CN115404361B - Method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution - Google Patents
Method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution Download PDFInfo
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- C22B34/00—Obtaining refractory metals
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- 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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- 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
- C22B7/04—Working-up slag
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Abstract
The invention discloses a method for preparing a high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution, and relates to the technical field of wet metallurgy separation and extraction of vanadium. Specifically, desilication agent is added to remove silicon in the leaching solution, then reducing agent is added to selectively reduce Cr (VI) in the solution to Cr (III), and a proper extraction system is selected to selectively extract vanadium, so that vanadium-chromium separation is realized. The vanadium loaded organic phase is washed and back extracted to obtain high purity vanadyl sulfate solution, and the raffinate is precipitated and calcined to obtain chromium oxide. The method for preparing the vanadyl sulfate solution has the advantages of short flow, low cost and high efficiency, and can obtain the high-purity vanadyl sulfate solution and chromium oxide.
Description
Technical Field
The invention relates to the technical field of wet metallurgy separation and extraction of vanadium, and discloses a method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution.
Background
In recent years, large-scale energy storage technology is becoming an important point for the development and utilization of renewable energy sources. The energy storage technology of the all-vanadium redox flow battery is one of the preferred technologies for large-scale energy storage due to the advantages of large energy storage scale, high safety, long cycle life, environmental friendliness and the like. Besides the characteristics, the all-vanadium redox flow battery uses the same metal ion (vanadium), so that the fatal problem of cross contamination of electrolyte is avoided, the all-vanadium redox flow battery has an infinite service life in theory, and the whole industry has entered the early stage of marketing. With the application of large-scale renewable energy sources, the all-vanadium redox flow battery becomes a large-scale energy storage system with wide application prospect.
The electrolyte is used as an important part of the all-vanadium redox flow battery, so that the energy storage capacity of the battery is determined, and the performance and cost of the energy storage system are directly influenced. Vanadyl sulfate is an active material for the electrochemical reaction of a vanadium battery, and the performance of the vanadyl sulfate directly influences the performance of the vanadium battery. Therefore, how to prepare the high-purity vanadyl sulfate solution has important significance for the all-vanadium redox flow battery. The prior vanadyl sulfate solution is mainly prepared by taking high-purity vanadyl pentoxide as a raw material and adopting a chemical reduction method. The method has the advantage that the cost for preparing the vanadyl sulfate solution is too high due to the too high price of raw materials. The invention is expected to develop a preparation method of high-purity vanadyl sulfate solution with short flow and low production cost by taking low-cost industrial vanadium slag sodium roasting water immersion liquid as a raw material.
Disclosure of Invention
The invention aims to provide a method for preparing a high-purity vanadyl sulfate solution by roasting water leaching solution of industrial vanadium slag sodium, in particular to a method for removing silicon in leaching solution by adding a desilication agent, then adding a reducing agent to selectively reduce Cr (VI) in the solution to Cr (III), and selectively extracting vanadium by selecting a proper extraction system to realize vanadium-chromium separation. The vanadium loaded organic phase is washed and back extracted to obtain high purity vanadyl sulfate solution, and the raffinate is precipitated and calcined to obtain chromium oxide.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a method for preparing a high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution, which comprises the following steps:
(1) Adding desilication agent into the industrial vanadium slag sodium-treatment roasting water immersion liquid, removing silicon in the industrial vanadium slag sodium-treatment roasting water immersion liquid, and filtering to obtain a leaching liquid;
(2) Adding a reducing agent into the leaching solution obtained in the step (1), and selectively reducing Cr (VI) in the leaching solution to Cr (III) to obtain a solution containing Cr (III);
(3) Preparing microemulsion by using mixed aqueous solution of quaternary ammonium salt, medium carbon chain alcohol, oil phase and NaOH and NaCl;
(4) Mixing the microemulsion obtained in the step (3) with the Cr (III) -containing solution obtained in the step (2) according to a certain volume ratio, vibrating for a certain time to extract, standing for layering, wherein the upper phase is a microemulsion phase, the lower phase is a water phase, and separating the microemulsion phase from the water phase;
(5) Washing, reducing and back-extracting the vanadium-loaded organic phase (upper microemulsion phase) obtained in the step (4) to prepare a high-purity vanadyl sulfate solution, wherein the vanadium yield is more than 90%, the vanadium concentration in the high-purity vanadyl sulfate solution is more than or equal to 1.5M, and the impurity concentration is lower than the concentration in table 1;
table 1 GB/T37204-2018 first order impurity concentration requirement
(6) Regulating the pH value of the lower water phase obtained in the step (4) to perform alkaline precipitation, and washing and calcining to prepare chromium oxide;
(7) And (3) recovering the organic phase (microemulsion phase) obtained after the reduction and back extraction in the step (5) through the mixed aqueous solution of neutralization and washing, naOH and NaCl, and replacing the microemulsion in the step (4) of the next reaction for recycling for extraction.
Based on the technical proposal, in the step (1), preferably, the concentration of vanadium in the industrial vanadium slag sodium roasting water immersion liquid is 20-40 g.L -1 。
Based on the above technical scheme, in the step (1), preferably, after adjusting the pH=8-11 of the industrial vanadium slag sodium roasting water leaching solution, adding a desilication agent, wherein the desilication agent is aluminum sulfate, al: si=0.8-2:1 (according to the molar ratio of Al in the industrial vanadium slag sodium roasting water leaching solution to Si in the desilication agent), the desilication temperature is 60-90 ℃, and the stirring time is 1-2 h.
Based on the above technical scheme, in the step (2), preferably, the reducing agent is added after adjusting the pH of the leaching solution to 3-6, wherein the reducing agent is at least one of sodium sulfite, sodium bisulphite, sodium metabisulfite and sulfurous acid, S is Cr=1-2:1 (calculated according to the molar ratio of S in the reducing agent to Cr in the solution), the reducing temperature is 45-70 ℃, and the stirring time is 20-60 min.
Based on the above technical scheme, preferably, in the step (1) and the step (2), the reagent used for adjusting the pH value is a sulfuric acid solution, and the concentration of the sulfuric acid solution is 4-16M.
Based on the above technical scheme, preferably, in the step (3), the mixed aqueous solution of quaternary ammonium salt, medium carbon chain alcohol, oil phase and NaOH and NaCl is mixed and vibrated, and the mixture is stood for layering, and the upper phase is the microemulsion.
Based on the above technical scheme, preferably, in the step (3), the quaternary ammonium salt is one of trioctyl methyl ammonium chloride, trinonyl methyl ammonium chloride and tri-dodecyl methyl ammonium chloride, and the mass concentration (mass fraction) of the quaternary ammonium salt in the microemulsion is 1% -35%; the medium carbon chain alcohol is one of n-butanol, isoamyl alcohol, n-hexanol, n-heptanol and n-octanol, and the mass concentration (mass fraction) of the medium carbon chain alcohol in the microemulsion is 5-35%; the oil phase is one of kerosene and n-heptane, and the mass concentration (mass fraction) of the oil phase in the microemulsion is 20% -93%; the concentration of NaOH and NaCl in the mixed aqueous solution of NaOH and NaCl is 0.1-2.0M, and the mass concentration (mass fraction) of the mixed aqueous solution of NaOH and NaCl in the microemulsion is 1-10%.
Based on the above technical scheme, preferably, in the step (4), the volume ratio O/A of the microemulsion to the solution containing Cr (III) is 1:1-10, and the oscillation time is 1-10 min.
Based on the above technical scheme, preferably, in the step (5), the washing process, the washing liquid is deionized water, and the O/a=1:1-2 of the organic phase loaded with vanadium (upper microemulsion phase) compared with the washing of the washing liquid, the washing time is 1-2 min; in the back extraction process, the back extraction agent is oxalic acid (H) 2 C 2 O 4 ) Vanadium V: H in the washed vanadium-loaded organic phase (upper microemulsion phase) 2 C 2 O 4 The stripping solution is prepared by adding a stripping agent into a sulfuric acid solution, wherein the concentration of the sulfuric acid solution is 4-6M, and the O/A=1-6:1 of the washed vanadium-loaded organic phase (upper microemulsion phase) is compared with the stripping of the stripping solution, and the stripping time is 1-2 h.
Based on the above technical scheme, preferably, in the step (6), the solution for adjusting the pH value is 1-6M NaOH solution, and the pH value of the solution is adjusted to 8-9; the washing process is characterized in that the washing liquid is deionized water, and washing is carried out according to the mass ratio of the sediment to the deionized water being 1-2:1; the calcination process is carried out at 800-1100 ℃ for 2-3 h.
Based on the above technical scheme, preferably, in the step (7), the neutralization washing solution is 1-6M NaOH solution, and the organic phase (microemulsion phase) is washed for 1-2 min with O/a=1:1-2 compared with the washing of 1-6M NaOH solution; the concentration of NaOH and NaCl in the mixed aqueous solution of NaOH and NaCl is 0.1-2.0M, and the recovery time of the organic phase (microemulsion phase) after neutralization and washing is 5-10 min compared with the recovery of the mixed aqueous solution of NaOH and NaCl.
Compared with the prior art, the invention has the following advantages:
1. the prior industrial vanadium slag sodium roasting water immersion liquid is used as a raw material to prepare a vanadyl sulfate solution, firstly, the vanadyl sulfate solution is prepared into high-purity vanadium pentoxide, and then, the vanadyl sulfate solution is prepared through dissolution reduction. In the process of preparing high-purity vanadium pentoxide, separation of vanadium and chromium is difficult, and the chromium can be removed by multistage impurity removal. The invention realizes the separation of vanadium and chromium by one step through microemulsion extraction, and synchronously realizes the separation with other impurity elements. The vanadyl sulfate solution can be directly prepared by reduction back extraction. Finally, the high-efficiency separation and enrichment of vanadium are realized.
2. The microemulsion belongs to a stable thermodynamic system, and is not easy to generate a third phase and an emulsifying phenomenon in the extraction process, so that the loss of an organic phase is reduced; after extraction, the two phases are separated easily and quickly, which is beneficial to improving the actual production efficiency.
3. Compared with the traditional solvent extraction, the microemulsion extraction has the advantages that as innumerable nanoscale water spheres are dispersed in the microemulsion, the specific surface area is obviously increased, the reaction speed is faster, and the production efficiency is improved for actual industrial production; meanwhile, the dispersed nano water spheres also increase the extraction saturation capacity of the microemulsion, and the organic phase with the same mass can extract more vanadium elements compared with the traditional solvent extraction microemulsion.
4. The method for preparing the vanadyl sulfate solution has the advantages of short flow, low cost and high efficiency, and can obtain the high-purity vanadyl sulfate solution and chromium oxide.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
1. Sodium treatment roasting water immersion liquid of vanadium slag in Pan steel vanadium factory is used as raw material, wherein the concentration of vanadium is 35 g.L -1 The pH was adjusted to 9 with a 16M sulfuric acid solution, aluminum sulfate was added thereto at Al: si=1:1 (molar ratio), the desilication temperature was 70 ℃, the stirring time was 2 hours, and the mixture was allowed to stand, cool and filtered.
2. Adjusting the pH of the leaching solution obtained in the step 1 to 3 by using a 16M sulfuric acid solution, adding sodium sulfite according to the ratio of S to Cr=1.67:1, reducing the temperature to 50 ℃, stirring for 30min, and selectively reducing Cr (VI) in the solution to Cr (III);
3. mixing and vibrating the mixed aqueous solution of trioctyl methyl ammonium chloride, isoamyl alcohol, kerosene and NaOH and NaCl for 5min, standing for layering, and obtaining the upper phase as the microemulsion. Wherein the concentration of each component in the microemulsion:
the trioctylmethyl ammonium chloride concentration was: 35% (w/w)
The concentration of isoamyl alcohol is: 25% (w/w)
The kerosene concentration was: 30% (w/w)
Mixed aqueous solution of NaOH and NaCl: 10% (w/w)
Wherein the concentration of NaOH in the mixed aqueous solution of NaOH and NaCl is as follows: 0.1M NaCl concentration: 0.1M.
4. Mixing the microemulsion in the step 3 with the solution obtained in the step 2 according to the volume ratio of O/A=1:1, vibrating for 5min for extraction, standing for layering, wherein the upper phase is a loaded microemulsion phase, the lower phase is a water phase, and separating the microemulsion phase from the water phase.
5. Taking the vanadium-loaded organic phase (the microemulsion-loaded phase) obtained in the step 4, and washing for 2min according to the washing ratio of O/A=1:1; according to V to H 2 C 2 O 4 =2.1:1 addition of H 2 C 2 O 4 Mixing and vibrating the solution and a washed organic phase in a sulfuric acid solution of 6M according to the ratio of O/A=3:1, and carrying out back extraction for 1h, thereby obtaining a high-purity vanadyl sulfate solution meeting the requirements of GB/T37204-2018 primary products, wherein the vanadium direct yield is 98.26%; wherein the concentration of vanadium in the obtained vanadyl sulfate solution is 1.9M, and the concentration of each impurity is shown in Table 2;
TABLE 2 impurity concentration of vanadyl sulfate solution
6. And (3) regulating the pH value of the lower water phase in the step (3) to 8.5 by using a NaOH solution with the concentration of 4M, washing the filtered precipitate according to the mass ratio of the precipitate to deionized water of 1:1, drying, and calcining at 800 ℃ for 2 hours. Chromium oxide with a purity of 98.84wt% was obtained with a direct yield of 96.06%.
7. Taking the organic phase (microemulsion phase) subjected to reduction back extraction in the step 5, and recovering the organic phase (microemulsion phase) after neutralization washing, wherein the washing solution is 4M NaOH solution, and the washing time is 2min compared with O/A=1:1; the microemulsion is reconstituted by selecting a mixed aqueous solution of 0.1M NaOH and 0.1M NaCl, wherein the replica ratio O/A=1:1, and the replica time is 5min. The microemulsion after the duplication is reused for extraction, and the extraction rate is 99.13 percent.
Example 2
1. Sodium treatment roasting water immersion liquid of vanadium slag in Pan steel vanadium factory is used as raw material, wherein the concentration of vanadium is 30 g.L -1 The pH was adjusted to 9 with a 16M sulfuric acid solution, aluminum sulfate was added thereto at Al: si=1:1 (molar ratio), the desilication temperature was 70 ℃, the stirring time was 2 hours, and the mixture was allowed to stand, cool and filtered.
2. Adjusting the pH of the leaching solution obtained in the step 1 to 4 by using a 16M sulfuric acid solution, adding sodium sulfite according to the ratio of S to Cr=1.65:1, reducing the temperature to 50 ℃, stirring for 30min, and selectively reducing Cr (VI) in the solution to Cr (III);
3. mixing and vibrating the mixed aqueous solution of trisnonylmethyl ammonium chloride, n-butanol, kerosene and NaOH and NaCl for 5min, standing for layering, and obtaining the upper phase as the microemulsion. Wherein the concentration of each component in the microemulsion:
the concentration of trisnonylmethyl ammonium chloride is: 35% (w/w)
The concentration of n-butanol is: 20% (w/w)
The kerosene concentration was: 35% (w/w)
Mixed aqueous solution of NaOH and NaCl: 10% (w/w)
Wherein the concentration of NaOH in the mixed aqueous solution of NaOH and NaCl is as follows: 0.1M NaCl concentration: 0.1M.
Mixing and vibrating the mixed aqueous solution of trisnonylmethyl ammonium chloride, n-butanol, kerosene and NaOH and NaCl for 5min, standing for layering, and obtaining the upper phase as the microemulsion. Wherein the concentration of each component in the microemulsion:
4. mixing the microemulsion in the step 3 with the solution obtained in the step 2 according to the volume ratio of O/A=1:1, vibrating for 5min for extraction, standing for layering, wherein the upper phase is a loaded microemulsion phase, the lower phase is a water phase, and separating the microemulsion phase from the water phase.
5. Taking the vanadium-loaded organic phase (the microemulsion-loaded phase) obtained in the step 4, and washing for 2min according to the washing ratio of O/A=1:1; according to V to H 2 C 2 O 4 =2.1:1 addition of H 2 C 2 O 4 Mixing and vibrating the solution and a washed organic phase in a sulfuric acid solution of 6M according to the ratio of O/A=3:1, and carrying out back extraction for 1h, thereby obtaining a high-purity vanadyl sulfate solution meeting the requirements of GB/T37204-2018 primary products, wherein the vanadium direct yield is 98.27%; wherein the concentration of vanadium in the obtained vanadyl sulfate solution is 1.7M, and the concentration of each impurity is shown in Table 3;
TABLE 3 impurity concentration of vanadyl sulfate solution
6. And (3) regulating the pH value of the lower water phase in the step (3) to 8.5 by using a NaOH solution with the concentration of 4M, washing the filtered precipitate according to the mass ratio of the precipitate to deionized water of 1:1, drying, and calcining at 800 ℃ for 2 hours. Chromium oxide with a purity of 98.85wt% was obtained with a direct yield of 96.07%.
7. Taking the organic phase (microemulsion phase) subjected to reduction back extraction in the step 5, and recovering the organic phase (microemulsion phase) after neutralization washing, wherein the washing solution is 4M NaOH solution, and the washing time is 2min compared with O/A=1:1; the microemulsion is reconstituted by selecting a mixed aqueous solution of 0.1M NaOH and 0.1M NaCl, wherein the replica ratio O/A=1:1, and the replica time is 5min. The microemulsion after the duplication is reused for extraction, and the extraction rate is 99.11 percent.
Example 3
1. Sodium treatment roasting water immersion liquid of vanadium slag in Pan steel vanadium factory is used as raw material, wherein the concentration of vanadium is 25 g.L -1 The pH was adjusted to 9 with a 16M sulfuric acid solution, aluminum sulfate was added thereto at Al: si=1:1 (molar ratio), the desilication temperature was 70 ℃, the stirring time was 2 hours, and the mixture was allowed to stand, cool and filtered.
2. Adjusting the pH of the leaching solution obtained in the step 1 to 3 by using a 16M sulfuric acid solution, adding sodium sulfite according to the ratio of S to Cr=1.65:1, reducing the temperature to 50 ℃, stirring for 30min, and selectively reducing Cr (VI) in the solution to Cr (III);
3. mixing and vibrating the mixed aqueous solution of trioctyl methyl ammonium chloride, isoamyl alcohol, kerosene and NaOH and NaCl for 5min, standing for layering, and obtaining the upper phase as the microemulsion. Wherein the concentration of each component in the microemulsion:
the trioctylmethyl ammonium chloride concentration was: 30% (w/w)
The concentration of isoamyl alcohol is: 25% (w/w)
The kerosene concentration was: 37% (w/w)
Mixed aqueous solution of NaOH and NaCl: 8% (w/w)
Wherein the concentration of NaOH in the mixed aqueous solution of NaOH and NaCl is as follows: 0.1M NaCl concentration: 0.1M.
4. Mixing the microemulsion in the step 3 with the solution obtained in the step 2 according to the volume ratio of O/A=1:1, vibrating for 5min for extraction, standing for layering, wherein the upper phase is a loaded microemulsion phase, the lower phase is a water phase, and separating the microemulsion phase from the water phase.
5. Taking the vanadium-loaded organic phase (the microemulsion-loaded phase) obtained in the step 4, and washing for 2min according to the washing ratio of O/A=1:1; according to V to H 2 C 2 O 4 =2.1:1 addition of H 2 C 2 O 4 Mixing and vibrating the solution and a washed organic phase in a sulfuric acid solution of 5M according to the ratio of O/A=4:1, and carrying out back extraction for 1h, thereby obtaining a high-purity vanadyl sulfate solution meeting the requirements of GB/T37204-2018 primary products, wherein the vanadium direct yield is 98.25%; wherein the concentration of vanadium in the obtained vanadyl sulfate solution is 1.9M, and the concentration of each impurity is shown in Table 4;
TABLE 4 impurity concentration of vanadyl sulfate solution
6. And (3) regulating the pH value of the lower water phase in the step (3) to 8.5 by using a NaOH solution with the concentration of 4M, washing the filtered precipitate according to the mass ratio of the precipitate to deionized water of 1:1, drying, and calcining at 800 ℃ for 2 hours. Chromium oxide with a purity of 98.83wt% was obtained with a direct yield of 96.05%.
7. Taking the organic phase (microemulsion phase) subjected to reduction back extraction in the step 5, and recovering the organic phase (microemulsion phase) after neutralization washing, wherein the washing solution is 4M NaOH solution, and the washing time is 2min compared with O/A=1:1; the microemulsion is reconstituted by selecting a mixed aqueous solution of 0.1M NaOH and 0.1M NaCl, wherein the replica ratio O/A=1:1, and the replica time is 5min. The microemulsion after the duplication is reused for extraction, and the extraction rate is 99.12 percent.
Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art without departing from the scope of the technology, or the technology can be modified to be equivalent. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall still fall within the scope of the technical solution of the present invention.
Claims (9)
1. The method for preparing the high-purity vanadyl sulfate solution by sodium roasting of industrial vanadium slag water leaching solution is characterized by comprising the following steps of:
(1) Adding desilication agent into the industrial vanadium slag sodium-treatment roasting water immersion liquid, removing silicon in the industrial vanadium slag sodium-treatment roasting water immersion liquid, and filtering to obtain a leaching liquid;
(2) Adding a reducing agent into the leaching solution obtained in the step (1), and reducing Cr (VI) in the leaching solution to Cr (III) to obtain a solution containing Cr (III);
(3) Preparing microemulsion by using mixed aqueous solution of quaternary ammonium salt, medium carbon chain alcohol, oil phase and NaOH and NaCl;
(4) Mixing the microemulsion obtained in the step (3) with the Cr (III) -containing solution obtained in the step (2) according to a certain volume ratio, vibrating for a certain time to extract, standing for layering, wherein the upper phase is a microemulsion phase, the lower phase is a water phase, and separating the microemulsion phase from the water phase;
(5) Washing, reducing and back-extracting the upper microemulsion phase obtained in the step (4) to prepare a high-purity vanadyl sulfate solution;
(6) Regulating the pH value of the lower water phase obtained in the step (4) to perform alkaline precipitation, and washing and calcining to prepare chromium oxide;
(7) Recovering the microemulsion phase obtained after the reduction back extraction in the step (5) through neutralization washing and a mixed aqueous solution of NaOH and NaCl, and replacing the microemulsion in the step (4) of the next reaction for recycling for extraction;
in the step (2), the pH of the leaching solution is regulated to 3-6, and then a reducing agent is added, wherein the reducing agent is at least one of sodium sulfite, sodium bisulphite, sodium metabisulfite and sulfurous acid, the molar ratio of S in the reducing agent to Cr in the leaching solution is 1-2:1, the reducing temperature is 45-70 ℃, and the reducing time is 20-60 min;
in the step (3), the quaternary ammonium salt is one of trioctyl methyl ammonium chloride, trinonyl methyl ammonium chloride and tri-decaalkyl methyl ammonium chloride; the medium carbon chain alcohol is one of n-butanol, isoamyl alcohol, n-hexanol, n-heptanol and n-octanol; the oil phase is one of kerosene and n-heptane;
in the step (5), the back extraction agent is oxalic acid, the molar ratio of vanadium to oxalic acid in the washed microemulsion phase is 2-3:1, the back extraction solution is prepared by adding the back extraction agent into sulfuric acid solution, the concentration of the sulfuric acid solution is 4-6M, the O/A=1-6:1 of the back extraction of the washed upper microemulsion phase and the back extraction solution is 1-2 h.
2. The method according to claim 1, wherein in the step (1), after adjusting the pH value of the industrial vanadium slag sodium roasting water leaching solution to 8-11, a desilication agent is added, wherein the desilication agent is aluminum sulfate, the molar ratio of Al in the industrial vanadium slag sodium roasting water leaching solution to Si in the desilication agent is 0.8-2:1, the desilication temperature is 60-90 ℃, and the desilication time is 1-2 h.
3. The method of claim 1, wherein in step (3), the quaternary ammonium salt, the medium carbon chain alcohol, the oil phase and the mixed aqueous solution of NaOH and NaCl are mixed and vibrated, and the mixture is left to stand for delamination, and the upper phase is the microemulsion.
4. A method according to claim 1 or 3, wherein in step (3) the mass concentration of the quaternary ammonium salt in the microemulsion is 1% to 35%; the mass concentration of the medium carbon chain alcohol in the microemulsion is 5-35%; the mass concentration of the oil phase in the microemulsion is 20% -93%; the concentration of NaOH and NaCl in the mixed aqueous solution of NaOH and NaCl is 0.1-2.0M, and the mass concentration of the NaOH and NaCl in the microemulsion is 1-10%.
5. The method according to claim 1, wherein in the step (4), the volume ratio O/A of the microemulsion to the Cr (III) -containing solution is 1:1-10, and the shaking time is 1-10 min.
6. The method according to claim 1, wherein in the step (5), the washing process, the washing liquid is deionized water, and the washing time of the microemulsion phase and the washing liquid is 1-2 min, wherein the ratio of O/A=1:1.
7. The method according to claim 1, wherein in the step (6), the solution for adjusting the pH value is 1-6M NaOH solution, and the pH value of the solution is adjusted to 8-9; the washing process is characterized in that the washing liquid is deionized water, and washing is carried out according to the mass ratio of the sediment to the deionized water being 1-2:1; the calcination process is carried out at 800-1100 ℃ for 2-3 h.
8. The method according to claim 1, wherein in the step (7), the neutralized washing solution is a 1-6M NaOH solution, and the washing time is 1-2 min, and the microemulsion phase is washed with 1-6M NaOH solution at O/a=1:1-2; the concentration of NaOH and NaCl in the mixed aqueous solution of NaOH and NaCl is 0.1-2.0M, and the recovery time of the neutralized and washed microemulsion phase is 5-10 min compared with the recovery of the mixed aqueous solution of NaOH and NaCl by O/A=1:1-2.
9. The method according to claim 1, wherein in the step (1), the concentration of vanadium in the industrial vanadium slag sodium roasting water immersion liquid is 20-40 g.L -1 。
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