CN111440908B - Method for converting titanium component in titanium-containing blast furnace slag into ilmenite - Google Patents
Method for converting titanium component in titanium-containing blast furnace slag into ilmenite Download PDFInfo
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- CN111440908B CN111440908B CN202010438869.XA CN202010438869A CN111440908B CN 111440908 B CN111440908 B CN 111440908B CN 202010438869 A CN202010438869 A CN 202010438869A CN 111440908 B CN111440908 B CN 111440908B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B3/00—General features in the manufacture of pig-iron
- C21B3/04—Recovery of by-products, e.g. slag
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B11/00—Making pig-iron other than in blast furnaces
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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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
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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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry 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
- 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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- 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
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Abstract
The invention discloses a method for converting a titanium component in titanium-containing blast furnace slag into ilmenite, and belongs to the field of comprehensive utilization of metallurgical solid wastes. The method comprises the following specific steps: (1) uniformly mixing the titanium-containing blast furnace slag, iron oxide scale, silicon dioxide and coke, pressing into a wafer, and controlling the mass ratio and the pressing pressure of the titanium-containing blast furnace slag, the iron oxide scale, the silicon dioxide and the coke; (2) and putting the obtained material sheet into an alumina crucible, putting the alumina crucible into a high-temperature furnace, introducing argon to drive away air in a furnace cavity, heating, reacting at 1300-1450 ℃ for 240-420min, cooling to 1000 ℃ along with the furnace after the reaction is finished, introducing argon for protection in the process, taking out the alumina crucible, and naturally cooling to room temperature. The reaction process is simple, ilmenite in the obtained synthetic slag can be separated and enriched through magnetic separation and is used as a titanium-extracting enriched material, and tailings after the magnetic separation can be used for manufacturing building materials, so that the efficient utilization of the titanium-containing blast furnace slag is realized.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of metallurgical solid wastes, and particularly relates to a method for converting a titanium component in titanium-containing blast furnace slag into ilmenite (FeTiO)3) The method of (1).
Background
Titanium is an important strategic resource, and titanium metal and compounds thereof are widely used in the fields of aviation, aerospace, vehicle engineering, biomedicine and the like. In China, the vanadium titano-magnetite resource reserves are abundant, particularly the vanadium titano-magnetite reserves in the Panzhihua area are abundant, which account for 1/3 of the titanium resource reserves in the world, but the utilization rate of the titanium resource in China is low at present. After the vanadium-titanium magnetite concentrate enters a blast furnace for smelting, iron and vanadium in the vanadium-titanium magnetite concentrate are reduced and converted into metal for recycling, and titanium enters a slag phase to form titanium-containing blast furnace slag with complex mineral phase composition and structure. The titanium content of the Panzhihua steel-containing blast furnace slag is 20-24%, the titanium-containing mineral phases mainly comprise perovskite, titanium-containing diopside, melilite and the like, the piling amount of the titanium-containing blast furnace slag in China reaches 8000 million tons, and the speed of the piling amount is increased by 360 million tons every year. The titanium-containing blast furnace slag accumulated like a mountain wastes precious titanium resources, occupies a large amount of land and causes serious pollution to the environment, so that the efficient utilization of the titanium-containing blast furnace slag is always the pursuit target of the utilization of the titanium resources in China.
In order to improve the comprehensive utilization rate of the titanium-containing blast furnace slag and reasonably and efficiently utilize the titanium resource therein, researchers at home and abroad put forward various methods for utilizing titanium in the titanium-containing blast furnace slag. Mainly comprises the following steps: (1) preparing a titanium alloy: the silicon-titanium alloy is produced mainly by adopting a silicothermic method or a direct current aluminothermic method and the like. However, the silicon-titanium alloy has narrow application range, small dosage, large process energy consumption and difficult treatment of generated solid waste, and limits the industrial production scale for preparing the titanium alloy by adopting the titanium-containing blast furnace slag. (2) Preparing titanium dioxide by an acid method: mainly adopts sulfuric acid or hydrochloric acid to carry out acidolysis and leaching on the titanium-containing mineral in the titanium-containing blast furnace slag, and the acidolysis solution is hydrolyzed and separated to obtain the titanium dioxide. However, the titanium-containing blast furnace slag has many kinds of impurities, high content and large acid consumption, which causes a large amount of waste acid and tailings and causes serious pollution to the environment. (3) Extracting titanium by an alkaline method: the method mixes the titanium-containing blast furnace slag with NaOH or Na2CO3The alkaline reagents react at high temperature and then are leached and separated to prepare the titanium dioxide, but the method has the disadvantages of high alkali consumption, high recovery cost and complex process in the leaching process, is only suitable for treating titanium-rich slag, and can cause serious air pollution in the high-temperature treatment. (4) High-temperature carbonization-low-temperature selective chlorination: the method is thatCarbonizing the titanium-containing blast furnace slag at a high temperature of more than 1500 ℃, and then selectively reacting with Cl at a low temperature2Reacting and separating gas phase TiCl4. But because of high energy consumption of high-temperature carbonization and large chlorine consumption in low-temperature chlorination, secondary pollution is generated. (5) Selective enrichment-beneficiation: selectively enriching titanium elements which are dispersed and distributed in the titanium-containing blast furnace slag in a perovskite phase through metallurgical modification treatment, and then separating the perovskite phase from impurities through gravity separation or flotation. The method has low titanium recovery rate due to the fact that perovskite phase has small granularity and low hardness and is difficult to obtain optional grain size, and secondary pollution is caused due to the fact that a large amount of reagents are used in the beneficiation process. Therefore, the existing titanium-extracting technology from titanium-containing blast furnace slag has some difficulties to overcome from the aspects of technology, cost, environmental protection and the like.
Disclosure of Invention
Aiming at the defects of the existing titanium-containing blast furnace slag separation titanium extraction technology, the invention provides a method for converting titanium components in the titanium-containing blast furnace slag into ilmenite, and the ilmenite in the slag can be separated by a magnetic separation enrichment method.
The invention is realized by the following technical scheme.
The invention provides a method for converting titanium components in titanium-containing blast furnace slag into ilmenite, which specifically comprises the following steps:
(1) drying and crushing the titanium-containing blast furnace slag and the ferric oxide scale, crushing the coke blocks, sieving the crushed coke blocks, and respectively taking 100-mesh and 300-mesh powder. And mixing the obtained titanium-containing blast furnace slag, iron oxide scale, coke powder and silicon dioxide according to the mass ratio of 10: (2.5-4.5): (0.15-0.45): (1.0-2.5) mixing, and pressing under 1-5Mpa to obtain the final product.
(2) And (2) putting the tablets obtained in the step (1) into an alumina crucible, and putting the alumina crucible into a high-temperature furnace. Introducing argon for 30min to drive away air in the furnace cavity, then starting to heat up, reacting at the temperature of 1300-1450 ℃ for 240-420min, cooling to 1000 ℃ along with the furnace after the reaction is finished, introducing the argon for protection in the process, then taking out the alumina crucible, and naturally cooling to room temperature.
Further, the granularity of the titanium-containing blast furnace slag, the iron oxide scale and the coke in the step (1) is 100-300 meshes.
Further, the diameter of the material sheet in the step (2) is 5-10 mm, and the thickness of the material sheet is 2-4 mm.
The process principle of the invention is as follows: the titaniferous minerals in the titaniferous blast furnace slag are mainly perovskites containing positive quadrivalence and titaniferous diopside containing low-valence titanium, iron oxide scales (mainly consisting of oxides of ferrous iron and ferric iron) are added to react at high temperature, in the process, the low-valence titanium in the titaniferous blast furnace slag is oxidized into the positive quadrivalent titanium under the action of high-valence iron, and the titaniferous blast furnace slag, the ferrous iron in the iron oxide scales and the reduced ferrous iron are converted into the magnetic ilmenite under the oxygen site condition controlled by coke powder.
Compared with the prior art, the invention has the following technical effects:
1. the method has simple process flow, and the obtained synthetic slag can separate the titanium-rich material ilmenite from the synthetic slag through magnetic separation, thereby providing a clean separation way for extracting titanium from the titanium-containing blast furnace slag.
2. The tailings obtained after separation can be used as building materials, and the efficient utilization of the titanium-containing blast furnace slag is realized.
Drawings
FIG. 1 is an XRD pattern of raw titanium-containing blast furnace slag and scale iron oxide;
as shown in the figure, the adopted raw material titanium-containing blast furnace slag mainly comprises 20.45 mass percent of TiO2、26.31％CaO、27.93％SiO2、6.67％MgO、15.22％Al2O3The main phase composition of the titanium-containing diopside-titanate is perovskite, titanium-containing diopside and melilite; the total iron content (mass percent) in the raw material iron oxide scale is 66.35 percent, and the main phase component of the raw material iron oxide scale is Fe2O3And Fe3O4。
FIG. 2 is an XRD pattern of the synthetic slag obtained in example 1 of the present invention;
as shown in the figure, the main phase composition of the synthetic slag obtained in example 1 of the present invention was ilmenite and a general diopside phase, and the titanium component in the raw material titanium-containing blast furnace slag had been converted into ilmenite.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
Drying and crushing the titanium-containing blast furnace slag and the ferric oxide scale, crushing the coke blocks, sieving the crushed coke blocks, and respectively taking 100-mesh and 300-mesh powder. And mixing the obtained titanium-containing blast furnace slag, iron oxide scale, coke powder and silicon dioxide according to the mass ratio of 10: 4.0: 0.45: 2.5 mixing, pressing into round pieces under 1Mpa, and making into tablet with diameter of 5mm and thickness of 2 mm. Putting the obtained material sheet into an alumina crucible, putting the alumina crucible into a high-temperature furnace, introducing argon for 30min to drive away air in a furnace cavity, then starting to heat up and react at 1375 ℃ for 240min, cooling to 1000 ℃ along with the furnace after the reaction is finished, introducing argon for protection in the process, then taking out the alumina crucible, naturally cooling to room temperature, and converting the titanium-containing component in the obtained synthetic slag into ilmenite, wherein the XRD diagram of the ilmenite is shown in figure 2.
Example 2
Drying and crushing the titanium-containing blast furnace slag and the ferric oxide scale, crushing the coke blocks, and sieving the crushed coke blocks to respectively obtain powder of 100 meshes and 200 meshes. And mixing the obtained titanium-containing blast furnace slag, iron oxide scale, coke powder and silicon dioxide according to the mass ratio of 10: 3.5: 0.4: 2, uniformly mixing, and pressing into a wafer under the pressure of 5MPa, wherein the diameter of the obtained tablet is 10mm, and the thickness of the tablet is 4 mm. Putting the obtained material sheet into an alumina crucible, putting the alumina crucible into a high-temperature furnace, introducing argon for 30min to drive away air in a furnace cavity, then starting to heat up and react at 1300 ℃ for 420min, introducing argon for protection in the heating and reaction processes, cooling to 1000 ℃ along with the furnace, taking out the alumina crucible after the reaction is finished, naturally cooling to room temperature, converting the titanium-containing component in the obtained synthetic slag into ilmenite, wherein the XRD pattern of the ilmenite is almost the same as that in figure 2.
Example 3
Drying and crushing the titanium-containing blast furnace slag and the ferric oxide scale, crushing the coke blocks, sieving the crushed coke blocks, and respectively taking 200-mesh and 300-mesh powder. And mixing the obtained titanium-containing blast furnace slag, iron oxide scale, coke powder and silicon dioxide according to the mass ratio of 10: 3.0: 0.3: 1.5 mixing, pressing into round pieces under 1Mpa, and making into tablet with diameter of 5mm and thickness of 2 mm. Putting the obtained material sheet into an alumina crucible, putting the alumina crucible into a high-temperature furnace, introducing argon for 30min to drive away air in a furnace cavity, then starting to heat up and react at 1450 ℃ for 240min, cooling to 1000 ℃ along with the furnace after the reaction is finished, introducing argon for protection in the process, then taking out the alumina crucible, naturally cooling to room temperature, converting the titanium-containing component in the obtained synthetic slag into ilmenite, wherein the XRD pattern of the ilmenite is almost the same as that in figure 2.
Claims (3)
1. A method for converting titanium components in titanium-containing blast furnace slag into ilmenite is characterized by comprising the following steps of:
(1) uniformly mixing the titanium-containing blast furnace slag, iron oxide scale, silicon dioxide and coke, pressing into wafers, and controlling the mass ratio of the titanium-containing blast furnace slag, the iron oxide scale, the silicon dioxide and the coke to be 10: 2.5-4.5: 1.0-2.5: 0.15-0.45, and the pressing pressure is 1-5 Mpa;
(2) and (2) putting the material sheet obtained in the step (1) into an alumina crucible, putting the alumina crucible into a high-temperature furnace, introducing argon to drive away air in a furnace cavity under the protection of argon, starting heating, reacting at 1300-1450 ℃ for 240-420min, cooling to 1000 ℃ along with the furnace after the reaction is finished, introducing argon to protect all the time in the process, taking out the alumina crucible, and naturally cooling to room temperature.
2. The method for converting titanium components in the titanium-containing blast furnace slag into ilmenite as claimed in claim 1, wherein the particle size of the titanium-containing blast furnace slag, the scale of iron oxide and the coke in step (1) is 100 to 300 mesh.
3. The method for converting titanium component in the titanium-containing blast furnace slag into ilmenite as claimed in claim 1, wherein the web in the step (2) has a diameter of 5 to 10mm and a thickness of 2 to 4 mm.
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