CN110484673B - Process for comprehensively utilizing vanadium-titanium magnetite through prereduction, electric furnace deep reduction and sulfuric acid method - Google Patents
Process for comprehensively utilizing vanadium-titanium magnetite through prereduction, electric furnace deep reduction and sulfuric acid method Download PDFInfo
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- CN110484673B CN110484673B CN201910859496.0A CN201910859496A CN110484673B CN 110484673 B CN110484673 B CN 110484673B CN 201910859496 A CN201910859496 A CN 201910859496A CN 110484673 B CN110484673 B CN 110484673B
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Abstract
The invention discloses a process for comprehensively utilizing vanadium-titanium magnetite by a prereduction-electric furnace deep reduction-sulfuric acid method. The method comprises the steps of firstly pre-reducing low-silicon vanadium titano-magnetite oxidized pellets, feeding the obtained pre-reduced pellets into an electric furnace for deep reduction to obtain vanadium-containing pig iron and titanium-containing furnace slag, adding a calcium-magnesium-containing flux in the smelting process of the electric furnace for slag adjustment to ensure that the main titanium-containing phase of the furnace slag is a magnesium metatitanate phase, preparing titanium dioxide from the titanium-containing furnace slag by adopting a sulfuric acid method to recover titanium, extracting vanadium from the vanadium-containing molten iron by adopting a converter, and realizing the comprehensive utilization of iron, vanadium and titanium. Compared with a blast furnace method, the process provided by the invention can realize the smelting of all-vanadium-titanium ore, the produced titanium slag has high grade, the titanium resource can be recycled, the serious pollution processes such as sintering, coking, a blast furnace and the like are reduced, the process has great environmental protection advantages, the investment and production cost can be reduced, and the process has great economic advantages.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of schreyerite, and relates to a process for comprehensively utilizing schreyerite by a prereduction-electric furnace deep reduction-sulfuric acid method.
Background
The vanadium titano-magnetite resource reserves in China are huge, but the overall development and utilization degree is low, taking vanadium titano-magnetite resources in Panxi areas as an example, in a production process taking steel as a leading factor, the recovery and utilization rate of titanium and vanadium is not high at present, and the resource waste is serious, so that the comprehensive utilization level of the vanadium titano-magnetite resources in China is improved, and the method has important significance for the development of steel and vanadium titano-magnetite industries in China.
In the existing treatment method for vanadium-titanium magnetite concentrate, the smelting of all vanadium-titanium ore can be realized by a non-blast furnace method, the recovery rates of iron, vanadium and titanium are high, and in the blast furnace smelting, coke is used as a reducing agent and also used as a reducing agentThe fuel provides the temperature required by smelting, so that the reduction potential in the blast furnace is stronger. When the vanadium titano-magnetite is smelted, the coke area is always in a carbon excess state, titanium oxide in slag is easy to be over-reduced to generate titanium carbonitride and other high-melting-point substances, slag becomes sticky and thick, the fluidity is poor, the slag is difficult to be discharged, and the slag contains much iron and has high iron loss. In order to inhibit the reduction of titanium oxide in this region, the blast furnace method adopts the addition of ordinary ore to reduce TiO in the slag2In turn, reduce the content of TiO2The activity of the iron ore is reduced to achieve the aims of inhibiting titanium oxide from being over-reduced, reducing titanium carbonitride generation and ensuring slag-iron separation and smooth smelting, but the addition of the common iron ore reduces TiO in the blast furnace slag2Content, TiO in the produced blast furnace titanium-containing slag2Low content (TiO)2About 20-25% mass fraction) cannot be economically recycled, and only iron and vanadium can be recycled. Compared with the blast furnace method, the prereduction-electric furnace method has great advantages in the aspects of iron, vanadium and titanium recovery, production scale, environmental protection and the like.
The specific process of the pre-reduction-electric furnace method is as follows: the vanadium-titanium magnetite concentrate is pre-reduced, the pre-reduced product is smelted in an electric furnace, and the separation of iron, vanadium and titanium can be completed in the electric furnace. From the aspect of smelting process, when smelting is carried out by the pre-reduction-electric furnace method, the heating process is provided by electric energy conversion, the added coke is only used as a reducing agent, and the reduction potential is controllable, so that the control difficulty of the smelting process is reduced, the main reason for realizing the smelting of the all-vanadium-titanium ore is that the slag titanium is high in grade, and favorable conditions are created for recycling titanium.
The process of smelting vanadium-titanium magnetite by an electric furnace can be divided into two major types of electric furnace melting and separation processes and electric furnace deep reduction processes according to the trend of vanadium in smelting. The electric furnace melting and separating process is to melt and separate the pre-reduced vanadium-titanium magnetite concentrate in an electric furnace, enrich vanadium and titanium in a slag phase, and extract vanadium and titanium from the slag phase. The electric furnace deep reduction process is to carry out deep reduction on the pre-reduced vanadium-titanium magnetite concentrate product in an electric furnace, so that vanadium enters molten iron and titanium is enriched in a slag phase. The main problems of the electric furnace melting process are that the required raw material metallization rate is high, the subsequent vanadium and titanium extraction is difficult, the vanadium and titanium-containing slag treatment process is long, and the production energy consumption is high. For the electric furnace deep reduction process, the method has the advantages of being beneficial to recovering vanadium, having shorter treatment process after deep reduction than that of the electric furnace melting process, low production energy consumption and relatively small environmental pollution, and adopting the electric furnace to deep reduce and smelt the vanadium-titanium magnetite in south Africa and New Zealand abroad. On the other hand, the vanadium-titanium-containing slag obtained by melting and separating the electric furnace is far larger than the vanadium slag obtained in the deep reduction process of the electric furnace, the treatment capacity of the vanadium slag is more, the environment pollution is serious in the vanadium extraction process, the subsequent vanadium extraction technology of the deep reduction process of the electric furnace is mature, the material treatment capacity in the vanadium extraction process is relatively low, the environment pollution load is relatively small, the control of the environment pollution is facilitated, but the trend control of the iron vanadium-titanium in the deep reduction process of the electric furnace is relatively difficult, if the trend problem of the vanadium-titanium can be solved, the deep reduction process of the electric furnace is relatively ideal as the smelting process of.
The key to realizing the smooth separation of slag and iron in the smelting process is to inhibit the over-reduction of titanium oxide in the smelting process of the vanadium titano-magnetite, and to feed vanadium iron and titanium into slag. In China, the perovskite is adopted as a slagging main phase when enterprises such as steel blast furnace smelting vanadium titano-magnetite and foreign south Africa enterprises and new Zealand enterprises adopt electric furnaces to smelt the vanadium titano-magnetite. The acidolysis of the perovskite phase is poor, which is not beneficial to the subsequent recovery of titanium by a sulfuric acid method. And ordinary ore is added in the steel-climbing blast furnace smelting to obtain titanium-containing blast furnace slag TiO2The grade is lower than 25 percent, quartz is added in the electric furnace smelting of the New Zealand in south Africa, and the obtained TiO containing titanium slag2The grade is lower than 35 percent, and the titanium resource in the product can not be effectively recycled, thereby causing the waste of precious titanium resource. Therefore, the development of the electric furnace smelting technology which can realize the trend control of vanadium and titanium in the electric furnace smelting process of the vanadium-titanium magnetite and the recovery of titanium resources has important functions and can promote the industrialized application of comprehensive utilization of the vanadium-titanium magnetite by the prereduction-electric furnace method in China.
Disclosure of Invention
Aiming at the problems that reduction trend of titanium and vanadium oxides is difficult to control, slag and iron are difficult to separate, titanium resources are difficult to recover and the like in the vanadium titano-magnetite smelting process in the prior art, the invention aims to provide a process for comprehensively utilizing the vanadium titano-magnetite by a pre-reduction-electric furnace deep reduction-sulfuric acid method, and provide technical support for industrial application of comprehensively utilizing the vanadium titano-magnetite by the pre-reduction-electric furnace method.
The invention provides the following technical scheme: a process for comprehensively utilizing vanadium titano-magnetite by a prereduction-electric furnace deep reduction-sulfuric acid method. The method comprises the following steps:
(1) pre-reducing the vanadium titano-magnetite oxidized pellets to obtain vanadium titano-magnetite pre-reduced pellets;
(2) loading the vanadium titano-magnetite pre-reduced pellets, calcium-containing flux, magnesium-containing flux and reducing agent into an electric furnace for deep reduction smelting, and separating to obtain vanadium-containing pig iron and titanium-containing slag, wherein the main titanium-containing phase of the obtained titanium-containing slag is magnesium metatitanate phase;
the amount of the calcium-containing flux is 0.6-1.0 (CaO: SiO) according to the pre-prepared alkalinity2Mass ratio) is added, and the amount of the magnesium-containing melt is determined according to the raw materials of MgO and TiO2Adding the mixture according to a molar ratio of (1.1-0.8) to 1;
(3) the obtained vanadium-containing molten iron is used for extracting vanadium in a converter or semisteel and vanadium slag are separated by converter blowing, and titanium-containing slag is used for preparing titanium dioxide by adopting a sulfuric acid method.
Further, in the step (1), the process for pre-reducing the vanadium-titanium magnet is one of a shaft furnace, a rotary kiln and a fluidization method.
Further, in the step (1), the silicon content in the vanadium-titanium magnet is lower than 4%.
Further, in the step (1), the metallization rate of the vanadium-titanium magnet pre-reduced pellet is more than or equal to 70%.
Further, in step (2), the added calcium-containing flux includes, but is not limited to, lime, limestone, dolomite, quicklime, calcium oxide, calcium carbonate.
Further, in the step (2), the magnesium-containing flux added includes but is not limited to magnesia, dolomite, and magnesite.
Further, in the step (2), the smelting temperature of the electric furnace is 1550-1650 ℃, and the smelting time is 20-60 min.
The invention has the advantages that:
the pre-reduction-electric furnace method adopts the smelting of vanadium titano-magnetite, compared with the blast furnace method, the process provided by the invention can realize the smelting of full vanadium titano-magnetite, the produced titanium slag has high grade, the titanium resource can be recycled, and the sintering and smelting are reduced at the same timeThe method has the advantages of high environmental protection, low investment and production cost and high economic advantage. According to the invention, magnesium metatitanate (MgTiO3) is used as a main slagging phase, and the temperature of titanium carbide for thickening slag generated by reduction is high, so that the reduction of titanium is inhibited, and the difficulty of smelting operation is reduced; the magnesium metatitanate has good acidolysis performance, and is used as a main phase of titanium slag to be beneficial to the recovery of titanium by a subsequent sulfuric acid process. Because the low-valence vanadium oxide belongs to an alkaline oxide, the addition of a calcium-containing reagent properly improves the alkalinity of the slag, is favorable for promoting the reduction of vanadium into molten iron, and realizes the control of the trend of vanadium and titanium. The invention adopts low-silicon vanadium titano-magnetite as raw material, and compared with blast furnace method and south Africa and New Zealand electric furnace method, the obtained titaniferous slag has high grade (TiO)2>47 percent), the obtained titanium slag can be used for preparing titanium dioxide by adopting a sulfuric acid method, vanadium is extracted from vanadium-containing molten iron through a converter, and the comprehensive utilization of vanadium-titanium magnetite iron vanadium titanium can be realized. The aim of inhibiting the reduction of titanium and simultaneously ensuring the recycling of titanium resources is fulfilled. In the process of smelting vanadium-titanium magnetite by the electric furnace, the slag with low magnesium content is easy to corrode the magnesium-containing furnace lining, and the magnesium metatitanic acid is used as a slagging material phase, so that the magnesium content of the slag is high, the corrosion of the slag on the electric furnace lining can be reduced, the service life is prolonged, and the production cost is reduced.
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FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following examples further illustrate embodiments of the present invention, but the embodiments of the present invention are not limited to the following examples.
Example 1
A process for comprehensively utilizing vanadium titano-magnetite by a pre-reduction-electric furnace deep reduction-sulfuric acid method comprises the following steps:
(1) the vanadium titano-magnetite oxidized pellet is pre-reduced to obtain the vanadium titano-magnetite pre-reduced pellet which mainly comprises the following components: 71.37% for TFe, 64.56% for MFe, TiO2＝15.53％，SiO23.71 percent of vanadium-titanium magnetite pre-reduced pellets with the metallization rate of 90.45 percent;
(2) pre-reducing ball of vanadium titano-magnetitePutting the agglomerate, limestone, magnesium oxide and reducing agent into an electric furnace for deep reduction smelting, adding the MgO and the TiO into quick lime according to the pre-prepared alkalinity of 0.62The mol ratio is 1.1:1, the smelting temperature is 1650 ℃, the smelting time is 20min, and vanadium-containing pig iron and TiO are obtained by separation245.90% titanium-containing slag;
(3) the obtained vanadium-containing molten iron is used for extracting vanadium in a converter or semisteel and vanadium slag are separated by converter blowing, and titanium-containing slag is used for preparing titanium dioxide by adopting a sulfuric acid method.
Example 2
A process for comprehensively utilizing vanadium titano-magnetite by a pre-reduction-electric furnace deep reduction-sulfuric acid method comprises the following steps:
(1) the vanadium titano-magnetite oxidized pellet is pre-reduced to obtain the vanadium titano-magnetite pre-reduced pellet which mainly comprises the following components: 71.37% for TFe, 64.56% for MFe, TiO2＝15.53％，SiO23.71 percent of vanadium-titanium magnetite pre-reduced pellets with the metallization rate of 90.45 percent;
(2) pre-reducing pellets of vanadium titano-magnetite, limestone, dolomite and a reducing agent are loaded into an electric furnace for deep reduction smelting, and the MgO and the TiO are added according to the pre-prepared alkalinity of 0.7 to quicklime2The mol ratio is 1:1, the smelting temperature is 1600 ℃, the smelting time is 40min, and vanadium-containing pig iron and TiO are obtained by separation246.45% titanium-containing slag;
(3) the obtained vanadium-containing molten iron is used for extracting vanadium in a converter or semisteel and vanadium slag are separated by converter blowing, and titanium-containing slag is used for preparing titanium dioxide by adopting a sulfuric acid method.
Example 3
A process for comprehensively utilizing vanadium titano-magnetite by a pre-reduction-electric furnace deep reduction-sulfuric acid method comprises the following steps:
(1) the vanadium titano-magnetite oxidized pellet is pre-reduced to obtain the vanadium titano-magnetite pre-reduced pellet which mainly comprises the following components: 71.37% for TFe, 64.56% for MFe, TiO2＝15.53％，SiO23.71 percent of vanadium-titanium magnetite pre-reduced pellets with the metallization rate of 90.45 percent;
(2) the vanadium titano-magnetite pre-reduction pellets, limestone, magnesium oxide and a reducing agent are put into an electric furnace for deep reduction smelting, and quicklime is addedAdding MgO and TiO with the alkalinity of 0.8 according to the pre-prepared proportion2The mol ratio is 0.8:1, the smelting temperature is 1550 ℃, the smelting time is 60min, and vanadium-containing pig iron and TiO are obtained by separation248.15% titanium-containing slag;
(3) the obtained vanadium-containing molten iron is used for extracting vanadium in a converter or semisteel and vanadium slag are separated by converter blowing, and titanium-containing slag is used for preparing titanium dioxide by adopting a sulfuric acid method.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (7)
1. A process for comprehensively utilizing vanadium titano-magnetite by a pre-reduction-electric furnace deep reduction-sulfuric acid method is characterized by comprising the following steps:
(1) pre-reducing the vanadium titano-magnetite oxidized pellets to obtain vanadium titano-magnetite pre-reduced pellets;
(2) loading the vanadium titano-magnetite pre-reduced pellets, calcium-containing flux, magnesium-containing flux and reducing agent into an electric furnace for deep reduction smelting, and separating to obtain vanadium-containing pig iron and titanium-containing slag, wherein the main titanium-containing phase of the obtained titanium-containing slag is magnesium metatitanate phase;
the calcium-containing flux is added according to the pre-prepared alkalinity of 0.6-1.0, and the magnesium-containing flux is added according to the raw materials of MgO and TiO2Adding the mixture according to a molar ratio of (1.1-0.8) to 1;
(3) the obtained vanadium-containing molten iron is used for extracting vanadium in a converter or semisteel and vanadium slag are separated by converter blowing, and titanium-containing slag is used for preparing titanium dioxide by adopting a sulfuric acid method.
2. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (1), characterized in that: the process for pre-reducing the vanadium-titanium magnet is one of a shaft furnace, a rotary kiln and a fluidization method.
3. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (1), characterized in that: the silicon content in the vanadium-titanium magnet is lower than 4 percent.
4. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (1), characterized in that: the metallization rate of the vanadium-titanium magnet pre-reduced pellet is more than or equal to 70 percent.
5. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (2), characterized in that: the added calcium-containing flux includes, but is not limited to, lime, limestone, dolomite, quicklime, calcium oxide, calcium carbonate.
6. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (2), characterized in that: magnesium-containing fluxes added include, but are not limited to, magnesia, dolomite, magnesite.
7. The process for comprehensively utilizing vanadium titano-magnetite by the pre-reduction-electric furnace deep reduction-sulfuric acid method according to claim 1, in the step (2), characterized in that: the smelting temperature of the electric furnace is 1550-1650 ℃, and the smelting time is 20-60 min.
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