CN110863074B - Harmless and resource utilization method for vanadium extraction tailings - Google Patents
Harmless and resource utilization method for vanadium extraction tailings Download PDFInfo
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- CN110863074B CN110863074B CN201911034299.1A CN201911034299A CN110863074B CN 110863074 B CN110863074 B CN 110863074B CN 201911034299 A CN201911034299 A CN 201911034299A CN 110863074 B CN110863074 B CN 110863074B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C1/00—Refining of pig-iron; Cast iron
- C21C1/02—Dephosphorising or desulfurising
- C21C1/025—Agents used for dephosphorising or desulfurising
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/064—Dephosphorising; Desulfurising
- C21C7/0645—Agents used for dephosphorising or desulfurising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
Abstract
The invention discloses a method for harmless and resource utilization of vanadium extraction tailings, which comprises the following steps: uniformly mixing the vanadium extraction tailings and semi-coke in proportion, pelletizing, and reducing and roasting to prepare pre-reduced pellets; crushing the pre-reduced pellets, mixing with a proper amount of lime, and grinding; and spraying the ground mixed material into a molten iron bath in the molten iron pretreatment process, stirring and slagging off. The metallic iron in the mixed material is melted into molten iron, and the toxic vanadium and chromium are deeply reduced by silicon and carbon in the molten iron and then enter the molten iron, so that the detoxification and valuable element recovery of the vanadium extraction tailings are realized, and the desulfurization effect of the reduction tailings on the molten iron is remarkable. The method directly realizes the detoxification and valuable metal recovery of the vanadium extraction tailings by means of the molten iron pretreatment procedure in the steelmaking process, completes the pre-desulfurization of the molten iron, has simple operation and low energy consumption, is easy to be linked with the steelmaking process, and has wide industrialization prospect.
Description
Technical Field
The invention belongs to the technical field of harmless and resource utilization of metallurgical solid wastes, and particularly relates to a method for harmless and resource utilization of vanadium extraction tailings in a molten iron pretreatment process.
Background
The vanadium extraction tailings are solid wastes generated in the vanadium extraction process of vanadium titano-magnetite smelting-vanadium slag. The annual discharge of vanadium extraction tailings in China exceeds 60 million tons, and due to increasing market demands, the vanadium productivity is continuously increased, and the discharge amount of the vanadium extraction tailings is also increased year by year. At present, most of vanadium extraction tailings are idle and stockpiled, which not only invades land resources, but also is more important to be toxic V in the vanadium extraction tailings5+And Cr6+And the like have great harm to the health of people and other organisms, and cause serious pollution when flowing into the natural environment. Therefore, the harmless treatment of the vanadium extraction tailings is necessary. Besides vanadium and chromium, the vanadium extraction tailings contain high content of iron, and metal elements such as iron, vanadium, chromium and the like have recycling value.
Patent CN200810106422.1 discloses a treatment method of vanadium extraction tailings, and specifically, the vanadium extraction tailings and a carbon source are mixed and heated, and then a magnetic separation method is adopted to separate reduction products to obtain magnetic powder and non-magnetic powder. The method carries out primary treatment on the vanadium extraction tailings, and although the patent indicates that magnetic powder rich in iron, manganese and chromium can be used for steel making, and non-magnetic powder can be used for extracting vanadium and titanium, no specific use method is given. Patent CN201310472042.0 discloses a method for efficiently recovering iron, vanadium and chromium from vanadium extraction tailings, and specifically, vanadium extraction tailings, a reducing agent, an additive and a binder are mixed and then pelletized, and vanadium-chromium sponge iron and titanium-containing slag are obtained through reduction and magnetic separation. The method adopts additive to act as catalyst or nucleating agent, can improve reduction condition, and reduce energy consumption to a certain extent. However, the product obtained by the method is still a primary industrial raw material, the added value is limited, and a specific using method is not given. In addition, the two methods have the problems of low reduction rate and incomplete magnetic separation. Patent CN201210331163.9 discloses a method for producing ferroalloy by reducing and smelting vanadium extraction tailings, and specifically, the vanadium extraction tailings are mixed with a carbon source and calcium oxide, and two-stage high-temperature smelting is carried out at 800-900 ℃ and 1350-1500 ℃ respectively to obtain ferroalloy containing vanadium and chromium. The method needs to be carried out in a high-temperature smelting furnace, the energy consumption is extremely high, and the tailings after the recovery of iron, vanadium and chromium cannot be effectively utilized.
The pretreatment of molten iron is an important process in the steel-making process, generally, the molten iron obtained by blast furnace smelting is pretreated to remove harmful element sulfur, and the molten iron can be added into a converter for steel making after the pretreatment and desulfurization. The industrial reactor for the molten iron pretreatment is a torpedo car or a ladle, the temperature of a molten iron bath in the torpedo car or the ladle is generally 1300-1400 ℃, and the molten iron pretreatment is generally carried out by spraying a desulfurizing agent into the molten iron bath by using a spray gun or adding the desulfurizing agent into the molten iron bath by using a KR stirring paddle and stirring. The method has the main function of removing sulfur in molten iron by using alkaline desulfurized slag so as to prevent the sulfur from remaining in steel to cause hot brittleness of the steel. The temperature of the molten iron is generally 1250-1450 ℃, more than 4% of carbon and 0.30-1.25% of silicon are usually dissolved in the molten iron, and the sensible heat of the molten iron and the existence of reducing agents such as silicon, carbon and the like provide possibility for harmless and resource utilization of the vanadium extraction tailings. If the vanadium extraction tailings can be subjected to pre-reduction treatment through carbon thermal reduction roasting and added into high-temperature molten iron in the molten iron pretreatment process, the sensible heat of the molten iron can be utilized to realize the melting separation and recovery of iron in the tailings. Meanwhile, the reducibility of silicon and carbon in high-temperature molten iron can be utilized to realize the reduction recovery of elements such as iron, vanadium, chromium and the like in the tailings in the molten iron, and the harmlessness and valuable metal resource recovery of the vanadium extraction tailings are realized. In order to ensure the realization of the desulfurization function in the pretreatment process of molten iron, the tailings are required to be modified properly to improve the sulfur capacity of the slag and improve the fluidity of the slag, and the tailings after extracting iron, vanadium and chromium are prepared into a molten iron desulfurizer to realize the maximum recycling of the vanadium extraction tailings.
If the harmless and resource utilization of the vanadium extraction tailings in the molten iron pretreatment process is realized, the problems of discharge and treatment of the vanadium extraction tailings can be solved to a great extent, the recovery of valuable metal elements and the removal of sulfur in molten iron are realized, and the environmental benefit and the economic benefit are very obvious.
Disclosure of Invention
In order to solve the problems, the invention provides a method for harmless and resource utilization of vanadium extraction tailings, which not only removes toxic V in the vanadium extraction tailings5+And Cr6+Meanwhile, valuable metal elements such as iron, vanadium, chromium and the like in the vanadium extraction tailings are recovered, the sulfur content in the molten iron can be effectively reduced, the quality of steel is improved, and the harmless and resource utilization of the vanadium extraction tailings in the molten iron pretreatment is realized.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for harmless and resource utilization of vanadium extraction tailings comprises the following specific process steps:
(1) preparing vanadium extraction tailings and semi-coke as raw materials, wherein the molar ratio of oxygen in iron oxide in the vanadium extraction tailings to carbon in the semi-coke is 1: 1.2-1.8, adding water into the raw materials, uniformly mixing, pelletizing, drying, and removing water to obtain carbon-containing pellets;
(2) reducing and roasting the carbon-containing pellets obtained in the step (1) at 700-1200 ℃ for 15-120 min to prepare pre-reduced pellets;
(3) crushing the pre-reduced pellets obtained in the step (2), uniformly mixing the pre-reduced pellets with lime, and grinding to obtain a mixed material with the particle size of less than or equal to 0.18 mm;
(4) and (3) spraying the mixed material obtained in the step (3) as a desulfurizer into a molten iron bath in the molten iron pretreatment process, stirring at 1300-1400 ℃, and slagging off.
In the step (1), the iron grade T.Fe of the vanadium extraction tailings is 15-50%, and the vanadium extraction tailings contain Cr according to weight percentage2O30～15％、V2O50～10％、Al2O30～5％、SiO25％～25％、Na2O 2％～15％、TiO25% -25% of MnO and 0-10% of MnO; the semi-coke contains more than or equal to 70 percent of fixed carbon and less than or equal to 0.15 percent of S according to weight percentage.
In the step (3), the lime contains more than or equal to 95 percent of CaO by weight percent, and the addition amount of the lime is 20 to 40 percent of the weight of the pre-reduced pellets.
In the step (4), the molten iron pretreatment is carried out in a molten iron tank or a torpedo tank car; the weight of the mixed material sprayed into the molten iron bath is 10-100 kg/t iron; the stirring time of the stirring treatment is 5-30 min.
The invention has the beneficial effects that:
1. the vanadium extraction tailings are pre-reduced and then mixed with lime, and the mixture is used as a desulfurizer and added into a molten iron molten pool for molten iron pretreatment and desulfurization. In addition to the desulfurization effect, the invention utilizes carbon thermal pre-reduction to reduce a large amount of iron oxide contained in the vanadium extraction tailings into metallic iron, and utilizes the high temperature of molten iron for steel making and the reducibility of carbon and silicon dissolved in the molten iron to deeply reduce and recycle iron, vanadium and chromium in the pre-reduced vanadium extraction tailings into the molten iron, thereby realizing the recovery of valuable metal elements and the harmlessness of the tailings while detoxifying the vanadium extraction tailings; the recovery rate of iron in the vanadium extraction tailings is more than or equal to 90 percent, the recovery rate of vanadium is more than or equal to 95 percent, and the recovery rate of chromium is more than or equal to 90 percent.
2. The invention utilizes lime to carry out component modification of the tailings after vanadium extraction by prereduction so as to reduce the melting point of the tailings and improve the sulfur capacity of the tailings, the modified tailings have obvious desulfurization effect on molten iron, the sulfur content in the molten iron can be reduced to be less than 0.01 percent, and the pretreatment desulfurization of the molten iron for steelmaking is directly realized.
3. The invention relates to a method for harmless and resource utilization of vanadium extraction tailings, which is simple and easy to operate and feed, separates slag and iron by utilizing the high temperature of molten iron for steel making, does not need to add extra high-temperature smelting equipment, has low energy consumption and low investment, and is easy to connect with a steel making process.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
Example 1
(1) Preparing vanadium extraction tailings and semi-coke as raw materials, wherein the iron grade T.Fe of the vanadium extraction tailings is 35.32%, and the vanadium extraction tailings contains Cr according to weight percentage2O37.08％、V2O51.78％、Al2O32.33％、SiO215.01％、Na2O 7.24％、TiO210.47% and MnO 4.05%. The semi-coke contains 74.3 percent of fixed carbon and 0.10 percent of S according to weight percentage. The molar ratio of oxygen in the vanadium extraction tailings iron oxide to carbon in the semi-coke is 1:1.2, water is added into the raw materials, the raw materials are uniformly mixed, pelletizing is carried out, and then drying is carried out to remove water, so that the carbon-containing pellets are obtained.
(2) Reducing and roasting the carbon-containing pellets for 30min at the temperature of 1000 ℃ to prepare pre-reduced pellets.
(3) And crushing the pre-reduced pellets, mixing the pre-reduced pellets with lime, and performing ball milling to obtain a mixed material with the particle size of less than or equal to 0.18 mm. The addition of lime is 21% of the weight of the roasted material.
(4) And (4) spraying the mixed material obtained in the step (3) into a molten pool in a molten iron tank in the molten iron pretreatment process, stirring for 12min, and slagging off. The weight of the mixed material injected into the molten iron bath was 45kg/t iron. Finally, the recovery rates of iron, vanadium and chromium in the vanadium extraction tailings in the molten iron are respectively 96.9%, 95.7% and 92.6%, and the content of sulfur in the molten iron is reduced to 0.004%.
Example 2
(1) Preparing vanadium extraction tailings and semi-coke as raw materials, wherein the iron grade T.Fe of the vanadium extraction tailings is 27.76%, and the vanadium extraction tailings contain Cr according to weight percentage2O35.26％、V2O50.97％、Al2O34.17％、SiO221.29％、Na2O 8.82％、TiO212.92 percent and MnO3.11 percent. The semi-coke comprises 72.6 percent of fixed carbon and 0.12 percent of S according to weight percentage. The molar ratio of oxygen in the vanadium extraction tailings iron oxide to carbon in the semi-coke is 1:1.8, water is added into the raw materials, the raw materials are uniformly mixed, pelletizing is carried out, and then drying is carried out to remove water, so as to obtain the carbon-containing pellets.
(2) Reducing and roasting the carbon-containing pellets for 120min at the temperature of 700 ℃ to prepare pre-reduced pellets.
(3) And crushing the pre-reduced pellets, mixing the pre-reduced pellets with lime, and performing ball milling to obtain a mixed material with the particle size of less than or equal to 0.18 mm. The lime is added in an amount of 35% by weight of the roasted material.
(4) And (4) spraying the mixed material obtained in the step (3) into a molten pool in a molten iron tank in the molten iron pretreatment process, stirring for 18min, and slagging off. The weight of the mixed material injected into the molten iron bath was 66kg/t iron. Finally, the recovery rates of iron, vanadium and chromium in the vanadium extraction tailings in the molten iron are respectively 93.4%, 97.1% and 92.3%, and the sulfur content in the molten iron is reduced to 0.007%.
Example 3
(1) Preparing vanadium extraction tailings and semi-coke as raw materials, wherein the iron grade T.Fe of the vanadium extraction tailings is 40.19%, and the vanadium extraction tailings contains Cr according to weight percentage2O39.33％、V2O52.38％、Al2O32.34％、SiO210.57％、Na2O 4.79％、TiO27.19 percent and MnO2.84 percent. The semi-coke contains 78.6 percent of fixed carbon and 0.08 percent of S according to weight percentage. The molar ratio of oxygen in the vanadium extraction tailings iron oxide to carbon in the semi-coke is 1:1.5, water is added into the raw materials, the raw materials are uniformly mixed, pelletizing is carried out, and then drying is carried out to remove water, so as to obtain the carbon-containing pellets.
(2) Reducing and roasting the carbon-containing pellets for 15min at the temperature of 1200 ℃ to prepare pre-reduced pellets.
(3) And crushing the pre-reduced pellets, mixing the pre-reduced pellets with lime, and performing ball milling to obtain a mixed material with the particle size of less than or equal to 0.18 mm. The lime is added in an amount of 27% by weight of the roasted material.
(4) And (3) spraying the mixed material into a molten pool in a molten iron tank in the molten iron pretreatment process, stirring for 9min, and slagging off. The weight of the mixed material injected into the molten iron bath was 31kg/t iron. Finally, the recovery rates of iron, vanadium and chromium in the vanadium extraction tailings in the molten iron are respectively 98.2%, 97.5% and 96.7%, and the sulfur content in the molten iron is reduced to 0.003%.
Claims (10)
1. A method for harmless and resource utilization of vanadium extraction tailings is characterized by comprising the following steps:
(1) the method comprises the following steps of taking vanadium extraction tailings and semi-coke as raw materials, controlling the molar ratio of oxygen in iron oxide in the vanadium extraction tailings to carbon in the semi-coke to be 1: 1.2-1.8, adding water into the raw materials, uniformly mixing, pelletizing, drying, and removing water to obtain carbon-containing pellets;
(2) reducing and roasting the carbon-containing pellets obtained in the step (1) at 700-1200 ℃ for 15-120 min to prepare pre-reduced pellets;
(3) crushing the pre-reduced pellets obtained in the step (2), mixing with lime, and grinding to obtain a mixed material;
(4) and (3) spraying the mixed material obtained in the step (3) as a desulfurizer into a molten iron bath in the molten iron pretreatment process, stirring at 1300-1400 ℃, and slagging off.
2. The method for harmless and resource utilization of the vanadium extraction tailings according to claim 1, wherein in the step (1), the iron grade T.Fe of the vanadium extraction tailings is 15-50%, and the vanadium extraction tailings contain Cr according to weight percentage2O30～15％、V2O50～10％、Al2O30～5％、SiO25％～25％、Na2O 2％～15％、TiO25% -25% of MnO and 0-10% of MnO; the semi-coke contains more than or equal to 70 percent of fixed carbon and less than or equal to 0.15 percent of S according to weight percentage.
3. The method for harmless and resource utilization of the vanadium extraction tailings according to claim 1 or 2, characterized in that in the step (3), CaO is contained in lime by weight percent of more than or equal to 95%, and the addition amount of the lime is 20-40% of the weight of the pre-reduced pellets.
4. The method for harmless and resource utilization of vanadium extraction tailings according to claim 1 or 2, wherein in the step (3), the particle size of the obtained mixed material is less than or equal to 0.18 mm.
5. The method for harmless and resource utilization of vanadium extraction tailings according to claim 3, wherein in the step (3), the particle size of the obtained mixed material is less than or equal to 0.18 mm.
6. The method for harmless and resource utilization of the vanadium extraction tailings according to claim 1, 2 or 5, wherein in the step (4), the weight of the mixed material sprayed into the molten iron bath is 10-100 kg/t iron.
7. The method for harmless and resource utilization of vanadium extraction tailings according to claim 3,
in the step (4), the weight of the mixed material sprayed into the molten iron bath is 10-100 kg/t iron.
8. The method for harmless and resource utilization of vanadium extraction tailings according to claim 4,
in the step (4), the weight of the mixed material sprayed into the molten iron bath is 10-100 kg/t iron.
9. The method for harmless and resource utilization of the vanadium extraction tailings according to the claim 1, 2, 5, 7 or 8, wherein in the step (4), the stirring time of the stirring treatment is 5-30 min.
10. The method for harmless and resource utilization of vanadium extraction tailings according to claim 6, wherein in the step (4), the stirring time of the stirring treatment is 5-30 min.
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| CN113736998B (en) * | 2021-09-07 | 2023-05-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Harmless treatment method for tailings of vanadium extraction by calcium method |
| CN115261608B (en) * | 2022-07-18 | 2023-07-21 | 中南大学 | Method and system for improving strength of vanadium extraction tailings pellets and strengthening reduction dealkalization |
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