CN112359231B - Method for extracting vanadium by directly calcifying hot vanadium slag - Google Patents
Method for extracting vanadium by directly calcifying hot vanadium slag Download PDFInfo
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- CN112359231B CN112359231B CN202011164298.1A CN202011164298A CN112359231B CN 112359231 B CN112359231 B CN 112359231B CN 202011164298 A CN202011164298 A CN 202011164298A CN 112359231 B CN112359231 B CN 112359231B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—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
- 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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- 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 the technical field of vanadium metallurgy, and particularly relates to a method for extracting vanadium by directly calcifying hot vanadium slag. The invention aims to solve the technical problem of providing a method for directly calcifying and extracting vanadium from hot vanadium slag, which has high vanadium recovery rate and low vanadium per ton cost. The method comprises the following steps: a. adding the hot vanadium slag obtained by extracting vanadium from the converter into a smelting furnace, and adding a calcium additive into the hot vanadium slag in a blowing mode by taking at least one of oxygen or air as a carrier to obtain calcium-containing hot vanadium slag; b. carrying out top-blowing oxidation on the calcium-containing hot vanadium slag to obtain vanadium slag clinker; c. crushing vanadium slag clinker, grinding, leaching, removing impurities, precipitating and calcining to obtain V 2 O 5 . The method improves the recovery rate of vanadium, has the advantages of low fuel consumption and low cost per ton of vanadium, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of vanadium metallurgy, and particularly relates to a method for extracting vanadium by directly calcifying hot vanadium slag.
Background
Vanadium-titanium magnetite is subjected to blast furnace ironmaking and vanadium extraction in a converter to obtain vanadium slag, wherein the vanadium slag is a main source of strategic rare metal vanadium. In the traditional process, vanadium slag is cooled and crushed, then iron particles are magnetically separated, the iron particles are ground and pelletized and enter a rotary kiln or a multi-hearth furnace for roasting, roasted clinker is used for producing vanadium oxide by a wet process, and the main processes for extracting vanadium from the vanadium slag at home and abroad comprise the following steps:
(1) Vanadium slag sodium salt roasting-water leaching-ammonium salt vanadium precipitation process
(2) Vanadium slag calcium salt roasting-acid leaching-hydrolysis vanadium precipitation process
(3) Vanadium slag calcium salt roasting-acid leaching-ammonium salt vanadium precipitation process (vanadium oxide clean production process)
(4) Sub-molten salt method
(5) Blank roasting-alkaline leaching process.
At present, most vanadium production enterprises at home and abroad adopt the traditional sodium salt roasting-water leaching-ammonium salt vanadium precipitation process, a Russian Tura vanadium plant adopts a vanadium slag calcium salt roasting-acid leaching-hydrolysis vanadium precipitation process to extract vanadium from vanadium slag, a Panzhi steel Xichang vanadium product plant adopts a vanadium slag calcium salt roasting-acid leaching-ammonium salt vanadium precipitation process to extract vanadium from vanadium slag, and a sub-molten salt method and a blank roasting-alkali leaching process are still in research, development or pilot-scale test at present. In the five processes, the cooled vanadium slag is used as a raw material for vanadium extraction, and the vanadium extraction thermal-state vanadium slag (the temperature is higher than 1300 ℃) of the converter contains a large amount of physical heat, so that the vanadium extraction heat loss is carried out after cooling, and the subsequent roasting needs to consume fuel for reheating and has more processes, thereby causing high vanadium cost per ton.
Patent document CN109971910A discloses a method for extracting vanadium from molten iron by calcium treatment, which comprises the following steps: adding molten iron into a converter, adding a coolant and lime for primary blowing oxidation to obtain vanadium slag and semisteel, pouring out the semisteel, keeping the vanadium slag in the converter, adding the lime into the converter for secondary blowing oxidation of the vanadium slag, and obtaining calcium-containing vanadium slag after blowing.
Patent document CN109971911A discloses a production and oxidation leaching method of calcium-containing vanadium slag, which comprises the following steps: adding molten iron into a converter, adding a coolant, lime and CaF 2 Performing primary blowing oxidation to obtain vanadium slag and semisteel, pouring the semisteel out, keeping the vanadium slag in the converter, performing secondary blowing oxidation on the vanadium slag in the converter, and obtaining calcium-containing vanadium slag after blowing.
Patent document CN109971909A discloses a method for producing calcium-containing vanadium slag and oxidizing leaching thereof in a converter, which comprises the following steps: adding molten iron into a converter, adding a coolant and lime for primary blowing oxidation to obtain vanadium slag and semisteel, pouring out the semisteel, keeping the vanadium slag in the converter, adding the lime into the converter for secondary blowing oxidation of the vanadium slag, and obtaining calcium-containing vanadium slag after blowing.
In all of the three patent documents, calcium additives are added into a converter in the process of extracting vanadium from the converter, and oxygen is blown and oxidized in two devices to obtain calcium-containing vanadium slag, although the heat in molten vanadium slag is fully utilized, the following defects exist: 1) High-melting-point substance spinel is formed in the process of extracting vanadium from a converter, so that the viscosity of vanadium slag is increased, the fluidity is deteriorated, and the deterioration of mass transfer kinetic conditions can not cause the addition of lime or CaF 2 The calcium-containing substance is homogenized in the vanadium slag, so that V and Ca cannot be fully contacted, the reaction is not thorough, and the recovery rate of vanadium is low; 2) The converter has no external heat supplement, the heat release of the oxidation reaction is not enough to maintain the system temperature, and the viscosity of the system is further increased along with the reduction of the system temperature, so that oxygen is diffused and received in the vanadium slagAnd V (III) cannot be oxidized Into V (IV) and V (V), so that the calcium-containing vanadium slag cannot be dissolved out in the leaching process.
In order to overcome the defect of low heat utilization efficiency in the process caused by the existing vanadium extraction process from vanadium slag and the cracking of the vanadium extraction process of the front-end converter, a new method for directly calcifying and extracting vanadium from thermal vanadium slag needs to be researched.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for directly calcifying hot vanadium slag to extract vanadium, which has high vanadium recovery rate and low vanadium cost per ton.
The invention adopts the technical scheme to solve the technical problems and provides a method for directly calcifying hot vanadium slag to extract vanadium. The method comprises the following steps:
a. adding the hot vanadium slag obtained by extracting vanadium in the converter into a smelting furnace, and adding a calcareous additive into the hot vanadium slag in a blowing mode by taking at least one of oxygen or air as a carrier to obtain calcium-containing hot vanadium slag;
b. carrying out top-blowing oxidation on the calcium-containing hot vanadium slag to obtain vanadium slag clinker;
c. crushing vanadium slag clinker, grinding, leaching, removing impurities, precipitating and calcining to obtain V 2 O 5 。
In the method for extracting vanadium by directly calcifying the thermal vanadium slag, in the step a, the smelting furnace is a straight-tube furnace, and the diameter of the straight-tube furnace is 1.4-2.6 m.
Further, in the step a, the adding amount of the hot vanadium slag enables the thickness of the hot vanadium slag in the smelting furnace to be 0.7-1.1 m.
Further, in the step a, the temperature of the hot vanadium slag is controlled to be 1400-1600 ℃.
Further, in the step a, the adding amount of the calcareous additive is 120-320 kg/t vanadium slag.
Further, in step a, the calcareous additive is at least one of calcium oxide or calcium carbonate.
Further, in the step a, the pressure of the blown gas is 0.7-1.0 MPa; the depth of the spray gun used for blowing inserted into the slag is 0.3-0.6 m.
In the method for extracting vanadium by directly calcifying the hot vanadium slag, in the step b, the gas adopted by top blowing is at least one of oxygen or air.
Further, in the step b, the strength of the top-blown gas is 5 to 25m 3 Per min per ton of vanadium slag; the top blowing time is 15-20 min.
The invention has the beneficial effects that:
the invention takes hot vanadium slag of vanadium extraction in a converter as a raw material, adds a calcium additive into the hot vanadium slag in a blowing mode by taking air or oxygen as a carrier to directly calcify so as to convert vanadium into acid-soluble calcium vanadate, and then obtains a product V by leaching, impurity removal, precipitation and calcination 2 O 5 The method shortens the vanadium extraction flow, realizes the effective connection of two steps of vanadium extraction by the converter and vanadium slag vanadium extraction, improves the recovery rate of vanadium, has the advantages of low fuel consumption and low vanadium cost per ton, can reduce the vanadium cost per ton by 5200-9700 yuan, is an advanced clean vanadium extraction process, and has wide application prospect.
Detailed Description
Specifically, the invention provides a method for extracting vanadium by directly calcifying hot vanadium slag. The method comprises the following steps:
a. adding hot vanadium slag obtained by extracting vanadium in a converter into a straight cylinder furnace with the diameter of 1.4-2.6 m, enabling the thickness of the hot vanadium slag in the straight cylinder furnace to be 0.7-1.1 m, blowing a calcium additive of 120-320 kg/t vanadium slag into the hot vanadium slag through a powder blowing system by taking at least one of oxygen or air as a carrier, controlling the temperature of the hot vanadium slag to be 1400-1600 ℃ through electric heating, and controlling the pressure of the blown gas to be 0.7-1.0 MPa; the depth of the spray gun used for spraying and blowing inserted into the slag is 0.3-0.6 m, and calcium-containing hot vanadium slag is obtained;
b. the calcium-containing hot vanadium slag is subjected to top blowing oxidation through an air supply system, the top blowing gas is at least one of oxygen or air, and the strength of the top blowing gas is 5-25 m 3 Min per ton of vanadium slag, wherein the top blowing time is 15-20 min to obtain vanadium slag clinker;
c. crushing vanadium slag clinker, grinding, leaching, removing impurities and precipitatingCalcining to obtain V 2 O 5 。
In the step a, the calcareous additive is added into the hot vanadium slag in a blowing mode, so that the homogenization of the calcareous additive in the vanadium slag is ensured, the viscosity of a slag system is reduced by controlling the temperature of the hot vanadium slag, and the dynamic mass transfer condition is improved. The temperature of the vanadium slag and the fluidity of the slag are controlled while the heat in the slag is utilized, so that oxygen is quickly diffused in the vanadium slag to oxidize V (III) into V (V) and the V (V) is combined with a calcareous additive to form an acid-soluble calcium salt, thereby ensuring the high-efficiency extraction of vanadium.
In the step a, the adding amount of the thermal vanadium slag enables the thickness of the thermal vanadium slag in the straight-tube furnace to be 0.7-1.1 m, so that the calcium additive and oxygen are effectively contacted with the vanadium slag, and the oxidation and calcification of vanadium in the vanadium slag are realized.
In the step a, the calcareous additive is added into the hot vanadium slag in a blowing mode by taking at least one of oxygen or air as a carrier, so that the calcareous additive can be uniformly dispersed in the vanadium slag, the vanadium-containing mineral and the calcareous additive are effectively combined to react, and the oxygen or the air can promote the oxidation of low-valence vanadium.
The present invention will be further illustrated by the following specific examples.
Example 1
Adding hot vanadium slag obtained by extracting vanadium in a converter into a straight-tube furnace, wherein the diameter of the straight-tube furnace is 1.8m, controlling the addition amount of the vanadium slag to enable the thickness of the vanadium slag in the straight-tube furnace to be 0.9m, controlling the temperature of the hot vanadium slag to be 1480 ℃ through electric heating, adding calcium oxide powder into the hot vanadium slag through a powder injection system by taking oxygen as a carrier to obtain calcium-containing hot vanadium slag, wherein the injection gas pressure is 0.9MPa, the depth of a spray gun inserted into the slag is 0.4m, and the addition amount of the calcium oxide powder is 150 kg/ton of vanadium slag;
oxygen is blown to the calcium-containing hot vanadium slag through a gas supply system for oxidation, and the strength of top-blown gas is 14m 3 (min. Ton vanadium slag), the top blowing time is 18min, get vanadium slag clinker;
crushing vanadium slag clinker, grinding, leaching with sulfuric acid, removing impurities, precipitating, and calcining to obtain V 2 O 5 . The vanadium yield is 88 percent, and the cost of per ton of vanadium is reduced by 5800 yuan.
Example 2
Adding hot vanadium slag obtained by extracting vanadium in a converter into a straight-barrel furnace, wherein the diameter of the straight-barrel furnace is 2.5m, controlling the addition amount of the vanadium slag to ensure that the thickness of the vanadium slag in the straight-barrel furnace is 1.0m, controlling the temperature of the hot vanadium slag to 1530 ℃ through electric heating, adding calcium carbonate powder into the hot vanadium slag through a powder injection system by taking air as a carrier to obtain calcium-containing hot vanadium slag, wherein the pressure of injection gas is 0.8MPa, the depth of a spray gun inserted into the slag is 0.3m, and the addition amount of the calcium carbonate powder is 300 kg/ton of vanadium slag;
air is blown to the top of the calcium-containing hot vanadium slag through an air supply system for oxidation, and the strength of the top blown air is 21m 3 (min. Ton vanadium slag), the top blowing time is 20min, obtain vanadium slag clinker;
crushing vanadium slag clinker, grinding, leaching with sulfuric acid, removing impurities, precipitating, and calcining to obtain V 2 O 5 . The vanadium yield is 96 percent, and the cost of vanadium per ton is reduced by 8900 yuan.
Example 3
Adding hot vanadium slag obtained by extracting vanadium from a converter into a straight cylinder furnace, wherein the diameter of the straight cylinder furnace is 2.0m, controlling the addition amount of the vanadium slag to ensure that the thickness of the vanadium slag in the straight cylinder furnace is 0.7m, controlling the temperature of the hot vanadium slag to be 1520 ℃ through electric heating, adding calcium carbonate powder into the hot vanadium slag through a powder injection system by taking oxygen as a carrier to obtain calcium-containing hot vanadium slag, wherein the pressure of injection gas is 1.0MPa, the depth of a spray gun inserted into the slag is 0.5m, and the addition amount of the calcium carbonate powder is 210 kg/ton of vanadium slag;
oxygen is blown to the calcium-containing hot vanadium slag through a gas supply system for oxidation, and the strength of top-blown gas is 9m 3 (min. Ton vanadium slag), the top blowing time is 16min, and vanadium slag clinker is obtained;
crushing vanadium slag clinker, grinding, leaching with sulfuric acid, removing impurities, precipitating, and calcining to obtain V 2 O 5 . The vanadium yield is 92 percent, and the cost of vanadium per ton is reduced by 7200 yuan.
Claims (5)
1. The method for extracting vanadium by directly calcifying hot vanadium slag is characterized by comprising the following steps: the method comprises the following steps:
a. adding hot vanadium slag obtained by extracting vanadium in a converter into a smelting furnace, adding a calcareous additive into the hot vanadium slag in a blowing mode by taking at least one of oxygen or air as a carrier, and controlling the temperature of the hot vanadium slag to be 1400-1600 ℃ to obtain calcium-containing hot vanadium slag; wherein the smelting furnace is a straight-tube furnace with the diameter of 1.4-2.6 m, and the calcareous additive is at least one of calcium oxide or calcium carbonate;
b. carrying out top blowing oxidation on the calcium-containing hot vanadium slag to obtain vanadium slag clinker, wherein the gas adopted by top blowing is oxygen or air;
c. crushing vanadium slag clinker, grinding, leaching, removing impurities, precipitating and calcining to obtain V 2 O 5 。
2. The method for extracting vanadium by direct calcification of hot vanadium slag as claimed in claim 1, wherein: in the step a, the adding amount of the thermal vanadium slag enables the thickness of the thermal vanadium slag in the smelting furnace to be 0.7-1.1 m.
3. The method for extracting vanadium by direct calcification of hot vanadium slag as claimed in claim 1, wherein: in the step a, the adding amount of the calcareous additive is 120-320 kg/t vanadium slag.
4. The method for extracting vanadium by direct calcification of hot vanadium slag as claimed in claim 1, wherein: in the step a, the pressure of the injected gas is 0.7-1.0 MPa; the depth of the spray gun used for blowing inserted into the slag is 0.3-0.6 m.
5. The method for extracting vanadium by direct calcification of hot vanadium slag according to any one of claims 1 to 4, wherein: in the step b, the strength of the top-blown gas is 5-25 m 3 Per min per ton of vanadium slag; the time of top blowing is 15-20 min.
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| CN114293032A (en) * | 2021-11-22 | 2022-04-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Grading treatment method for sodium vanadium slag |
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