step includes: drying and dehydrating the hydrated titanium oxide precipitate and the hydrated niobium oxide precipitate in an oven at 100-120° C., respectively, to obtain 8.64 kg of titanium oxide and 7.93 kg of niobium oxide.

[0043] Example 2

[0044] Embodiment 2 of the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, the method comprising: a step of removing a coating layer, a step of preparing a chlorination reaction precursor, a step of chlorination reaction, a step of separation in a distillation tower, a step of hydrolysis, and a step of drying and dehydration.

[0045] The step of removing the coating layer comprises: weighing 30 kg of the same niobium-titanium superconducting alloy waste as in Example 1 and 10 kg of nitric acid solution (50%), and then immersing the niobium-titanium superconducting alloy waste in the nitric acid solution (50%) to remove the coating layer of the outer layer of the niobium-titanium superconducting alloy waste to obtain the inner layer of niobium-titanium alloy, which weighs about 11.31 kg;

[0046] The steps of preparing the chlorination reaction precursor include: cutting the inner layer of niobium-titanium alloy into small pieces, washing and drying the pieces with deionized water, and then mixing the pieces with 1.70 kg of carbon powder in a mass ratio of 100:15 to obtain the chlorination reaction precursor.

[0047] The steps of the chlorination reaction include: placing a chlorination reaction precursor into a chlorination furnace, introducing nitrogen and setting a temperature rise program for the chlorination furnace to replace the air in the chlorination furnace and take away the moisture introduced by the material; after the temperature of the chlorination furnace reaches the set 900°C, the chlorination reaction is carried out for 4 hours, and then the temperature is lowered to 100°C to take out the melt in the chlorination furnace to obtain a mixed chlorination melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride).

[0048] The steps of separation in the distillation tower include: after nitrogen is passed through the distillation equipment in advance to replace the air, the distillation tower temperature program is set, the bottom temperature of the distillation tower is set to 300°C, the middle layer temperature of the tower is set to 248°C, and the top temperature of the tower is set to 134°C. After the bottom, middle layer and top of the distillation tower reach the set temperature, the mixed chlorinated melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride) is transferred to the distillation tower. The melt collected in the middle layer of the distillation tower is the separated niobium chloride melt, and the melt collected at the top of the tower is the separated titanium tetrachloride melt. The niobium chloride melt and the titanium tetrachloride melt are stored in transfer tanks and other equipment.

[0049] The hydrolysis step comprises: adding titanium tetrachloride melt to dilute hydrochloric acid (pH controlled at 4) for hydrolysis, the mass of the dilute hydrochloric acid being three to five times that of titanium tetrachloride, keeping the temperature at 20°C, stirring for 4 hours, filtering to obtain a hydrated titanium oxide precipitate; adding the obtained niobium chloride melt to dilute hydrochloric acid water (pH controlled at 4) for hydrolysis, the mass of the dilute hydrochloric acid being four to five times that of niobium chloride, keeping the temperature at 20°C, stirring for 4 hours, and centrifuging to obtain a hydrated niobium oxide precipitate.

[0050] The drying and dehydration step includes: drying and dehydrating the hydrated titanium oxide precipitate and the hydrated niobium oxide precipitate in an oven at 100-120° C., respectively, to obtain 8.43 kg of titanium oxide and 7.68 kg of niobium oxide.

[0051] Example 3

[0052] Embodiment 3 of the present application provides a method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, the method comprising: a step of removing a coating layer, a step of preparing a chlorination reaction precursor, a step of chlorination reaction, a step of separation in a distillation tower, a step of hydrolysis, and a step of drying and dehydration.

[0053] The step of removing the coating layer comprises: weighing 30 kg of the same niobium-titanium superconducting alloy waste as in Example 1 and 10 kg of nitric acid solution (50%), and then immersing the niobium-titanium superconducting alloy waste in the nitric acid solution (50%) to remove the coating layer of the outer layer of the niobium-titanium superconducting alloy waste to obtain the inner layer of niobium-titanium alloy, which weighs about 11.31 kg;

[0054] The steps of preparing the chlorination reaction precursor include: cutting the inner layer of niobium-titanium alloy into small pieces, washing and drying the pieces with deionized water, and then mixing the pieces with 1.70 kg of carbon powder in a mass ratio of 100:15 to obtain the chlorination reaction precursor.

[0055] The steps of the chlorination reaction include: placing a chlorination reaction precursor into a chlorination furnace, introducing nitrogen and setting a temperature rise program for the chlorination furnace to replace the air in the chlorination furnace and take away the moisture introduced by the material; after the temperature of the chlorination furnace reaches the set 900°C, the chlorination reaction is carried out for 8 hours, and then the temperature is lowered to 120°C to take out the melt in the chlorination furnace to obtain a mixed chlorination melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride).

[0056] The steps of separation in the distillation tower include: after nitrogen is passed through the distillation equipment in advance to replace the air, the distillation tower temperature rising program is set, the bottom temperature of the distillation tower is set to 280°C, the middle layer temperature of the tower is set to 245°C, and the top temperature of the tower is set to 130°C. After the bottom, middle layer and top of the distillation tower reach the set temperature, the mixed chlorinated melt (titanium tetrachloride melt, niobium chloride and a small amount of niobium oxychloride) is transferred to the distillation tower. The melt collected in the middle layer of the distillation tower is the separated niobium chloride melt, and the melt collected at the top of the tower is the separated titanium tetrachloride melt. The niobium chloride melt and the titanium tetrachloride melt are stored in transfer tanks and other equipment.

[0057] The hydrolysis step includes: adding titanium tetrachloride melt to dilute hydrochloric acid (pH controlled at 3.5) for hydrolysis, the mass of the dilute hydrochloric acid is three to five times that of titanium tetrachloride, keeping the temperature at 40°C, stirring for 4 hours, filtering to obtain hydrated titanium oxide precipitate; adding the obtained niobium chloride melt to dilute hydrochloric acid water (pH controlled at 3.5) for hydrolysis, the mass of the dilute hydrochloric acid is four to five times that of niobium chloride, keeping the temperature at 60°C, stirring for 4 hours, and centrifuging to obtain hydrated niobium oxide precipitate.

[0058] The drying and dehydration step includes: drying and dehydrating the hydrated titanium oxide precipitate and the hydrated niobium oxide precipitate in an oven at 100-120° C., respectively, to obtain 8.72 kg of titanium oxide and 7.85 kg of niobium oxide.

[0059] Experimental Example 4

[0060] This Experimental Example 4 is the recovery data of the method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste provided in Examples 1-3.

[0061] Table 1: Recovery data of niobium and titanium in the method provided in Example 1

[0062]

[0063] Table 2: Recovery data of niobium and titanium in the method provided in Example 2

[0064]

[0065] Table 3: Recovery data of niobium and titanium in the method provided in Example 2

[0066]

[0067] It can be seen from Table 1-3 that 30 kg of niobium-titanium superconducting alloy waste contains about 5.89 kg of niobium and about 5.42 kg of titanium, while the method provided in Example 1 can recover 7.93 kg of niobium oxide (Nb2O5), containing about 5.54 kg of niobium, and the recovery rate of niobium is about 94%, and can recover 8.64 kg of titanium oxide (TiO2), containing about 5.18 kg of titanium, and the recovery rate of titanium is about 95%; this shows that the method provided in this embodiment directly obtains a niobium-titanium mixed chlorinated melt by chlorinating the niobium-titanium alloy into small pieces, and the recovery rate of niobium and titanium is good, avoiding the defect of poor effect of water leaching separation of niobium and titanium after strong alkali calcination, and at the same time, utilizing the large difference in boiling points between niobium chloride and titanium tetrachloride, niobium chloride and titanium tetrachloride are effectively separated, thereby improving the purity of niobium and titanium and avoiding mutual doping of niobium and titanium. Therefore, the method provided in this embodiment is a method for efficiently recovering niobium and titanium.

[0068] It can be further seen from Tables 1-3 that after adjusting the temperature and the pH value of hydrochloric acid hydrolysis in Example 2-3, the effect of recovering niobium and titanium changed slightly, but the recovery rate was still maintained at more than 91%.

[0069] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, a person skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some or all of the technical features thereof may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste, characterized in that: Includes steps: Step S1, placing niobium-titanium superconducting alloy waste in an acidic solution to remove the coating layer to obtain an inner layer of niobium-titanium alloy; Step S2, forming the niobium-titanium alloy into small pieces or powders and mixing them with carbon powder to obtain a chlorination reaction precursor; Step S3, placing the chlorination reaction precursor in a chlorination furnace for chlorination to obtain a mixed chlorinated melt; Step S4, under a nitrogen atmosphere, sending the mixed chlorinated melt into a distillation tower with a middle layer temperature of 240-250° C. and a top layer temperature of 130-135° C. for separation, collecting the niobium chloride melt in the middle layer of the distillation tower and the titanium tetrachloride melt at the top layer of the distillation tower; Step S5, placing the niobium chloride melt and the titanium tetrachloride melt in an acidic aqueous solution for hydrolysis, respectively, to obtain a hydrated niobium oxide precipitate and a hydrated titanium oxide precipitate; Step S6: drying and dehydrating the hydrated niobium oxide precipitate and the hydrated titanium oxide precipitate respectively to obtain niobium oxide and titanium oxide.

2. A method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S1, the acidic solution is a nitric acid solution with a concentration of 20-80%.

3. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S2, the method of making small pieces is cutting, and the method of making powder is grinding.

4. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S2, the mass ratio of the niobium-titanium alloy to the carbon powder is 100:10-30.

5. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S3, the temperature of the chlorination reaction is 800-900° C., and the time is 4-12 hours.

6. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S4, the bottom temperature of the distillation tower is 280-300°C.

7. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S5, the acidic aqueous solution is a hydrochloric acid aqueous solution with a pH of 3.5-4.

8. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S5, the niobium chloride melt is placed in an acidic aqueous solution for hydrolysis at a temperature of 20-60° C. for a time of 2-4 hours.

9. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S5, the titanium chloride melt is placed in an acidic aqueous solution for hydrolysis at a temperature of 20-40° C. for a time of 2-4 hours.

10. The method for efficiently recovering niobium and titanium from niobium-titanium superconducting alloy waste according to claim 1, characterized in that: In step S6, the temperature of the drying and dehydration is 100-120°C.

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