CN113736998B - Harmless treatment method for tailings of vanadium extraction by calcium method - Google Patents

Harmless treatment method for tailings of vanadium extraction by calcium method Download PDF

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CN113736998B
CN113736998B CN202111042019.9A CN202111042019A CN113736998B CN 113736998 B CN113736998 B CN 113736998B CN 202111042019 A CN202111042019 A CN 202111042019A CN 113736998 B CN113736998 B CN 113736998B
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vanadium
tailings
slag
calcium
vanadium extraction
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CN113736998A (en
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陈炼
陈均
梁新腾
戈文荪
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B11/00—Making pig-iron other than in blast furnaces
    • C21B11/10—Making pig-iron other than in blast furnaces in electric furnaces
    • 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
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
    • 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
    • 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
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for innocent treatment of tailings of vanadium extraction by a calcium method, which comprises the following steps: a certain amount of carbonaceous material is added into the tailings after the vanadium extraction by a calcium method, dehydration, desulfurization and reduction are carried out in a pushed slab kiln at 1500-1650 ℃, valuable elements such as vanadium, iron and the like in the slag are reduced by carbon, so that vanadium-containing iron blocks and slag are obtained, the iron blocks can be used for alloying molten steel, and the slag can be used for producing cement, thereby realizing the recycling and harmless treatment of the tailings after the vanadium extraction. The invention can effectively utilize valuable elements in the vanadium extraction tailings, effectively recycle vanadium, iron and other elements, realize the green utilization of industrial waste resources and is beneficial to the efficient utilization of the resources. The method is suitable for enterprises producing vanadium products by adopting the vanadium slag and adopting the calcium method vanadium extraction process, and solves the problem of recycling of tailings generated after vanadium products are produced by adopting the calcium method vanadium extraction process by using the vanadium slag in a vanadium product factory.

Description

Harmless treatment method for tailings of vanadium extraction by calcium method
Technical Field
The invention belongs to the technical field of vanadium-titanium technology, and particularly relates to a method for innocent treatment of tailings from vanadium extraction by a calcium method.
Background
Vanadium (V) is a transition metal element, and the chemical property of the metal vanadium is stable at normal temperature and active at high temperature. The valence electron structure of the vanadium atom is 3d 3 4s 2 Is a typical valence-changing element, five valence electrons can participate in the bond, with +2, +3, +4, and +5 valence states. The stable compounds of vanadium are different at different oxygen partial pressures and temperatures, and lowering the oxygen partial pressure to raise the temperature is beneficial to the stable existence of trivalent vanadium oxides. In addition to vanadium, there are also various non-stoichiometric oxides of the general formula V n O 2n-1 And (3) a group oxide represented by n.ltoreq.9. At V 2 O 4 And V 2 O 5 Between them, V is known to 3 O 5 、V 3 O 7 、V 4 O 7 、V 4 O 9 、V 5 O 9 、V 6 O 11 、V 6 O 13 And the like. Industrial vanadium oxides are mainly V 2 O 3 、VO 2 And V 2 O 5 Wherein V is 2 O 5 And is particularly important.
Vanadium has excellent strength, hardness and fatigue resistance, and is widely used in the fields of steel, chemical industry, aviation and the like. About 84% of vanadium is used for dissolution of steel as an alloying element into steel to form VC and VN, refine grains, inhibit the development of bainite and pearlite to increase the strength of martensite, thereby improving the hardness, strength, toughness and wear resistance of steel, and the product is mainly composed of vanadium iron and VN. Vanadium is used for the nonferrous alloy mainly used for structural materials represented by V-Al series alloy, such as excellent high-temperature aviation structural materials Ti-6Al-4V, ti-8Al-1V-Mo, ti-6Al-6V-2Sn and other alloys. Vanadium products used in the chemical industry mainly comprise V 2 O 5 、NH 4 VO 3 、V 2 O 3 、VOCl 3 VCl 4 And the like, as catalysts, colorants, electrode materials for large-capacity batteries. It is worth mentioning that the vanadium is used as the positive electrode material of lithium battery or developed into super capacitor and other energy storage devices due to the multivalent state of vanadium, and has the advantages of rapid charging, high specific energy, low cost and the like, and has a good application prospect. In addition, about 2% of vanadium products are also used in the fields of medicine, protective materials, film materials, etc. The prior researches show that the vanadium compound has the function of insulin-like, can promote the synthesis of hepatic glycogen and myoglycogen, inhibit the decomposition of the hepatic glycogen into glucose, promote the synthesis of fat and inhibit the decomposition of the fat. In summary, vanadium and vanadium products are widely used as additives to improve material properties or accelerate chemical reaction processes.
The existing industrial vanadium extraction process mainly comprises a process flow of blast furnace ironmaking, converter vanadium extraction and deep processing of vanadium slag to obtain vanadium products, and two processes of stone coal vanadium extraction. The vanadium extraction process of the vanadium slag comprises two processes of sodium treatment vanadium extraction and calcification vanadium extraction, wherein the calcification vanadium extraction process is to perform oxidation roasting on the vanadium slag and lime, the obtained clinker is treated by sulfuric acid to obtain vanadium-containing solution and tailings, and the obtained tailings contain a large amount of CaSO 4 The water content is also up to more than 30%, so the utilization difficulty is extremely high, the environmental protection risk is high, and the problem to be solved in the utilization of vanadium resources is always solvedOne of them.
Disclosure of Invention
In view of the above, the invention aims to provide a harmless treatment method for the tailings of the vanadium extraction by the calcium method, and the treatment method provided by the invention can enable the tailings of the vanadium extraction by the calcium method to be better utilized as resources.
The invention provides a method for innocent treatment of tailings of vanadium extraction by a calcium method, which comprises the following steps:
mixing the calcium-method vanadium extraction tailings and the carbonaceous material, and carrying out first heating treatment for dehydration and desulfurization to obtain dehydrated desulfurization tailings;
and (3) carrying out second heating treatment reduction on the dehydrated desulfurization tailings to obtain vanadium-containing molten iron and slag.
Preferably, the second temperature raising treatment reduction process further includes:
mixing the dehydrated desulfurization tailings with a reducing agent for reduction by a second heating treatment;
the reducing agent comprises: carbonaceous reducing agents and/or ferrosilicon.
Preferably, the components of the tailings of the vanadium extraction by the calcium method comprise:
4.4 to 5wt% of S;
8.5 to 10.4 weight percent of CaO;
1.1 to 1.4 weight percent MgO;
4.2 to 5.0wt% of MnO;
27.1 to 29.2wt% TFe;
11.1 to 12.8 weight percent of SiO 2 ；
9.7 to 10.5 weight percent of TiO 2 ；
1.7～2.2wt％V 2 O 5 ；
1.4 to 1.8wt% of Al 2 O 3 ；
1.02 to 1.09wt% of Cr 2 O 3 。
Preferably, the carbonaceous material is selected from one or more of coke breeze and anthracite coal.
Preferably, the mass of the carbonaceous material is 5-30% of the mass of the tailings of the vanadium extraction by a calcium method.
Preferably, the temperature of the first heating treatment is 1300-1500 ℃ and the treatment time is 30-180 min.
Preferably, the mass content of water in the dehydrated desulfurization tailings is less than 1%; the mass content of sulfur is less than 0.01 percent.
Preferably, the carbon reducing agent is selected from one or two of diced coke and anthracite.
Preferably, the mass of the reducing agent is 1-21% of the mass of the low-sulfur tailings.
Preferably, the temperature of the second heating treatment is 1500-1700 ℃, and the treatment time is 15-30 min.
The invention provides a harmless treatment method of vanadium extraction tailings by a calcium method, which comprises the steps of dewatering, desulfurizing and reducing the vanadium extraction tailings in a pushed slab kiln or a rotary kiln, desulfurizing the flue gas by adopting a flue gas desulfurization method, and reducing and recovering valuable elements such as vanadium, iron and the like in the slag by a carbonaceous reducing agent; and the obtained low-sulfur tailings are moved into an electric furnace, the tailings are melted through an electrode and reduced by adding a carbonaceous reducing agent, the obtained iron blocks or molten iron can be used for alloying molten steel, and slag can be used for producing cement, so that the recycling utilization of the vanadium extraction tailings is realized. The treatment method provided by the invention can effectively utilize valuable elements in the vanadium extraction tailings, effectively recycle vanadium, iron and other elements, realize the green utilization of industrial waste resources, facilitate the efficient utilization of resources, solve the harmless treatment of the tailings and create benefits.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other examples of modifications and alterations will be apparent to those skilled in the art based on the examples herein, and are intended to be within the scope of the invention. It should be understood that the embodiments of the present invention are only used for illustrating the technical effects of the present invention, and are not used for limiting the scope of the present invention. In the examples, the methods used are conventional methods unless otherwise specified.
The invention provides a method for innocent treatment of tailings of vanadium extraction by a calcium method, which comprises the following steps:
mixing the calcium-method vanadium extraction tailings and the carbonaceous material, and carrying out first heating treatment for dehydration and desulfurization to obtain dehydrated desulfurization tailings;
and (3) carrying out second heating treatment reduction on the dehydrated desulfurization tailings to obtain vanadium-containing molten iron and slag.
In the invention, the calcium-method vanadium extraction tailings are prepared by oxidizing and roasting vanadium slag and lime, and the obtained clinker is treated by sulfuric acid to obtain vanadium-containing solution and tailings, wherein the tailings are calcium-method vanadium extraction tailings and contain a large amount of CaSO 4 The moisture content is also up to 30%.
In the invention, the components of the calcium-method vanadium extraction tailings can comprise:
4.4 to 5wt% of S;
8.5 to 10.4 weight percent of CaO;
1.1 to 1.4 weight percent MgO;
4.2 to 5.0wt% of MnO;
27.1 to 29.2wt% TFe;
11.1 to 12.8 weight percent of SiO 2 ；
9.7 to 10.5 weight percent of TiO 2 ；
1.7～2.2wt％V 2 O 5 ；
1.4 to 1.8wt% of Al 2 O 3 ；
1.02 to 1.09wt% of Cr 2 O 3 。
In the present invention, the mass content of S is preferably 4.5 to 4.9%, more preferably 4.6 to 4.8%, and most preferably 4.7%; the mass content of CaO is preferably 9 to 10%, more preferably 9.3 to 9.7%, most preferably 9.5%; the mass content of MgO is preferably 1.2-1.3%; the mass content of the MnO is preferably 4.3 to 4.8%, more preferably 4.4 to 4.6%, and most preferably 4.5%; the TFe is preferably 27.5-29% by mass, more preferably 28-28.5% by mass, and is metallic iron and Fe 2 O 3 Iron oxides such as FeO, etc., namely 27.1 to 29.2 weight percent of Fe can be included in the tailings of the vanadium extraction by the calcium method 2 O 3 And 27.1 to 29.2wt% FeO; the SiO is 2 Preferably 11 mass percent.5 to 12.5%, more preferably 11.8 to 12.2%, most preferably 12%; the TiO 2 The mass content of (2) is preferably 9.8 to 10.2%, more preferably 10%; the V is 2 O 5 The mass content of (2) is preferably 1.8 to 2%, more preferably 1.9%; the Al is 2 O 3 The mass content of (2) is preferably 1.5 to 1.7%, more preferably 1.6%; the Cr 2 O 3 The mass content of (2) is preferably 1.03 to 1.08%, more preferably 1.04 to 1.07%, and most preferably 1.05 to 1.06%.
In the invention, the calcium-method vanadium extraction tailings preferably further comprise: and (3) water.
In the present invention, the water content is preferably 8 to 12% by mass, more preferably 9 to 11% by mass, and most preferably 10% by mass.
In the present invention, the carbonaceous material has a relatively high carbon content, and is preferably one or both of diced coke and anthracite.
In the present invention, the mass of the carbonaceous material is preferably 5 to 30%, more preferably 10 to 25%, and most preferably 15 to 20% of the mass of the tailings of the calcium vanadium extraction.
In the present invention, the mass of the carbonaceous material is preferably 5 to 25%, more preferably 10 to 20%, and most preferably 15% of the mass of the tailings of the calcium vanadium extraction.
In the invention, the mass of the carbonaceous material is preferably 10-20%, more preferably 12-18%, and most preferably 14-16% of the mass of the tailings of the calcium-process vanadium extraction.
In the present invention, the mass of the carbonaceous material is preferably 20 to 30%, more preferably 22 to 28%, and most preferably 24 to 26% of the mass of the tailings of the calcium vanadium extraction.
In the present invention, the first temperature raising treatment and the second temperature raising treatment are preferably performed in a pushed slab kiln; preferably, the mixed material is placed in a graphite crucible and placed in a pusher kiln for heating treatment.
In the present invention, the temperature of the first temperature raising treatment is preferably 1300 to 1500 ℃, more preferably 1350 to 1450 ℃, and most preferably 1400 ℃.
In the present invention, the temperature of the first temperature-raising treatment (dehydration and desulfurization) is preferably 1300 to 1450 ℃, more preferably 1350 to 1400 ℃, and most preferably 1360 to 1380 ℃.
In the present invention, the temperature of the first temperature-raising treatment is preferably 1400 to 1500 ℃, more preferably 1420 to 1480 ℃, and most preferably 1440 to 1460 ℃.
In the present invention, the time of the first temperature raising treatment is preferably 30 to 180 minutes, more preferably 50 to 160 minutes, still more preferably 70 to 140 minutes, still more preferably 90 to 120 minutes, and most preferably 100 to 110 minutes.
In the present invention, the first temperature-raising treatment time is preferably 30 to 60 minutes, more preferably 40 to 50 minutes, and most preferably 45 minutes.
In the present invention, the time of the first temperature-raising treatment (dehydration and desulfurization) is preferably 30 to 120 minutes, more preferably 50 to 100 minutes, and most preferably 60 to 80 minutes.
In the present invention, the time of the first temperature-raising treatment (dehydration and desulfurization) is preferably 60 to 180 minutes, more preferably 80 to 160 minutes, still more preferably 100 to 140 minutes, and most preferably 120 minutes.
In the invention, the first temperature rising treatment is preferably to raise the temperature of the first 1/3 section of the pushed slab kiln to 1400-1500 ℃ for dehydration and desulfurization, and the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln is controlled to be 30-60 min.
In the invention, the mass content of water in the dehydrated desulfurization tailings is preferably less than 1%; the mass content of sulfur is preferably <0.01%.
In the present invention, the preparation method of the low sulfur tailings preferably comprises:
placing the calcium-method vanadium extraction tailings into a rotary kiln, adding carbonaceous materials with higher carbon content such as diced coke or anthracite, and the like, wherein the carbonaceous materials account for 5-25% of the weight of the calcium-method vanadium extraction tailings, raising the temperature in the rotary kiln to 1300-1450 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the rotary kiln to 30-120 min, so as to ensure that the moisture content in the low-sulfur tailings is less than 1% and the sulfur content is less than 0.01%.
In the present invention, the preparation method of the low sulfur tailings preferably comprises:
placing the calcium-method vanadium extraction tailings into a pushed slab kiln, adding carbonaceous materials with higher carbon content such as diced coke or anthracite, and the like, wherein the carbonaceous materials account for 10-20% of the weight of the calcium-method vanadium extraction tailings, raising the temperature in the pushed slab kiln to 1400-1500 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the pushed slab kiln to be 60-180 min, so that the moisture content of the low-sulfur tailings is less than 1wt% and the sulfur content of the low-sulfur tailings is less than 0.01wt%.
In the invention, the flue gas generated in the dehydration and desulfurization process is preferably subjected to desulfurization treatment by adopting a flue gas desulfurization method, and the obtained gypsum is preferably used for cement production.
In the present invention, the second temperature increasing treatment reduction process preferably further includes:
mixing the dehydrated desulfurization tailings with a reducing agent for reduction by a second heating treatment;
the reducing agent comprises: carbonaceous reducing agents and/or ferrosilicon.
In the present invention, the carbonaceous reducing agent is preferably a carbonaceous material having a relatively high carbon content, and more preferably one or both of the group consisting of coke breeze and anthracite.
In the present invention, the mass of the reducing agent (carbonaceous reducing agent) is preferably 1 to 21%, more preferably 5 to 20%, still more preferably 10 to 15%, and most preferably 12 to 13% of the mass of the low sulfur tailings.
In the present invention, the mass of the ferrosilicon is preferably 3 to 10%, more preferably 4 to 8%, still more preferably 5 to 7%, and most preferably 6% of the mass of the low-sulfur tailings.
In the present invention, the reduction is preferably performed in an electric furnace; the reduction is preferably carried out by melting the low sulfur tailings by means of electrodes and adding ferrosilicon.
In the invention, the reduction is to reduce and recycle valuable elements such as vanadium, iron and the like in the low-sulfur tailings; the vanadium-containing iron block with economic benefit is obtained by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like.
In the present invention, the temperature of the second temperature-raising treatment is preferably 1500 to 1700 ℃, more preferably 1550 to 1650 ℃, and most preferably 1600 ℃.
In the present invention, the temperature of the second temperature-raising treatment (reduction) is preferably 1500 to 1600 ℃, more preferably 1520 to 1580 ℃, and most preferably 1540 to 1560 ℃.
In the present invention, the temperature of the second temperature-increasing treatment is preferably 1500 to 1650 ℃, more preferably 1550 to 1600 ℃, and most preferably 1570 to 1580 ℃.
In the present invention, the time of the second temperature increasing treatment is preferably 15 to 30 minutes, more preferably 20 to 25 minutes.
In the invention, the second heating treatment is preferably to raise the temperature to 1500-1650 ℃ in the middle 1/6 section of the pushed slab kiln, the vanadium-containing molten iron with economic benefit is obtained by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like, the layering of the molten iron and slag is realized, and the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln is controlled to be 15-30 min.
In the present invention, the method of the second temperature increasing treatment (reduction) preferably includes:
transferring low-sulfur tailings obtained from the vanadium tailings obtained by extracting the vanadium from the calcium method after the treatment of the rotary kiln into an electric furnace through a slag pot, electrifying to melt the low-sulfur tailings, heating to 1500-1700 ℃, and adding carbonaceous materials with higher carbon content, such as diced coke or anthracite, and the like, wherein the carbonaceous materials account for 1-21% of the weight of the low-sulfur tailings; the vanadium-containing iron block with economic benefit is obtained by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like.
In the present invention, the method of the second temperature increasing treatment (reduction) preferably includes:
transferring low-sulfur tailings obtained by extracting vanadium tailings by a calcium method after being processed by a pushed slab kiln into an electric furnace through a slag pot, electrifying to melt the low-sulfur tailings, heating to 1500-1600 ℃, and adding ferrosilicon accounting for 3-10% of the weight of the low-sulfur tailings; the vanadium-containing iron block with economic benefit is obtained by utilizing the reduction effect of silicon on elements such as iron, vanadium and the like.
In the present invention, the second temperature increasing treatment (reduction) is preferably performed after the mass content of iron in the slag is less than 0.1% and the mass content of vanadium is less than 0.05%.
In the present invention, the method for obtaining vanadium-containing molten iron preferably further comprises:
and (5) cooling the vanadium-containing iron with water to obtain an iron block.
In the invention, the cooling method is preferably that the second half section of the pushed slab kiln is not heated, the temperature of the crucible is naturally cooled down, and slag-iron separation is carried out after the crucible is discharged from the pushed slab kiln, so that iron blocks and slag are obtained.
In the present invention, the iron nuggets are preferably used for steel-making alloying; the slag is preferably used in cement production.
In the invention, the vanadium-containing molten iron is preferably cast to obtain vanadium-containing iron blocks for molten steel alloying.
In the present invention, the slag is preferably used for cement production after water quenching.
In the invention, the tail gas generated by adopting the pushed slab kiln for heating treatment is preferably desulfurized in the whole process.
In the invention, the method for innocent treatment of the tailings of the vanadium extraction by the calcium method preferably comprises the following steps:
fully mixing the calcium-method vanadium extraction tailings and carbonaceous materials with higher carbon content such as diced coke or anthracite, and the like, wherein the carbonaceous materials are 20-30% of the weight of the calcium-method vanadium extraction tailings, placing the mixture into a graphite crucible and placing the graphite crucible into a pushed slab kiln, heating the first 1/3 section of the pushed slab kiln to 1400-1500 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln to 30-60 min so as to ensure that the moisture content in the tailings is less than 1% and the sulfur content is less than 0.01%;
raising the temperature to 1500-1650 ℃ in the middle 1/6 section of the pushed slab kiln, obtaining vanadium-containing molten iron with economic benefit by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like, realizing layering of the molten iron and slag, and controlling the treatment time of vanadium extraction tailings in the section of the pushed slab kiln to be 15-30 min;
the second half section of the pusher kiln is not heated, the temperature of the crucible is naturally cooled down, slag and iron separation is carried out after the crucible is discharged out of the pusher kiln, slag is used for cement production, and iron blocks are used for steelmaking alloying;
the tail gas obtained by the pushed slab kiln treatment is desulfurized in the whole process.
The treatment method provided by the invention can effectively utilize valuable elements in the vanadium extraction tailings, effectively recycle vanadium, iron and other elements, realize the green utilization of industrial waste resources, facilitate the efficient utilization of resources, solve the harmless treatment of the tailings and create benefits.
The components of the calcium-method vanadium extraction tailings adopted in the following examples of the invention comprise: 4.6wt% of S, 9.7wt% of CaO, 1.4wt% of MgO, 4.5wt% of MnO, 28.6wt% of TFe and SiO 2 12.1wt％、TiO 2 9.8wt％、V 2 O 5 2.0wt％、Al 2 O 3 1.6wt％、Cr 2 O 3 1.06wt％。
Example 1
Fully mixing the calcium-method vanadium extraction tailings and the diced coke accounting for 20% of the weight of the calcium-method vanadium extraction tailings, placing the mixture into a graphite crucible and placing the graphite crucible into a pushed slab kiln, raising the temperature of the first 1/3 section of the pushed slab kiln to 1400 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln to be 60min, so as to ensure that the moisture content in the tailings is less than 1% and the sulfur content in the tailings is less than 0.01%; raising the temperature to 1650 ℃ in the middle 1/6 section of the pushed slab kiln, obtaining vanadium-containing molten iron with economic benefit by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like, realizing layering of the molten iron and slag, and controlling the treatment time of vanadium extraction tailings in the section of the pushed slab kiln to be 30min; the second half of the pushed slab kiln is not heated, the crucible temperature is naturally cooled down, slag and iron separation is carried out after the crucible is discharged from the pushed slab kiln, slag is used for cement production, and iron blocks are used for steelmaking alloying. The tail gas obtained by the pushed slab kiln treatment is desulfurized in the whole process.
And detecting the contents of C and V in the iron block by adopting a direct-reading spectrometer, wherein the detection result shows that the mass content of C in the iron block is 5.21% and the mass content of V is 3.11%.
The vanadium yield in the slag is 90.9% (mineral detection method).
Example 2
Fully mixing the calcium-method vanadium extraction tailings and anthracite accounting for 30% of the weight of the calcium-method vanadium extraction tailings, placing the mixture into a graphite crucible and placing the graphite crucible into a pushed slab kiln, raising the temperature of the first 1/3 section of the pushed slab kiln to 1500 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln to be 30min so as to ensure that the moisture content in the tailings is less than 1% and the sulfur content in the tailings is less than 0.01%; raising the temperature to 1500 ℃ in the middle 1/6 section of the pushed slab kiln, obtaining vanadium-containing molten iron with economic benefit by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like, realizing layering of the molten iron and slag, and controlling the treatment time of vanadium extraction tailings in the section of the pushed slab kiln to be 15min; the second half of the pushed slab kiln is not heated, the crucible temperature is naturally cooled down, slag and iron separation is carried out after the crucible is discharged from the pushed slab kiln, slag is used for cement production, and iron blocks are used for steelmaking alloying. The tail gas obtained by the pushed slab kiln treatment is desulfurized in the whole process.
The mass contents of C and V in the iron nuggets obtained in example 2 of the present invention were examined in the same manner as in example 1, and as a result, the mass content of C in the iron nuggets was 5.18%, the mass content of V was 3.07%, and the vanadium yield in the slag was 88.4%.
Example 3
Fully mixing the calcium-method vanadium extraction tailings and carbonaceous materials with high coke content, wherein the coke content is 25% of the weight of the calcium-method vanadium extraction tailings, placing the mixture into a graphite crucible and placing the graphite crucible into a pusher kiln, raising the temperature of the first 1/3 section of the pusher kiln to 1450 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the section of the pusher kiln to 40min so as to ensure that the moisture content in the tailings is less than 1% and the sulfur content is less than 0.01%; raising the temperature to 1600 ℃ in the middle 1/6 section of the pushed slab kiln, obtaining vanadium-containing molten iron with economic benefit by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like, realizing the layering of the molten iron and slag, and controlling the treatment time of the vanadium extraction tailings in the section of the pushed slab kiln to be 20min; the second half of the pushed slab kiln is not heated, the crucible temperature is naturally cooled down, slag and iron separation is carried out after the crucible is discharged from the pushed slab kiln, slag is used for cement production, and iron blocks are used for steelmaking alloying. The tail gas obtained by the pushed slab kiln treatment is desulfurized in the whole process.
The mass contents of C and V in the iron nuggets obtained in example 3 of the present invention were examined in the same manner as in example 1, and as a result, the mass content of C in the iron nuggets was 4.93%, the mass content of V was 2.98%, and the vanadium yield in the slag was 88.1%.
Example 4
Putting the vanadium extraction tailings by a calcium method into a rotary kiln, adding diced coke accounting for 5% of the weight of the vanadium extraction tailings by the calcium method, increasing the temperature in the rotary kiln to 1450 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the rotary kiln to 120min, so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the rotary kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium-extracting tailings treated by the rotary kiln into an electric furnace through a slag pot, electrifying to melt the tailings, heating to 1700 ℃, adding coke butyl accounting for 21% of the weight of the tailings, and obtaining vanadium-containing iron blocks with economic benefits by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The composition of the vanadium-containing iron block obtained in example 4 of the present invention was examined in accordance with the method of example 1, and the examination result was: 4.23wt% of [ C ] and 3.10wt% of [ V ] in the vanadium-containing iron block, and the vanadium yield in the slag is 90.3%.
Example 5
Placing the vanadium extraction tailings by a calcium method into a rotary kiln, adding anthracite accounting for 25% of the weight of the vanadium extraction tailings by the calcium method, raising the temperature in the rotary kiln to 1300 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the rotary kiln to 30min so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content in the obtained low-sulfur tailings is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the rotary kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium extraction tailings treated by the rotary kiln into an electric furnace through a slag pot, electrifying to melt the low-sulfur tailings, heating to 1500 ℃, adding anthracite accounting for 1% of the weight of the low-sulfur tailings, and obtaining vanadium-containing iron blocks with economic benefits by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The vanadium-containing iron nuggets prepared in example 5 of the present invention were subjected to composition detection in accordance with the method of example 1, and as a result, the vanadium-containing iron nuggets were found to have [ C ] of 3.89wt% and [ V ] of 2.94wt%, and the vanadium yield in the slag was 87.2%.
Example 6
Putting the vanadium extraction tailings by a calcium method into a rotary kiln, adding diced coke accounting for 15% of the weight of the vanadium extraction tailings by the calcium method, raising the temperature in the rotary kiln to 1350 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the rotary kiln to be 100min, so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the rotary kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium extraction tailings treated by the rotary kiln into an electric furnace through a slag pot, electrifying to melt the low-sulfur tailings, heating to 1600 ℃, adding anthracite accounting for 11% of the weight of the low-sulfur tailings, and obtaining vanadium-containing iron blocks with economic benefits by utilizing the reduction effect of carbon on elements such as iron, vanadium and the like; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The vanadium-containing iron block prepared in example 6 of the present invention was subjected to component detection according to the method of example 1, and the detection results were that [ C ] was 4.33wt% and [ V ] was 2.87wt% in the vanadium-containing iron block, and the vanadium yield in the slag was 87.8%.
Example 7
Placing the vanadium extraction tailings by a calcium method into a pushed slab kiln, adding diced coke accounting for 10% of the weight of the vanadium extraction tailings by the calcium method, raising the temperature in the pushed slab kiln to 1500 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the pushed slab kiln to 180min so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the pushed slab kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium-extracting tailings treated by the pushed slab kiln into an electric furnace through a slag pot, electrifying to melt the tailings and heating to 1600 ℃, and adding 15% of ferrosilicon by weight of the tailings to reduce elements such as iron, vanadium and the like to obtain vanadium-containing iron blocks with economic benefits; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The composition of the vanadium-containing iron block obtained in example 7 of the present invention was examined in accordance with the method of example 1, and the examination result was: 3.23wt% of [ C ] and 3.04wt% of [ V ] in the vanadium-containing iron block, and the vanadium yield in the slag is 88.1%.
Example 8
Placing the vanadium extraction tailings by a calcium method into a pushed slab kiln, adding anthracite accounting for 20% of the weight of the vanadium extraction tailings by the calcium method, raising the temperature in the pushed slab kiln to 1400 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the pushed slab kiln to be 60min so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the pushed slab kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium-extracting tailings treated by the pushed slab kiln into an electric furnace through a slag pot, electrifying to melt the tailings, heating to 1500 ℃, and adding ferrosilicon accounting for 3% of the weight of the tailings to reduce elements such as iron, vanadium and the like to obtain vanadium-containing iron blocks with economic benefits; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The vanadium-containing iron nuggets prepared in example 8 of the present invention were subjected to composition detection in accordance with the method of example 1, and as a result, the vanadium-containing iron nuggets were found to have [ 4.08wt% of C ] and [ 3.14wt% of V ] and the vanadium yield in slag was found to be 89.6%.
Example 9
Placing the calcium-method vanadium extraction tailings into a pushed slab kiln, adding diced coke accounting for 15% of the weight of the calcium-method vanadium extraction tailings, increasing the temperature in the pushed slab kiln to 1450 ℃ for dehydration and desulfurization, and controlling the treatment time of the vanadium extraction tailings in the pushed slab kiln to be 100min, so as to ensure that the moisture content in the obtained low-sulfur tailings is less than 1wt% and the sulfur content in the obtained low-sulfur tailings is less than 0.01wt%; desulfurizing the flue gas by adopting a flue gas desulfurization method in the pushed slab kiln treatment process, wherein the obtained gypsum is used for cement production;
transferring the calcium-method vanadium extraction tailings treated by the pushed slab kiln into an electric furnace through a slag pot, electrifying to melt the tailings, heating to 1550 ℃, and adding ferrosilicon accounting for 8% of the weight of the tailings to reduce elements such as iron, vanadium and the like to obtain vanadium-containing iron blocks with economic benefits; in the electric furnace smelting process, when iron content in the obtained slag is less than 0.1wt% and vanadium content is less than 0.05wt%, stopping electrifying, discharging the obtained molten iron into a molten iron tank, and casting into blocks to obtain vanadium-containing iron blocks; the liquid slag is used for cement production after water quenching.
The vanadium-containing iron block prepared in example 9 of the present invention was subjected to component detection according to the method of example 1, and the detection results were that [ C ] was 3.93wt% and [ V ] was 2.91wt% in the vanadium-containing iron block, and the vanadium yield in the slag was 87.5%.
From the above examples, it is known that a certain amount of carbonaceous material is added into the tailings of vanadium extraction by the calcium method, dehydration, desulfurization and reduction are performed in a pushed slab kiln at 1500-1650 ℃, valuable elements such as vanadium, iron and the like in the slag are reduced by carbon, so as to obtain vanadium-containing iron blocks and slag, the iron blocks can be used for alloying molten steel, and the slag can be used for producing cement, thereby realizing the recycling and harmless treatment of the tailings of vanadium extraction. The invention can effectively utilize valuable elements in the vanadium extraction tailings, effectively recycle vanadium, iron and other elements, realize the green utilization of industrial waste resources and is beneficial to the efficient utilization of the resources. The method is suitable for enterprises producing vanadium products by adopting the vanadium slag and adopting the calcium method vanadium extraction process, and solves the problem of recycling of tailings generated after vanadium products are produced by adopting the calcium method vanadium extraction process by using the vanadium slag in a vanadium product factory.
The invention provides a method for recycling tailings generated in the vanadium extraction by a calcium method, which comprises the following steps: adding a certain amount of carbonaceous material into the tailings of vanadium extraction by a calcium method, dehydrating and desulfurizing in a rotary kiln at 1300-1450 ℃, desulfurizing the flue gas by adopting a flue gas desulfurization method, transferring the obtained low-sulfur tailings into an electric furnace, melting the tailings by an electrode, adding a carbonaceous reducing agent for reduction to obtain vanadium-containing iron blocks and slag, wherein the iron blocks can be used for molten steel alloying, and the slag can be used for cement production, so that the recycling utilization of the tailings of vanadium extraction is realized. The invention solves the problem of recycling the tailings generated after the vanadium product factory adopts the vanadium slag to produce the vanadium product by adopting the calcium method to extract the vanadium, and provides the recycling method of the tailings for extracting the vanadium by adopting the calcium method, which is suitable for enterprises which adopt the vanadium slag as a raw material to produce the vanadium product by adopting the calcium method vanadium extraction process.
The invention provides a method for recovering valuable resources of vanadium extraction tailings by a calcium method, which comprises the following steps: adding a certain amount of carbonaceous material into the tailings after vanadium extraction by a calcium method, dehydrating and desulfurizing in a pushed slab kiln at 1400-1500 ℃, desulfurizing the flue gas by adopting a flue gas desulfurization method, transferring the obtained low-sulfur tailings into an electric furnace, melting the tailings by an electrode, adding ferrosilicon to reduce valuable elements such as vanadium, iron and the like in the slag, and obtaining vanadium-containing iron blocks and slag, wherein the iron blocks can be used for alloying molten steel, and the slag can be used for cement production, so that the recycling utilization of the tailings after vanadium extraction is realized. The invention solves the problem of recycling the tailings generated after the vanadium product factory adopts the vanadium slag to produce the vanadium product by adopting the calcium method to extract the vanadium, and provides the recycling method of the tailings for extracting the vanadium by adopting the calcium method, which is suitable for enterprises which adopt the vanadium slag as a raw material to produce the vanadium product by adopting the calcium method vanadium extraction process.
While the invention has been described with respect to the preferred embodiments, it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be within the scope of the present invention.

Claims (7)

1. A method for innocent treatment of tailings of vanadium extraction by a calcium method comprises the following steps:
mixing the calcium-method vanadium extraction tailings and the carbonaceous material, and carrying out first heating treatment for dehydration and desulfurization to obtain dehydrated desulfurization tailings;
carrying out second heating treatment reduction on the dehydrated desulfurization tailings to obtain vanadium-containing molten iron and slag;
the second heating treatment reduction process further comprises the following steps:
mixing the dehydrated desulfurization tailings with a reducing agent for reduction by a second heating treatment;
the reducing agent comprises: carbonaceous reducing agents and/or ferrosilicon;
the temperature of the first heating treatment is 1300-1500 ℃ and the treatment time is 30-180 min;
the temperature of the second heating treatment is 1500-1700 ℃, and the treatment time is 15-30 min.
2. The method according to claim 1, wherein the components of the calcium-extracted vanadium tailings comprise:
4.4 to 5wt% of S;
8.5 to 10.4 weight percent of CaO;
1.1 to 1.4 weight percent MgO;
4.2 to 5.0wt% of MnO;
27.1 to 29.2wt% TFe;
11.1 to 12.8 weight percent of SiO 2 ；
9.7 to 10.5 weight percent of TiO 2 ；
1.7～2.2wt％V 2 O 5 ；
1.4 to 1.8wt% of Al 2 O 3 ；
1.02 to 1.09wt% of Cr 2 O 3 。
3. The method of claim 1, wherein the carbonaceous material is selected from one or both of pyrodine and anthracite.
4. The method according to claim 1, wherein the mass of the carbonaceous material is 5-30% of the mass of the tailings of the calcium-process vanadium extraction.
5. The method according to claim 1, characterized in that the mass content of water in the dewatered desulfurization tailings is < 1%; the mass content of sulfur is less than 0.01 percent.
6. The method of claim 1, wherein the carbon reductant is selected from one or both of pyro-butyl and anthracite.
7. The method according to claim 1, wherein the mass of the reducing agent is 1-21% of the mass of the low sulfur tailings.
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