CN111575496A - Method for extracting vanadium by low-calcium roasting of vanadium slag - Google Patents
Method for extracting vanadium by low-calcium roasting of vanadium slag Download PDFInfo
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- CN111575496A CN111575496A CN202010608225.0A CN202010608225A CN111575496A CN 111575496 A CN111575496 A CN 111575496A CN 202010608225 A CN202010608225 A CN 202010608225A CN 111575496 A CN111575496 A CN 111575496A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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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- 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to the technical field of vanadium hydrometallurgy, in particular to a method for extracting vanadium by low-calcium roasting of vanadium slag. The invention aims to solve the technical problem of providing a vanadium slag low-calcium roasting vanadium extraction method which can realize vanadium slag low-calcium roasting and reduce the calcium and sulfur content in the residue. 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 into the roasted clinker for leaching to obtain leached slurry; c. and adding a pH regulator into the leached slurry until the pH value is 2.5-3.5, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues. The inventionThe method can recycle vanadium and manganese resources in the vanadium slag and simultaneously 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 by low-calcium roasting of vanadium slag.
Background
The 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 calcium extraction processA vanadium extraction process by chemical roasting. 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 providing a vanadium slag low-calcium roasting vanadium extraction method which can realize vanadium slag low-calcium roasting and reduce the calcium and sulfur content in the residue.
The invention adopts the technical scheme to solve the technical problems and provides a method for extracting vanadium from vanadium slag by low-calcium roasting. 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 into the roasted clinker for leaching to obtain leached slurry;
c. and adding a pH regulator into the leached slurry until the pH value is 2.5-3.5, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues.
In the method for extracting vanadium by low-calcium roasting 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 5-12% of metal vanadium and 3-8% of metal manganese by mass percent.
Further, in the step a, the particle sizes of the vanadium slag and 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 by low-calcium roasting of vanadium slag, in the step b, the granularity of the roasted clinker is less than 0.12 mm.
Further, in the step b, the leaching agent is recycled water and/or tap water after wastewater treatment.
Further, in step b, the leaching conditions are as follows: the leaching pH value is 1.5-2.2; the solid-to-solid ratio of the leaching solution is 2-4: 1; leaching at 25-40 ℃; the leaching time is 20-40 min.
Further, in the step b, a sulfuric acid solution with the mass fraction of 30-95% is adopted to control the pH value of leaching.
In the method for extracting vanadium by low-calcium roasting of vanadium slag, in the step c, the leachate is subjected to vanadium precipitation by using an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate, and the ammonium polyvanadate is oxidized and calcined to generate vanadium pentoxide or is reduced to generate vanadium trioxide.
Further, in step c, the pH adjusting agent is at least one of ammonia water or lime.
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. The inventionThe method controls the pH value of the roasted clinker to be 1.5-2.2 during leaching, which is beneficial to destroying the phase of the clinker and rapidly dissolving vanadium into the solution. And after leaching, controlling the pH value of the leached slurry to be 2.5-3.5 by adopting a pH regulator so as to prevent vanadium from hydrolyzing and precipitating under the condition of low pH, and 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
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 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.
Specifically, the method for extracting vanadium by low-calcium roasting of vanadium slag 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 into the roasted clinker for leaching to obtain leached slurry;
c. and adding a pH regulator into the leached slurry until the pH value is 2.5-3.5, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues.
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 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 roasted clinker is controlled to be 1.5-2.2 in the leaching process, so that the phases in the clinker are damaged, and vanadium is rapidly dissolved into the solution.
In the step c, after leaching, a pH regulator is adopted to control the pH value of the leached slurry to be 2.5-3.5 so as to prevent vanadium from hydrolyzing and precipitating under the condition of low pH and simultaneously remove impurities such as iron, silicon and the like in the solution.
The present invention will be further illustrated by the following specific examples.
Example 1
Taking vanadium slag (containing 10.14 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 120min, cooling, pulverizing, and sieving with 120 mesh sieve; performing acid leaching reaction on the clinker and a leaching agent at 25 ℃ for 30min according to a liquid-solid ratio of 4:1 and a pH value of 1.8, adding ammonia water to adjust the pH value to 2.5, and performing solid-liquid separation to obtain a leaching solution and a leaching residue (containing 1.28 percent of vanadium, 3.41 percent of manganese, 2.55 percent of calcium and 1.74 percent of sulfur)). The leaching rate of vanadium is 90.1% and the leaching rate of manganese is 64.1% in the roasting and leaching process. 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 99.2%. And further oxidizing and calcining the ammonium polyvanadate to obtain vanadium pentoxide, wherein the product quality meets the requirements of the standard YB/T5304-2011.
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 0.15, calcining at 850 deg.C for 60min, cooling, pulverizing, and sieving with 120 mesh sieve; performing acid leaching reaction on the clinker and a leaching agent at 30 ℃ for 20min according to a liquid-solid ratio of 3:1 and a pH value of 1.5, adding ammonia water to adjust the pH value to 3.0, and performing solid-liquid separation to obtain a leaching solution and a leaching residue (containing 1.02% of vanadium, 1.90% of manganese, 1.54% of calcium and 1.03% of sulfur). The leaching rate of vanadium in the roasting leaching process is 89.2 percent, and the leaching rate of manganese is 73.1 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 99.0%. And further oxidizing and calcining the ammonium polyvanadate to obtain vanadium pentoxide, wherein the product quality meets the requirements of the standard YB/T5304-2011.
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 0.20, calcining at 900 deg.C for 30min, cooling, pulverizing, and sieving with 120 mesh sieve; performing acid leaching reaction on the clinker and a leaching agent at 40 ℃ for 40min according to a liquid-solid ratio of 2:1 and a pH value of 2.2, adding ammonia water to adjust the pH value to 3.0, and performing solid-liquid separation to obtain a leaching solution and a leaching residue (containing 0.75% of vanadium, 1.45% of manganese, 1.84% of calcium and 1.27% of sulfur). The leaching rate of vanadium is 87.8 percent and the leaching rate of manganese is 69.5 percent in the roasting and leaching process. 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 99.1%. And further oxidizing and calcining the ammonium polyvanadate to obtain vanadium pentoxide, wherein the product quality meets the requirements of the standard YB/T5304-2011.
Claims (10)
1. The method for extracting vanadium by low-calcium roasting of vanadium slag is characterized by comprising the following steps: 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 into the roasted clinker for leaching to obtain leached slurry;
c. and adding a pH regulator into the leached slurry until the pH value is 2.5-3.5, and carrying out solid-liquid separation to obtain a leaching solution and leaching residues.
2. The method for extracting vanadium from vanadium slag through low-calcium roasting according to claim 1, which is characterized by comprising the following steps of: in the step c, the leachate is subjected to vanadium precipitation by using an acidic ammonium salt vanadium precipitation method to obtain ammonium polyvanadate, and the ammonium polyvanadate is oxidized and calcined to generate vanadium pentoxide or is reduced to generate vanadium trioxide.
3. The method for extracting vanadium from vanadium slag through low-calcium roasting according to claim 1 or 2, characterized by comprising the following steps: in the step a, the vanadium slag contains 5-12% of metal vanadium and 3-8% of metal manganese by mass percent.
4. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 3, characterized by comprising the following steps: in the step a, the particle sizes of the vanadium slag and the limestone are both less than 0.12 mm.
5. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 4, characterized by comprising the following steps: in the step a, the roasting temperature is 800-900 ℃; the roasting time is 30-180 min.
6. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 5, characterized by comprising the following steps: in the step b, the particle size of the roasted clinker is less than 0.12 mm.
7. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 6, characterized by comprising the following steps: in the step b, the leaching agent is recycled water and/or tap water after wastewater treatment.
8. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 7, characterized by comprising the following steps: in the step b, the leaching conditions are as follows: the leaching pH value is 1.5-2.2; the solid-to-solid ratio of the leaching solution is 2-4: 1; leaching at 25-40 ℃; the leaching time is 20-40 min.
9. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 8, characterized by comprising the following steps: in the step b, a sulfuric acid solution with the mass fraction of 30-95% is adopted to control the pH value of leaching.
10. The method for extracting vanadium through low-calcium roasting of vanadium slag according to any one of claims 1 to 9, characterized by comprising the following steps: in the step c, the pH regulator is at least one of ammonia water or lime.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN112111661A (en) * | 2020-09-24 | 2020-12-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium by calcium-manganese composite roasting of vanadium slag |
| CN112410569A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Method for recovering vanadium from acidic vanadium-containing underflow slag |
| CN112430740A (en) * | 2020-11-30 | 2021-03-02 | 东北大学 | Method for strengthening vanadium-chromium separation by cooperatively roasting vanadium slag through calcium salt and manganese salt |
| CN113957272A (en) * | 2021-09-23 | 2022-01-21 | 攀钢集团研究院有限公司 | Vanadium slag vanadium extraction method using sintering process red mud as additive |
| CN114350964A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide by using high-phosphorus high-calcium vanadium slag and recycling leachate |
| CN115611309A (en) * | 2022-08-10 | 2023-01-17 | 新疆盛安新材料科技有限公司 | Industrial method for preparing high-quality vanadium oxide from calcium vanadate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN112080651B (en) * | 2020-09-23 | 2022-07-19 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN112111661A (en) * | 2020-09-24 | 2020-12-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium by calcium-manganese composite roasting of vanadium slag |
| CN112410569A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Method for recovering vanadium from acidic vanadium-containing underflow slag |
| CN112430740A (en) * | 2020-11-30 | 2021-03-02 | 东北大学 | Method for strengthening vanadium-chromium separation by cooperatively roasting vanadium slag through calcium salt and manganese salt |
| CN112430740B (en) * | 2020-11-30 | 2022-05-10 | 东北大学 | Method for strengthening vanadium-chromium separation by cooperatively roasting vanadium slag through calcium salt and manganese salt |
| CN113957272A (en) * | 2021-09-23 | 2022-01-21 | 攀钢集团研究院有限公司 | Vanadium slag vanadium extraction method using sintering process red mud as additive |
| CN113957272B (en) * | 2021-09-23 | 2023-02-03 | 攀钢集团研究院有限公司 | Vanadium slag vanadium extraction method using sintering process red mud as additive |
| CN114350964A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide by using high-phosphorus high-calcium vanadium slag and recycling leachate |
| 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 |
| CN115611309A (en) * | 2022-08-10 | 2023-01-17 | 新疆盛安新材料科技有限公司 | Industrial method for preparing high-quality vanadium oxide from calcium vanadate |
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