CN113373312A - Method for separating and recovering tantalum, scandium and aluminum - Google Patents
Method for separating and recovering tantalum, scandium and aluminum Download PDFInfo
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- CN113373312A CN113373312A CN202110647128.7A CN202110647128A CN113373312A CN 113373312 A CN113373312 A CN 113373312A CN 202110647128 A CN202110647128 A CN 202110647128A CN 113373312 A CN113373312 A CN 113373312A
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C01F17/00—Compounds of rare earth metals
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- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C22B21/00—Obtaining aluminium
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- C22B21/0023—Obtaining aluminium by wet processes from waste materials
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Abstract
The invention provides a method for separating and recovering tantalum, scandium and aluminum, which comprises the following steps: s1, crushing the tantalum crucible scrap to obtain fragments, pickling, collecting pickling solution, and drying the fragments; s2, heating the dried fragments, and introducing hydrogen to embrittle the fragments; s3, further crushing and grinding the fragments into powder after the embrittlement treatment, then removing impurities by acid washing, and collecting acid washing liquid; s4, drying the powder obtained in the step S3, and carrying out dehydrogenation treatment to obtain tantalum powder; s5, concentrating the pickling solution obtained in the step S1 and S3, adding an extraction solution into the concentrated solution to extract scandium, collecting raffinate, carrying out acid pickling on an organic phase obtained by extraction, and adding a stripping agent to carry out stripping treatment to obtain a scandium-containing precipitate, wherein the extraction solution comprises an extraction agent and a diluent; s6, calcining the precipitate obtained in the step S5 to obtain scandium oxide or scandium fluoride; s7, adding sodium hydroxide into the raffinate obtained in the step S6 to adjust the pH value to obtain a precipitate, and calcining the precipitate to obtain the alumina.
Description
Technical Field
The disclosure relates to the field of secondary resource recovery, in particular to a method for separating and recovering tantalum, scandium and aluminum.
Background
The aluminum-scandium alloy has comprehensive properties of high strength, corrosion resistance, high temperature resistance and good weldability, and has wide application in advanced scientific and technological fields of aerospace, nuclear engineering and the like, and fields of transportation, household appliances and the like. With the rapid development of science and technology and the emphasis of various countries on the research of key materials for the key field, the demand of aluminum-scandium alloy targets with high scandium content is increasing day by day. However, during the target processing and production process, a small amount of scandium may adhere to the fragments or scraps of the tantalum crucible, resulting in scandium loss, and therefore, if tantalum and scandium in the scrap can be efficiently recovered, the production cost of the aluminum scandium target and the solid waste pollution generated in the production process can be greatly reduced.
Disclosure of Invention
In view of the problems of the background art, the present disclosure aims to provide a method for separating and recovering tantalum, scandium and aluminum, which has a short process flow, low equipment investment, simple operation, no generation of fluorine-containing wastewater, waste gas and waste residues, and can obtain 3N5 high-purity tantalum metal powder and scandium oxide powder.
In some embodiments, the method for separating and recovering tantalum scandium aluminum provided by the present disclosure includes the following steps: s1, crushing the tantalum crucible scrap to obtain fragments, pickling, collecting pickling solution, and drying the fragments; s2, heating the dried chips obtained in the step S1, and introducing hydrogen to embrittle the chips; s3, further crushing and grinding the fragments into powder after the embrittlement treatment, removing impurities by acid washing, and collecting acid washing liquid; s4, drying the powder obtained in the step S3, and then carrying out dehydrogenation treatment to obtain tantalum powder; s5, concentrating the pickling solution obtained in the step S1 and S3, adding an extraction solution into the concentrated solution to extract and enrich scandium elements, collecting raffinate, carrying out acid pickling on an organic phase obtained by extraction, and adding a stripping agent to carry out stripping treatment to obtain a scandium-containing element precipitate, wherein the extraction solution comprises an extracting agent and a diluting agent; s6, calcining the precipitate obtained in the step S5 to obtain scandium oxide or scandium fluoride; s7, adding sodium hydroxide into the raffinate obtained in the step S6 to adjust the pH value to obtain a precipitate, and calcining the precipitate to obtain the alumina.
In some embodiments, in step S1, the acid used for acid washing is at least one of hydrochloric acid or sulfuric acid; the acid used for pickling has the volume fraction of 10-20%, the pickling temperature is 70-90 ℃, and the pickling time is 2-4 h.
In some embodiments, in step S2, the process conditions of the embrittlement treatment are: putting the fragments into a tubular furnace for embrittlement treatment, firstly introducing protective gas argon into the tubular furnace to remove air and moisture in the fragments, and then introducing hydrogen into the tubular furnace, wherein the heating temperature is 700-800 ℃, the flow rate of the hydrogen is 1.5-2L/min, and the time is 60-120 min.
In some embodiments, in step S3, the prepared powder has a particle size of-120 mesh to +200 mesh, the acid used for acid washing is one or a mixture of two of sulfuric acid and hydrochloric acid, the acid concentration is 10% to 30%, the acid washing time is 2h to 4h, and the acid washing temperature is 70 ℃ to 90 ℃.
In some embodiments, in step S4, the process conditions for dehydrogenation are: and putting the dried powder into a tubular furnace, setting the temperature to be 700-900 ℃, and introducing argon with the gas flow rate of 1-2L/min for 2-4 h.
In some embodiments, in step S5: the extractant is one or a mixture of more than two of bis (2-ethylhexyl) phosphate, bis (2,4, 4-trimethylpentyl) phosphinic acid and tributyl phosphate; the stripping agent is at least one of sodium hydroxide solution, oxalic acid, ammonia water and ammonium fluoride solution; washing with sulfuric acid or hydrochloric acid; the diluent is kerosene.
In some embodiments, in step S5: the concentration of scandium element in the obtained concentrated solution is 200mg/L to 500 mg/L; the volume fraction of the extractant in the extraction liquid is 5 to 10 percent; the acid concentration adopted by acid washing is 2mol/L to 4 mol/L; the concentration of the stripping agent is 5 to 10 percent, and the stripping temperature is 25 to 70 ℃.
In some embodiments, in step S6, the temperature of the calcination is 700 ℃ to 800 ℃.
In some embodiments, in step S7, the pH is adjusted in the range of 4 to 5.
In some embodiments, in step S1, the composition of the tantalum crucible scrap includes metallic tantalum and adhered aluminum scandium alloy or scrap.
The beneficial effects of this disclosure are as follows: the method combines the wet method and the pyrogenic method, has short total process flow, avoids leaching of hydrofluoric acid in the separation and purification process, has no problem of treatment of fluorine-containing waste liquid, reduces the investment of extraction equipment, can simultaneously separate and recover tantalum and scandium, has high separation efficiency, achieves the recovery rate of metal tantalum above 98 percent and the purity of the metal tantalum above 99.95 percent, achieves the recovery rate of scandium oxide obtained by separation above 95 percent and achieves the purity of 99.95 percent. The process can realize the efficient recycling of the valuable metals of tantalum and scandium in the tantalum crucible fragments for the aluminum-scandium target material, and reduces the energy consumption and the product research and development cost.
Drawings
Fig. 1 is a schematic flow chart of the method for separating and recovering tantalum, scandium and aluminum according to the present disclosure.
Detailed Description
It is to be understood that the disclosed embodiments are merely exemplary of the disclosure that may be embodied in various forms, and that specific details of the disclosure are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the disclosure. In the description of the present disclosure, terms and terms not specifically described are common general knowledge of those skilled in the art, and methods not specifically described are conventional methods known to those skilled in the art.
In the description of the present disclosure, the stripping agent may be an aqueous solution, the concentration of the stripping agent being the concentration of the solute in water; the concentration of the extracting agent is the volume concentration of the extracting agent in an organic extraction liquid formed by the extracting agent and an organic diluent (and a modifier), wherein the modifier can be selectively added, and the organic diluent comprises kerosene.
The method for separating and recovering tantalum, scandium and aluminum of the present disclosure is described next.
The method aims at tantalum-scandium-containing waste materials, provides a technological method of pickling pretreatment, physical method and extraction enrichment for separating, purifying and enriching tantalum scandium, and can effectively avoid the problems of corrosion of high-temperature chlorination to equipment, fluorine-containing wastewater caused by hydrofluoric acid leaching and the like. The tantalum scandium-containing waste material of the present disclosure may be derived from, but is not limited to, tantalum crucible fragments for aluminum scandium targets.
In some embodiments, the method for separating and recovering tantalum scandium aluminum provided by the present disclosure includes the following steps: s1, crushing the tantalum crucible scrap to obtain fragments, pickling, collecting pickling solution, and drying the fragments; s2, heating the dried chips obtained in the step S1, and introducing hydrogen to embrittle the chips; s3, further crushing and grinding the fragments into powder after the embrittlement treatment, removing impurities by acid washing, and collecting acid washing liquid; s4, drying the powder obtained in the step S3, and then carrying out dehydrogenation treatment to obtain tantalum powder; s5, concentrating the pickling solution obtained in the step S1 and S3, adding an extraction solution into the concentrated solution to extract and enrich scandium elements, collecting raffinate, carrying out acid pickling on an organic phase obtained by extraction, and adding a stripping agent to carry out stripping treatment to obtain a scandium-containing element precipitate, wherein the extraction solution comprises an extracting agent and a diluting agent; s6, calcining the precipitate obtained in the step S5 to obtain scandium oxide or scandium fluoride; s7, adding sodium hydroxide into the raffinate obtained in the step S6 to adjust the pH value to obtain a precipitate, and calcining the precipitate to obtain the alumina.
In some embodiments, in step S1, the tantalum crucible waste material may be in the shape of a crucible or a block, and may be processed into chips by a jaw crusher, the maximum size of the chips being less than 8 cm.
In some embodiments, in step S1, the acid used for acid washing is at least one of hydrochloric acid or sulfuric acid; the volume fraction of acid used for acid washing is 10-20%, the acid washing temperature is 70-90 ℃, the acid washing time is 2-4 h, and the acid washing aims at removing other impurities and improving the separation and recovery purity.
The hydrogen embrittlement treatment of step S2 is to utilize the characteristics of tantalum itself, and can absorb hydrogen to generate hydride at a temperature of more than 400 ℃, and can effectively separate from other metals. In some embodiments, to further ensure the separation effect, the process conditions of the embrittlement treatment in step S2 may be: putting the fragments into a tubular furnace for embrittlement treatment, firstly introducing protective gas argon into the tubular furnace to remove air and moisture in the fragments, and then introducing hydrogen into the tubular furnace, wherein the heating temperature is 700-800 ℃, the flow rate of the hydrogen is 1.5-2L/min, and the time is 60-120 min.
In some embodiments, in step S3, the particle size of the powder is-120 mesh to +200 mesh, the acid used for acid washing is one or a mixture of two of sulfuric acid and hydrochloric acid, the acid concentration is 10% to 30%, the acid washing time is 2h to 4h, the acid washing temperature is 70 ℃ to 90 ℃, and the acid washing in this step is aimed at further reducing the chemical impurities in the tantalum hydride powder, particularly the chemical impurities introduced by stripping Ti, Cu and the like from the target material.
In some embodiments, in step S4, the process conditions for dehydrogenation are: and placing the dried powder in a tubular furnace, setting the temperature to be 700-900 ℃, introducing argon with the flow rate of 1-2L/min, introducing the argon for 2-4 h, wherein the hydrogenated metal tantalum has the characteristic of releasing hydrogen under the conditions of high temperature and low hydrogen partial pressure, and obtaining the metallurgical-grade tantalum powder by a dehydrogenation process.
In some embodiments, in step S5: the extractant is one or a mixture of more than two of bis (2-ethylhexyl) phosphate (P204), bis (2,4, 4-trimethylpentyl) phosphinic acid (Cyanex272) and tributyl phosphate (TBP); the stripping agent is at least one of sodium hydroxide solution, oxalic acid, ammonia water and ammonium fluoride solution; washing with sulfuric acid or hydrochloric acid; the diluent is kerosene.
In some embodiments, in step S5: the concentration of scandium element in the obtained concentrated solution is 200mg/L to 500 mg/L; the volume fraction of the extractant in the extraction liquid is 5 to 10 percent; the acid concentration adopted by acid washing is 2mol/L to 4 mol/L; the concentration of the stripping agent is 5 to 10 percent, and the stripping temperature is 25 to 70 ℃.
In some embodiments, in step S6, the temperature of the calcination is 700 ℃ to 800 ℃.
In some embodiments, in step S7, the pH is adjusted in the range of 4 to 5.
In some embodiments, in step S1, the composition of the tantalum crucible scrap includes metallic tantalum and adhered aluminum scandium alloy or scrap.
By the method for separating and recovering tantalum, scandium and aluminum, the recovery rate of tantalum can reach more than 98%, and the purity can reach more than 99.95%; the recovery rate of scandium oxide obtained by separation reaches 95%, and the purity of scandium oxide can reach 99.95%; the extraction waste liquid can be separated and recycled by a precipitation method to obtain alumina, and the waste liquid reaches the national wastewater discharge standard. For the tantalum crucible fragments for the aluminum scandium target material, the process disclosed by the invention can realize effective recycling of valuable metals of tantalum and scandium, and reduce the research and development cost of products.
The disclosure is further illustrated with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure. In the following examples and comparative examples, reagents, materials and instruments used were commercially available or prepared by methods known in the art, unless otherwise specified.
Example 1
Simply crushing the aluminum-scandium target material by using tantalum crucible fragment waste to obtain fragments, cleaning the fragments by using sulfuric acid with the concentration of 10% for 2 hours, drying, and collecting pickling solution; putting the acid-washed fragments into a tube furnace for hydrogen embrittlement treatment: introducing argon for 30min to remove air and water, setting the heating temperature at 700 deg.C, and introducing hydrogen at 1.5L/min for 80 min; preparing the hydrogen embrittlement treated fragments into powder with the granularity of-120 meshes to +200 meshes by using a sample preparation machine, cleaning for 3 hours by using sulfuric acid with the concentration of 10%, wherein the pickling temperature is 90 ℃, and collecting pickling solution; drying the powder subjected to acid washing in the previous step, and performing dehydrogenation treatment: the dehydrogenation process is carried out in a tubular furnace, the temperature is set to be 700 ℃, argon gas with the speed of 2L/min is introduced for 2 hours, and tantalum powder is obtained; concentrating the pickling solution obtained in the previous step to obtain a concentrated solution with scandium concentration of 200mg/L, adding an extraction liquid (the extraction liquid is composed of an extracting agent di (2-ethylhexyl) phosphate (P204) and a diluent kerosene, the volume fraction of the P204 is 10%) into the concentrated solution to extract and enrich scandium, and collecting a raffinate; then washing an organic phase obtained by extraction by adopting 4mol/L hydrochloric acid, adding a sodium hydroxide solution stripping agent with the concentration of 5% to strip scandium at the temperature of 80 ℃, and obtaining scandium-containing precipitate; calcining the scandium-containing precipitate at 800 ℃ to prepare scandium oxide; and adding sodium hydroxide into the obtained raffinate to adjust the pH value to 4 to obtain an aluminum-containing precipitate, and calcining the precipitate to obtain the aluminum oxide.
Example 2
Simply crushing the aluminum scandium target material by using tantalum crucible fragment waste to obtain fragments smaller than 8cm, cleaning the fragments by using hydrochloric acid with the concentration of 20% for 4h, drying, and collecting pickling solution; putting the acid-washed fragments into a tube furnace for hydrogen embrittlement treatment: introducing argon for 30min to remove air and water, setting the heating temperature at 750 deg.C, and introducing hydrogen at 2L/min for 60 min; preparing the hydrogen embrittlement treated fragments into powder with the granularity of-120 meshes to +200 meshes by using a sample preparation machine, cleaning for 2 hours by using hydrochloric acid with the concentration of 20%, wherein the acid cleaning temperature is 70 ℃, and collecting acid cleaning solution; drying the powder subjected to acid washing in the previous step, and performing dehydrogenation treatment: the dehydrogenation process is carried out in a tubular furnace, the temperature is set to be 900 ℃, argon gas with the speed of 2L/min is introduced for 2 hours, and tantalum powder is obtained; concentrating the pickling solution obtained in the previous step to obtain a concentrated solution with the scandium concentration of 500mg/L, adding an extraction liquid (the extraction liquid consists of an extraction agent bis (2,4, 4-trimethylpentyl) phosphinic acid (Cyanex272) and a diluent kerosene, the volume fraction of the Cyanex272 is 5%) into the concentrated solution to extract and enrich scandium, and collecting a raffinate; then washing an organic phase obtained by extraction by using 5mol/L hydrochloric acid, adding an oxalic acid solution stripping agent with the concentration of 10% to strip scandium at 60 ℃ to obtain scandium-containing precipitate; calcining the scandium-containing precipitate at 800 ℃ to prepare scandium oxide; and adding sodium hydroxide into the obtained raffinate to adjust the pH value to 4 to obtain an aluminum-containing precipitate, and calcining the precipitate to obtain the aluminum oxide.
Example 3
Simply crushing the aluminum scandium target material by using tantalum crucible fragment waste to obtain fragments smaller than 8cm, cleaning the fragments by using hydrochloric acid with the concentration of 10% for 2h, drying, and collecting pickling solution; putting the acid-washed fragments into a tube furnace for hydrogen embrittlement treatment: introducing argon for 30min to remove air and water, setting the heating temperature at 800 deg.C, and introducing hydrogen at a rate of 1.5L/min for 120 min; preparing the hydrogen embrittlement treated fragments into powder with the granularity of-120 meshes to +200 meshes by using a sample preparation machine, cleaning for 4 hours by adopting hydrochloric acid with the concentration of 5%, wherein the acid cleaning temperature is 90 ℃, and collecting acid cleaning solution; drying the powder subjected to acid washing in the previous step, and performing dehydrogenation treatment: the dehydrogenation process is carried out in a tubular furnace, the temperature is set to be 800 ℃, argon gas with the speed of 2L/min is introduced for 4 hours, and tantalum powder is obtained; concentrating the pickling solution obtained in the previous step to obtain a concentrated solution with the scandium concentration of 500mg/L, adding an extraction liquid into the concentrated solution, wherein the extraction liquid consists of an extracting agent tributyl phosphate (TBP), bis (2,4, 4-trimethylpentyl) phosphinic acid (Cyanex272) and a diluent kerosene, the volume fractions of the TBP and the Cyanex272 are respectively 5% and 10%, and extracting and enriching scandium, and collecting a raffinate; then washing an organic phase obtained by extraction by adopting 6mol/L hydrochloric acid, adding an ammonium fluoride solution stripping agent with the concentration of 10% to strip scandium at 25 ℃, and obtaining scandium-containing precipitate; calcining the scandium-containing precipitate at 800 ℃ to prepare scandium fluoride; and adding sodium hydroxide into the obtained raffinate to adjust the pH value to 4 to obtain an aluminum-containing precipitate, and calcining the precipitate to obtain the aluminum oxide.
Example 4
Simply crushing the aluminum scandium target material by using tantalum crucible fragment waste to obtain fragments of 1cm to 8cm, cleaning the fragments by using sulfuric acid with the concentration of 10 percent for 2 hours, drying, and collecting pickling solution; putting the acid-washed fragments into a tube furnace for hydrogen embrittlement treatment: introducing argon for 30min to remove air and water, setting the heating temperature at 750 deg.C, and introducing hydrogen at 2L/min for 80 min; preparing the hydrogen embrittlement treated fragments into powder with the granularity of-120 meshes to +200 meshes by using a sample preparation machine, cleaning for 3 hours by using sulfuric acid with the concentration of 5%, wherein the pickling temperature is 80 ℃, and collecting pickling solution; drying the powder subjected to acid washing in the previous step, and performing dehydrogenation treatment: the dehydrogenation process is carried out in a tubular furnace, the temperature is set to be 900 ℃, argon gas with the speed of 2L/min is introduced for 3 hours, and tantalum powder is obtained; concentrating the pickling solution obtained in the previous step to obtain a concentrated solution with scandium concentration of 300mg/L, adding an extraction liquid (the extraction liquid consists of an extracting agent of tributyl phosphate (TBP), di (2-ethylhexyl) phosphate (P204) and a diluent of kerosene, the volume fractions of TBP and Cyanex272 are 5% and 10% respectively) to extract and enrich scandium, and collecting a raffinate; then washing an organic phase obtained by extraction by adopting 4mol/L hydrochloric acid, adding an ammonia water stripping agent with the concentration of 10% to strip scandium at 60 ℃ to obtain scandium-containing precipitate; calcining the scandium-containing precipitate at 800 ℃ to prepare scandium oxide; and adding sodium hydroxide into the obtained raffinate to adjust the pH value to 4 to obtain an aluminum-containing precipitate, and calcining the precipitate to obtain the aluminum oxide.
The scrap pieces of the tantalum crucible for the aluminum scandium target material in examples 1 to 4 were derived from the same batch of scrap pieces, and the analysis of impurities in the tantalum powder and scandium oxide recovered in each example is shown in table 1 to 2. Analysis of impurity levels can be determined by standard, methods known in the industry or in the art.
TABLE 1 analysis of impurities in tantalum powder%
| Numbering | Al | Sc | Ni | Fe | Si | Ti | W | Mo | O | H |
| Example 1 | 0.006 | 0.001 | 0.003 | 0.003 | 0.002 | 0.01 | 0.01 | 0.01 | 0.15 | 0.003 |
| Example 2 | 0.003 | 0.001 | 0.002 | 0.001 | 0.002 | 0.01 | 0.01 | 0.01 | 0.13 | 0.001 |
| Example 3 | 0.007 | 0.001 | 0.002 | 0.002 | 0.002 | 0.01 | 0.01 | 0.01 | 0.15 | 0.003 |
| Example 4 | 0.005 | 0.001 | 0.002 | 0.002 | 0.002 | 0.01 | 0.01 | 0.01 | 0.14 | 0.002 |
TABLE 2 analysis of impurities in scandium oxide%
| Numbering | SiO2 | Fe2O3 | CaO | ZrO2 | Al2O3 | TiO2 | CuO | V2O5 |
| Example 1 | 0.01 | 0.005 | 0.004 | 0.002 | 0.006 | 0.008 | 0.01 | 0.001 |
| Example 2 | 0.01 | 0.003 | 0.002 | 0.003 | 0.002 | 0.008 | 0.01 | 0.001 |
| Example 3 | 0.01 | 0.004 | 0.004 | 0.003 | 0.004 | 0.008 | 0.01 | 0.001 |
| Example 4 | 0.01 | 0.005 | 0.005 | 0.003 | 0.003 | 0.008 | 0.01 | 0.001 |
From the results obtained in the different examples, it can be seen that 99.95% Ta can be obtained by the process2O5Or Sc2O3Al and Sc can be leached more efficiently by hydrochloric acid leaching, and Al and Sc can also be leached effectively by sulfuric acid leaching. For high-content aluminum scandium waste, the hydrochloric acid leaching and washing effects are better, and for low-content aluminum scandium waste, the sulfuric acid has less corrosion to equipment in the hydrochloric acid leaching process, less acid mist and good operating environment.
The above description is only exemplary of the present disclosure and should not be taken as limiting the present disclosure in any way, and although the present disclosure has been described in terms of preferred embodiments, it is not intended to limit the present disclosure, and those skilled in the art can make modifications and equivalents without departing from the scope of the present disclosure.
Claims (10)
1. A method for separating and recovering tantalum, scandium and aluminum is characterized by comprising the following steps:
s1, crushing the tantalum crucible scrap to obtain fragments, pickling, collecting pickling solution, and drying the fragments;
s2, heating the dried chips obtained in the step S1, and introducing hydrogen to embrittle the chips;
s3, further crushing and grinding the fragments into powder after the embrittlement treatment, removing impurities by acid washing, and collecting acid washing liquid;
s4, drying the powder obtained in the step S3, and then carrying out dehydrogenation treatment to obtain tantalum powder;
s5, concentrating the pickling solution obtained in the step S1 and S3, adding an extraction solution into the concentrated solution to extract and enrich scandium elements, collecting raffinate, carrying out acid pickling on an organic phase obtained by extraction, and adding a stripping agent to carry out stripping treatment to obtain a scandium-containing element precipitate, wherein the extraction solution comprises an extracting agent and a diluting agent;
s6, calcining the precipitate obtained in the step S5 to obtain scandium oxide or scandium fluoride;
s7, adding sodium hydroxide into the raffinate obtained in the step S6 to adjust the pH value to obtain a precipitate, and calcining the precipitate to obtain the alumina.
2. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S1, acid used for acid washing is at least one of hydrochloric acid or sulfuric acid; the acid used for pickling has the volume fraction of 10-20%, the pickling temperature is 70-90 ℃, and the pickling time is 2-4 h.
3. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S2, the process conditions of the embrittlement treatment are as follows: putting the fragments into a tubular furnace for embrittlement treatment, firstly introducing protective gas argon into the tubular furnace to remove air and moisture in the fragments, and then introducing hydrogen into the tubular furnace, wherein the heating temperature is 700-800 ℃, the flow rate of the hydrogen is 1.5-2L/min, and the time is 60-120 min.
4. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S3, the prepared powder has a particle size of-120 mesh to +200 mesh, the acid used for acid washing is one or a mixture of two of sulfuric acid and hydrochloric acid, the acid concentration is 10% to 30%, the acid washing time is 2h to 4h, and the acid washing temperature is 70 ℃ to 90 ℃.
5. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S4, the dehydrogenation process conditions are as follows: and putting the dried powder into a tubular furnace, setting the temperature to be 700-900 ℃, and introducing argon with the gas flow rate of 1-2L/min for 2-4 h.
6. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S5: the extractant is one or a mixture of more than two of bis (2-ethylhexyl) phosphate, bis (2,4, 4-trimethylpentyl) phosphinic acid and tributyl phosphate; the stripping agent is at least one of sodium hydroxide solution, oxalic acid, ammonia water and ammonium fluoride solution; washing with sulfuric acid or hydrochloric acid; the diluent is kerosene.
7. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S5: the concentration of scandium element in the obtained concentrated solution is 200mg/L to 500 mg/L; the volume fraction of the extractant in the extraction liquid is 5 to 10 percent; the acid concentration adopted by acid washing is 2mol/L to 4 mol/L; the concentration of the stripping agent is 5 to 10 percent, and the stripping temperature is 25 to 70 ℃.
8. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S6, the temperature of calcination is 700 ℃ to 800 ℃.
9. The method for separating and recovering tantalum, scandium and aluminum according to claim 1, wherein in step S7, the pH value is adjusted in a range of 4 to 5.
10. The method of claim 1, wherein the tantalum, scandium and aluminum separation and recovery method is characterized in that in step S1, the components of the tantalum crucible scrap pieces comprise metallic tantalum and adhered aluminum-scandium alloy or scraps.
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