CN110079643A - Using the method for lime treatment vanadium-bearing hot metal vanadium extraction - Google Patents
Using the method for lime treatment vanadium-bearing hot metal vanadium extraction Download PDFInfo
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- CN110079643A CN110079643A CN201910409592.5A CN201910409592A CN110079643A CN 110079643 A CN110079643 A CN 110079643A CN 201910409592 A CN201910409592 A CN 201910409592A CN 110079643 A CN110079643 A CN 110079643A
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- vanadium
- blowing
- oxygen
- hot metal
- slag
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
- C21C5/28—Manufacture of steel in the converter
- C21C5/30—Regulating or controlling the blowing
- C21C5/35—Blowing from above and through the bath
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
- C21C5/28—Manufacture of steel in the converter
- C21C5/36—Processes yielding slags of special composition
-
- 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
-
- 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
-
- 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
-
- 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 belongs to Ferrous Metallurgy and vanadium titanium chemical technology fields, and in particular to using the method for lime treatment vanadium-bearing hot metal vanadium extraction.That the technical problem to be solved by the present invention is to the oxygenation efficiency of vanadium slag production process vanadium is low, Vanadium in Vanadium Residue leaching rate is low.The invention discloses the methods using the vanadium extraction of lime treatment vanadium-bearing hot metal.Step are as follows: molten iron is blended into converter, addition coolant, lime carry out phase blowing oxidation, obtain vanadium slag and half steel, half steel is poured out, and vanadium slag is stayed in converter, and vanadium slag carries out the second stage of blowing oxidation in converter, obtain calcic vanadium slag after finishing blowing.The present invention can reduce operation quantity of the molten iron production containing vanadium leachate, and the oxygenation efficiency and leaching rate, reduction Process Energy consumption, the utilization and vanadium extraction production cost for being conducive to resource that can improve vanadium reduce.
Description
Technical field
The invention belongs to Ferrous Metallurgy and vanadium titanium chemical technology fields, and in particular to use the vanadium extraction of lime treatment vanadium-bearing hot metal
Method.
Background technique
Vanadium (V) is a kind of transiting group metal elements, and chemical property is more stable at normal temperature, relatively active under high temperature.Vanadium because
It is widely used in the fields such as steel, chemical industry, aviation with excellent intensity, hardness and antifatigue effect.About 84%
Vanadium is dissolved into formation VC and VN in steel as alloying element for steel, refines crystal grain, inhibits the development of bainite and pearlite
Increase martensite intensity, to improve the hardness of steel, intensity, toughness and wear resistance.Vanadium for non-ferrous alloy mainly with
V-Al system alloy is the structural material of representative, such as excellent high temperature Aircraft Structure Materials Ti-6Al-4V, Ti-8Al-1V-Mo and
The alloys such as Ti-6Al-6V-2Sn.Vanadium product for chemical field mainly has V2O5、NH4VO3、V2O3、VOCl3And VCl4Deng use
It is used as the electrode material of catalyst, colorant, high capacity cell.
Vanadium resource disperses very much in distributed in nature, main association in sulphur navajoite, lead navajoite, vanadium marble, potassium vanadate uranium ore with
And in the mineral such as vanadium titano-magnetite.Because of vanadium raw materials type, mineral characteristic and wherein content of vanadium differs greatly, and mentions from vanadium-containing material
It takes technique and the method for vanadium also varied, mainly there is pyrometallurgical smelting, wet-leaching and the wet method combined extraction process of pyrogenic process-.Fire
Method is smelted usually using vanadium titano-magnetite as primary raw material, obtains vanadium-bearing hot metal by blast furnace or other ironmaking processes, then in converter
In be blown into oxygen and make the vanadium oxidization enrichment in metal into slag, obtained vanadium slag or v-bearing steel slag is by roasting-leaching or directly
The mode of leaching carries out subsequent extracted.Wet-leaching is relatively specific for the wastes such as dead catalyst, flying dust and petroleum lime-ash, also has
It is applied in bone coal on a small quantity, the raw ores such as vanadium titano-magnetite, but since wherein vanadium all mainly exists in the form of the trivalent vanadium of indissoluble, directly
It is lower compared with pyrometallurgical smelting and the wet method combined extraction process rate of recovery of pyrogenic process-to connect leaching.Pyrogenic process-is wet method combined to be extracted it is generally necessary to will
Vanadium roasts under oxidizing atmosphere is converted to high price compound in favor of leaching, and the wet method combined extraction process of traditional pyrogenic process-has sodium
Salt roasting-water logging, blank roasting-acidleach (alkali leaching), few salt roasting-circulating leaching and calcium salt roasting-acidleach (alkali leaching) etc..
CN102086487A discloses a kind of vanadium slag treatment method of energy-saving and emission-reduction, comprising the following steps: firstly, will be with iron
1200 DEG C or more of high-temperature liquid state vanadium slag after water separation is placed in slag ladle；Then, sodium is added into slag ladle according to v slag grade
Then compound is supplied oxygen with water cooling supersonic speed or subsonic speed oxygen rifle into slag ladle, cause strong oxidizing property atmosphere, while can play and stir
The effect of mixing promotes to quickly generate water-soluble sodium vanadate in vanadium slag, is fully oxidized to most to guarantee that oxygen-supplying amount is greater than each component in slag
Oxygen amount needed for high oxide, the V that need to be generated using the FeO/TFe in slag as the index for examining degree of oxidation, in vanadium slag2O5
The water-soluble sodium vanadate of generation is reacted with the sodium compound of addition, finally, the obtained bits containing water-soluble sodium vanadate, processing
Obtain V2O5, wherein the dissolution rate of vanadium is 90~94%.But the above method joined a large amount of sodium compound: in sodium compound
Na2O and V2O5Molar ratio be 1~10, Na in embodiment2O and V2O5Molar ratio be 2.3~3, this is because sodium compound
At high temperature be easy decomposition gasification, at high temperature be added sodium compound will lead to sodium compound loss it is larger；Above-mentioned side simultaneously
The vanadium slag that the raw material of method can only use vanadium extraction by converter blowing to produce, production line is long, at high cost.
Summary of the invention
Low, Vanadium in Vanadium Residue leaching rate that the technical problem to be solved by the present invention is to the oxygenation efficiency of vanadium slag production process vanadium
It is low.
The technical solution used to solve the technical problems of the present invention is that providing using lime treatment vanadium-bearing hot metal vanadium extraction
Method.Include the following steps: for molten iron to be blended into converter, be added coolant, lime carry out a phase blowing oxidation, obtain vanadium slag and
Half steel pours out half steel, and vanadium slag is stayed in converter, and vanadium slag carries out second phase blowing oxidation in converter, obtains calcic after finishing blowing
Vanadium slag.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the additional amount of the coolant is 15~
35kg/tFe；The coolant is ferriferous oxide.
Further, the coolant is added in the preceding 3min that a phase blows oxidation beginning, and 2min after coolant is added
Interior addition lime.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, lime is added in the phase blowing oxidation
Amount is 3~4kg/tFe.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the phase blowing oxidation is same using top bottom
It blows, top blast carries out oxygen blast gas, bottom blowing nitrogen using oxygen rifle.
Further, rifle position is controlled using " high-low-high " mode when the oxygen gun blowing, i.e., oxygen blast rifle position is being blown
0.5~1.5min that refining starts is 1.7~2.0m, and blowing mid-term is 1.6~1.8m, and 1.0~1.5min before finishing blowing is
1.7~2.0m；Top blast oxygen supply intensity is 2.0~3.0m3/ (mintFe), oxygen blow duration are 5~6.5min, and oxygen pressure is
0.7~0.9MPa；Bottom blowing nitrogen flow is 0.1~0.5m3/(min·tFe)。
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the second phase blowing oxidation uses BOTTOM OXYGEN
Gas.
Further, the flow of the bottom blowing oxygen is 0.25~0.75m3/(min·tFe)；The time of bottom blowing oxygen is
2~3min.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, vanadium slag after the second phase blowing oxidation
Middle CaO/V2O5Mass ratio is controlled 0.55~0.65.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, calcic is being prepared using the above method
It is isolated to contain vanadium leachate by calcic vanadium slag through cooling, broken, magnetic separation, ball milling, acidleach after vanadium slag.
The beneficial effects of the present invention are:
The method of the present invention generates calcic vanadium slag using the blowing oxidation of two phases, and phase blowing is added lime and uses top blast oxygen,
Bottom blowing nitrogen, second phase blowing carry out bottom blowing oxygen to vanadium slag in converter, and compared with prior art, the method for the present invention can reduce iron
Aquatic operation quantity of the production containing vanadium leachate, can improve the oxygenation efficiency and leaching rate of vanadium, can efficiently use the self-heating of vanadium slag, make
V in vanadium slag2O3It is oxidized to V2O5, roasting bring heat consumption is carried out again after reducing vanadium slag cooling, is conducive to the utilization of resource
And vanadium extraction production cost reduces.
Specific embodiment
Specifically, the invention discloses the methods using the vanadium extraction of lime treatment vanadium-bearing hot metal.Include the following steps: molten iron
Be blended into converter, be added coolant, lime carry out a phase blowing oxidation, obtain vanadium slag and half steel, half steel poured out, vanadium slag stay in
In converter, vanadium slag carries out second phase blowing oxidation in converter, obtains calcic vanadium slag after finishing blowing.
For the present invention using two phases blowing oxidation production calcic vanadium slag, phase blowing oxidation is by the vanadium oxidation separation in molten iron
Vanadium slag is formed, second phase blowing oxidation is the barium oxide aoxidized in vanadium slag under the state existing for no molten iron, by the V in vanadium slag2O3
It is oxidized to V2O5, and promote V2O5Water-soluble calcium vanadate is generated with CaO.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the additional amount of the coolant is 15~
35kg/tFe；The coolant is ferriferous oxide.The purpose that coolant is added and is aoxidized in molten iron to control molten iron temperature
Vanadium formed vanadium slag.
Further, the coolant is added in the preceding 3min that a phase blows oxidation beginning, and 2min after coolant is added
Interior addition lime.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, lime is added in the phase blowing oxidation
Amount is 3~4kg/tFe.Lime is added into molten iron in phase blowing oxidation process by the present invention, can not only improve slag state, moreover it is possible to
Be conducive to the formation of subsequent calcium vanadate, and the fusing point reduction of vanadium slag after lime is added, slag iron separation effect is good, iron-content in slag
Few, the process oxygen utilization rate for aoxidizing vanadium slag is higher.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the phase blowing oxidation is same using top bottom
It blows, top blast carries out oxygen blast gas, bottom blowing nitrogen using oxygen rifle.
Further, rifle position is controlled using " high-low-high " mode when the oxygen gun blowing, i.e., oxygen blast rifle position is being blown
0.5~1.5min that refining starts is 1.7~2.0m, and blowing mid-term is 1.6~1.8m, and 1.0~1.5min before finishing blowing is
1.7~2.0m；Top blast oxygen supply intensity is 2.0~3.0m3/ (mintFe), oxygen blow duration are 5~6.5min, and oxygen pressure is
0.7~0.9MPa；Bottom blowing nitrogen flow is 0.1~0.5m3/(min·tFe).The present invention utilizes high pressure oxygen pair in converter
Vanadium slag blows, and mixing effect greatly improves so that in slag CaO mix it is more uniform, be more advantageous to and aoxidized from molten iron
Vanadium obtains vanadium slag.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, the second phase blowing oxidation uses BOTTOM OXYGEN
Gas.It in the present invention, is in order to by the V in vanadium slag using second phase blowing oxidation2O3It is oxidized to V2O5, and promote V2O5It is raw with CaO
At water-soluble calcium vanadate.After half steel is poured out, vanadium slag temperature at this time is relatively high and CaO is uniformly distributed in slag, at this time
Second phase blowing oxidation is carried out, the more conducively production of calcium vanadate further increases the leaching rate for realizing vanadium.
Further, the flow of the bottom blowing oxygen is 0.25~0.75m3/(min·tFe)；The time of bottom blowing oxygen is
2~3min.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, vanadium slag after the second phase blowing oxidation
Middle CaO/V2O5Mass ratio is controlled 0.55~0.65.Inventor is had found by a large number of experiments, will be contained after second phase blowing oxidation
CaO/V in calcium vanadium slag2O5Mass ratio is controlled 0.55~0.65, the ratio highest of calcium vanadate is generated, most beneficial for Vanadium in Vanadium Residue
It extracts.
Wherein, in the above-mentioned method using lime treatment vanadium-bearing hot metal vanadium extraction, calcic is being prepared using the above method
It is isolated to contain vanadium leachate by calcic vanadium slag through cooling, broken, magnetic separation, ball milling, acidleach after vanadium slag.
Further, after second phase blowing oxidation, cooling, control cooling time are covered after vanadium slag is poured into vanadium slag tank
By vanadium slag, at 120 mesh fine powders, fine powder is mixed with water by weight 1:2 for broken, magnetic separation, ball milling after 36~72h, cooling
Afterwards, it is leached using the sulfuric acid solution of 1:1, pH value controls between 2.8~3.2, and leaching process is using mechanical stirring (stirring
300~400r/min of paddle revolving speed) and 50 ± 2 DEG C of temperature of holding is heated, it is filtered by vacuum after 1h, gained filtrate is to leach containing vanadium
Liquid.
In the present invention, initial molten iron temperature is generally 1190~1360 DEG C, and converting process temperature is no more than 1400 DEG C.
The present invention will further be elaborated by specific embodiment below.
Embodiment 1
Molten iron is blended into converter, oxygen blast oxidation is carried out using oxygen rifle, addition 35kg/tFe is cold in 3min before oxygen blast starts
But the interior addition 4kg/tFe lime of 2min after coolant is added in agent.It is blown using top blast oxygen bottom blowing nitrogen, rifle when oxygen gun blowing
Position is controlled using " high-low-high " mode, i.e., oxygen blast rifle position is 1.7m in the 0.5min that blowing starts, and blowing mid-term is
1.6m, the 1.0min before finishing blowing are 1.7m.The control of top blast oxygen supply intensity is 3.0m3/ (mintFe), oxygen blow duration control
In 5.5min, oxygen pressure 0.9MPa, bottom blowing nitrogen flow is controlled in 0.4m3/(min·tFe)。
Half steel is poured into half cylinder of steel after finishing blowing, vanadium slag is stayed in converter, after converter is returned to blowing position, by bottom blowing
Gas is switched to oxygen, and bottom blowing oxygen flow is 0.75m3/ (mintFe), gassing time 3min.
After vanadium slag finishing blowing, cooling is covered after vanadium slag is poured into vanadium slag tank, control cooling time is in 36h, cooling knot
By vanadium slag, broken, magnetic separation, ball milling are molten using the sulfuric acid of 1:1 after fine powder is mixed with water by weight 1:2 at 120 mesh fine powders after beam
Liquid is leached, and pH value controls between 2.8~3.2, and leaching process uses mechanical stirring (300~400r/ of rotating speed of agitator
Min) and 50 ± 2 DEG C of temperature of holding is heated, is filtered by vacuum after 1h, gained filtrate is containing vanadium leachate.The oxygen of whole process vanadium
Rate is 91.09%, V leaching rate 94.69%.
Embodiment 2
Molten iron is blended into converter, oxygen blast oxidation is carried out using oxygen rifle, addition 29kg/tFe is cold in 3min before oxygen blast starts
But the interior addition 4kg/tFe lime of 2min after coolant is added in agent.It is blown using top blast oxygen bottom blowing nitrogen, rifle when oxygen gun blowing
Position is controlled using " high-low-high " mode, i.e., oxygen blast rifle position is 1.7m in the 1.5min that blowing starts, and blowing mid-term is
1.65m, the 1.0min before finishing blowing are 1.7m.The control of top blast oxygen supply intensity is 2.2m3/ (mintFe), oxygen blow duration control
System is controlled in 6min, oxygen pressure 0.75MPa, bottom blowing nitrogen flow in 0.25m3/(min·tFe)。
Half steel is poured into half cylinder of steel after finishing blowing, vanadium slag is stayed in converter, after converter is returned to blowing position, by bottom blowing
Gas is switched to oxygen, and bottom blowing oxygen flow is 0.55m3/ (mintFe), gassing time 3min.
After vanadium slag finishing blowing, cooling is covered after vanadium slag is poured into vanadium slag tank, control cooling time is in 51h, cooling knot
By vanadium slag, broken, magnetic separation, ball milling are molten using the sulfuric acid of 1:1 after fine powder is mixed with water by weight 1:2 at 120 mesh fine powders after beam
Liquid is leached, and pH value controls between 2.8~3.2, and leaching process uses mechanical stirring (300~400r/ of rotating speed of agitator
Min) and 50 ± 2 DEG C of temperature of holding is heated, is filtered by vacuum after 1h, gained filtrate is containing vanadium leachate.The oxygen of whole process vanadium
Rate is 90.76%, V leaching rate 94.46%.
Claims (10)
1. using the method for lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that include the following steps: for molten iron to be blended into converter,
Coolant is added, lime carries out phase blowing oxidation, obtain vanadium slag and half steel, half steel poured out, vanadium slag stays the converter in converter
Interior vanadium slag carries out second phase blowing oxidation, obtains calcic vanadium slag after finishing blowing.
2. the method according to claim 1 using lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that: the coolant
Additional amount be 15~35kg/tFe；The coolant is ferriferous oxide.
3. the method according to claim 1 or 2 using lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that: described cold
But agent is added in the preceding 3min that a phase blows oxidation beginning, and lime is added in 2min after addition coolant.
4. described in any item methods using lime treatment vanadium-bearing hot metal vanadium extraction according to claim 1~3, it is characterised in that:
The amount that lime is added in the one phase blowing oxidation is 3~4kg/tFe.
5. the method according to any one of claims 1 to 4 using lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that:
Using top bottom with blowing, top blast carries out oxygen blast gas, bottom blowing nitrogen using oxygen rifle for the one phase blowing oxidation.
6. the method according to claim 5 using lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that: the oxygen rifle is blown
Rifle position is controlled using " high-low-high " mode when oxygen, i.e., oxygen blast rifle position 0.5~1.5min that blowing starts be 1.7~
2.0m, blowing mid-term are 1.6~1.8m, and 1.0~1.5min before finishing blowing is 1.7~2.0m；Top blast oxygen supply intensity is 2.0
~3.0m3/ (mintFe), oxygen blow duration are 5~6.5min, and oxygen pressure is 0.7~0.9MPa；Bottom blowing nitrogen flow is
0.1~0.5m3/(min·tFe)。
7. described in any item methods using lime treatment vanadium-bearing hot metal vanadium extraction according to claim 1~6, it is characterised in that:
The second phase blowing oxidation uses bottom blowing oxygen.
8. the method according to claim 7 using lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that: the BOTTOM OXYGEN
The flow of gas is 0.25~0.75m3/(min·tFe)；The time of bottom blowing oxygen is 2~3min.
9. described in any item methods using lime treatment vanadium-bearing hot metal vanadium extraction according to claim 1~8, it is characterised in that:
CaO/V in vanadium slag after the second phase blowing oxidation2O5Mass ratio is controlled 0.55~0.65.
10. using the method for lime treatment vanadium-bearing hot metal vanadium extraction, it is characterised in that: on the basis of any one of claim 1~9
On, it is isolated to contain vanadium leachate by calcic vanadium slag through cooling, broken, magnetic separation, ball milling, acidleach.
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| CN201910409592.5A CN110079643A (en) | 2019-05-16 | 2019-05-16 | Using the method for lime treatment vanadium-bearing hot metal vanadium extraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020228750A1 (en) * | 2019-05-16 | 2020-11-19 | 成都先进金属材料产业技术研究院有限公司 | Method for producing calcium-containing vanadium slag by adding lime to converter molten iron and leaching method therefor |
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2019
- 2019-05-16 CN CN201910409592.5A patent/CN110079643A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020228750A1 (en) * | 2019-05-16 | 2020-11-19 | 成都先进金属材料产业技术研究院有限公司 | Method for producing calcium-containing vanadium slag by adding lime to converter molten iron and leaching method therefor |
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Application publication date: 20190802 |