CN112239808A - Method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag - Google Patents
Method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag Download PDFInfo
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- CN112239808A CN112239808A CN202011186980.0A CN202011186980A CN112239808A CN 112239808 A CN112239808 A CN 112239808A CN 202011186980 A CN202011186980 A CN 202011186980A CN 112239808 A CN112239808 A CN 112239808A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the technical field of vanadium extraction, in particular to a method for extracting vanadium by utilizing vanadium-containing high-calcium high-phosphorus slag. The method comprises the following steps: a: carrying out primary crushing and primary sieving on the vanadium-containing high-calcium high-phosphorus slag to obtain a material with the particle size of less than 5mm, and then carrying out wet grinding and secondary sieving to obtain a material with the particle size of less than 0.175 mm; b: mixing the material obtained in the step a with water, then introducing sulfur dioxide gas under stirring until the pH value is 4-7, and then filtering to obtain low-calcium vanadium-containing slag and a calcium-rich solution; c: roasting the low-calcium vanadium-containing slag to obtain clinker, crushing the clinker, and then performing acid leaching to obtain vanadium-containing solution; d: heating the calcium-rich solution to obtain sulfur dioxide gas, and then returning to the step b for use. The method pretreats the vanadium-containing high-calcium high-phosphorus slag, and greatly reduces the content of calcium in the vanadium-containing high-calcium high-phosphorus slag and improves the grade of vanadium through the processes of iron removal, water grinding, decalcification and vanadium extraction.
Description
Technical Field
The invention relates to the technical field of vanadium extraction, in particular to a method for extracting vanadium by utilizing vanadium-containing high-calcium high-phosphorus slag.
Background
The vanadium titano-magnetite is the main resource for extracting vanadium oxide at present, the vanadium extraction process mainly comprises direct vanadium extraction and blast furnace process, and the vanadium oxide grade (V) in some foreign vanadium titano-magnetite is higher2O5Content is more than 1 wt%), and direct vanadium extraction process is adopted, so thatThe grade of vanadium oxide in most of domestic vanadium titano-magnetite is generally low (V)2O5The content is less than 0.5 percent), and when a blast furnace process is adopted, vanadium in the molten iron is oxidized and enriched in the vanadium slag of the converter and is used as a raw material for further extracting vanadium. In addition, 8-10% of vanadium resources enter the dephosphorization slag for steel making in the blast furnace process, and the vanadium resources cannot be used as raw materials for extracting vanadium due to the fact that the vanadium resources contain very high calcium oxide and phosphorus.
At present, part of the vanadium-containing high-calcium high-phosphorus slag is still used in the construction industry, which causes the waste of vanadium resources. In Pan Steel preparation of Steel slag composite micropowder and application thereof in concrete, the steel slag composite micropowder is prepared from vanadium-containing high-calcium high-phosphorus slag, and concrete preparation tests are carried out. The result shows that the activity index of the prepared steel slag composite micro powder in 28 days reaches more than 90 percent, the prepared concrete has better workability, and the compressive strength meets the design requirement.
In the research on the experiment of directly acid-leaching vanadium-containing high-calcium high-phosphorus slag by using new sulfuric acid and titanium white waste acid, the research on the direct acid-leaching vanadium-extracting of the new sulfuric acid and the titanium white waste acid is carried out by using the vanadium-containing high-calcium high-phosphorus slag as a raw material. Vanadium is dispersed in various minerals in the vanadium-containing high-calcium high-phosphorus slag, and V4+The dense large-particle vanadium-titanium-calcium oxide formed by the vanadium-titanium-calcium-titanium. The direct acid leaching is difficult to damage the structure, and the ball milling of the vanadium-containing high-calcium high-phosphorus slag is needed to improve the leaching rate of vanadium. Elements such as Ca, Si, V, O and the like form ore phases such as dicalcium silicate and the like, and the vanadium content in the ore phases is low and is relatively dispersed, but the vanadium is easily leached directly by acid. The direct acid leaching of the vanadium-containing high-calcium high-phosphorus slag shows that the stirring speed at normal temperature is 200r/min, the sulfuric acid concentration is 30 percent, the granularity of the vanadium-containing high-calcium high-phosphorus slag is 65 percent of-120 meshes, the liquid-solid ratio is 7: 1, the acid leaching time is 1h, the acid leaching condition is better, and the leaching rate of vanadium can reach 79 percent. When the titanium white waste acid is used for leaching, the leaching rate of vanadium reaches 74 percent, and the vanadium leaching rates of new sulfuric acid and the waste acid are not greatly different. Because the vanadium-containing high-calcium high-phosphorus slag has higher CaO and FeO content and large acid consumption, the cost is too high by leaching with new sulfuric acid, while the titanium white waste acid is waste and can not be directly discharged, the traditional treatment process adopts calcium carbonate for neutralization and adopts vanadium-containing high-phosphorus slagThe titanium white waste acid neutralized by the calcium high-phosphorus slag can greatly consume the titanium white waste acid, reduce the calcium carbonate consumption of the single neutralized waste acid, and simultaneously extract vanadium in the vanadium-containing high-calcium high-phosphorus slag, thereby realizing high-value utilization of the vanadium-containing high-calcium high-phosphorus slag. However, in the process, under the condition that vanadium has a system with high acidity and high impurities, the further extraction with high yield is the key of the next research.
In "melting Na2CO3Research on roasting process of vanadium-containing high-calcium high-phosphorus slag in system aiming at molten Na2CO3The roasting process of the vanadium-containing high-calcium high-phosphorus slag in the system is researched. The roasting temperature and Na are investigated through a single-factor experiment2CO3The influence of the addition amount and the roasting time on the leaching rate of vanadium in the vanadium-containing high-calcium high-phosphorus slag is realized by optimizing process conditions by adopting orthogonal design on the basis of a single-factor experiment and analyzing a reaction mechanism. The results show that molten Na2CO3The optimized experimental conditions for roasting the vanadium-containing high-calcium high-phosphorus slag in the system are that the roasting temperature is 900 ℃ and Na2CO3The addition amount is 40 percent, the roasting time is 60min, and the vanadium leaching rate is stabilized to be more than 90 percent at the moment. On the whole, although the process obtains higher vanadium yield, the cost is high, and further impurity removal and vanadium precipitation of the leaching with high alkalinity are huge technical difficulties.
Regarding the removal of calcium in the vanadium-containing high-calcium high-phosphorus slag, the process research of calcium leaching by ammonium salt and vanadium leaching by acid leaching is carried out on the vanadium-containing high-calcium high-phosphorus slag in the way of purification and recovery of negative component calcium in the vanadium-containing high-calcium high-phosphorus slag. In the process of leaching calcium by using ammonium salt, the leaching agent ammonium chloride can be recycled, and good economic and environment-friendly effects are achieved. The leached calcium ions can be prepared into calcium carbonate with higher purity by a precipitation method, so that the effective recycling of calcium is realized. In the acid leaching vanadium extraction process, not only is the roasting procedure omitted, the problem of waste gas pollution of the traditional sodium treatment roasting is solved, but also a novel leaching agent A with good vanadium leachability is selected for acid leaching vanadium extraction, so that the content of impurities in the leaching solution is reduced, and the problem of large acid consumption in the acid leaching vanadium extraction is solved. Although the process reduces the calcium in the vanadium-containing high-calcium high-phosphorus slag, the process is substantially an acid decalcification process, the recovery cost is high, and chloride ions seriously corrode equipment.
From the analysis of the current research situation, the research on direct vanadium extraction of vanadium-containing high-calcium high-phosphorus slag in the prior art is still incomplete, an effective decalcification and vanadium extraction process is lacked, and a great amount of intensive research is needed to realize industrial application.
Disclosure of Invention
The invention aims to solve the problems of difficult iron and calcium removal, low vanadium grade, complex process, high cost and low vanadium extraction rate in the prior art, and provides a method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag.
In order to achieve the aim, the invention provides a method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag, which comprises the following steps:
a: carrying out primary crushing and primary sieving on the vanadium-containing high-calcium high-phosphorus slag to obtain a material with the particle size of less than 5mm, and then carrying out wet grinding and secondary sieving to obtain a material with the particle size of less than 0.175 mm;
b: mixing the material obtained in the step a with water, then introducing sulfur dioxide gas under the stirring condition until the pH value is 4-7, and then filtering to obtain low-calcium vanadium-containing slag and a calcium-rich solution;
c: b, roasting the low-calcium vanadium-containing slag obtained in the step a to obtain a clinker, crushing the clinker, and then performing acid leaching to obtain a vanadium-containing solution;
d: and c, heating the calcium-rich solution obtained in the step b to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step b for use.
Preferably, in the step a, the content of vanadium pentoxide in the vanadium-containing high-calcium high-phosphorus slag is more than 1 wt%, and the content of calcium oxide in the vanadium-containing high-calcium high-phosphorus slag is more than 20 wt%.
Preferably, in step a, the wet milling is carried out in a wet ball mill.
Preferably, in the step a, the volume ratio of water to materials in the wet grinding is (0.1-0.8): 1.
Preferably, in the step b, the liquid-solid ratio of the water to the material is 5-10 mL/g.
Preferably, in the step b, the stirring speed is 100-300 r/min.
Preferably, in step c, the firing conditions include: the roasting temperature is 800-1000 ℃, and the roasting time is 30-180 min.
Preferably, in step c, the clinker is crushed to a particle size of less than 120 mesh.
Preferably, in step c, the specific process of acid leaching comprises: mixing water and clinker according to a liquid-solid ratio of 0.5-5 mL/g, adjusting the pH value to 0.5-3, and leaching for 30-240 min.
Preferably, in step d, the heating temperature is 60 ℃ to 100 ℃.
The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag comprises the steps of pretreating the vanadium-containing high-calcium high-phosphorus slag in advance, and greatly reducing the content of calcium in the vanadium-containing high-calcium high-phosphorus slag and improving the grade of vanadium through the processes of removing iron, grinding with water, decalcifying and extracting vanadium. The method not only changes the vanadium-containing high-calcium high-phosphorus slag waste resources into valuable, but also has the advantages of simple and easy process, low equipment requirement, convenient operation, low cost and the like, and has good social benefit and economic benefit.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag, which comprises the following steps:
a: carrying out primary crushing and primary sieving on the vanadium-containing high-calcium high-phosphorus slag to obtain a material with the particle size of less than 5mm, and then carrying out wet grinding and secondary sieving to obtain a material with the particle size of less than 0.175 mm;
b: mixing the material obtained in the step a with water, then introducing sulfur dioxide gas under the stirring condition until the pH value is 4-7, and then filtering to obtain low-calcium vanadium-containing slag and a calcium-rich solution;
c: b, roasting the low-calcium vanadium-containing slag obtained in the step a to obtain a clinker, crushing the clinker, and then performing acid leaching to obtain a vanadium-containing solution;
d: and c, heating the calcium-rich solution obtained in the step b to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step b for use.
In the method, the vanadium-containing high-calcium high-phosphorus slag can be steel slag generated in the dephosphorization process of steel making of vanadium-containing molten iron.
Preferably, in the step a, the content of vanadium pentoxide in the vanadium-containing high-calcium high-phosphorus slag is more than 1 wt%, and the content of calcium oxide in the vanadium-containing high-calcium high-phosphorus slag is more than 20 wt%. Further preferably, the content of vanadium pentoxide in the vanadium-containing high-calcium high-phosphorus slag is 1-5 wt%, and the content of calcium oxide is more than 25-50 wt%.
Preferably, in step a, the wet milling is carried out in a wet ball mill.
In the method, in the step a, the volume ratio of water to the material during wet grinding can be (0.1-0.8): 1.
Preferably, in step a, the second screening has a mesh size of 120 meshes.
In the method, in the step b, the liquid-solid ratio of water to the material can be 5-10 mL/g. Specifically, for example, the concentration may be 5mL/g, 6mL/g, 7mL/g, 8mL/g, 9mL/g or 10 mL/g.
In the method of the present invention, in step b, there is no particular limitation on the source of the sulfur dioxide gas, and it may be a conventional choice in the art. In a preferred embodiment, the sulphur dioxide is otherwise technical grade sulphur dioxide or high concentration concentrated sulphur dioxide from flue gas.
In the method, in the step b, the stirring speed can be 100-300 r/min. Specifically, for example, the concentration may be 100r/min, 120r/min, 140r/min, 160r/min, 180r/min, 200r/min, 220r/min, 240r/min, 260r/min, 280r/min or 300 r/min.
Preferably, in step c, the roasting conditions include: the roasting temperature is 800-1000 ℃, and the roasting time is 30-180 min. Specifically, the roasting temperature can be 800 ℃, 810 ℃, 820 ℃, 850 ℃, 880 ℃, 900 ℃, 910 ℃, 920 ℃, 930 ℃, 940 ℃, 950 ℃, 960 ℃, 970 ℃, 980 ℃, 990 ℃ or 1000 ℃; the roasting time can be 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180 min.
In the method of the present invention, there is no particular requirement for the selection of the equipment used for calcination, and it may be a routine choice in the art. In a specific embodiment, the firing is performed in a muffle furnace.
Preferably, in step c, the temperature of the material taken out after the roasting is more than or equal to 650 ℃.
Preferably, in step c, the clinker is crushed to a particle size of less than 120 mesh.
In the method of the present invention, in step c, the specific process of acid leaching includes: mixing water and clinker according to a liquid-solid ratio of 0.5-5 mL/g, adjusting the pH value to 0.5-3, and leaching for 30-240 min. Specifically, the liquid-solid ratio of the water to the clinker can be 0.5mL/g, 1mL/g, 1.5mL/g, 2mL/g, 2.5mL/g, 3mL/g, 3.5mL/g, 4mL/g, 4.5mL/g or 5 mL/g; the leaching time can be 30min, 50min, 60min, 75min, 90min, 120min, 150min, 180min, 210min or 240 min.
In the method of the present invention, in step c, the vanadium-containing solution obtained can be used for preparing ammonium polyvanadate.
Preferably, the acid is immersed and stirred at a stirring speed of 100 to 300 r/min.
In the method of the present invention, in the step d, the heating temperature is 60 ℃ to 100 ℃. Preferably, the heating temperature is 70-90 ℃.
In the method of the present invention, in step d, the calcium-rich solution is heated to obtain calcium sulfite, and the calcium sulfite can be continuously heated to obtain a part of sulfur dioxide, and can also be directly sold as a product.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
Example 1
a: 10kg of blocky vanadium-containing high-calcium high-phosphorus slag (the main chemical components are shown in table 1) is subjected to primary crushing and primary sieving to obtain a material with the particle size of less than 5mm and an oversize product MFe of 1.25kg, then 4.38kg of water is added, wet grinding is carried out for 30min, then the material passes through a 120-mesh sieve, and drying is carried out to obtain an oversize product 0.32kgMFe, so as to obtain 8.43kg of the material with the particle size of less than 0.175 mm;
b: mixing 500g of the material obtained in the step a with 5000mL of water, then introducing sulfur dioxide gas under the stirring condition until the pH value is 6-7, and then filtering to obtain 333.19g of low-calcium vanadium-containing slag (V)2O54.02 wt%, CaO 5.87 wt%) and a calcium rich solution (calcium hydrogen sulfite solution);
c: b, roasting the low-calcium vanadium-containing slag (200g) obtained in the step b in a muffle furnace (roasting temperature is 850 ℃, roasting time is 2 hours), taking out at 650 ℃ to obtain clinker, crushing the clinker to be below 120 meshes, mixing 100g of clinker with 200mL of water, adding sulfuric acid to adjust the pH value to be 0.5, leaching for 30min under the condition of continuously stirring at 50 ℃ (stirring speed is 200r/min) to obtain 185mL of vanadium-containing leachate, wherein V is2O518.09g/L and the leaching rate is 90 percent;
d: and (c) heating the calcium-rich solution obtained in the step (b) (the heating temperature is 70 ℃, and the heating time is kept for 120min) to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step (b) for use.
The acid leaching rate in this example was 90%, and V was found in the resulting leachate2O5Is 18.09g/L, and the sulfur dioxide gas in the whole process can be recycled.
Example 2
a: 10kg of blocky vanadium-containing high-calcium high-phosphorus slag (the main chemical components are shown in table 1) is subjected to primary crushing and primary sieving to obtain a material with the particle size of less than 5mm and an oversize product MFe1.24kg, then 4.35kg of water is added, wet grinding is carried out for 30min, then the material passes through a 120-mesh sieve, and drying is carried out to obtain an oversize product 0.32kgMFe, so as to obtain 8.44kg of the material with the particle size of less than 0.175 mm;
b: mixing 500g of the material obtained in the step a with 4000mL of water, then introducing sulfur dioxide gas under the stirring condition until the pH value is 5-6, and then filtering to obtain 323.38g of low-calcium vanadium-containing slag (V)2O54.14 wt%, CaO 3.93 wt%) and a calcium rich solution (calcium hydrogen sulfite solution);
c: b, roasting the low-calcium vanadium-containing slag (200g) obtained in the step a in a muffle furnace (roasting temperature is 1000 ℃, roasting time is 2 hours), taking out at 650 ℃ to obtain clinker, crushing the clinker to be below 120 meshes, mixing 100g of clinker with 200mL of water, adding sulfuric acid to adjust the pH value to be 1.7, leaching for 120min under the condition of continuously stirring at 50 ℃ (stirring speed is 150r/min) to obtain 180mL of vanadium-containing leachate, wherein V is2O519.66g/L and the leaching rate is 95 percent;
d: and (c) heating the calcium-rich solution obtained in the step (b) (the heating temperature is 90 ℃, and the temperature is kept for 60min) to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step (b) for use.
In this example, the acid leaching rate was 95%, and V was contained in the resulting leachate2O5Is 19.66g/L, and the sulfur dioxide gas in the whole process can be recycled.
Example 3
a: carrying out primary crushing and primary sieving on 10kg of blocky vanadium-containing high-calcium high-phosphorus slag (the main chemical components are shown in table 1) to obtain a material with the particle size of less than 5mm and an oversize product MFe1.23kg, then adding 4.36kg of water, carrying out wet grinding for 30min, then sieving by a 120-mesh sieve, and drying to obtain an oversize product 0.33kgMFe to obtain a material with the particle size of less than 0.175mm 8.42 kg;
b: mixing 500g of the material obtained in the step a with 4000mL of water, and then stirringThen, sulfur dioxide gas is introduced until the pH value is 6-7, and then, the mixture is filtered to obtain 343.0g of low-calcium vanadium-containing slag (V)2O53.91 wt%, CaO 7.85 wt%) and a calcium rich solution (calcium hydrogen sulfite solution);
c: b, roasting the low-calcium vanadium-containing slag (200g) obtained in the step a in a muffle furnace (roasting temperature is 1000 ℃, roasting time is 2 hours), taking out at 650 ℃ to obtain clinker, crushing the clinker to be below 120 meshes, mixing 100g of clinker with 200mL of water, adding sulfuric acid to adjust the pH value to be 2.0, leaching for 120min under the condition of continuously stirring at 50 ℃ (stirring speed is 250r/min) to obtain 180mL of vanadium-containing leachate, wherein V is2O515.64g/L and the leaching rate is 95 percent;
d: and (c) heating the calcium-rich solution obtained in the step (b) (the heating temperature is 100 ℃, and the heating time is kept for 40min) to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step (b) for use.
In this example, the acid leaching rate was 95%, and V was contained in the resulting leachate2O5Is 15.64g/L, and the sulfur dioxide gas in the whole process can be recycled.
Comparative example 1
The procedure is as described in example 1, except that the pretreatment stage of step a is not carried out and steps b-d are carried out directly.
The acid leaching rate of the comparative example is 50%, and V in the obtained leaching solution2O5It was 8.23 g/L.
Comparative example 2
The process is carried out as described in example 1, except that in step b, sulfur dioxide is passed to a pH of 8.5.
The acid leaching rate of the comparative example is 70%, and V in the obtained leaching solution2O5The concentration was 11.52 g/L.
TABLE 1 main chemical composition of vanadium-containing high calcium high phosphorus slag (% by weight)
V2O5 | CaO | FeO | MFe | TFe | SiO2 | TiO2 | Al2O3 | P2O5 | MgO |
2.68 | 39.25 | 12.54 | 16.25 | 25.95 | 12.8 | 1.03 | 3.25 | 3.37 | 8.69 |
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag is characterized by comprising the following steps:
a: carrying out primary crushing and primary sieving on the vanadium-containing high-calcium high-phosphorus slag to obtain a material with the particle size of less than 5mm, and then carrying out wet grinding and secondary sieving to obtain a material with the particle size of less than 0.175 mm;
b: mixing the material obtained in the step a with water, then introducing sulfur dioxide gas under the stirring condition until the pH value is 4-7, and then filtering to obtain low-calcium vanadium-containing slag and a calcium-rich solution;
c: b, roasting the low-calcium vanadium-containing slag obtained in the step a to obtain a clinker, crushing the clinker, and then performing acid leaching to obtain a vanadium-containing solution;
d: and c, heating the calcium-rich solution obtained in the step b to obtain sulfur dioxide gas, and then returning the obtained sulfur dioxide gas to the step b for use.
2. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein in step a, the content of vanadium pentoxide and the content of calcium oxide in the vanadium-containing high-calcium high-phosphorus slag are respectively greater than 1% and 20% by weight.
3. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1 or 2, wherein in step a, the wet grinding is carried out in a wet ball mill.
4. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 3, wherein in the step a, the volume ratio of water to the material during wet grinding is (0.1-0.8): 1.
5. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein in the step b, the liquid-solid ratio of water to the material is 5-10 mL/g.
6. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein in the step b, the stirring speed is 100-300 r/min.
7. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein in the step c, the roasting conditions comprise: the roasting temperature is 800-1000 ℃, and the roasting time is 30-180 min.
8. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein in step c, the slag is crushed until the particle size of the clinker is less than 120 meshes.
9. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1 or 8, wherein in the step c, the specific process of acid leaching comprises the following steps: mixing water and clinker according to a liquid-solid ratio of 0.5-5 mL/g, adjusting the pH value to 0.5-3, and leaching for 30-240 min.
10. The method for extracting vanadium from vanadium-containing high-calcium high-phosphorus slag according to claim 1, wherein the heating temperature in step d is 60 ℃ to 100 ℃.
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113774237A (en) * | 2021-09-15 | 2021-12-10 | 中冶赛迪工程技术股份有限公司 | Method for preparing vanadium-rich liquid by using vanadium-rich slag |
CN115323199A (en) * | 2021-11-12 | 2022-11-11 | 虔东稀土集团股份有限公司 | Method for recovering rare earth elements |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES240054A1 (en) * | 1958-02-11 | 1958-10-16 | Yehuda Arieh Gruenstein | A procedure for the concentration of mineral phosphate (Machine-translation by Google Translate, not legally binding) |
US4118458A (en) * | 1972-05-12 | 1978-10-03 | Robinson Murry C | Separating magnesium and calcium from mineral mixtures containing zinc sulphides |
CN101899582A (en) * | 2010-07-30 | 2010-12-01 | 四川省川威集团有限公司 | Method for extracting vanadium pentoxide from vanadium slag |
CN103014321A (en) * | 2012-12-26 | 2013-04-03 | 攀枝花钢城卓越钒钛有限公司 | Raw material pretreatment process for extracting vanadium from vanadium slag |
CN109136534A (en) * | 2018-08-06 | 2019-01-04 | 陕西福盛钒业科技有限公司 | The method of powder containing navajoite and the baking mixed vanadium extraction of v-bearing steel slag |
-
2020
- 2020-10-29 CN CN202011186980.0A patent/CN112239808B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES240054A1 (en) * | 1958-02-11 | 1958-10-16 | Yehuda Arieh Gruenstein | A procedure for the concentration of mineral phosphate (Machine-translation by Google Translate, not legally binding) |
US4118458A (en) * | 1972-05-12 | 1978-10-03 | Robinson Murry C | Separating magnesium and calcium from mineral mixtures containing zinc sulphides |
CN101899582A (en) * | 2010-07-30 | 2010-12-01 | 四川省川威集团有限公司 | Method for extracting vanadium pentoxide from vanadium slag |
CN103014321A (en) * | 2012-12-26 | 2013-04-03 | 攀枝花钢城卓越钒钛有限公司 | Raw material pretreatment process for extracting vanadium from vanadium slag |
CN109136534A (en) * | 2018-08-06 | 2019-01-04 | 陕西福盛钒业科技有限公司 | The method of powder containing navajoite and the baking mixed vanadium extraction of v-bearing steel slag |
Non-Patent Citations (1)
Title |
---|
叶国华等: "含钒钢渣的选矿预处理及其对后续浸出的影响", 《中国有色金属学报》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113774237A (en) * | 2021-09-15 | 2021-12-10 | 中冶赛迪工程技术股份有限公司 | Method for preparing vanadium-rich liquid by using vanadium-rich slag |
CN115323199A (en) * | 2021-11-12 | 2022-11-11 | 虔东稀土集团股份有限公司 | Method for recovering rare earth elements |
CN115323199B (en) * | 2021-11-12 | 2023-09-29 | 虔东稀土集团股份有限公司 | Rare earth element recovery method |
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