CN111807411A - Method for removing and recycling vanadium in molybdate by using copper salt - Google Patents
Method for removing and recycling vanadium in molybdate by using copper salt Download PDFInfo
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Abstract
The invention discloses a method for removing and recycling vanadium in molybdate by using copper salt, which comprises the following steps: s1, dissolving molybdate to obtain a molybdate solution, and adjusting the pH of the molybdate solution to 6-10; s2, preparing a copper sulfate solution with the concentration of 10-150 g/L, and adding ammonia water to obtain a copper ammonia solution; s3, adding the prepared cuprammonia solution into the molybdate solution, keeping the pH value at 6-10 and the residual ammonia concentration at 100-1000 mg/L, filtering and taking the filtrate and the like. According to the method, the copper salt is used for removing and recovering vanadium in molybdate, the characteristic that cuprammonia formed by the copper salt and ammonia has selective adsorbability on vanadium and molybdenum is utilized, molybdenum and vanadium are thoroughly separated, the direct yield of vanadium is more than 99%, the molybdenum loss rate is less than 0.1%, the V/Mo ratio of slag is more than 10 times, the content of V in a vanadium product is more than 39%, and the content of Mo is less than 0.1%, so that the comprehensive utilization of molybdenum and vanadium is realized, meanwhile, the used copper salt can be reused, the process cost is low, and the method is particularly suitable for industrial application.
Description
Technical Field
The invention relates to the technical field of molybdate purification, in particular to a method for removing and recycling vanadium in molybdate by using copper salt.
Background
Because molybdenum and vanadium have more chemical commonalities and are similar in neutral substances of aqueous solution and difficult to separate, researchers at home and abroad carry out a great deal of research on vanadium removal of molybdate in order to improve the quality of molybdenum products, and ammonium salt precipitation, vulcanization, extraction, ion exchange and other methods are respectively developed to separate molybdenum and vanadium, for example, vanadium is removed by mainly adopting chemical precipitation with ferric salt as a precipitator according to the condition that the molar ratio of iron to vanadium is 40 and the system pH is 7.5-10.8, the vanadium removal rate can reach 97 percent, and the molybdenum loss rate is less than 5 percent (vanadium removal, Chengxing and the like in the tungsten-molybdenum smelting process, Chinese non-ferrous metal declaration, volume 24, and phase 7), however, when vanadium is recovered by the method in industrial application, the yield of vanadium recovered from iron-vanadium slag is less than 70 percent, the molybdenum loss rate is more than 10 percent, and the molybdenum loss is larger along with the increase of ferric salt, the molybdenum loss is unsatisfactory, the molybdenum and vanadium separation effect is not effectively realized, And comprehensively recycling the vanadium. Chinese patent CN109455761A discloses a method for removing vanadium from molybdate solution, which adopts iron salt to remove vanadium, the vanadium removal rate is more than or equal to 97%, the molybdenum loss rate is less than or equal to 1%, and similarly, the method still can not overcome the problems of difficult vanadium recovery, large molybdenum loss and non-ideal vanadium removal effect.
For another example, the prior art discloses the use of ion exchange to remove and recover vanadium, the general process is: under the acidic condition, respectively adding a reducing agent and an oxidizing agent to adjust the oxidation-reduction potential of the solution, so that vanadium exists in a cation form and molybdenum exists in an anion form, and enriching vanadium through ion exchange, which is characterized in that the concentration of vanadium and molybdenum solution in the pre-exchange solution is 1-10 g/L, the exchange speed is controlled according to the contact time of 10-50 min, and the saturated adsorption capacity of vanadium is 40 mg/g.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the method for removing and recovering vanadium in molybdate by using the copper salt is provided, vanadium in molybdate is removed and recovered by using the copper salt, molybdenum and vanadium are separated thoroughly, the direct yield of vanadium is more than 99%, the molybdenum loss is less than 0.1%, the V/Mo ratio of slag is more than 10 times, molybdenum and vanadium can be effectively separated, vanadium is recovered from slag to prepare a vanadium product, the comprehensive utilization of molybdenum and vanadium is realized, and the defects of the existing process are overcome.
The technical scheme adopted by the invention is as follows: a method for removing vanadium in molybdate by using copper salt is characterized by comprising the following steps:
s1, dissolving molybdate to obtain a molybdate solution, and adjusting the pH of the molybdate solution to 6-10;
s2, preparing a copper sulfate solution with the concentration of 10-150 g/L, and adding ammonia water to obtain a copper ammonia solution;
s3, adding the prepared cuprammonia solution into the molybdate solution, keeping the pH value at 6-10 and the residual ammonia concentration at 100-1000 mg/L, and filtering to obtain the filtrate.
In the invention, the vanadium removal mode of the cuprammonia solution is similar to the vanadium removal mode of an iron salt, and vanadium is also removed in an adsorption mode, but the cuprammonia solution is essentially different from the iron salt in the adsorption process, a cuprammonia complex in the cuprammonia solution has selectivity on the absorption of molybdenum and vanadium in the presence of ammonia, namely the presence of ammonia can inhibit the combination of copper and molybdenum and is beneficial to the combination of copper and vanadium, most of vanadium in a molybdate solution is separated through filter residue (copper vanadium slag) in a subsequent separation mode, molybdenum exists in the solution in the form of molybdic acid, the adsorption rate of vanadium is more than 99%, the adsorption rate of molybdenum is less than 0.1%, and the separation effect of molybdenum and vanadium is far higher than that of the iron salt. Accordingly, since ammonia cannot form an amino-iron complex with iron, it does not improve the separation effect of vanadium and molybdenum even in the presence of ammonia since iron itself is not selective for molybdenum and vanadium. Further, in the invention, the cuprammonia can also be replaced by silver ammonia liquid, but the silver ammonia liquid has high toxicity and high use cost, and is not suitable for industrial application.
In the invention, ammonia water is used for preparing cuprammonia according to the molar ratio of Cu/NH3·H2O ═ 1 to 5: 1 in a ratio of 1.
Further, in S3, the amount of the ammoniacal copper solution added is set to 1 to 5: 1, the reaction temperature is 20-80 ℃, and the reaction time is 1-5 h.
The invention also comprises a method for recovering vanadium from molybdate, which is characterized by comprising the following steps:
s4.1, washing the obtained filter residue, and then performing alkaline leaching treatment on the filter residue to obtain an alkaline leaching solution and alkaline leaching residue;
s4.2, carrying out vanadium precipitation treatment on the alkaline leaching solution, namely recovering to obtain a vanadium-containing product.
In the invention, the filter residue obtained by treating the cuprammonium solution is the copper-vanadium slag, the copper-vanadium slag is subjected to alkaline leaching treatment, vanadium and molybdenum in the copper-vanadium slag are leached and remain in an alkaline leaching solution, copper remains in the alkaline leaching slag, the leaching rate of vanadium is more than 99.5%, and then the alkaline leaching solution is subjected to vanadium precipitation treatment, for example, ammonium chloride or high alkali (NaOH) can be added, or direct freezing treatment (crystallization at 4-5 ℃) is adopted, so that a vanadium-containing product is obtained, the recovery of vanadium is realized, the direct yield of vanadium is more than 99.5%, and the defect that the vanadium is difficult to recover from the existing iron-vanadium slag is overcome.
Further, in alkaline leaching, the liquid-solid mass ratio is 1-10: 1, the alkaline leaching temperature is 40-100 ℃, the alkaline leaching time is 1-5 h, and the residual alkaline concentration is 5-100 g/L.
In the invention, in order to recycle copper salt and reduce the use cost and copper consumption, the alkaline leaching residue is subjected to acid leaching treatment to obtain copper sulfate solution, the leaching rate of copper is more than 99.8%, and the copper sulfate solution is used as a raw material for preparing the copper ammonia solution for reuse.
Further, during acid leaching, the mass ratio of liquid to solid is 1-10: 1, the acid leaching temperature is 40-100 ℃, the reaction time is 1-5 h, and the residual acid concentration is 5-100 g/L.
Preferably, when the alkaline leaching solution is subjected to vanadium precipitation treatment, ammonium chloride is added to the alkaline leaching solution in an amount of NH (NH) per mole4Cl/V ═ 1 to 6: 1, and filtering after the precipitation is finished, wherein the filter residue is an ammonium metavanadate product.
Further, the filtered mother liquor is subjected to an ion exchange method to recover molybdenum.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the method, the vanadium in the molybdate is removed and recovered through the copper salt, the characteristic that cuprammonia formed by the copper salt and ammonia has selective adsorbability on the vanadium and the molybdenum is utilized, the molybdenum and the vanadium are thoroughly separated, after alkali leaching and vanadium precipitation are carried out subsequently, the direct yield of the vanadium is more than 99%, the molybdenum loss rate is less than 0.1%, the V/Mo ratio of slag is more than 10 times, the vanadium is recovered from the slag to prepare a vanadium product, the content of V in the vanadium product is more than 39%, and the content of Mo is less than 0.1%, so that the comprehensive utilization of the molybdenum and the vanadium is realized, meanwhile, the used copper salt can be reused after acid leaching treatment, the loss of the copper salt is less than 0.2%, the use cost is low, the practicability.
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FIG. 1 is a schematic flow diagram of a method for removing and recovering vanadium from molybdate according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Taking sodium molybdate solid containing vanadium obtained by adding a reagent for roasting, leaching and evaporative crystallization from petroleum waste as an example, the main component (mass fraction) of the raw material is Mo 5-40%; v1-20%; the NaOH 1-10%, named as sodium molybdate solid, as shown in figure 1, is a method for removing and recovering vanadium from molybdate by using copper salt, comprising the following steps:
s1, dissolving: taking a certain amount of the sodium molybdate solid raw material, adding water, stirring and dissolving, adding acid to adjust the pH value to 6-8 after dissolving, and obtaining a sodium molybdate solution;
s2, preparing a copper ammonia solution: preparing copper sulfate solution with the concentration of 80-90 g/L, adding ammonia water, and adding the ammonia water according to the molar ratio of Cu/NH3·H2O is 3: 1 to obtain copper ammonia solution;
s3, precipitating vanadium: slowly adding the prepared cuprammonia into a sodium molybdate solution, adding the solution according to the molar ratio of Cu/V to 4, performing pressure filtration and washing to obtain the sodium molybdate solution and copper vanadium slag (containing about 40% of copper and the content of vanadium is about 15%) at the reaction temperature of 20-30 ℃ for 3h and the residual ammonia concentration of 500-600 mg/L;
s4, alkaline leaching of copper vanadium slag: according to the mass ratio of liquid to solid: 4: 1, carrying out alkaline leaching, wherein an alkaline solution is NaOH solution, the alkaline leaching temperature is 40-50 ℃, the residual alkali concentration is 15-25 g/L, reacting for 5 hours, carrying out filter pressing and washing to obtain copper hydroxide slag and an alkaline leaching solution, and the leaching rate of vanadium is more than 99.5%;
s5, acid leaching of copper hydroxide slag: according to the mass ratio of liquid to solid: 5: 1, carrying out acid leaching at the temperature of 40-45 ℃ and the residual acid concentration of 20-30 g/L, reacting for 4 hours to obtain a copper sulfate solution, wherein the leaching rate of copper is more than 99.8%, and adding ammonia water into the copper sulfate solution to return to continue vanadium precipitation;
s6, precipitating vanadium from the alkaline leaching solution: adding solid ammonium chloride into the alkaline leaching solution, wherein the adding amount of the ammonium chloride is NH according to the molar ratio4Cl/V ═ 3: 1, filtering and washing to obtain an ammonium metavanadate product (the content of V is more than 39 percent, and the content of Mo is less than 0.1 percent), and recovering molybdenum from the mother liquor by an ion exchange method.
Example 2
Still using the sodium molybdate solid of example 1 as the starting material, the method for removing and recovering vanadium from molybdate includes the following steps:
s1, dissolving: taking a certain amount of the sodium molybdate solid raw material, adding water, stirring and dissolving, adding acid to adjust the pH value to 6-8 after dissolving, and obtaining a sodium molybdate solution;
s2, preparing a copper ammonia solution: preparing copper sulfate solution with the concentration of 100-120 g/L, adding ammonia water, wherein the ammonia water is Cu/NH in molar ratio3·H2O is 5: 1 to obtain copper ammonia solution;
s3, precipitating vanadium: slowly adding the prepared cuprammonia into a sodium molybdate solution, adding the solution according to the molar ratio of Cu/V to 2, performing pressure filtration and washing to obtain the sodium molybdate solution and copper vanadium slag (containing about 40% of copper and the content of vanadium is about 15%) at the reaction temperature of 20-30 ℃ for 3h and the residual ammonia concentration of 100-plus-150 mg/L;
s4, alkaline leaching of copper vanadium slag: according to the mass ratio of liquid to solid: 8: 1, carrying out alkaline leaching, wherein an alkaline solution is NaOH solution, the alkaline leaching temperature is 50-65 ℃, the residual alkali concentration is 60-70 g/L, reacting for 1.5h, carrying out filter pressing and washing to obtain copper hydroxide slag and an alkaline leaching solution, and the leaching rate of vanadium is more than 99.5%;
s5, acid leaching of copper hydroxide slag: according to the mass ratio of liquid to solid: 3: 1, carrying out acid leaching at the temperature of 40-45 ℃ and the residual acid concentration of 20-30 g/L, reacting for 5 hours to obtain a copper sulfate solution, wherein the leaching rate of copper is more than 99.8%, and adding ammonia water into the copper sulfate solution to return to continue vanadium precipitation;
s6, precipitating vanadium from the alkaline leaching solution: adding solid ammonium chloride into the alkaline leaching solution, wherein the adding amount of the ammonium chloride is NH according to the molar ratio4Cl/V ═ 2: 1, filtering and washing to obtain an ammonium metavanadate product (the content of V is more than 39 percent, and the content of Mo is less than 0.1 percent), and recovering molybdenum from the mother liquor by an ion exchange method.
Example 3
The method for removing and recovering vanadium in molybdate by using the sodium molybdate solid in the example 1 as a raw material comprises the following steps:
s1, dissolving: taking a certain amount of the sodium molybdate solid raw material, adding water, stirring and dissolving, adding acid to adjust the pH value to 8-9 after dissolving, and obtaining a sodium molybdate solution;
s2, preparing a copper ammonia solution: preparing 40-50 g/L copper sulfate solution, adding ammonia water, and adding Cu/NH according to molar ratio3·H2O is 3: 1 to obtain copper ammonia solution;
s3, precipitating vanadium: slowly adding the prepared cuprammonia into a sodium molybdate solution, adding the solution according to the molar ratio of Cu/V to 4, performing pressure filtration and washing to obtain the sodium molybdate solution and copper vanadium slag (containing about 40% of copper and about 15% of vanadium), wherein the reaction temperature is 20-40 ℃, the reaction time is 2 hours, and the residual ammonia concentration is 450 mg/L;
s4, alkaline leaching of copper vanadium slag: according to the mass ratio of liquid to solid: 5: 1, carrying out alkaline leaching, wherein an alkaline solution is NaOH solution, the alkaline leaching temperature is 40-50 ℃, the residual alkali concentration is 60g/L, reacting for 3 hours, carrying out filter pressing and washing to obtain copper hydroxide slag and an alkaline leaching solution, and the leaching rate of vanadium is more than 99.5%;
s5, acid leaching of copper hydroxide slag: according to the mass ratio of liquid to solid: 6: 1, carrying out acid leaching at the temperature of 40-50 ℃ and the residual acid concentration of 50g/L, reacting for 3.5 hours to obtain a copper sulfate solution, wherein the leaching rate of copper is more than 99.8%, and adding ammonia water into the copper sulfate solution to return to continue vanadium precipitation;
s6, precipitating vanadium from the alkaline leaching solution: adding solid ammonium chloride into the alkaline leaching solution, wherein the adding amount of the ammonium chloride is NH according to the molar ratio4Cl/V ═ 3: 1, filtering and washing to obtain an ammonium metavanadate product (the content of V is more than 39 percent, and the content of Mo is less than 0.1 percent), and recovering molybdenum from the mother liquor by an ion exchange method.
Example 4
The method for removing and recovering vanadium in molybdate by using the sodium molybdate solid in the example 1 as a raw material comprises the following steps:
s1, dissolving: taking a certain amount of the sodium molybdate solid raw material, adding water, stirring and dissolving, adding acid to adjust the pH value to 6-8 after dissolving, and obtaining a sodium molybdate solution;
s2, preparing a copper ammonia solution: preparing copper sulfate solution with the concentration of 70-80 g/L, adding ammonia water, and adding the ammonia water according to the molar ratio of Cu/NH3·H2O is 3: 1 to obtain copper ammonia solution;
s3, precipitating vanadium: slowly adding the prepared cuprammonia into a sodium molybdate solution, adding the solution according to the molar ratio of Cu/V to 3, reacting at the temperature of 20-30 ℃ for 3 hours, wherein the concentration of the residual ammonia is 400mg/L, and performing pressure filtration and washing to obtain the sodium molybdate solution and copper vanadium slag (containing about 40% of copper and about 15% of vanadium);
s4, alkaline leaching of copper vanadium slag: according to the mass ratio of liquid to solid: 7: 1, carrying out alkaline leaching, wherein an alkaline solution is NaOH solution, the alkaline leaching temperature is 40-50 ℃, the residual alkali concentration is 70g/L, reacting for 2 hours, carrying out filter pressing and washing to obtain copper hydroxide slag and an alkaline leaching solution, and the leaching rate of vanadium is more than 99.5%;
s5, acid leaching of copper hydroxide slag: according to the mass ratio of liquid to solid: 7: 1, carrying out acid leaching at the temperature of 40-50 ℃ and the residual acid concentration of 5-100 g/L, reacting for 2 hours to obtain a copper sulfate solution, wherein the leaching rate of copper is more than 99.8%, and adding ammonia water into the copper sulfate solution to return to continue vanadium precipitation;
s6, precipitating vanadium from the alkaline leaching solution: adding solid ammonium chloride into the alkaline leaching solution, wherein the adding amount of the ammonium chloride is NH according to the molar ratio4Cl/V ═ 5: 1, filtering and washing to obtain an ammonium metavanadate product (V content)The amount is more than 39 percent, the Mo content is less than 0.1 percent), and the molybdenum is recovered from the mother liquor by an ion exchange method.
In the above examples 1-4, the direct yield of vanadium is greater than 99.5%, the molybdenum loss rate is less than 0.1%, and the V/Mo ratio of slag is greater than 10 times, so that the comprehensive utilization of molybdenum and vanadium is realized, the process cost is low, the medicament consumption is low, and the method is particularly suitable for industrial application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A method for removing vanadium in molybdate by using copper salt is characterized by comprising the following steps:
s1, dissolving molybdate to obtain a molybdate solution, and adjusting the pH of the molybdate solution to 6-10;
s2, preparing a copper sulfate solution with the concentration of 10-150 g/L, and adding ammonia water to obtain a copper ammonia solution;
s3, adding the prepared cuprammonia solution into the molybdate solution, keeping the pH value at 6-10 and the residual ammonia concentration at 100-1000 mg/L, and filtering to obtain the filtrate.
2. The method for removing vanadium from molybdate according to claim 1, wherein the ammoniacal copper solution is prepared by using ammonia water in a molar ratio of Cu/NH3·H2O ═ 1 to 5: 1 in a ratio of 1.
3. The method for removing vanadium from molybdate according to claim 2, wherein the amount of the ammoniacal copper solution added in S3 is 1-5: 1, the reaction temperature is 20-80 ℃, and the reaction time is 1-5 h.
4. A method for recovering vanadium from molybdate, which is characterized by comprising the filter residue obtained by the method for removing vanadium from molybdate by using copper salt as claimed in any one of claims 1 to 3, wherein the method for recovering vanadium comprises the following steps:
s4.1, washing filter residues, and then performing alkaline leaching treatment on the filter residues to obtain alkaline leaching solution and alkaline leaching residues;
s4.2, carrying out vanadium precipitation treatment on the alkaline leaching solution, namely recovering to obtain a vanadium-containing product.
5. The method for recovering vanadium from molybdate according to claim 4, wherein the ratio of liquid to solid mass in alkaline leaching is 1 to 10: 1, the alkaline leaching temperature is 40-100 ℃, the alkaline leaching time is 1-5 h, and the residual alkaline concentration is 5-100 g/L.
6. The method for recovering vanadium from molybdate according to claim 4, wherein the alkaline leaching residue is subjected to acid leaching to obtain a copper sulfate solution, and the copper sulfate solution is reused as a raw material for preparing the cuprammonium solution.
7. The method for recovering vanadium from molybdate according to claim 6, wherein the liquid-solid mass ratio in the acid leaching is 1 to 10: 1, the acid leaching temperature is 40-100 ℃, the reaction time is 1-5 h, and the residual acid concentration is 5-100 g/L.
8. The method for recovering vanadium from molybdate according to claim 4, wherein ammonium chloride is added to the alkaline leaching solution in an amount of NH in terms of molar ratio when the alkaline leaching solution is subjected to the vanadium precipitation treatment4Cl/V ═ 1 to 6: 1, and filtering after the precipitation is finished, wherein the filter residue is an ammonium metavanadate product.
9. The method for recovering vanadium from molybdate according to claim 8 wherein the filtered mother liquor is subjected to ion exchange to recover molybdenum.
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| CN101062785A (en) * | 2006-04-26 | 2007-10-31 | 中南大学 | Method for deeply removing vanadium of vanadium-containing molybdate solution |
| BRPI0703015A2 (en) * | 2007-07-25 | 2008-11-25 | Diaz Samuel Aguirre | process for the production of molybdenum derivatives from depleted molybdenum catalysts |
| CN103602807A (en) * | 2013-09-18 | 2014-02-26 | 崇义章源钨业股份有限公司 | Treating method of removed molybdenum slag produced from tungsten smelting processes |
| CN108754125A (en) * | 2018-08-21 | 2018-11-06 | 中南大学 | A kind of vanadium-containing material sodium roasting vanadium-extracting cleaning procedure |
| CN109468468A (en) * | 2018-11-29 | 2019-03-15 | 成都虹波钼业有限责任公司 | A method for comprehensive utilization and treatment of molybdenum copper slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062785A (en) * | 2006-04-26 | 2007-10-31 | 中南大学 | Method for deeply removing vanadium of vanadium-containing molybdate solution |
| BRPI0703015A2 (en) * | 2007-07-25 | 2008-11-25 | Diaz Samuel Aguirre | process for the production of molybdenum derivatives from depleted molybdenum catalysts |
| CN103602807A (en) * | 2013-09-18 | 2014-02-26 | 崇义章源钨业股份有限公司 | Treating method of removed molybdenum slag produced from tungsten smelting processes |
| CN108754125A (en) * | 2018-08-21 | 2018-11-06 | 中南大学 | A kind of vanadium-containing material sodium roasting vanadium-extracting cleaning procedure |
| CN109468468A (en) * | 2018-11-29 | 2019-03-15 | 成都虹波钼业有限责任公司 | A method for comprehensive utilization and treatment of molybdenum copper slag |
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Application publication date: 20201023 |
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| RJ01 | Rejection of invention patent application after publication |