CN111719053A - Method for extracting vanadium and manganese by roasting vanadium slag - Google Patents
Method for extracting vanadium and manganese by roasting vanadium slag Download PDFInfo
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- CN111719053A CN111719053A CN202010608423.7A CN202010608423A CN111719053A CN 111719053 A CN111719053 A CN 111719053A CN 202010608423 A CN202010608423 A CN 202010608423A CN 111719053 A CN111719053 A CN 111719053A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22B7/04—Working-up slag
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/10—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of chromium or manganese
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Abstract
The invention relates to the technical field of hydrometallurgy of vanadium and manganese, in particular to a method for extracting vanadium and manganese by roasting vanadium slag. The invention aims to solve the technical problem of providing a method for simultaneously extracting vanadium and manganese in vanadium slag. The method comprises the following steps: a. mixing vanadium slag and manganese-containing substances, and roasting to obtain roasted clinker; b. adding a leaching agent into the roasted clinker for leaching to obtain leached slurry, adjusting the pH value, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues; c. and (3) precipitating vanadium from the leachate by adopting an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and a vanadium precipitation supernatant, adding an impurity removing agent into the vanadium precipitation supernatant, and electrolyzing to obtain manganese metal and anolyte. The method can realize the simultaneous recycling of vanadium and manganese resources in the vanadium slag, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy of vanadium and manganese, in particular to a method for extracting vanadium and manganese by roasting vanadium slag.
Background
Vanadium slag is a main raw material for preparing vanadium oxide, and the current industrialized vanadium extraction processes mainly comprise two processes, namely a sodium roasting vanadium extraction process and a calcification roasting vanadium extraction process. The sodium salt vanadium extraction process adopts sodium salt additive to oxidize trivalent vanadium in vanadium slag into pentavalent vanadium at high temperature and convert the pentavalent vanadium into soluble vanadate, and some pollution is inevitably generated in productionOf (e.g. SO)2、HCl、Cl2Etc.) and wastes which are difficult to recycle (such as vanadium extraction tailings, vanadium chromium slag, by-product sodium sulfate, etc.), so that the limitation of the sodium vanadium extraction process is more and more obvious when steel enterprises face more and more strict environmental requirements. The process of calcium roasting-acid leaching vanadium extraction of vanadium slag is characterized in that calcium salt is used as an additive, roasting is carried out in a high-temperature oxidizing atmosphere to oxidize low-valence vanadium in the vanadium slag into pentavalent vanadium, calcium vanadate which is insoluble in water and soluble in acid is generated, a vanadium-containing solution is obtained by leaching in a dilute sulfuric acid solution, then a vanadium pentoxide product is obtained by removing impurities and precipitating vanadium, and vanadium precipitation wastewater can be returned for use after being simply treated. Because a large amount of calcium salt is added in the roasting process, the calcium sulfate enters the vanadium extraction tailings in the acid leaching process, so that the tailings have high sulfur content and high comprehensive utilization cost.
Patent document CN103898329B discloses a vanadium extraction method of manganese roasted vanadium slag, which is to mix vanadium slag with a high-valence manganese oxidant and then roast the mixture at a high temperature, so that vanadium and manganese are combined in the roasting process to form a manganese vanadate compound, and obtain a vanadium-containing leachate and a vanadium extraction tailings through acid leaching.
Patent document CN105671340B discloses a method for extracting vanadium from a vanadium-containing raw material, which comprises mixing the vanadium-containing raw material with a manganese source, roasting, leaching the obtained vanadium-containing clinker with an ammonium salt solution to obtain a vanadium-containing solution and vanadium extraction tailings. The method adopts high concentration of leaching agent and large solid-to-solid ratio of reaction solution, which is not beneficial to the subsequent treatment of the leaching solution.
Patent document CN109666789A discloses a method for preparing vanadium pentoxide by using vanadium-chromium slag and manganese carbonate, which comprises mixing vanadium-chromium slag and manganese carbonate, roasting at high temperature to obtain roasted clinker, and then performing acid leaching to obtain vanadium-containing leachate and chromium-containing leached slag; precipitating vanadium in the vanadium-containing leaching solution to obtain ammonium polyvanadate precipitate and manganese-containing supernatant, and further preparing a vanadium pentoxide product from the ammonium polyvanadate precipitate; and carbonizing the manganese-containing supernatant to obtain manganese carbonate precipitate and vanadium precipitation waste liquid, circulating the manganese carbonate back to the roasting system as a roasting additive to participate in the next roasting, and circulating the vanadium precipitation waste liquid back to the leaching system as a leaching medium after removing impurities. The method realizes the high-efficiency separation of vanadium and chromium in the high-chromium vanadium slag, but a large amount of sodium ions are introduced in the carbonization process of recovering manganese, only ammonia nitrogen is removed in the treatment of vanadium precipitation waste liquid, the treatment of the sodium ions is not mentioned, and sodium can be enriched in the system in the recycling process of water.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for simultaneously extracting vanadium and manganese in vanadium slag.
The invention adopts the technical scheme to solve the technical problems and provides a method for extracting vanadium and manganese by roasting vanadium slag. The method comprises the following steps:
a. mixing vanadium slag and manganese-containing substances, and roasting to obtain roasted clinker;
b. adding a leaching agent into the roasted clinker for leaching to obtain leached slurry, adjusting the pH value, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues;
c. and (3) precipitating vanadium from the leachate by adopting an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and a vanadium precipitation supernatant, adding an impurity removing agent into the vanadium precipitation supernatant, and electrolyzing to obtain manganese metal and anolyte.
In the method for extracting vanadium and manganese by roasting vanadium slag, in the step a, the vanadium slag is converter vanadium slag generated in the smelting process of vanadium titano-magnetite.
Further, the vanadium slag contains 5-12% by mass of vanadium and 3-8% by mass of manganese.
Further, in the step a, the manganese-containing substance is a manganese-containing mineral.
Preferably, the manganese-containing substance is pyrolusite and/or rhodochrosite.
Further preferably, the manganese-containing substance is pyrolusite. Manganese dioxide and/or manganese carbonate with higher purity can also be selected in the invention.
Further, in the step a, the vanadium slag and the manganese-containing substance are mixed according to the mass ratio of Mn/V of 0.8-1.5.
Furthermore, the particle sizes of the vanadium slag and the manganese-containing substances are both less than 0.12 mm.
Further, in the step a, the roasting temperature is 800-900 ℃; the roasting time is 60-180 min.
In the method for extracting vanadium and manganese by roasting vanadium slag, in the step b, the leaching agent is at least one of tap water or the anolyte.
Further, in the step b, the leaching is to leach the roasted clinker and a leaching agent for 20-40 min at 25-40 ℃ according to a liquid-solid ratio of 2-4 mL:1g and under a condition that the pH value is 1.5-2.2.
Furthermore, the grain size of the roasted clinker is controlled to be less than 0.12 mm.
Further, in the step b, a sulfuric acid solution with the mass fraction of 30-95% is adopted in the leaching process to control the pH value of the leaching solution.
Further, in the step b, the pH value is adjusted to 2.5-3.5.
Furthermore, in the step b, 20-30 g/L, Mn 15-30 g/L of TV in the obtained leaching solution.
In the method for extracting vanadium and manganese by roasting vanadium slag, in the step c, the impurity removing agent is at least one of ferrous sulfate, sulfurous acid and scrap iron.
Preferably, the impurity removing agent is ferrous sulfate.
Further, the molar ratio of the impurity removing agent to vanadium is 1-2: 1.
Further, in the step c, direct current electrolysis is adopted in the electrolysis process, and the concentration of manganese in the anolyte is controlled to be 5-10 g/L.
Further, in the step c, the pH value of the acidic ammonium salt in the vanadium precipitation process is controlled to be 1.8-2.2.
The invention has the beneficial effects that:
according to the invention, a manganese-containing substance is added into the manganese-containing vanadium slag, manganese vanadate is generated in the roasting process, and vanadium and manganese enter the solution simultaneously by adopting acid leaching, so that vanadium and manganese resources in the vanadium slag are recycled simultaneously. The method controls the pH value to be 1.5-2.2 in the clinker leaching process, is beneficial to destroying the phase in the clinker, and enables vanadium and manganese to be rapidly dissolved into the solution. And adjusting the pH value of the leached slurry obtained after leaching to 2.5-3.0 to prevent vanadium from hydrolyzing and precipitating under the condition of low pH value, and simultaneously removing impurities such as iron, silicon and the like in the solution. The method has the advantages of simple and easy process, wide application range, low cost and wide application prospect.
Detailed Description
The raw material vanadium slag used for extracting vanadium in the invention not only contains vanadium, but also contains a large amount of manganese. If the vanadium slag is calcified and roasted, in the roasting process, low-valence vanadium is oxidized and then forms vanadate or double salt with calcium, manganese and the like, such as calcium vanadate, manganese vanadate, calcium manganese vanadate and the like. Under the condition that a large amount of calcium exists, the calcium vanadate accounts for a relatively high proportion, the manganese vanadate accounts for a relatively low proportion, and redundant manganese in vanadium slag exists in a high valence form and is difficult to enter a solution in the leaching process. On the basis of this, the method is suitable for the production,
through a large number of experimental researches, the inventor adds a manganese-containing substance into the manganese-containing vanadium slag, generates manganese vanadate in the roasting process, and adopts acid leaching to ensure that vanadium and manganese enter a solution simultaneously, thereby realizing the purpose of simultaneously recycling vanadium and manganese resources in the vanadium slag.
Specifically, the method for extracting vanadium and manganese by roasting vanadium slag comprises the following steps:
a. mixing vanadium slag and manganese-containing substances, and roasting to obtain roasted clinker;
b. adding a leaching agent into the roasted clinker for leaching to obtain leached slurry, adjusting the pH value, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues;
c. and (3) precipitating vanadium from the leachate by adopting an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and a vanadium precipitation supernatant, adding an impurity removing agent into the vanadium precipitation supernatant, and electrolyzing to obtain manganese metal and anolyte.
In the invention, the vanadium slag is converter vanadium slag generated in the vanadium titano-magnetite smelting process. The vanadium slag contains 5-12% of vanadium and 3-8% of manganese by mass.
In the step a, vanadium slag and a manganese-containing substance are mixed, so that vanadium and manganese in the vanadium slag generate manganese vanadate, and in order to ensure higher vanadium leaching rate and avoid manganese resource waste, the vanadium slag and the manganese-containing substance are mixed according to the mass ratio of Mn/V of 0.8-1.5. The vanadium leaching rate is low due to the excessively low Mn/V mass ratio; too high a mass ratio results in excess manganese in a high-valence form, which is difficult to enter the solution during leaching, and thus manganese resources are wasted.
In the step b, a leaching agent is added into the roasted clinker for leaching under the conditions of liquid-solid ratio of 2-4 mL:1g at 25-40 ℃ and pH value of 1.5-2.2, so that vanadium and manganese enter a solution at the same time, and vanadium and manganese resources in vanadium slag are recovered at the same time.
In the step c, the concentration of manganese in the anolyte is controlled to be 5-10 g/L. Too low manganese concentration can cause serious hydrogen evolution side reaction in the electrolysis process and high unit consumption of recovered manganese.
The present invention will be further illustrated by the following specific examples.
Example 1
Taking 500g of vanadium slag (containing 10.35% of vanadium and 6.17% of manganese) and 41.4g of pyrolusite (containing 38.05% of manganese), uniformly mixing, roasting at 800 ℃ for 100min, cooling, crushing, and sieving with a 120-mesh sieve; and performing acid leaching reaction on the clinker and water at 25 ℃ for 40min according to a liquid-solid ratio of 4:1 and a pH value of 1.5, adding ammonia water to adjust the pH value to 2.5, and performing solid-liquid separation to obtain a leaching solution (TV 22.75g/L and Mn17.04g/L) and leaching residues (containing 1.34% of vanadium and 2.17% of manganese). The vanadium yield in the roasting and leaching process is 85.4 percent, and the manganese yield is 75.3 percent. The leaching solution is subjected to an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and vanadium precipitation supernatant, and the vanadium precipitation rate is 98.9%. The ammonium polyvanadate is further oxidized and calcined to obtain vanadium pentoxide, and the product quality meets the requirements of the standard YB/T5304-one 2011. After the vanadium precipitation supernatant is reduced by ferrous sulfate to remove vanadium, a manganese metal product (with the purity of 99.91%) and an acidic anolyte are obtained by direct current electrolysis, and the anolyte (with the pH value of 0.8 and the Mn value of 8.50g/L) can be used for leaching vanadium-containing clinker.
Example 2
Taking 500g of vanadium slag (containing 8.86% of vanadium and 5.85% of manganese) and 64.3g of pyrolusite (containing 38.05% of manganese), uniformly mixing, roasting at 900 ℃ for 120min, cooling, crushing, and sieving with a 120-mesh sieve; and performing acid leaching reaction on the clinker and water at 40 ℃ for 20min according to a liquid-solid ratio of 2.5:1 and a pH value of 2.2, adding lime slurry to adjust the pH value to 3.0, and performing solid-liquid separation to obtain a leaching solution (TV 26.58g/L, Mn 28.63.63 g/L) and leaching residues (containing 1.12% of vanadium and 2.44% of manganese). The vanadium yield in the roasting and leaching process is 86.2 percent, and the manganese yield is 73.8 percent. The leaching solution is subjected to an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and vanadium precipitation supernatant, and the vanadium precipitation rate is 98.5%. The ammonium polyvanadate is further oxidized and calcined to obtain vanadium pentoxide, and the product quality meets the requirements of the standard YB/T5304-one 2011. After the vanadium is removed from the upper layer solution of the precipitated vanadium through sulfurous acid reduction, a manganese metal product (with the purity of 99.85%) and an acidic anolyte are obtained through direct current electrolysis, and the anolyte (with the pH value of 1.0 and the Mn value of 10.0g/L) can be used for leaching vanadium-containing clinker.
Example 3
Taking 500g of vanadium slag (containing 10.35% of vanadium and 6.17% of manganese) and 80.0g of pyrolusite (containing 38.05% of manganese), uniformly mixing, roasting at 850 ℃ for 60min, cooling, crushing, and sieving with a 120-mesh sieve; the anolyte obtained in example 1 (pH 0.8, Mn 8.50g/L) was added to the clinker, water was added to make the liquid-solid ratio 4:1, acid leaching was performed at 30 ℃ and pH 1.8 for 30min, ammonia was added to adjust the pH to 3.5, and solid-liquid separation was performed to obtain a leachate (TV 23.48g/L, Mn 26.25.25 g/L) and a leaching residue (containing 1.25% vanadium, 3.14% manganese). The vanadium yield in the roasting and leaching process is 86.5 percent, and the manganese yield is 72.9 percent. The leaching solution is subjected to an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and vanadium precipitation supernatant, and the vanadium precipitation rate is 98.6%. The ammonium polyvanadate is further oxidized and calcined to obtain vanadium pentoxide, and the product quality meets the requirements of the standard YB/T5304-one 2011. After the vanadium precipitation supernatant is reduced by ferrous sulfate to remove vanadium, a manganese metal product (with the purity of 99.88%) and an acidic anolyte are obtained by direct current electrolysis, and the anolyte (with the pH value of 0.9 and the Mn value of 9.20g/L) can be used for leaching vanadium-containing clinker.
Claims (10)
1. The method for extracting vanadium and manganese by roasting vanadium slag is characterized by comprising the following steps: the method comprises the following steps:
a. mixing vanadium slag and manganese-containing substances, and roasting to obtain roasted clinker;
b. adding a leaching agent into the roasted clinker for leaching to obtain leached slurry, adjusting the pH value, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues;
c. and (3) precipitating vanadium from the leachate by adopting an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate and a vanadium precipitation supernatant, adding an impurity removing agent into the vanadium precipitation supernatant, and electrolyzing to obtain manganese metal and anolyte.
2. The method for extracting vanadium and manganese by roasting vanadium slag according to claim 1, characterized by comprising the following steps: in the step a, the mass content of vanadium in the vanadium slag is 5-12%, and the mass content of manganese is 3-8%.
3. The method for extracting vanadium and manganese by roasting vanadium slag according to claim 1 or 2, characterized by comprising the following steps: in the step a, the manganese-containing substance is a manganese-containing mineral; preferably, the manganese-containing substance is pyrolusite and/or rhodochrosite.
4. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 3, which is characterized by comprising the following steps: in the step a, mixing the vanadium slag and a manganese-containing substance according to the mass ratio of Mn/V of 0.8-1.5.
5. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 4, which is characterized by comprising the following steps: in the step a, the roasting temperature is 800-900 ℃; the roasting time is 60-180 min.
6. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 5, which is characterized by comprising the following steps: in the step b, the leaching agent is at least one of tap water or the anolyte.
7. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 6, which is characterized by comprising the following steps: in the step b, the leaching is to leach the roasted clinker and a leaching agent for 20-40 min at 25-40 ℃ according to a liquid-solid ratio of 2-4 mL:1g and under the condition that the pH value is 1.5-2.2.
8. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 7, which is characterized by comprising the following steps: in the step b, the pH value is adjusted to 2.5-3.5.
9. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 8, which is characterized by comprising the following steps: in the step c, the impurity removing agent is at least one of ferrous sulfate, sulfurous acid and scrap iron.
10. The method for extracting vanadium and manganese by roasting vanadium slag according to any one of claims 1 to 9, characterized by comprising the following steps: in the step c, direct current electrolysis is adopted in the electrolysis process, and the concentration of manganese in the anolyte is controlled to be 5-10 g/L.
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Cited By (2)
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| CN113957262A (en) * | 2021-10-29 | 2022-01-21 | 东北大学 | Method for precipitating vanadium from vanadium-chromium leaching solution without ammonium |
| CN114350965A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium, manganese and recycling wastewater by using vanadium slag calcified roasting clinker |
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| CN113957262A (en) * | 2021-10-29 | 2022-01-21 | 东北大学 | Method for precipitating vanadium from vanadium-chromium leaching solution without ammonium |
| CN113957262B (en) * | 2021-10-29 | 2022-09-23 | 东北大学 | Method for precipitating vanadium from vanadium-chromium leaching solution without ammonium |
| CN114350965A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium, manganese and recycling wastewater by using vanadium slag calcified roasting clinker |
| CN114350965B (en) * | 2021-11-30 | 2024-02-23 | 攀钢集团研究院有限公司 | Method for extracting vanadium, manganese and recycling wastewater from vanadium slag calcified roasting clinker |
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