CN114164310B - Method for smelting vanadium-containing pig iron and by-product vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime - Google Patents

Method for smelting vanadium-containing pig iron and by-product vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime Download PDF

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CN114164310B
CN114164310B CN202111477248.3A CN202111477248A CN114164310B CN 114164310 B CN114164310 B CN 114164310B CN 202111477248 A CN202111477248 A CN 202111477248A CN 114164310 B CN114164310 B CN 114164310B
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CN114164310A (en
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岳庆丰
贾怡晗
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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
    • C21B13/08—Making spongy iron or liquid steel, by direct processes in rotary furnaces
    • C21B13/085—Making spongy iron or liquid steel, by direct processes in rotary furnaces wherein iron or steel is obtained in a molten state
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • C21B13/0006—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state
    • C21B13/0013—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state introduction of iron oxide into a bath of molten iron containing a carbon reductant
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • C21B13/006—Starting from ores containing non ferrous metallic oxides
    • 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
    • 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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    • 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

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Abstract

The invention relates to the technical field of metallurgy, and provides a method for smelting vanadium-containing pig iron and byproduct vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime. The method comprises the steps of smelting furnace burden comprising vanadium-titanium magnetite by using an ore-smelting furnace, wherein a submerged arc smelting method is adopted at the initial stage, after the furnace burden is melted to form a naked molten pool, self-adaptive feeding is carried out in a mode of controlling automatic metering and continuous feeding by using an electronic computer, a strong-reduction saturated carburization layer is formed on a slag-iron interface by using a massive carbonaceous reducing agent, molten iron is carburized, vanadium in slag is reduced to enter the molten iron, titanium which is difficult to reduce is left in the slag, acid-soluble titanium slag and vanadium-containing molten iron are obtained after the slag-iron is separated, and oxygen blowing is further carried out on the vanadium-containing molten iron to extract vanadium, so that vanadium slag is obtained; and (3) removing sulfur and phosphorus from the molten iron after vanadium removal to obtain low-sulfur and phosphorus trace vanadium-containing pig iron. The product obtained by the method provided by the invention has high quality and high value, can improve economic benefit, and realizes high-value utilization of the vanadium-titanium-iron ore.

Description

Method for smelting vanadium-containing pig iron and by-product vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for smelting vanadium-containing pig iron by using vanadium titano-magnetite without adding desulfurized slag-making material lime or vanadium titano-magnetite reduced by a rotary kiln to obtain vanadium slag and acid-soluble titanium slag as byproducts.
Background
The vanadium titano-magnetite is a kind of complex mineral with many metal elements, mainly containing iron, vanadium and titanium. Due to its close intergrowth of ferrotitanium, most of the vanadium and iron minerals occur in the titanomagnetite in a homogeneous image, which is commonly referred to as vanadium titanomagnetite.
The vanadium titano-magnetite is a difficult-to-smelt ore recognized in the world, and the comprehensive utilization difficulty is high. The existing smelting method of vanadium titano-magnetite comprises the following steps: blast furnace-converter method, rotary kiln-electric furnace method, reduction-grinding method. Wherein, the blast furnace-converter method is used for low-titanium vanadium titano-magnetite (TiO) 2 Less than 12 percent) has advantages in smelting and good economic benefits. The disadvantage is that it can not smelt high Titanium (TiO) 2 Content of 13% by weight or more), titanium slag could not be recovered. The rotary kiln-electric furnace method can smelt vanadium-titanium magnetite ore with high titanium content, but because the smelting needs to add desulfurization material lime to make alkaline slag, titanium enters lime waste slag, and thus titanium slag can not be recovered. The reduction-grinding method is not suitable for large-scale production due to the defects that the vanadium-titanium magnetite is difficult to reduce, the scale is small, the distribution recovery rate of vanadium in iron powder and titanium slag is low, and the like.
The invention patent with publication number CN110592303A provides a vanadium-titanium magnetMethod for smelting vanadium-containing pig iron by ore, wherein CaO, mgO and Al are added during smelting 2 O 3 And SiO 2 In the smelting process, titanium enters lime furnace slag to become waste slag, and the recovery of titanium slag cannot be realized.
In the invention patent with publication number CN109943719A, a method for simultaneously preparing titanium slag and vanadium-containing pig iron by taking vanadium-titanium magnetite as a raw material is provided, wherein an electric furnace is adopted for smelting, and V in the titanium slag obtained by the method 2 O 5 The content is high (0.35-0.89 wt%), which affects the quality of titanium slag and the quality of vanadium-containing raw iron and sulfur.
Disclosure of Invention
The invention aims to provide a method for smelting vanadium-containing pig iron and producing vanadium slag and acid-soluble titanium slag as byproducts from vanadium titano-magnetite. The process according to the invention makes it possible to recover high-quality 15-30% V by smelting vanadium-containing pig iron from vanadium titano-magnetite 2 O 5 Vanadium slag and 50-80% of TiO 2 Acid-soluble titanium slag.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for smelting vanadium-containing pig iron and byproduct vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime comprises the following steps:
(1) Flatly paving a massive carbonaceous reducing agent at the bottom of a submerged arc furnace, then electrifying to perform arc striking, then adding part of furnace burden to perform reduction smelting, adding the rest furnace burden into a molten pool in a continuous feeding mode to perform melting reduction after the furnace burden is melted out of an exposed molten pool, and then performing slag-iron separation to obtain vanadium-containing molten iron and acid-soluble titanium slag; the furnace charge comprises the following components in parts by weight: 1.7 to 1.8 portions of vanadium titano-magnetite, 0 to 0.5 portion of ilmenite and 0.4 to 0.5 portion of granular carbonaceous reducing agent; lime is not required to be added into the submerged arc furnace for desulfurization and slagging;
(2) Carrying out oxygen blowing on the vanadium-containing molten iron in a foundry ladle to extract vanadium slag, carrying out sulfur and phosphorus removal on the molten iron after the vanadium slag is extracted, and then casting into blocks to obtain low-sulfur and phosphorus trace vanadium-containing pig iron; the low sulfur and phosphorus trace vanadium-containing pig iron contains less than 0.02wt% of S, less than 0.03wt% of P and less than or equal to 0.05wt% of V.
Preferably, the vanadium titano-magnetite comprises the following chemical components in percentage by mass: TFe 50-62%, tiO 2 12～23％、V 2 O 5 0.51～2.3％、SiO 2 0～2％、Al 2 O 3 0～3.5％、CaO 0～0.5％、MgO 0～1.0％、P<0.05％、S<0.1％；
The ilmenite comprises the following chemical components: TFe 29-35%, tiO 2 46～55％、V 2 O 5 0～0.6％、SiO 2 0～3.5％、Al 2 O 3 0～5％、CaO 0～0.3％、MgO 0～1.0％、P<0.05％、 S<0.1％；
Preferably, the lumped carbonaceous reducing agents and the particulate carbonaceous reducing agents have a fixed carbon content independently of > 85 wt. -%, a sulphur content independently of <0.05 wt. -% and a phosphorus content independently of <0.05 wt. -%.
Preferably, the lump carbonaceous reducing agent and the granular carbonaceous reducing agent independently comprise one or more of anthracite, semi coke, coke breeze and petroleum coke.
Preferably, the total time of the reduction smelting and the melting reduction is 4 to 6 hours, and the time of the melting reduction is counted from the beginning of the continuous feeding; the residual furnace burden is granules with the particle size less than 5mm; the particle size of the massive carbonaceous reducing agent is 10-80 mm; the particle size of the granular carbonaceous reducing agent is less than 5mm.
Preferably, the continuous feeding is automatically metered by using an electronic computer control.
Preferably, before the charging materials are added into the submerged arc furnace, the charging materials are reduced in a rotary kiln, then reduced materials are obtained through magnetic separation, and the reduced materials are smelted in the submerged arc furnace.
Preferably, when the reducing material is smelted, the reducing material is mixed with a carbonaceous reducing agent accounting for 3-5% of the total mass of the pre-reducing material.
Preferably, the submerged arc furnace is a graphite electrode submerged arc furnace; the capacity of the submerged arc furnace is 1800-50000 KVA.
Preferably, the desulfurization and the dephosphorization are carried out in an LF furnace, and the desulfurizing agent for the desulfurization comprises soda powder and magnesium powder.
The invention provides a method for smelting vanadium-containing pig iron by-products of vanadium slag and acid-soluble titanium slag from vanadium titano-magnetite without adding desulfurized slag-making material lime, which comprises the following steps: (1) Flatly paving a massive carbonaceous reducing agent at the bottom of a submerged arc furnace, then electrifying to perform arc striking, then adding part of furnace burden to perform reduction smelting, adding the rest furnace burden into a molten pool in a continuous feeding mode to perform melting reduction after the furnace burden is melted out of an exposed molten pool, and then performing slag-iron separation to obtain vanadium-containing molten iron and acid-soluble titanium slag; the furnace charge comprises the following components in parts by weight: 1.7 to 1.8 portions of vanadium titano-magnetite, 0 to 0.5 portion of ilmenite and 0.4 to 0.5 portion of granular carbonaceous reducing agent; the heat expansion furnace does not need to add lime for desulfurization and slagging (2), the vanadium-containing molten iron is subjected to hot metal ladle oxygen blowing to extract vanadium slag, molten iron after the vanadium slag is extracted is subjected to sulfur and phosphorus removal, and then the molten iron is cast into blocks to obtain low-sulfur and phosphorus trace vanadium-containing pig iron; the low-sulfur-phosphorus trace vanadium-containing pig iron contains less than 0.02wt% of S, less than 0.03wt% of P and less than or equal to 0.05wt% of V. The method comprises the steps of smelting furnace materials containing vanadium-titanium magnetite by using an ore furnace, adopting a submerged arc smelting method at the initial stage, converting the furnace materials into a continuous feeding mode to carry out smelting reduction smelting after the furnace materials are melted to form a naked molten pool, forming a strongly reduced saturated carburized layer on a slag-iron interface by using a massive carbonaceous reducing agent, carburizing molten iron, so that vanadium in slag is reduced and enters the molten iron, titanium which is difficult to reduce is remained in the slag, separating the slag-iron to obtain acid-soluble titanium slag and vanadium-containing molten iron, and carrying out sulfur removal after oxygen blowing is carried out on the vanadium-containing molten iron in a foundry ladle to extract vanadium slag, thereby obtaining low-sulfur-phosphorus trace vanadium-containing pig iron. The method provided by the invention can obtain high-quality low-sulfur phosphorus trace vanadium-containing pig iron, and V in the obtained acid-soluble titanium slag 2 O 5 The content is low, and the results of the examples show that the low-sulfur and low-phosphorus trace vanadium-containing pig iron obtained by the invention has the content of V less than 0.04 percent, the content of S and P less than 0.03 percent and the content of V in acid-soluble titanium slag 2 O 5 The content is less than 0.13wt%.
In addition, in the furnace charge, the dosage of the ilmenite can be 0, and when the ilmenite is not added, tiO in the obtained acid-soluble titanium slag 2 The content of the ilmenite is 50 to 60 percent, and part of ilmenite is addedThen, tiO can be obtained 2 The acid-soluble titanium slag with the content of 72-80 percent.
The invention combines reduction smelting and smelting reduction of the submerged arc furnace, so that vanadium is transferred from titanium slag into molten iron, and then acid soluble titanium slag containing vanadium iron and low vanadium content is obtained, and low-sulfur and low-phosphorus trace vanadium-containing pig iron is obtained from the vanadium-containing molten iron through vanadium extraction and phosphorus desulfurization. By adopting the method, the low-sulfur and phosphorus trace vanadium-containing pig iron, the vanadium slag and the acid-soluble titanium slag can be obtained by smelting the vanadium-titanium iron ore, the low-sulfur and phosphorus trace vanadium-containing pig iron can be used for steelmaking and high-quality cast iron, the vanadium slag can be used as a raw material for preparing vanadium pentoxide and ferrovanadium, and the acid-soluble titanium slag is a raw material for producing titanium dioxide and ferrotitanium by a sulfuric acid method.
In addition, in the art, blast furnace smelting is not applicable to high titanium ores, with slag containing TiO 2 But the slag is not easy to discharge, and the furnace bottom is easy to rise, so that the smelting can not be carried out. The traditional ore-smelting furnace smelting needs to add desulfurizer lime, and the produced vanadium-containing pig iron has high sulfur content and is unqualified without adding the desulfurizer lime, so that the vanadium-containing pig iron is a waste defective product, and the slag has high melting point, high viscosity and high energy consumption. The method realizes the smelting of the vanadium-titanium magnetite by the submerged arc furnace under the condition of desulfurization and slagging without adding lime, realizes the recovery of high-quality acid-soluble titanium slag, and reduces the iron-making cost.
Detailed Description
The invention provides a method for smelting vanadium-containing pig iron by-products of vanadium slag and acid-soluble titanium slag from vanadium titano-magnetite without adding desulfurized slag-making material lime, which comprises the following steps:
(1) Flatly paving a massive carbonaceous reducing agent at the bottom of a submerged arc furnace, then electrifying to perform arc striking, then adding part of furnace burden to perform reduction smelting, adding the rest furnace burden into a molten pool in a continuous feeding mode to perform melting reduction after the furnace burden is melted out of an exposed molten pool, and then performing slag-iron separation to obtain vanadium-containing molten iron and acid-soluble titanium slag; the furnace charge comprises the following components in parts by weight: 1.7 to 1.8 portions of vanadium titano-magnetite, 0 to 0.5 portion of ilmenite and 0.4 to 0.5 portion of granular carbonaceous reducing agent; lime does not need to be added into the heat expansion furnace for desulfurization and slagging;
(2) Carrying out hot metal ladle oxygen blowing on the vanadium-containing molten iron to extract vanadium slag, carrying out dephosphorization on the molten iron after the vanadium slag is extracted, and then casting into blocks to obtain low-sulfur phosphorus trace vanadium-containing pig iron; the low sulfur and phosphorus trace vanadium-containing pig iron contains less than 0.02wt% of S, less than 0.03wt% of P and less than or equal to 0.05wt% of V.
The method comprises the steps of flatly paving a blocky carbonaceous reducing agent at the bottom of a submerged arc furnace, then striking an arc by electrifying current, then adding part of furnace burden and striking an arc for reduction smelting, adding the rest furnace burden into a molten pool for melting reduction by adopting a continuous feeding mode after the furnace burden is melted out of an exposed molten pool, and then carrying out slag-iron separation to obtain vanadium-containing molten iron and acid-soluble titanium slag. In the invention, the furnace charge comprises the following components in parts by mass: 1.7 to 1.8 parts of vanadium titano-magnetite, preferably 1.73 to 1.75 parts, 0 to 0.5 part of ilmenite, preferably 0.1 to 0.4 part, and 0.4 to 0.5 part of granular carbonaceous reducing agent, preferably 0.44 to 0.45 part. In the present invention, the residual charge is preferably a granulate having a particle size of < 5mm.
In the present invention, the vanadium titano-magnetite preferably comprises the following chemical components in mass fraction: TFe 50-62%, preferably 55-60%, tiO 2 12 to 23%, preferably 15 to 20%, V 2 O 5 0.51 to 2.3%, preferably 1.5 to 2%, siO 2 0 to 2%, preferably 0.5 to 1.5%, al 2 O 3 0 to 3.5%, preferably 0.5 to 3%, caO 0 to 0.5%, preferably 0.2 to 0.4%, mgO 0 to 1.0%, preferably 1 to 9%, P<0.05%, preferably < 0.03%, S<0.1%, preferably < 0.05%. The invention uses vanadium titano-magnetite with higher vanadium and titanium content as raw material, which can improve economic benefit.
In the present invention, the ilmenite preferably comprises the following chemical components in mass fraction: TFe 29 to 35%, preferably 30 to 34%, tiO 2 46 to 55%, preferably 47 to 53%, V 2 O 5 0 to 0.6%, preferably 0.1 to 0.5%, siO 2 0 to 3.5%, preferably 0.3 to 3%, al 2 O 3 0 to 5%, preferably 0 to 3%, caO 0 to 0.3%Preferably 0 to 0.01%, mgO 0 to 1.0%, preferably 0.2 to 0.6%, P<0.05%, preferably<0.05％、S<0.1%, preferably<0.03 percent; in the present invention, the ilmenite is preferably mosangbicg ilmenite or chender ilmenite concentrate; in the invention, the mass fraction of the ilmenite in the furnace charge can be 0, and when no ilmenite is added, tiO in the obtained acid-soluble titanium slag 2 The content of the titanium dioxide is 50-60 percent, and TiO can be obtained after adding partial ilmenite 2 The acid-soluble titanium slag with the content of 72-80 percent.
In the present invention, the particulate carbonaceous reducing agent preferably has a fixed carbon content of > 85 wt.%, more preferably 88 wt.%, a sulphur content of preferably <0.05 wt.%, more preferably < 0.03 wt.%, and a phosphorus content of preferably <0.05 wt.%, more preferably < 0.03 wt.%. In the present invention, the particulate carbonaceous reducing agent preferably includes one or more of anthracite, semi coke, coke dust and petroleum coke; the particle size of the particulate carbonaceous reducing agent is preferably < 5mm, more preferably 1 to 4mm.
The preparation method of the furnace charge has no special requirements, and the raw materials are uniformly mixed according to the proportion.
In the invention, the submerged arc furnace is preferably a graphite electrode submerged arc furnace; the capacity of the submerged arc furnace is preferably 1800-50000 KVA, more preferably 2800-40000 KVA; the particle size of the massive carbonaceous reducing agent is preferably 10-80 mm; the lump carbonaceous reducing agent preferably has a fixed carbon content of > 85 wt.%, more preferably 88 wt.%, a sulphur content of <0.05 wt.%, more preferably < 0.03 wt.%, and a phosphorus content of <0.05 wt.%, more preferably < 0.03 wt.%. In the present invention, the lump carbonaceous reducing agent preferably includes one or more of anthracite, semi coke, coke dust and petroleum coke; the tiled thickness of the massive carbonaceous reducing agent is preferably 200-300mm, more preferably 230-250 mm, the tiled massive carbonaceous reducing agent is used as an initial carbon layer for arc striking, and in the subsequent smelting process, the massive carbonaceous reducing agent forms a saturated carburized layer on a slag-iron interface to promote vanadium to be reduced into molten iron; in a specific embodiment of the present invention, the specific operation of arc striking is preferably: adjusting the voltage of the submerged arc furnace to the minimum, introducing current into the initial carbon layer for arc striking, and then gradually increasing the voltage and the current until the voltage and the current of the submerged arc furnace reach the normal level; the process of boosting the voltage and current is preferably controlled by an automatic distributor of the submerged arc furnace. After the voltage and current of the submerged arc furnace reach the normal level, adding part of furnace burden; in the present invention, the weight of said portion of charge preferably represents 50% of the total weight of the charge. After part of furnace burden is added, continuing submerged arc reduction smelting until the furnace burden is melted out of an exposed molten pool, and then adding the rest furnace burden in a continuous feeding mode for melting reduction, wherein the particle size of the rest furnace burden is preferably less than 5mm; in the specific embodiment of the invention, the continuous feeding preferably adopts self-adaptive continuous feeding which is automatically metered and melted under the control of an electronic computer, and the thin-layer foam slag is kept at the heat preservation during feeding; in the present invention, the total time of the reduction smelting and the melting reduction is preferably 4 to 6 hours, more preferably 4.5 to 5.5 hours; the time of the melt reduction was timed from the start of the continuous feed.
In the invention, before the charging materials are added into the ore smelting furnace, the charging materials are preferably reduced in a rotary kiln, then reduced materials are obtained through magnetic separation, and the reduced materials are smelted in the ore smelting furnace; the invention has no special requirement on the temperature of the reducing material, and hot materials or cold materials can be smelted in a submerged arc furnace; in the invention, the metal pellets or metal blocks are obtained by metallizing the furnace charge after reduction, and the metallization rate of the reduced material is preferably 87 to 93 percent, and more preferably 90 percent.
In the invention, when the reducing material is adopted for smelting, the reducing material is preferably mixed with a carbonaceous reducing agent accounting for 3-5% (preferably 4%) of the total mass of the reducing material, and the obtained mixture is used as a furnace charge for smelting; the carbonaceous reducing agent is preferably a particulate carbonaceous reducing agent of less than 5mm; the invention does not require special measures for the mixing. In the invention, the specific operation method of smelting is consistent with the scheme, namely, firstly, a massive carbonaceous reducing agent is paved at the bottom of the submerged arc furnace to be used as an initial carbon layer, then, current is supplied to initiate arc, after the voltage and current in the furnace reach a normal level, a mixture of a partial reducing material and the carbonaceous reducing agent is added, reduction smelting is carried out until a molten pool is dissolved out, then, a continuous feeding mode is adopted for feeding and melting reduction, and slag-iron separation is carried out after smelting is finished, so that vanadium-containing molten iron and acid-soluble titanium slag can be obtained; the control conditions of the smelting process and the method for separating the iron slag are consistent with the scheme, and are not described again. The invention carries out pre-reduction on the furnace burden, and then adds the furnace burden into the submerged arc furnace for smelting, thus reducing the power consumption of smelting and being beneficial to reducing the production cost.
The specific operation method for separating the slag and the iron is not particularly required by the invention, and the method well known by the technical personnel can be adopted, in the specific embodiment of the invention, tapping and deslagging are preferably carried out when the temperature in the submerged arc furnace is more than 1650 ℃, the components of the vanadium-containing molten iron and slag are preferably tested before tapping and deslagging, and the C in the vanadium-containing molten iron is preferably selected>4wt%, V is preferably>1.35 wt.%), feO in the slag is preferred<5wt％、TiO 2 Preference is given to>72wt% (when the charge composition includes ilmenite) or > 50wt% (when ilmenite is not included in the charge composition); in the specific embodiment of the invention, the molten iron containing vanadium is preferably received by a ladle during tapping, slag is received by a slag pan during slag tapping, part of the slag iron in the furnace is preferably kept electrified during tapping and slag, and when a furnace bottom carbon layer is observed to be insufficient, part of the massive carbonaceous reducing agent is preferably supplemented to keep the thickness of the carbon layer; when the bottom of the furnace is expanded, the bottom of the furnace is preferably reduced by adding part of vanadium-titanium magnetite powder or ilmenite powder. In the embodiment of the invention, when the slag has high viscosity and can not be discharged, vanadium titano-magnetite or ilmenite powder is preferably added into the ore heating furnace from the electrode hole, and is electrified to melt, or oxygen is blown from a slag hole to destroy carbonitride of high melting point titanium, and slag is discharged after being diluted.
In the invention, slag obtained by separating slag iron is acid-soluble titanium slag; tiO in the acid-soluble titanium slag 2 The content of the acid-soluble titanium slag is preferably 50-80%, and particularly, when the charging material does not contain ilmenite, tiO in the acid-soluble titanium slag 2 Preferably 50-60%, when the charging material comprises ilmenite, tiO in the acid-soluble titanium slag 2 The content of (b) is preferably 72 to 80%. In the invention, the content of FeO in the acid-soluble titanium slag is preferably<5.0wt％，Al 2 O 3 Preferably 4 to 6wt% of SiO 2 Preferably in an amount of 3 to 4wt％、 V 2 O 5 Is preferably contained in<0.13wt%, C content is preferred<0.1wt%, S content is preferred<0.15 wt.%, the P content preferably being <0.05 wt.%.
In the invention, the molten iron obtained by slag-iron separation is vanadium-containing molten iron, and the vanadium-containing molten iron preferably comprises the following components in percentage by mass: c is more than 4.0 percent, V is preferably more than 1.3 percent, ti is less than 0.3 percent, si is less than 0.3 percent, P is preferably less than or equal to 0.05 percent, S is preferably less than or equal to 0.15 percent, and the rest is TFe.
After the vanadium-containing molten iron is obtained, the vanadium-containing molten iron is preferably subjected to ladle oxygen blowing to extract vanadium slag, the molten iron after the vanadium slag is extracted is subjected to sulfur and phosphorus removal, and then the molten iron is cast into blocks to obtain low-sulfur and phosphorus trace vanadium-containing pig iron; s in the low-sulfur and low-phosphorus trace vanadium-containing pig iron is less than 0.02wt%, P is less than 0.03wt%, V is less than or equal to 0.05%, and TFe in the low-sulfur and low-phosphorus trace vanadium-containing pig iron is preferably more than 95wt%; the product of the scheme of the invention comprises acid-soluble titanium slag, vanadium slag and low-sulfur phosphorus trace vanadium-containing pig iron; the vanadium slag preferably comprises the following components in percentage by mass: v 2 O 5 15-30％，TiO 2 8-10.5％，FeO20-25％，SiO 2 8-11.5％， C0.1-0.3％、S<0.15 percent and P is less than 0.05 percent; in the specific embodiment of the invention, the vanadium slag is preferably subjected to crushing and magnetic separation in sequence, iron particles are recovered, the residual vanadium slag is packaged and warehoused, and the recovered iron particles are returned to the oxygen blowing vanadium extraction step to be used as a coolant.
In the present invention, the desulfurising phosphorus is preferably carried out in an LF furnace; preferably, the ladle after oxygen blowing and vanadium extraction is transported to an LF furnace station, and then molten iron is heated and a desulfurizer is sprayed to remove sulfur and phosphorus; the desulfurizer preferably comprises soda powder and/or magnesium powder; the method has no special requirements on the specific operation conditions of the sulfur and phosphorus removal, and can ensure that the sulfur and phosphorus in the molten iron can meet the requirements by adopting the conditions well known by the technical personnel in the field.
Casting the molten iron after the sulfur and phosphorus removal into blocks to obtain low-sulfur and phosphorus trace vanadium-containing pig iron, wherein the low-sulfur and phosphorus trace vanadium-containing pig iron can be directly sold.
The embodiments of the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Smelting by adopting a 2500kVA graphite electrode submerged arc furnace. The chemical components of the used raw materials are as follows (all the mass fractions):
south africa vanadium titano-magnetite: TFe 56%, tiO 2 13％、V 2 O 5 1.6％、SiO 2 1.4％、Al 2 O 3 3.0％、CaO 0.01％、MgO 0.7％、P 0.05％、S 0.03％；
The petroleum coke requirement is as follows: the carbon content is more than or equal to 85%, the ash content is less than or equal to 3%, the volatile content is less than or equal to 10%, P is less than 0.05%, and S is less than 0.1%.
The proportioning is as follows: petroleum coke =1.8t, and is uniformly mixed to be used as ore-heating burden material.
The coke block with the thickness of 200-300mm is added into the furnace bottom when the furnace is opened, the furnace is electrified with low voltage and low current for arc striking, the voltage and the current are gradually increased to the normal smelting level under the automatic control of an automatic distributor, the furnace burden with the proportion is added for submerged arc smelting, after a molten pool is exposed, the automatic charging (namely the self-adaptive melting and the adding amount of the molten material are controlled by the electronic computer) is carried out in a continuous metering charging mode by adopting an electronic computer, the charging is carried out while melting, the operation of a thin layer of foam slag is kept during the charging, and the carburizing coke layer in an arc area is kept. And (3) testing the components of the slag iron at the temperature of more than 1650 ℃ after a reduction period and a carbon-supplementing strong reduction refining period, tapping iron, and deslagging to obtain vanadium-containing molten iron and acid-soluble titanium slag.
The vanadium-containing molten iron comprises the following chemical components: c4.1%, V1.37%, ti 0.3%, si 0.4%, P0.05%, S0.15%, and the rest is TFe.
Acid-soluble titanium slag components: tiO 2 2 57％、FeO 4.2％、Al 2 O 3 5.1％、SiO 2 3.6％、V 2 O 5 0.12％、C 0.08％、P 0.04％、S 0.13％；
Oxygen is blown into the foundry ladle to extract vanadium slag, and the obtained vanadium-removing molten iron and vanadium slag comprise the following components:
the vanadium-removing molten iron comprises the following components: 96.2% of TFe, 0.04% of V, 0.01% of Si, 0.05% of P and 0.10% of S;
composition of vanadium slag％：V 2 O 5 25.3％、TiO 2 11.1％、FeO 21.6％、Al 2 O 3 1.1％、SiO 2 11.1％、MgO 10.8％、C 0.1％、S 0.15％；
Heating and spraying soda powder to desulfurize phosphorus and alloying at a station of a vanadium-removing ladle LF furnace to produce low-phosphorus-sulfur molten iron: the molten iron with low sulfur and phosphorus content comprises the following components: 95.8 percent of TFe, 0.03 percent of V, 0.01 percent of Si, 0.028 percent of P and 0.017 percent of S, and obtaining the low-sulfur phosphorus pig iron from the ingot.
Example 2
Smelting by adopting a 2500kVA graphite electrode submerged arc furnace. The chemical components of the raw materials are as follows (all mass fractions):
the vanadium-titanium magnetite powder comprises the following chemical components: TFe 56%, tiO 2 13％、V 2 O 5 1.6％、SiO 2 1.4％、 Al 2 O 3 3.0％、CaO 0.01％、MgO 0.7％、P 0.05％、S 0.03％；
Composition of mosangbicg ilmenite: TFe 32.9%, tiO 2 50.2％、V 2 O 5 0.15％、SiO 2 0.45％、Al 2 O 3 0.55％、CaO 0.01％、MgO 0.28％、P 2 O 5 0.03％、S 0.03％；
The petroleum coke requirement is as follows: more than or equal to 85 percent of fixed carbon, less than or equal to 3 percent of ash, less than or equal to 10 percent of volatile matter, less than 0.05 percent of P and less than 0.01 percent of S.
The proportioning is as follows: vanadium titano-magnetite Mosang bisque titanium concentrate, petroleum coke = 1.7t.
Firstly adding carburized coke blocks with the grain size of 20-80mm and the thickness of 200-300mm into the furnace bottom, electrifying, carrying out low-voltage and low-current arc striking, adopting an automatic distributor to automatically control and gradually increase the voltage and the current to the normal smelting level, adding the furnace burden for submerged arc smelting, after an exposed molten pool is formed, adopting an electronic computer to control a continuous metering automatic feeding mode, carrying out melting and feeding at the same time, keeping the operation of thin-layer foamed slag, and keeping carburized coke in an arc area. And (3) testing the components of the slag iron to discharge iron and discharging slag when the total smelting time is 5h and the temperature is more than 1650 ℃ through a reduction period and a carbon-supplementing strong reduction refining period to obtain vanadium-containing molten iron and acid-soluble titanium slag.
The vanadium-containing molten iron comprises the following chemical components: 4.6% of C, 1.41% of V, 0.34% of Ti, 0.3% of Si, 0.05% of P, 0.13% of S and the balance of TFe;
acid-soluble titanium slag components: tiO 2 2 72.8％、FeO 4.5％、Al 2 O 3 5.1％、SiO 2 3.3％、V 2 O 5 0.11％、CaO 0.2％、MgO 1.1％、C 0.07％、P 0.03％、S 0.13％；
Oxygen blowing is carried out on the vanadium-containing molten iron to extract vanadium slag, and the obtained vanadium-removed molten iron and vanadium slag comprise the following components:
the vanadium-removing molten iron comprises the following components: TFe 95.7%, V0.027%, si 0.009%, P0.04%, S0.08%;
the vanadium slag comprises the following components: v 2 O 5 22.2％、TiO 2 10.3％、FeO 20.4％、Al 2 O 3 0.9％、SiO 2 11.2％、MgO 1.8％、C 0.1％、P 0.048％、S 0.07％；
Heating and spraying soda powder to desulfurize and phosphor to alloy and produce low-phosphor sulfur pig iron at an LF (ladle furnace) station, wherein the low-phosphor molten iron comprises the following components: 96.8% of TFe, 0.02% of V, 0.008% of Si, 0.026% of P and 0.019% of S, and obtaining low-sulfur phosphorus pig iron by casting.
Example 3
Smelting by adopting a 2500kVA graphite electrode submerged arc furnace, wherein the raw materials comprise the following chemical components:
chemical components of vanadium-titanium magnetite powder: TFe 53.8%, tiO 2 12.31％、V 2 O 5 0.53％、SiO 2 2.49％、Al 2 O 3 2.13％、CaO 0.01％、MgO 1.447％、P 0.05％、S 0.03％；
The titanium concentrate component: TFe 35% and TiO 2 45.5％、V 2 O 5 0.28％、SiO 2 1.64％、Al 2 O 3 1.2％、CaO 0.15％、MgO 0.79％、P 2 O 5 0.05％、S 0.13％；
The proportioning is as follows: vanadium titano-magnetite, chengdu titanium concentrate, petroleum coke = 1.7t.
The method comprises the steps of opening a furnace, firstly adding carburized coke with the particle size of 20-80mm into the bottom of the furnace, conducting low-voltage low-current arc striking, automatically controlling by an automatic distributor to gradually increase the voltage and the current to normal smelting levels, adding the furnace charge for submerged arc smelting, melting an exposed molten pool, then continuously metering in an automatic feeding mode under the control of an electronic computer, melting while feeding, keeping the operation of thin-layer foam slag, keeping the carburized coke in an arc area, testing the iron slag components when the temperature is higher than 1650 ℃ through a reduction period and a carbon-supplementing strong reduction refining period, tapping iron, and tapping to obtain vanadium-containing molten iron and acid-soluble titanium slag.
The vanadium-containing molten iron comprises the following chemical components: c5.0%, V1.55%, ti 0.3%, si 0.3%, cr 0.55%/P0.05%, S0.13%, TFe the remainder;
acid-soluble titanium slag components: tiO 2 2 75.6％、FeO 4.6％、Al 2 O 3 4.2％、SiO 2 3.7％、V 2 O 5 0.08％、C 0.05％、P 0.03％、S 0.10％；
Oxygen blowing is carried out on the vanadium-containing molten iron to extract vanadium slag, and vanadium-removed molten iron and vanadium slag are obtained:
the vanadium-removing molten iron comprises the following components: 96.4% of TFe, 0.04% of V, 0.01% of Si, 0.05% of P and 0.10% of S;
the vanadium slag comprises the following components: v 2 O 5 15.4％、TiO 2 9.3％、FeO 20.6％、Al 2 O 3 1.1％、SiO 2 10.7％、 MgO 9.4％、C 0.16％、P 0.045％、S 0.09％；
And (3) carrying out heating spraying on soda powder and magnesium powder for dephosphorizing and alloying to produce low-phosphorus sulfur pig iron at the station of the LF furnace by the vanadium-removing foundry ladle:
low sulfur phosphorus molten iron component: 97.1 percent of TFe, 0.025 percent of V, 0.02 percent of Si, 0.025 percent of P and 0.016 percent of S, and obtaining low-sulfur phosphorus pig iron by casting.
Example 4
Smelting by using a 2500kVA graphite electrode submerged arc furnace. The chemical components of the used raw materials are as follows:
the vanadium-titanium-iron ore powder comprises the following chemical components: TFe 56.5%, tiO 2 13.1％、V 2 O 5 1.6％、SiO 2 1.4％、 Al 2 O 3 3.0％、CaO 0.01％、MgO 0.7％、P 0.05％、S 0.03％；
Chemical components of Mosangbicg ilmenite: TFe 32.9%, tiO 2 50.2％、V 2 O 5 0.15％ SiO 2 0.45％、Al 2 O 3 0.55％、CaO≤0.11％、MgO 0.28％、P 2 O 5 0.03％、S 0.03％；
The petroleum coke requirement is as follows: more than or equal to 85 percent of fixed carbon, less than or equal to 3 percent of ash, less than or equal to 10 percent of volatile matter, less than 0.05 percent of P and less than 0.01 percent of S.
The proportioning is as follows: vanadium titano-magnetite, mosangbise titanium concentrate, petroleum coke = 1.7t.
Adding the mixture into a rotary kiln for pre-reduction to obtain a reduced material, wherein the metallization rate of the reduced material is 90 +/-3%, pellets or metal blocks are formed after pre-reduction, and the reduced material is used as a submerged arc furnace burden; chemical composition of reducing material%: TFe 64.5%, tiO 2 27.4％、V 2 O 5 1.75％、SiO 2 1.6％、Al 2 O 3 3.3％、MgO 1.1％、P 0.02％、S 0.06％。
And (3) adding 4% of petroleum coke into the reducing material, and uniformly mixing to obtain ore heating furnace charge. Firstly, adding a carburized coke block with the grain diameter of 20-80mm and the thickness of 200-300mm into the furnace bottom, electrifying, carrying out low-voltage and low-current arc striking, adopting an automatic distributor to automatically control and gradually increase the voltage and the current to the normal smelting level, adding part of the furnace burden, carrying out submerged arc smelting, after an exposed molten pool is formed, adopting an electronic computer to control a continuous metering automatic feeding mode, carrying out melting and feeding at the same time, keeping the operation of a thin layer of foam slag, and keeping carburized coke in an arc area. And (3) testing the iron components of the slag through a reduction period and a carbon-supplementing strong reduction refining period, wherein the total smelting time is 4h, and the temperature is more than 1650 ℃, tapping iron and deslagging to obtain vanadium-containing molten iron and acid-soluble titanium slag.
The vanadium-containing molten iron comprises the following chemical components: 4.4% of C, 1.39% of V, 0.3% of Ti, 0.3% of Si, 0.05% of P, less than 0.13% of S and the balance of TFe;
acid-soluble titanium slag components: tiO 2 2 77.3％、FeO 4.2％、Al 2 O 3 4.6％、SiO 2 3.8％、V 2 O 5 0.122％、CaO 0.2％、MgO 1.1％、C 0.07％、P 0.048％、S 0.13％；
And (3) blowing oxygen to extract vanadium slag from the vanadium-containing foundry ladle to obtain vanadium-removed molten iron and vanadium slag.
Vanadium-removing molten iron components: 95.2% of TFe, 0.04% of V, 0.01% of Si, 0.05% of P and 0.15% of S;
the vanadium slag comprises the following components: v 2 O 5 20.4％、TiO 2 9.5％、TFe 32.2％、FeO 24.1％、Al 2 O 3 1.2％、 SiO 2 11.3％、C 0.19％、S 0.10％、P 0.038％。
The vanadium-removing foundry ladle is heated and sprayed with soda ash to remove sulfur and phosphorus and alloy at an LF furnace station to produce low-phosphorus and sulfur pig iron and low-sulfur and phosphorus molten iron components: TFe95.8%, V0.035%, si0.008%, P0.025%, S0.015%, and casting to obtain low-sulfur phosphorus pig iron.
The above examples show that the invention overcomes the defects that the blast furnace-converter method can not smelt the high-titanium magnetite and can not recover the titanium slag and the rotary kiln pre-reduction-electric furnace method can not recover the titanium slag.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A method for smelting vanadium-containing pig iron and producing vanadium slag and acid-soluble titanium slag as byproducts from vanadium titano-magnetite without adding desulfurized slag-making material lime comprises the following steps:
(1) Flatly spreading a blocky carbonaceous reducing agent at the bottom of a submerged arc furnace, then electrifying to strike an arc, then adding part of furnace burden to carry out reduction smelting, adding the rest furnace burden to a molten pool by adopting a continuous feeding mode to carry out melting reduction after the furnace burden is melted out of an exposed molten pool in the reduction smelting, and then carrying out slag-iron separation to obtain vanadium-containing ironWater and acid soluble titanium slag; the furnace charge comprises the following components in parts by weight: 1.7 to 1.8 portions of vanadium titano-magnetite, 0.1 to 0.5 portion of ilmenite and 0.4 to 0.5 portion of granular carbonaceous reducing agent; lime does not need to be added into the submerged arc furnace for desulfurization and slagging; v in the acid-soluble titanium slag 2 O 5 In an amount of<0.13wt%; the part of furnace burden accounts for 50 percent of the total weight of the furnace burden; the particle size of the rest furnace burden is less than 5mm;
(2) Carrying out oxygen blowing on the vanadium-containing molten iron in a foundry ladle to extract vanadium slag, carrying out sulfur and phosphorus removal on the molten iron after the vanadium slag is extracted, and then casting into blocks to obtain low-sulfur and phosphorus trace vanadium-containing pig iron; the low-sulfur-phosphorus trace vanadium-containing pig iron contains less than 0.02wt% of S, less than 0.03wt% of P and less than or equal to 0.05wt% of V.
2. The method according to claim 1, wherein the vanadium titanomagnetite comprises the following chemical composition in mass fraction: TFe 50-62%, tiO 2 12～23％、V 2 O 5 0.51～2.3％、SiO 2 0～2％、Al 2 O 3 0～3.5％、CaO 0～0.5％、MgO 0～1.0％、P<0.05％、S<0.1％；
The ilmenite comprises the following chemical components: TFe 29-35%, tiO 2 46～55％、V 2 O 5 0～0.6％、SiO 2 0～3.5％、Al 2 O 3 0～5％、CaO 0～0.3％、MgO 0～1.0％、P<0.05％、S<0.1％；
3. The process of claim 1 wherein the lumped carbonaceous reducing agents and the particulate carbonaceous reducing agents have a fixed carbon content independently of > 85 wt.%, a sulfur content independently of <0.05 wt.%, and a phosphorus content independently of <0.05 wt.%.
4. The method of claim 1 or 3, wherein the bulk carbonaceous reducing agent and the particulate carbonaceous reducing agent independently comprise one or more of anthracite, semi-coke, coke breeze, and petroleum coke.
5. The method according to claim 1, wherein the total time of the reduction smelting and the melt reduction is 4 to 6 hours, and the time of the melt reduction is counted from the start of the continuous feeding; the particle size of the massive carbonaceous reducing agent is 10-80 mm; the particle size of the granular carbonaceous reducing agent is less than 5mm.
6. The method according to claim 1 or 5, wherein the continuous feed is metered automatically using computer control.
7. The method as claimed in claim 1 or 5, wherein the charging material is added in front of the ore smelting furnace, and the method further comprises the steps of reducing the charging material in a rotary kiln, then obtaining reducing material through magnetic separation, and smelting the reducing material in the ore smelting furnace.
8. The method of claim 7, wherein the reducing material is smelted, and the method further comprises mixing the reducing material with a carbonaceous reducing agent accounting for 3-5% of the total mass of the pre-reducing material.
9. The method of claim 1 or 8, wherein the submerged arc furnace is a graphite electrode submerged arc furnace; the capacity of the submerged arc furnace is 1800-50000 KVA.
10. The method as claimed in claim 1, characterized in that the said desulfation is carried out in a LF furnace, and the desulfating desulfurizing agents include soda ash and magnesium powder.
CN202111477248.3A 2021-12-06 2021-12-06 Method for smelting vanadium-containing pig iron and by-product vanadium slag and acid-soluble titanium slag from vanadium-titanium magnetite without adding desulfurized slag-making material lime Active CN114164310B (en)

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