CN111719051A - Method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching - Google Patents
Method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching Download PDFInfo
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- 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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- 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
- 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
- C22B47/00—Obtaining manganese
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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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention relates to the technical field of vanadium hydrometallurgy, in particular to a method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching. The invention aims to solve the technical problem of improving the method for extracting vanadium by low-calcium roasting and acid leaching of vanadium slag, which can realize low-calcium roasting of vanadium slag and reduce the content of calcium and sulfur in secondary residues. The method comprises the following steps: a. vanadium slag and limestone according to CaO/V2O5Mixing and roasting at a weight ratio of 0.15-0.25 to obtain roasted clinker; b. adding a leaching agent 1 into the roasted clinker for primary leaching, and performing solid-liquid separation to obtain primary vanadium-containing leaching solution and primary residue; c. adding a leaching agent 2 into the primary residue for secondary leaching, controlling the pH value of a leaching end point, and performing solid-liquid separation to obtain a secondary vanadium-containing leaching solution and a secondary residue; the secondary vanadium-containingAnd (c) returning the leachate as a leaching agent 1 to the step b for use. The method can recycle vanadium and manganese resources in the vanadium slag and reduce the content of calcium and sulfur in the tailings.
Description
Technical Field
The invention relates to the technical field of vanadium hydrometallurgy, in particular to a method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching.
Background
Vanadium slag is a main raw material for preparing vanadium oxide, and currently, vanadium slag is a main raw material for preparing vanadium oxideThere are two main industrialized vanadium extraction 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 pollutant gas (such as SO) is inevitably generated in production2、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.
Patent document CN101161831A discloses a method for calcifying and roasting vanadium slag, which comprises the steps of mixing CaO and V2O5Roasting the vanadium slag with the weight ratio of 0.5-0.7 in a roasting furnace at the temperature of 600-950 ℃. The method needs to add high-content calcium to roast the vanadium slag, and because a large amount of calcium salt is added in the roasting process, the calcium salt enters the vanadium extraction tailings in the form of calcium sulfate in the acid leaching process, the tailings have high sulfur content, and the comprehensive utilization cost is high.
Disclosure of Invention
The invention aims to solve the technical problem of improving a vanadium slag low-calcium roasting acid leaching vanadium extraction method which can realize low-calcium roasting of vanadium slag and reduce the contents of calcium and sulfur in secondary residues.
The invention provides a method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching, which is used for solving the technical problems. The method comprises the following steps:
a. vanadium slag and limestone according to CaO/V2O5Mixing and roasting at a weight ratio of 0.15-0.25 to obtain roasted clinker;
b. adding a leaching agent 1 into the roasted clinker for primary leaching, and performing solid-liquid separation to obtain primary vanadium-containing leaching solution and primary residue;
c. adding a leaching agent 2 into the primary residue for secondary leaching, controlling the pH value of a leaching end point, and performing solid-liquid separation to obtain a secondary vanadium-containing leaching solution and a secondary residue; and (c) returning the secondary vanadium-containing leaching solution as a leaching agent 1 to the step (b) for use.
In the method for extracting vanadium by low-calcium roasting and acid leaching of 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 6-12% of metal vanadium and 3-8% of metal manganese by mass percent.
Further, in the step a, the particle size of the vanadium slag and the particle size of the limestone are both less than 0.12 mm.
Further, in the step a, the roasting temperature is 800-900 ℃; the roasting time is 30-180 min.
In the method for extracting vanadium from the vanadium slag by low-calcium roasting and acid leaching, in the step b, the primary leaching condition is as follows: the leaching pH value is 2.6-3.0; the solid-to-solid ratio of the leaching solution is 2-4 mL:1 g; leaching at 25-60 ℃; the leaching time is 40-100 min.
Further, in the step b, the particle size of the roasted clinker is less than 0.12 mm.
Further, in the step b and the step c, a sulfuric acid solution with the mass fraction of 30-95% is adopted to control the pH values of the primary leaching and the secondary leaching.
In the method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching, in the step c, the leaching agent 2 is recycled water and/or tap water after wastewater treatment.
Further, in step c, the conditions of the secondary leaching are as follows: the leaching pH value is 1.0-1.2; the solid-to-solid ratio of the leaching solution is 1.5-3: 1; leaching at 25-40 ℃; the leaching time is 5-20 min.
Further, in the step c, the pH value of the secondary leaching end point is controlled to be 2.5-3.0.
Further, in the step c, at least one of ammonia water or lime slurry is adopted to control the pH value of the leaching end point.
The invention has the beneficial effects that:
the invention adopts low calcium roasting to mix vanadium slag and limestone according to CaO/V2O5Mixing and roasting the vanadium slag and the limestone in a weight ratio of 0.15-0.25, adding a small amount of calcium source to generate calcium vanadate, calcium manganese vanadate and manganese vanadate salts in the roasting process, and performing acid leaching to ensure that vanadium and manganese enter a solution simultaneously, thereby realizing the recycling of vanadium and manganese resources in the vanadium slag and simultaneously reducing the content of calcium and sulfur in tailings. According to the method, the roasted clinker is leached twice, the pH value of the first leaching is controlled to be 2.6-3.0, most of vanadium and manganese in the clinker enter a solution, and impurities such as iron and silicon are less dissolved out; and performing secondary leaching on the obtained primary residue, and controlling the pH value of leaching to be 1.0-1.2, so that the ore phase in the slag can be damaged, and the vanadium can be further dissolved, thereby improving the yield of the vanadium. The secondary vanadium-containing leaching solution obtained by the invention is directly used as a leaching agent to return to the primary leaching process of the clinker, thereby recovering vanadium resources. The method has the advantages of simple and easy process, wide application range, low cost and wide application prospect.
Detailed Description
In the process of calcifying and roasting vanadium slag, 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. Because the mass ratio of calcium to vanadium in the existing vanadium slag roasting process is 0.5-0.8, Ca is easily generated when calcium pyrovanadate is easily generated in the roasting process2V2O7During the sulfuric acid leaching process of clinker, vanadium enters into the solution, and calcium reacts with sulfate radicals to generate calcium sulfate which enters into the residue, so that the content of calcium and sulfur in the residue is high. In addition, the vanadium slag used as a raw material for extracting vanadium not only contains vanadium, but also contains a large amount of manganese, and under the condition that calcium exists in a large amount, the generated calcium vanadate accounts for a relatively high amount, the generated manganese vanadate accounts for a relatively low amount, and redundant manganese in the vanadium slag exists in a high-valence form, so that the vanadium slag is difficult to enter a solution in the leaching process.
Through a large amount of experimental researches, the inventor adopts low-calcium roasting to mix vanadium slag and limestone according to CaO/V2O5Mixing and roasting the mixture according to the weight ratio of 0.15-0.25, adding a small amount of calcium source to enable the vanadium slag and the limestone to generate calcium vanadate, calcium manganese vanadate and manganese vanadate salts in the roasting process, and then adopting acid leaching to enable vanadium and manganese to be obtainedAnd simultaneously, the vanadium and manganese resources in the vanadium slag are recycled, and the content of calcium and sulfur in the tailings is reduced.
Specifically, the method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching comprises the following steps:
a. vanadium slag and limestone according to CaO/V2O5Mixing and roasting at a weight ratio of 0.15-0.25 to obtain roasted clinker;
b. adding a leaching agent 1 into the roasted clinker for primary leaching, and performing solid-liquid separation to obtain primary vanadium-containing leaching solution and primary residue;
c. adding a leaching agent 2 into the primary residue for secondary leaching, controlling the pH value of a leaching end point, and performing solid-liquid separation to obtain a secondary vanadium-containing leaching solution and a secondary residue; and (c) returning the secondary vanadium-containing leaching solution as a leaching agent 1 to the step (b) for use.
In the invention, the vanadium slag is converter vanadium slag generated in the vanadium titano-magnetite smelting process. The vanadium slag contains 6-12% of metal vanadium and 3-8% of metal manganese by mass percent.
In the step a, low-calcium roasting is adopted, and the vanadium slag and the limestone are roasted according to CaO/V2O5Mixing and roasting the vanadium slag and the limestone in a weight ratio of 0.15-0.25 to generate calcium vanadate, calcium manganese vanadate and manganese vanadate salts in the roasting process, and then adopting acid leaching to enable vanadium and manganese to enter a solution simultaneously, so that vanadium and manganese resources in the vanadium slag are recycled, and the content of calcium and sulfur in tailings is reduced.
When CaO/V2O5When the weight ratio is increased, the leaching rate of manganese is reduced, and when CaO/V is increased2O5When the leaching rate is more than 0.5, the leaching rate of manganese is reduced to 30 percent due to the combination of vanadium and calcium, and in order to ensure the leaching rate of vanadium and fully utilize manganese in vanadium slag, CaO/V is added into the vanadium slag2O5The weight ratio is controlled to be 0.25 to 0.5.
In the step b, the pH value of the first leaching is controlled to be 2.6-3.0, so that most of vanadium and manganese in the clinker enter the solution, and meanwhile, impurities such as iron, silicon and the like are less dissolved out.
In the step c, the obtained primary residue is leached for the second time, the pH value of leaching is controlled to be 1.0-1.2, the ore phase in the residue is favorably damaged, and vanadium is further dissolved, so that the yield of the vanadium is improved.
The present invention will be further illustrated by the following specific examples.
Example 1
Taking vanadium slag (containing 10.86 percent of vanadium and 6.82 percent of manganese) and limestone powder (containing CaO54.5 percent) according to CaO/V2O5Mixing at weight ratio of 0.25, calcining at 800 deg.C for 90min, cooling, pulverizing, and sieving with 120 mesh sieve; and performing acid leaching reaction on the clinker and a leaching agent 1 at 40 ℃ for 60min under the conditions of a liquid-solid ratio of 3:1 and a pH value of 2.6, and performing solid-liquid separation to obtain vanadium-containing leaching solution (28.1 g/L vanadium and 11.8g/L manganese) and primary leaching residue. And performing acid leaching reaction on the primary leaching residue and a leaching agent 2 for 10min at the liquid-solid ratio of 1.5:1, the pH value of 1.0 and the temperature of 25 ℃, adjusting the pH value to 2.5 by using ammonia water, and performing solid-liquid separation to obtain a low-vanadium leaching solution (containing 2.5g/L vanadium and 0.2g/L manganese) and a secondary residue (containing 0.92% vanadium, 3.08% manganese, 3.08% calcium and 1.86% sulfur). The vanadium leaching rate and the manganese leaching rate in the whole roasting and leaching process are respectively 91.7% and 65.2%.
Example 2
Vanadium slag (containing 8.45 percent of vanadium and 5.42 percent of manganese) and limestone powder (containing 54.5 percent of CaO54%) are taken according to CaO/V2O5Mixing at weight ratio of 0.2, calcining at 850 deg.C for 120min, cooling, pulverizing, and sieving with 120 mesh sieve; and performing acid leaching reaction on the clinker and a leaching agent 1 at 25 ℃ for 80min under the conditions that the liquid-solid ratio is 2.3:1 and the pH value is 2.8, and performing solid-liquid separation to obtain vanadium-containing leachate (containing 28.3g/L vanadium and 8.0g/L manganese) and primary leaching residue. And carrying out acid leaching reaction on the primary leaching residue and a leaching agent 2 for 15min under the conditions of a liquid-solid ratio of 3:1, a pH value of 1.2 and 40 ℃, adjusting the pH value to 2.8 by using ammonia water, and carrying out solid-liquid separation to obtain a low-vanadium leaching solution (containing vanadium 4.5g/L and manganese 3.2g/L) and a secondary residue (containing vanadium 0.90%, manganese 1.78%, calcium 1.92% and sulfur 1.15%). The vanadium leaching rate and the manganese leaching rate in the whole roasting and leaching process are respectively 90.8% and 74.8%.
Example 3
Vanadium slag (containing 6.64 percent of vanadium and 4.51 percent of manganese) and limestone powder (containing 54.5 percent of CaO54%) are taken according to CaO/V2O5Mixing at weight ratio of 0.15, calcining at 900 deg.C for 30min, cooling, pulverizing, and sieving with 120 mesh sieve; cookingThe materials are subjected to acid leaching reaction for 80min with a leaching agent 1 at a liquid-solid ratio of 2:1 and a pH value of 2.8 at 50 ℃, and a vanadium-containing leaching solution (containing 25.9g/L vanadium and 5.4g/L manganese) and primary leaching residues are obtained through solid-liquid separation. And carrying out acid leaching reaction on the primary leaching residue and a leaching agent 2 for 20min at the liquid-solid ratio of 2:1, the pH value of 1.2 and the temperature of 30 ℃, adjusting the pH value to 3.0 by adopting ammonia water, and carrying out solid-liquid separation to obtain a low-vanadium leaching solution (containing vanadium 3.8g/L and manganese 4.4g/L) and a secondary residue (containing vanadium 0.75%, manganese 1.50%, calcium 0.95% and sulfur 0.58%). The vanadium leaching rate and the manganese leaching rate in the whole roasting and leaching process are respectively 89.6% and 72.5%.
Claims (10)
1. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching is characterized by comprising the following steps of: the method comprises the following steps:
a. vanadium slag and limestone according to CaO/V2O5Mixing and roasting at a weight ratio of 0.15-0.25 to obtain roasted clinker;
b. adding a leaching agent 1 into the roasted clinker for primary leaching, and performing solid-liquid separation to obtain primary vanadium-containing leaching solution and primary residue;
c. adding a leaching agent 2 into the primary residue for secondary leaching, controlling the pH value of a leaching end point, and performing solid-liquid separation to obtain a secondary vanadium-containing leaching solution and a secondary residue; and (c) returning the secondary vanadium-containing leaching solution as a leaching agent 1 to the step (b) for use.
2. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching is characterized by comprising the following steps of: in the step a, the vanadium slag contains 6-12% of metal vanadium and 3-8% of metal manganese by mass percent.
3. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching is characterized by comprising the following steps of: in the step a, the particle sizes of the vanadium slag and the limestone are both less than 0.12 mm.
4. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 3, characterized by comprising the following steps: in the step a, the roasting temperature is 800-900 ℃; the roasting time is 30-180 min.
5. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 4, characterized by comprising the following steps: in the step b, the conditions of the primary leaching are as follows: the leaching pH value is 2.6-3.0; the solid-to-solid ratio of the leaching solution is 2-4 mL:1 g; leaching at 25-60 ℃; the leaching time is 40-100 min.
6. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 5, characterized by comprising the following steps: in the step b and the step c, the pH values of the primary leaching and the secondary leaching are controlled by adopting a sulfuric acid solution with the mass fraction of 30-95%.
7. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 6, characterized by comprising the following steps: in the step c, the leaching agent 2 is recycled water and/or tap water after wastewater treatment.
8. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 7, characterized by comprising the following steps: in the step c, the conditions of the secondary leaching are as follows: the leaching pH value is 1.0-1.2; the solid-to-solid ratio of the leaching solution is 1.5-3: 1; leaching at 25-40 ℃; the leaching time is 5-20 min.
9. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 8, characterized by comprising the following steps: in the step c, the pH value of the secondary leaching end point is controlled to be 2.5-3.0.
10. The method for extracting vanadium from vanadium slag by low-calcium roasting and acid leaching according to any one of claims 1 to 9, characterized by comprising the following steps: in the step c, at least one of ammonia water or lime slurry is adopted to control the pH value of the leaching end point.
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| CN114350964B (en) * | 2021-11-30 | 2024-01-26 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide by utilizing high-phosphorus high-calcium vanadium slag and recycling leaching liquid |
| CN114990360A (en) * | 2022-07-22 | 2022-09-02 | 攀枝花市阳润科技有限公司 | Method for extracting vanadium from vanadium slag by acid leaching |
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