CN110317917B - Method for treating vanadium-titanium magnetite through fluidized reduction, electric arc melting and converter sodium treatment - Google Patents
Method for treating vanadium-titanium magnetite through fluidized reduction, electric arc melting and converter sodium treatment Download PDFInfo
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- CN110317917B CN110317917B CN201910640291.3A CN201910640291A CN110317917B CN 110317917 B CN110317917 B CN 110317917B CN 201910640291 A CN201910640291 A CN 201910640291A CN 110317917 B CN110317917 B CN 110317917B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0033—In fluidised bed furnaces or apparatus containing a dispersion of the material
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/12—Making spongy iron or liquid steel, by direct processes in electric furnaces
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/14—Multi-stage processes processes carried out in different vessels or 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
- 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
- C22B34/1204—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1213—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by wet processes, e.g. using leaching methods or flotation techniques
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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
A method for treating vanadium-titanium magnetite by fluidized reduction, electric arc melting and converter sodium treatment comprises the following steps: putting the vanadium-titanium magnet concentrate powder into a storage bin, and conveying the concentrate powder into a primary cyclone separator; under the action of negative pressure, primary solid-gas separation is carried out on the vanadium-titanium magnetite concentrate powder, and primary solid materials enter a suspension heating furnace; the high-temperature flue gas heats the primary solid material and keeps the primary solid material in a suspension state; then the mixture enters a secondary cyclone separator, a secondary solid material is separated out and enters a reduction reactor, the formed reduction material enters a converter for sodium oxide roasting under the condition of arc melting of an electric arc furnace, roasted clinker is cooled and ground, and TiO is separated by water immersion2Concentrate and sodium vanadate solution. The method can efficiently separate each component, has simple process and short flow, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for treating vanadium-titanium magnetite through fluidized reduction, electric arc melting and converter sodium treatment.
Background
Vanadium-titanium is an important strategic resource in China, is widely applied to core high-technology fields such as aerospace, high-speed steel rails, national defense and military, and is mainly contained in vanadium-titanium magnetite. At present, the vanadium-titanium magnetite concentrate is mainly processed by adopting a blast furnace-converter industrial process, but the vanadium-titanium magnetite concentrate is limited by blast furnace smelting conditions, titanium in the vanadium-titanium magnetite concentrate is not recycled, and the recovery rate of vanadium is only about 45%, so that the vanadium-titanium resource is greatly wasted. Therefore, research and development are urgently needed for the efficient utilization technology and equipment of the iron, vanadium and titanium all components of the vanadium-titanium magnetite.
The effective separation of iron and vanadium and titanium can be realized by fluidized bed direct reduction-electric furnace melting separation, wherein the fluidized bed method has prominent advantages in the direct reduction process because the powder ore is directly fed into the furnace, the process flow is short, the required temperature is low. The fluidized bed method is a method for making mineral particles in suspension state and reducing them by utilizing reducing gas through ore bed, and the petroleum catalytic cracking in the 20 th century and 40 th century developed the modern fluidized bed reaction technology and introduced into the gas-based direct reduction industry. The fluidized bed method has the advantages of no coke for reduction and less pollutant discharge, and is a direct reduction process capable of directly feeding fine ores into a furnace. Compared with the pellet material, the specific surface area of the powder particles is multiplied, and the reaction rate of the fluidized bed at the same temperature is improved. Therefore, the research and development of the novel vanadium-titanium magnetite full-component efficient utilization technology and equipment based on the fluidized bed direct reduction-electric furnace melting separation technology are significant.
Disclosure of Invention
The invention aims to provide a method for treating vanadium-titanium magnetite through fluidized reduction-electric arc melting-converter sodium treatment, which is characterized in that the vanadium-titanium magnetite is pre-reduced (the iron metallization rate is more than or equal to 90%) by utilizing a fluidized bed direct reduction technology, then an electric arc furnace is adopted for melting and separating to generate molten iron and vanadium-titanium slag, the vanadium-titanium slag is subjected to sodium oxidation roasting, and then vanadium is extracted by water, and finally high-grade titanium slag is obtained, so that the full-component efficient utilization of the vanadium-titanium magnetite is realized.
The method of the invention is carried out according to the following steps:
(1) putting the vanadium-titanium magnet concentrate powder into a stock bin, and conveying the concentrate powder into a primary cyclone separator through a discharge port of the stock bin;
(2) the gas outlet of the first-stage cyclone separator is communicated with the feed inlet of the dust removing equipment, the gas outlet of the dust removing equipment is communicated with the induced draft fan, the discharge hole of the first-stage cyclone separator is communicated with the lower part of the suspension heating furnace, the top of the suspension heating furnace is communicated with the feed inlet of the second-stage cyclone separator through a conveying pipeline, and the gas outlet of the second-stage cyclone separator is communicated with the feed inlet of the first-stage cyclone separator; starting an induced draft fan to enable negative pressure to be formed inside the primary cyclone separator, the suspension heating furnace and the secondary cyclone separator, carrying out solid-gas separation on the vanadium-titanium magnetite concentrate powder in the primary cyclone separator under the action of the negative pressure, and enabling the formed primary solid material to enter the suspension heating furnace;
(3) introducing high-temperature flue gas at 1100-1300 ℃ from the bottom of the suspension heating furnace, wherein the high-temperature flue gas enables the primary solid material to be heated and in a suspension state;
(4) the heated primary solid material enters a secondary cyclone separator through a conveying pipeline under the action of negative pressure to carry out secondary solid-gas separation, and the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator;
(5) the discharge hole of the secondary cyclone separator is communicated with the feed inlet of the reduction reactor; under the condition of introducing reducing gas into the reduction reactor, after the secondary solid material enters the reduction reactor, reducing the iron oxide in the secondary solid material into metallic iron, discharging the formed reduced material from a discharge hole of the reduction reactor, and entering an electric arc furnace;
(6) under the condition that the electric arc furnace carries out electric arc melting, reducing materials are added into the electric arc furnace for electric arc melting to form liquid slag and molten iron which are respectively discharged from a slag discharging port and a molten iron outlet;
(7) the slag discharging port of the electric arc furnace is communicated with a converter through a pipeline, liquid slag enters the converter, sodium carbonate or sodium sulfate is added into the converter, oxygen is introduced into the converter, and the liquid slag and the sodium carbonate or sodium sulfate are mixed and then subjected to sodium oxide roasting to obtain roasted clinker; oxidizing vanadium trioxide in the roasted clinker into vanadium pentoxide, and further reacting with sodium carbonate or sodium sulfate to generate sodium vanadate dissolved in water;
(8) discharging the roasted clinker from the converter, cooling to room temperature, and then crushing and grinding to obtain roasted powder; placing the roasted powder into water for water leaching, dissolving sodium vanadate into the water, filtering and separating the obtained water leaching material to obtain a sodium vanadate solution and water leaching residues, and allowing titanium dioxide in the roasted clinker to enter the water leaching residues; washing and drying the water-soaked slag to prepare TiO2And (5) concentrating.
The particle size of the vanadium-titanium magnet concentrate powder is less than or equal to 0.8 mm.
In the method, the reduction reactor is of a box-type structure, the top of the reduction reactor is provided with a feed inlet, the upper part of the side wall of the reduction reactor is provided with a discharge outlet, the bottom of the reduction reactor is provided with an air inlet, and the reduction reactor is internally provided with an air distribution plate and at least one partition plate; the air distribution plate is positioned at the lower part of the reduction reactor, and the space between the air distribution plate and the bottom plate of the reduction reactor is used as an air chamber; the baffle plate is positioned above the air distribution plate, two side edges of the baffle plate are fixed on the inner wall of the reduction reactor, the space between the top edge of the baffle plate and the top of the reduction reactor is an upper channel, and the space between the bottom edge of the baffle plate and the air distribution plate is a lower channel; the feed inlet and the discharge outlet are respectively positioned at two sides of the partition plate; each clapboard uniformly divides the interior of the reduction reactor into at least two reduction chambers; under the condition of introducing reducing gas, the secondary solid material entering the reduction reactor is in a suspension state in each reduction chamber and is reduced.
In the method, the electric arc furnace comprises a furnace body and an electrode, wherein the electrode is fixed above the furnace body and is inserted into the furnace body from the top of the furnace body; a feed inlet is arranged above the furnace body and is communicated with a discharge outlet of the reduction reactor through a pipeline, the interior of the furnace body is divided into an upper space, a slag layer space and a molten iron layer space from top to bottom, a gas outlet is arranged on the side wall of the upper space, a slag discharge port is arranged on the side wall of the slag layer space, and a molten iron outlet is arranged on the side wall of the molten iron layer space; the bottom end of the electrode is positioned in the slag layer space; when the electric arc furnace is used for smelting, after the reducing materials enter the electric arc furnace, liquid slag and molten iron formed by electric arc smelting respectively enter a slag layer space and a molten iron layer space.
In the method, after the vanadium-titanium magnetite concentrate powder is subjected to solid-gas separation in the primary cyclone separator, the generated primary tail gas enters the dust remover, and the dust-removing tail gas after dust removal is discharged by the induced draft fan.
In the method, the gas outlet of the electric arc furnace is communicated with the bottom of the suspension heating furnace through a high-temperature flue gas pipeline, and high-temperature flue gas generated during electric arc smelting is introduced into the suspension heating furnace through the high-temperature flue gas pipeline.
In the method, when the secondary cyclone separator performs secondary solid-gas separation, the generated secondary tail gas enters the feed inlet of the primary cyclone separator.
The iron grade TFe of the vanadium-titanium magnet concentrate powder is 55-62%, and the iron grade TFe comprises 26-34% of FeO and SiO according to mass percentage2 2～10％，Al2O3 2～10％，CaO 0.1～1.2％，MgO 0.5～11％。
In the method, the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.15-0.25 m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 800-900 ℃.
The reducing gas is carbon monoxide and/or hydrogen or a mixed gas consisting of carbon monoxide and/or hydrogen and nitrogen, and the volume percentage of the nitrogen in the mixed gas is less than or equal to 40 percent.
In the method, the ratio of the volume flow of the reducing gas entering the reduction reactor to the mass flow of the secondary solid material is 0.05-0.15 m3And/kg, the retention time of the secondary solid material in the reduction reactor is 40-60 min, and the temperature of the material in the reduction reactor is 750-850 ℃.
In the method, when the induced draft fan is started, the negative pressure in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace is-0.1 kPa to-2.5 kPa.
In the method, the metallization rate of iron in the reduction reactor is more than or equal to 90 percent.
In the method, the smelting temperature of the electric arc furnace for arc smelting is 1600-1800 ℃, and the retention time of the reducing materials in the electric arc furnace is 40-60 min.
The Fe content of the molten iron is more than or equal to 95 percent by mass.
In the method, the temperature of sodium oxide roasting is 1250-1500 ℃, and the time is 20-40 min; the using amount of the sodium carbonate or the sodium sulfate is 15-20% of the total mass of the liquid slag; the mass ratio of the total amount of the introduced oxygen to the liquid slag in the sodium oxide roasting process is 75-115 m3/kg。
In the method, the granularity of the roasted powder is less than or equal to 0.074mm, the water immersion temperature is 70-100 ℃, and the time is 40-60 min; the water consumption during water immersion is 4-6L/kg according to the liquid-solid ratio of water to the roasted material.
The above TiO2TiO content in the concentrate according to mass percentage2≥50％。
The principle of the invention is as follows: the iron in the vanadium-titanium magnetite concentrate is reduced by suspension preheating of a suspension heating furnace and reduction, and vanadium and titanium still exist in the form of oxides; when the electric arc melting is carried out, iron is separated from vanadium and titanium, then sodium salt roasting is carried out in a converter, and then vanadium is recovered by water leaching, so that the separation of three elements of iron, vanadium and titanium is realized; the method can efficiently separate each component, has simple process and short flow, and has good application prospect.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to the present invention;
FIG. 2 is a schematic view of the reduction reactor of FIG. 1;
in the figure, the device comprises a material bin 1, a material bin 2, a primary cyclone separator 3, a dust remover 4, an induced draft fan 5, a suspension heating furnace 6, a conveying pipeline 7, a secondary cyclone separator 8, a reduction reactor discharge port 9, a reduction reactor 10, an electrode 11, an electric arc furnace feed port 12, a furnace body 13, a slag discharge port 14, a molten iron outlet 15, a high-temperature flue gas pipeline 16, a converter oxygen nozzle 17, a converter body 18, a converter discharge port 19, a reduction reactor feed port 20, a partition plate 21 and a wind distribution plate.
Detailed Description
In the embodiment of the invention, the granularity of the powdery vanadium titano-magnetite is less than or equal to 0.8mm, wherein the mass of the particles with the granularity of less than 0.074mm accounts for 40-90% of the total mass.
The N partition plates in the reduction reactor of the present invention equally divide the reduction reactor into N +1 reduction chambers in the width direction.
In the embodiment of the invention, the TFe of the powdery vanadium-titanium magnetite concentrate is 55-62%, and the powdery vanadium-titanium magnetite concentrate contains 26-34% of FeO and SiO by mass2 2～10％，Al2O3 2～10％，CaO 0.1～1.2％，MgO 0.5～11％。
The structure of the device for treating vanadium-titanium magnetite by fluidized reduction-electric arc smelting-converter sodium treatment in the embodiment of the invention is shown in figure 1, and the device comprises a storage bin 1, a primary cyclone separator 2, a dust remover 3, an induced draft fan 4, a suspension heating furnace 5, a suspension material channel 6, a secondary cyclone separator 7, a reduction reactor 9 and an electric arc furnace; a discharge port of the storage bin 1 is communicated with a feed inlet of the primary cyclone separator 2, a discharge port of the primary cyclone separator 2 is communicated with the lower part of the suspension heating furnace 5, the top of the suspension heating furnace 5 is communicated with a feed inlet of the secondary cyclone separator 7 through a conveying pipeline 6, and an air outlet of the secondary cyclone separator 7 is communicated with a feed inlet of the primary cyclone separator 2; the discharge hole of the secondary cyclone separator 7 is communicated with the reduction reactor feed inlet 19 of the reduction reactor 9;
the reduction reactor 9 is in a box-type structure as shown in FIG. 2, the top of the reduction reactor is provided with a reduction reactor feed inlet 19, the upper part of the side wall of the reduction reactor is provided with a reduction reactor discharge outlet 8, the bottom of the reduction reactor is provided with an air inlet, and the reduction reactor is internally provided with an air distribution plate 21 and two partition plates 20; the air distribution plate 21 is positioned at the lower part of the reduction reactor 9, and the space between the air distribution plate 21 and the bottom plate of the reduction reactor 9 is used as an air chamber; the baffle plate 20 is positioned above the air distribution plate 21, two side edges of the baffle plate 20 are fixed on the inner wall of the reduction reactor 9, the space between the top edge of the baffle plate 20 and the top of the reduction reactor 9 is an upper channel, and the space between the bottom edge of the baffle plate 20 and the air distribution plate 21 is a lower channel; and the reduction reactor feed port 19 and the reduction reactor discharge port 8 are respectively positioned at both sides of all the partition plates 20; the two clapboards 20 divide the interior of the reduction reactor 9 into three reduction chambers along the horizontal direction;
the electric arc furnace comprises a furnace body 12 and an electrode 10, wherein the electrode 10 is fixed above the furnace body 12, and the electrode 10 is inserted into the furnace body 12 from the top of the furnace body 12; an electric arc furnace feed inlet 11 is arranged above a furnace body 12 and is communicated with a reduction reactor discharge outlet 8 through a pipeline, the interior of the furnace body 12 is divided into an upper space, a slag layer space and a molten iron layer space from top to bottom, an air outlet is arranged on the side wall of the upper space, a slag discharge port 13 is arranged on the side wall of the slag layer space, and a molten iron outlet 14 is arranged on the side wall of the molten iron layer space; the bottom end of the electrode 10 is positioned in the slag layer space; the gas outlet is communicated with the bottom of the suspension heating furnace 5 through a high-temperature flue gas pipeline 15;
the converter comprises a converter body 17 and a converter oxygen nozzle 16, and a converter discharge hole 18 is arranged on the side wall.
In the embodiment of the invention, the metallization rate of the secondary solid material in the reduction reactor is more than or equal to 90 percent.
The following are preferred embodiments of the present invention.
Example 1
The vanadium-titanium magnet concentrate powder comprises, by mass, TFe 58.95%, FeO 31.12%, and SiO2 2.04％，Al2O33.49％，CaO 0.21％，MgO 0.66％；
Putting the vanadium-titanium magnet concentrate powder into a stock bin, and conveying the concentrate powder into a primary cyclone separator through a discharge port of the stock bin; the particle size of the vanadium-titanium magnetite concentrate powder is less than or equal to 0.8 mm;
the gas outlet of the first-stage cyclone separator is communicated with the feed inlet of the dust removing equipment, the gas outlet of the dust removing equipment is communicated with the induced draft fan, the discharge hole of the first-stage cyclone separator is communicated with the lower part of the suspension heating furnace, the top of the suspension heating furnace is communicated with the feed inlet of the second-stage cyclone separator through a conveying pipeline, and the gas outlet of the second-stage cyclone separator is communicated with the feed inlet of the first-stage cyclone separator; starting an induced draft fan to enable negative pressure to be formed inside the primary cyclone separator, the suspension heating furnace and the secondary cyclone separator, carrying out solid-gas separation on the vanadium-titanium magnetite concentrate powder in the primary cyclone separator under the action of the negative pressure, and enabling the formed primary solid material to enter the suspension heating furnace;
introducing high-temperature flue gas at 1100-1300 ℃ from the bottom of the suspension heating furnace, wherein the high-temperature flue gas enables the primary solid material to be heated and in a suspension state;
the heated primary solid material enters a secondary cyclone separator through a conveying pipeline under the action of negative pressure to carry out secondary solid-gas separation, and the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator;
the discharge hole of the secondary cyclone separator is communicated with the feed inlet of the reduction reactor; under the condition of introducing reducing gas into the reduction reactor, after the secondary solid material enters the reduction reactor, reducing the iron oxide in the secondary solid material into metallic iron, discharging the formed reduced material from a discharge hole of the reduction reactor, and entering an electric arc furnace;
under the condition that the electric arc furnace carries out electric arc melting, reducing materials are added into the electric arc furnace for electric arc melting, liquid slag and molten iron formed by electric arc melting respectively enter a slag layer space and a molten iron layer space and are respectively discharged from a slag discharging port and a molten iron outlet; introducing high-temperature flue gas generated in the electric arc smelting into the suspension heating furnace through a high-temperature flue gas pipeline;
the slag discharging port of the electric arc furnace is communicated with a converter through a pipeline, liquid slag enters the converter, sodium carbonate is added into the converter, oxygen is introduced into the converter, and sodium oxide roasting is carried out after the liquid slag and the sodium carbonate are mixed to obtain roasted clinker; oxidizing vanadium trioxide in the roasted clinker into vanadium pentoxide, and further reacting with sodium carbonate or sodium sulfate to generate sodium vanadate dissolved in water;
discharging the roasted clinker from the converter, cooling to room temperature, and then crushing and grinding to obtain roasted powder; placing the roasted powder into water for water leaching, dissolving sodium vanadate into the water, filtering and separating the obtained water leaching material to obtain a sodium vanadate solution and water leaching residues, and allowing titanium dioxide in the roasted clinker to enter the water leaching residues; washing and drying the water-soaked slag to prepare TiO2Concentrate;
after solid-gas separation is carried out on the vanadium-titanium magnetite concentrate powder in a primary cyclone separator, generated primary tail gas enters a dust remover, and the dust-removing tail gas after dust removal is discharged by a draught fan;
when the secondary cyclone separator performs secondary solid-gas separation, the generated secondary tail gas enters a feed inlet of the primary cyclone separator;
wherein the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.15m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 800 ℃;
the reducing gas is a mixed gas of carbon monoxide and nitrogen, and the volume percentage of the nitrogen is 25 percent;
the ratio of the volume flow of the reducing gas entering the reduction reactor to the mass flow of the secondary solid material is 0.1m3The residence time of the secondary solid material in the reduction reactor is 50min, and the material temperature in the reduction reactor is 780 ℃;
when the induced draft fan is started, the negative pressures in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace are respectively-2.2, -1.1, -0.36 and-0.13 kPa;
the metallization rate of iron in the reduction reactor is more than or equal to 90 percent;
the smelting temperature of the electric arc furnace for arc smelting is 1600 ℃, and the retention time of the reducing materials in the electric arc furnace is 60 min;
the molten iron contains 96 percent of Fe, 1.50 percent of C, 0.01 percent of P, 0.01 percent of S, 0.02 percent of Si and 0.03 percent of Al according to mass percentage;
the sodium oxide roasting temperature is 1300 deg.C, and the time is 40min; the using amount of the sodium carbonate is 17 percent of the total mass of the liquid slag; the mass ratio of the total amount of oxygen introduced in the sodium oxide roasting process to the liquid slag is 80m3/kg；
The granularity of the roasted powder is less than or equal to 0.074mm, the water immersion temperature is 70 ℃, and the time is 60 min; the water consumption during water immersion is 6L/kg according to the liquid-solid ratio of water to the roasted material;
TiO2TiO content in the concentrate according to mass percentage2 54.5％。
Example 2
The vanadium-titanium magnet concentrate powder comprises, by mass, TFe 59.63%, FeO 30.93%, and SiO2 1.78％，Al2O33.14％，CaO 0.20％，MgO 0.76％；
The method is the same as example 1, except that:
(1) the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.25m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 900 ℃;
(2) the reducing gas is a mixed gas of hydrogen and nitrogen, and the volume percentage of the nitrogen is 35 percent;
(3) the ratio of the volume flow of the reducing gas entering the reduction reactor to the mass flow of the secondary solid material is 0.15m3The residence time of the secondary solid material in the reduction reactor is 40min, and the material temperature in the reduction reactor is 810 ℃;
(4) when the induced draft fan is started, the negative pressures in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace are respectively-1.95, -1.15, -0.33 and-0.17 kPa;
(5) the electric arc melting temperature is 1700 ℃, and the retention time of the reducing materials in the electric arc furnace is 50 min;
(6) the molten iron contains 95.2 percent of Fe, 1.41 percent of C, 0.02 percent of P, 0.02 percent of S, 0.04 percent of Si and 0.04 percent of Al according to mass percentage;
(7) adding sodium sulfate into the converter; the temperature of sodium oxide roasting is 1350 ℃ and the time is 30 min; the using amount of the sodium sulfate is 16 percent of the total mass of the liquid slag; total oxygen gas introduced during sodium oxide roastingThe mass ratio of the amount to the liquid slag is 85m3/kg；
(8) The water immersion temperature is 80 ℃, and the time is 55 min; the liquid-solid ratio of water to the roasted material is 4L/kg;
(9)TiO2TiO content in the concentrate according to mass percentage2 52.3％。
Example 3
The vanadium-titanium magnet concentrate powder comprises, by mass, TFe 60.58%, FeO 31.24%, and SiO2 1.08％，Al2O33.02％，CaO 0.14％，MgO 0.68％；
The method is the same as example 1, except that:
(1) the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.2m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 850 ℃;
(2) reducing gas mixed gas of carbon monoxide, hydrogen and nitrogen, wherein the volume percentage of the nitrogen is 15%; the volume percentage of carbon monoxide is 60 percent;
(3) the ratio of the volume flow of the reducing gas entering the reduction reactor to the mass flow of the secondary solid material is 0.06m3The residence time of the secondary solid material in the reduction reactor is 45min, and the material temperature in the reduction reactor is 850 ℃;
(4) when the induced draft fan is started, the negative pressure in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace is respectively-2.35, -1.25, -0.34 and-0.16 kPa;
(5) the electric arc melting temperature is 1750 ℃, and the retention time of the reducing material in the electric arc furnace is 45 min;
(6) the molten iron comprises 96.8 percent of Fe, 1.04 percent of C, 0.01 percent of P, 0.01 percent of S, 0.03 percent of Si and 0.02 percent of Al in percentage by mass;
(7) the temperature of sodium oxide roasting is 1400 ℃, and the time is 25 min; the using amount of the sodium carbonate is 15 percent of the total mass of the liquid slag; the mass ratio of the total amount of oxygen introduced in the sodium oxide roasting process to the liquid slag is 75m3/kg；
(8) The water immersion temperature is 85 deg.C, and the time is 50 min; the liquid-solid ratio of water to the roasted material is 5L/kg;
(9)TiO2TiO content in the concentrate according to mass percentage2 51.6％。
Example 4
The vanadium-titanium magnet concentrate powder comprises, by mass, TFe 57.44%, FeO 29.25%, and SiO2 3.11％，Al2O34.16％，CaO 0.27％，MgO 7.83％；
The method is the same as example 1, except that:
(1) the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.22m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 870 ℃;
(2) the reducing gas is a mixed gas of carbon monoxide and hydrogen in equal volume;
(3) the ratio of the volume flow of the reducing gas entering the reduction reactor to the mass flow of the secondary solid material is 0.05m3The residence time of the secondary solid material in the reduction reactor is 60min, and the material temperature in the reduction reactor is 750 ℃;
(4) when the induced draft fan is started, the negative pressure in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace is respectively-2.35, -1.25, -0.34 and-0.16 kPa;
(5) the electric arc melting temperature is 1800 ℃, and the retention time of the reducing material in the electric arc furnace is 40 min;
(6) the molten iron comprises 95.4 percent of Fe, 1.1 percent of C, 0.02 percent of P, 0.01 percent of S, 0.04 percent of Si and 0.03 percent of Al in percentage by mass;
(7) adding sodium sulfate into the converter; the temperature of sodium oxide roasting is 1450 ℃, and the time is 20 min; the using amount of the sodium sulfate is 18 percent of the total mass of the liquid slag; the mass ratio of the total amount of oxygen introduced in the sodium oxide roasting process to the liquid slag is 95m3/kg；
(8) The water immersion temperature is 90 deg.C, and the time is 40 min; the liquid-solid ratio of water to the roasted material is 4.5L/kg;
(9)TiO2TiO content in the concentrate according to mass percentage2 53.1％。
Claims (10)
1. A method for treating vanadium titano-magnetite by fluidized reduction-electric arc melting-converter sodium treatment is characterized by comprising the following steps:
(1) putting the vanadium-titanium magnet concentrate powder into a stock bin, and conveying the concentrate powder into a primary cyclone separator through a discharge port of the stock bin;
(2) the gas outlet of the first-stage cyclone separator is communicated with the feed inlet of the dust removing equipment, the gas outlet of the dust removing equipment is communicated with the induced draft fan, the discharge hole of the first-stage cyclone separator is communicated with the lower part of the suspension heating furnace, the top of the suspension heating furnace is communicated with the feed inlet of the second-stage cyclone separator through a conveying pipeline, and the gas outlet of the second-stage cyclone separator is communicated with the feed inlet of the first-stage cyclone separator; starting an induced draft fan to enable negative pressure to be formed inside the primary cyclone separator, the suspension heating furnace and the secondary cyclone separator, carrying out solid-gas separation on the vanadium-titanium magnetite concentrate powder in the primary cyclone separator under the action of the negative pressure, and enabling the formed primary solid material to enter the suspension heating furnace; when a draught fan is started, the negative pressure in the dust remover, the primary cyclone separator, the secondary cyclone separator and the suspension heating furnace is-0.1 kPa to-2.5 kPa;
(3) introducing high-temperature flue gas at 1100-1300 ℃ from the bottom of the suspension heating furnace, wherein the high-temperature flue gas enables the primary solid material to be heated and in a suspension state; the ratio of the volume flow of the high-temperature flue gas entering the suspension heating furnace to the mass flow of the primary solid material is 0.15-0.25 m3Per kg; the temperature of the first-stage solid material in the suspension heating furnace is 800-900 ℃;
(4) the heated primary solid material enters a secondary cyclone separator through a conveying pipeline under the action of negative pressure to carry out secondary solid-gas separation, and the formed secondary solid material is discharged from a discharge hole of the secondary cyclone separator;
(5) the discharge hole of the secondary cyclone separator is communicated with the feed inlet of the reduction reactor; under the condition of introducing reducing gas into the reduction reactor, after the secondary solid material enters the reduction reactor, reducing the iron oxide in the secondary solid material into metallic iron, discharging the formed reduced material from a discharge hole of the reduction reactor, and entering an electric arc furnace; into a reduction reactorThe ratio of the volume flow of the reducing gas to the mass flow of the secondary solid material is 0.05-0.15 m3The residence time of the secondary solid material in the reduction reactor is 40-60 min, and the temperature of the material in the reduction reactor is 750-850 ℃;
(6) under the condition that the electric arc furnace carries out electric arc melting, reducing materials are added into the electric arc furnace for electric arc melting to form liquid slag and molten iron which are respectively discharged from a slag discharging port and a molten iron outlet;
(7) the slag discharging port of the electric arc furnace is communicated with a converter through a pipeline, liquid slag enters the converter, sodium carbonate or sodium sulfate is added into the converter, oxygen is introduced into the converter, and the liquid slag and the sodium carbonate or sodium sulfate are mixed and then subjected to sodium oxide roasting to obtain roasted clinker; oxidizing vanadium trioxide in the roasted clinker into vanadium pentoxide, and further reacting with sodium carbonate or sodium sulfate to generate sodium vanadate dissolved in water;
(8) discharging the roasted clinker from the converter, cooling to room temperature, and then crushing and grinding to obtain roasted powder; placing the roasted powder into water for water leaching, dissolving sodium vanadate into the water, filtering and separating the obtained water leaching material to obtain a sodium vanadate solution and water leaching residues, and allowing titanium dioxide in the roasted clinker to enter the water leaching residues; washing and drying the water-soaked slag to prepare TiO2And (5) concentrating.
2. The method for treating vanadium-titanium magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, wherein the particle size of vanadium-titanium magnetite concentrate powder is less than or equal to 0.8 mm.
3. The method for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, characterized in that the reduction reactor is of a box structure, the top is provided with a feed inlet, the side wall is provided with a discharge outlet, the bottom is provided with an air inlet, and the inside is provided with an air distribution plate and at least one baffle plate; the air distribution plate is positioned at the lower part of the reduction reactor, and the space between the air distribution plate and the bottom plate of the reduction reactor is used as an air chamber; the baffle plate is positioned above the air distribution plate, two side edges of the baffle plate are fixed on the inner wall of the reduction reactor, the space between the top edge of the baffle plate and the top of the reduction reactor is an upper channel, and the space between the bottom edge of the baffle plate and the air distribution plate is a lower channel; the feed inlet and the discharge outlet are respectively positioned at two sides of the partition plate; each clapboard uniformly divides the interior of the reduction reactor into at least two reduction chambers; under the condition of introducing reducing gas, the secondary solid material entering the reduction reactor is in a suspension state in each reduction chamber and is reduced.
4. The method for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, characterized in that the electric arc furnace comprises a furnace body and an electrode, the electrode is fixed above the furnace body, the electrode is inserted into the furnace body from the top of the furnace body; a feed inlet is arranged above the furnace body and is communicated with a discharge outlet of the reduction reactor through a pipeline, the interior of the furnace body is divided into an upper space, a slag layer space and a molten iron layer space from top to bottom, a gas outlet is arranged on the side wall of the upper space, a slag discharge port is arranged on the side wall of the slag layer space, and a molten iron outlet is arranged on the side wall of the molten iron layer space; the bottom end of the electrode is positioned in the slag layer space; when the electric arc furnace is used for smelting, after the reducing materials enter the electric arc furnace, liquid slag and molten iron formed by electric arc smelting respectively enter a slag layer space and a molten iron layer space.
5. The method for treating the vanadium-titanium magnetite by the fluidized reduction-electric arc melting-converter sodium treatment according to the claim 1, wherein in the step (2), after the vanadium-titanium magnetite concentrate powder is subjected to solid-gas separation in a primary cyclone separator, the generated primary tail gas enters a dust remover, and the dust-removed tail gas after dust removal is discharged by a draught fan.
6. The method for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, characterized in that the gas outlet of the electric arc furnace is communicated with the bottom of the suspension heating furnace through a high temperature flue gas pipeline, and the high temperature flue gas generated during electric arc melting is introduced into the suspension heating furnace through the high temperature flue gas pipeline.
7. The method for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, characterized in that in step (4), secondary tail gas generated during secondary solid-gas separation in the secondary cyclone enters the feed inlet of the primary cyclone.
8. The method of claim 1, wherein the iron grade TFe of the vanadium titano-magnetite powder is 55-62% and contains 26-34% FeO and SiO by mass2 2~10%，Al2O3 2~10%，CaO 0.1~1.2%，MgO 0.5~11%。
9. The method of claim 1, wherein the reducing gas is carbon monoxide and/or hydrogen, or a mixture of carbon monoxide and/or hydrogen and nitrogen, and the volume percentage of nitrogen in the mixture is less than or equal to 40%.
10. The method for treating vanadium titano-magnetite by fluidized reduction-arc melting-converter sodium treatment according to claim 1, characterized in that the molten iron contains Fe by mass percent of more than or equal to 95%.
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| CN114045404A (en) * | 2021-11-16 | 2022-02-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium concentrate hydrogen reduction method |
| CN114574712A (en) * | 2022-03-14 | 2022-06-03 | 沈阳铝镁设计研究院有限公司 | Roasting system and roasting process for reducing roasting temperature by adopting fluidized bed |
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