CN114480882B - Method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite - Google Patents
Method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite Download PDFInfo
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Abstract
The application provides a method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite, which comprises the following steps: s1, extracting vanadium: concentrating the vanadium titano-magnetite to obtain vanadium titano-magnetite concentrate and titanium concentrate; carrying out wet vanadium extraction on the vanadium-titanium magnetite concentrate to obtain a leaching material; s2, smelting reduction: the immersed material is put into a smelting reduction furnace for reduction smelting, and molten slag is obtained; s3, smelting titanium slag: combining titanium concentrate or melt slag with the titanium concentrate, and carrying out reduction smelting in a titanium slag furnace to obtain titanium slag; s4, alkali fusion: taking titanium slag or melt-separated slag or combining the titanium slag and the melt-separated slag, and performing alkali fusion treatment for 0.5-2 h at 450-750 ℃; s5, soaking in water; s6, acid leaching to obtain titanium-rich slag. According to the application, vanadium titano-magnetite is firstly separated into vanadium titano-magnetite concentrate and titanium concentrate through mineral separation, and the vanadium titano-magnetite concentrate and the titanium concentrate are treated respectively, so that the efficient utilization of titanium is realized.
Description
Technical Field
The application belongs to the technical field of titanium dioxide preparation, and particularly relates to a method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite.
Background
China has rich titanium resources, but the grade of the titanium-containing minerals in China is lower, the content of impurities such as calcium and magnesium is high, and the utilization rate is low. At present, about 90% of the titanium resources in China are assigned to the Panzhihua area in the form of vanadium titanomagnetite, wherein Panzhihua vanadium titanomagnetite belongs to complex multi-metal rock ore, and has complex mineral composition and assignment state, compact structure and difficult grinding and selection. The vanadium titano-magnetite is beneficiated, about 46 percent of titanium enters tailings, and the rest of titanium enters slag in the iron-making process to form largeAmount of titanium-containing slag (TiO) 2 The content reaches 25 percent), and the process for further removing impurities and enriching titanium is complex because the content of impurities in the titanium-containing slag is higher, the titanium in the titanium-containing slag can not be recovered basically, and the titanium-containing slag can not be utilized effectively, so that a great amount of titanium resources are wasted. Therefore, the method has important strategic significance in fully utilizing the iron resources and simultaneously effectively utilizing the titanium and vanadium resources.
At present, the titanium-containing slag in China is mainly divided into three categories: titanium-containing blast furnace slag, electric furnace titanium slag and molten titanium slag. Wherein, the titanium content in the titanium-containing blast furnace slag obtained by iron-making is lower, about 20-29%, and the utilization difficulty is higher because the mineral composition and the mineral phase structure are complex; the titanium content of the electric furnace titanium slag obtained after the electric furnace smelting of the titanium concentrate is generally above 75%, and the electric furnace titanium slag is a main raw material for preparing titanium white; the molten titanium slag is a titanium-containing slag obtained by directly reducing vanadium titanomagnetite to extract iron and then smelting and separating the iron by an electric furnace, and the titanium content of the titanium-containing slag is about 10-40%. At present, the utilization direction of the melted titanium slag is mainly to prepare the sulfuric acid process titanium white, the product value is low, the cost is high, and secondary pollution to the environment is easy to cause.
In order to fully utilize titanium resources in vanadium titano-magnetite, the blast furnace slag and the melted titanium slag with lower titanium grade are required to be subjected to impurity removal treatment again to enrich titanium, and the existing clean production process is less, for example, the treatment method of the blast furnace slag mainly comprises the following steps: acid leaching, high temperature carbonization, high temperature selective crystallization separation and alkaline process.
Patent document CN201711241777.7 discloses a method for extracting titanium from titanium-containing blast furnace slag by vacuum reduced pressure carbonization reduction. The method in the document needs to uniformly mix titanium-containing blast furnace slag, coke powder and coal dust, pelletize and dry to obtain partial reaction materials, and also needs to carry out vacuum decompression carbonization reduction metallurgical reaction in a vacuum reduction reaction device, and then cool, crush, ball mill and magnetic separator reaction products to obtain titanium carbide concentrate products. The method adopts vacuum decompression carbonization reduction reaction to extract titanium from the titanium-containing blast furnace slag, the titanium recovery rate reaches 55-85%, the waste of titanium resources of the titanium-containing blast furnace slag is greatly reduced, but the method has high equipment requirement, high reaction temperature and higher cost.
In order to fully utilize the titanium resources in vanadium titano-magnetite, a cleaner and more environment-friendly process is needed to be searched for effectively utilizing the titanium in the titanium-containing slag.
Disclosure of Invention
The application aims to provide a method for fully utilizing ferrotitanium and vanadium resources in vanadium-titanium magnetite to solve the defects in the prior art.
A method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite comprises the following steps:
s1, extracting vanadium: concentrating the vanadium titano-magnetite to obtain vanadium titano-magnetite concentrate and titanium concentrate; carrying out wet vanadium extraction on the vanadium-titanium magnetite concentrate, and carrying out solid-liquid separation to obtain a leaching material;
s2, smelting reduction: mixing the leaching material with a reducing agent in a smelting reduction furnace for reduction smelting to obtain semisteel and molten slag; detecting the titanium content of the melt slag, if the titanium content in the melt slag is more than 35%, carrying out a step S3 on the melt slag and the titanium concentrate together, and if the titanium content in the melt slag is less than or equal to 35%, directly carrying out a step S4 on the melt slag;
s3, smelting titanium slag: mixing the titanium concentrate or the melt slag with the titanium concentrate, and mixing with a reducing agent to perform reduction smelting in a titanium slag furnace to obtain semisteel and titanium slag, and if the grade of the obtained titanium slag is less than 75%, continuing to perform step S4;
s4, alkali fusion: taking the titanium slag, or the molten slag, or the combination of the titanium slag and the molten slag, adding alkali metal hydroxide and water, and performing alkali fusion treatment for 0.5-2 h at 450-750 ℃; wherein the mass ratio of the alkaline slag is (0.6-1.3) 1, and the addition amount of the water is 7-15% of the mass of the slag to obtain alkaline slag;
s5, soaking in water: soaking the alkali slag in water at 20-60 ℃ to obtain water soaked slag;
s6, acid leaching: and mixing the water leaching slag with acid, and performing acid leaching treatment to obtain titanium-rich slag.
Preferably, the wet vanadium extraction in the step S1 adopts powdery vanadium-titanium magnetite concentrate, static leaching is carried out at normal temperature, leaching solution is 0.3-1.5 mol/L dilute acid, and leaching time is 7-30 d.
Preferably, in the step S2, the reduction smelting raw material is powdery vanadium-titanium magnetite concentrate, the reducing agent is pulverized coal, and an auxiliary material is additionally added, wherein the auxiliary material is dolomite or lime, the mass ratio of the vanadium-titanium magnetite concentrate, the pulverized coal and the auxiliary material is (10-15): (3-5): (0.3-1.0), the reduction smelting reaction temperature is 1200-1600 ℃, and the reaction time is 4-13 h.
Preferably, if the grade of the titanium slag obtained in the step S3 is more than or equal to 75%, the titanium slag is used as a raw material for producing titanium dioxide by a sulfuric acid method or a raw material by a molten salt chlorination method.
Preferably, the reducing smelting reducing agent in the step S3 is one or more of anthracite, metallurgical coke and petroleum coke, and the reducing temperature is 1600-2000 ℃.
Preferably, the alkali metal hydroxide in step S4 is sodium hydroxide and/or potassium hydroxide.
Preferably, in the step S5, the alkali-soluble residue is firstly ground and sieved through a 150-250 mesh sieve, and then the water leaching treatment is carried out.
Preferably, after the water leaching treatment in the step S5, the water leaching treatment is washed to be neutral by water, and the water leaching residue is obtained by filtering.
Preferably, in the step S6, acid and alkali are subjected to a pressurizing or normal-pressure acid leaching method;
the pressure of the pressurized acid leaching is 0.3-0.5 MPa, and the stirring is carried out under the stirring condition, the stirring speed is 500-800 r/min, the temperature of the pressurized acid leaching is 120-140 ℃, and the time is 3-5 h;
the normal pressure acid leaching step comprises the following steps: reflux reaction is carried out for 5 to 10 hours at the temperature of 100 to 110 ℃;
the leaching acid liquid is hydrochloric acid solution with the concentration of 0.6-1.2 mol/L or sulfuric acid solution with the concentration of 0.6-1.5 mol/L, and the liquid-solid ratio is 40-70:1, ml/g.
Preferably, the titanium-rich slag obtained in the step S6 is used as a raw material for producing titanium dioxide by a molten salt chlorination method.
According to the method for fully utilizing titanium resources in the vanadium titano-magnetite, firstly, the vanadium titano-magnetite is subjected to mineral separation and separated into vanadium titano-magnetite concentrateAnd titanium concentrate, and respectively treating the titanium concentrate and the titanium concentrate; carrying out reduction smelting on iron concentrate in advance, and separating slag iron obtained by smelting to obtain low-grade titanium-containing smelting slag; detecting the titanium content in the molten slag, and when the titanium content in the molten slag is higher, carrying out reduction smelting on the molten slag and the titanium concentrate in a titanium slag furnace together to obtain higher-grade titanium slag; when the titanium content in the molten slag is low, directly carrying out high-temperature alkali fusion to obtain alkali slag; the titanium content in the obtained higher-grade titanium slag is also detected, when the titanium content is higher, the titanium slag is directly used for sulfuric acid method titanium white raw material or molten salt chlorination raw material, subsequent alkali melting, acid leaching and other treatments are not carried out, when the obtained higher-grade titanium slag is lower, high-temperature alkali melting is carried out, and the alkali slag is subjected to water leaching, water washing, acid leaching hydrolysis and other procedures to remove impurities to obtain TiO 2 Enriching the product, the TiO can be 2 The enriched product is used for fused salt chlorination, thereby realizing the high-efficiency utilization of titanium.
Compared with the prior art, the application has the advantages that:
(1) In the prior art, the vanadium removal process is generally carried out after crude titanium tetrachloride is prepared, and the vanadium-titanium magnetite concentrate is smelted after vanadium removal, so that the smelting and subsequent impurity removal effects can be improved, and the titanium grade in the titanium-rich material can be improved;
(2) According to the application, the smelting reduction furnace (SRV furnace) is utilized to carry out smelting reduction smelting on the vanadium-titanium magnetite concentrate, the advantage of strong adaptability to raw materials is utilized by using the HIsmolt smelting reduction technology, the powdery iron concentrate can be directly used, the pelletization is not needed, and the cost is saved; in addition, coke can be not used, pulverized coal can be directly used, the flow is short, and the emission of harmful substances is low;
(3) The application combines HIsmolt smelting reduction technology (SRV furnace), titanium slag smelting technology (titanium slag furnace) and alkali smelting technology, can fully exert the advantages of each technology, furthest recycle titanium, iron and vanadium resources, improve the energy utilization rate, ensure that the utilization rate of titanium reaches about 90 percent, ensure that the utilization rate of iron reaches about 90 percent and ensure that the utilization rate of vanadium reaches more than 60 percent, which cannot be realized by a single traditional technology;
(4) The melt slag produced by the SRV furnace contains part of TiO 2 (TiO 2 The content is 10-40 percent), and the titanium content in the melt slag is greatly changed, so that different treatment methods are respectively given to the melt slag according to the difference of the titanium content after the titanium content is detected for high-efficiency recycling of the titanium in the melt slag, specifically, when the titanium content in the melt slag is more than 35 percent, the melt slag and titanium concentrate can be jointly fed into a titanium slag furnace for smelting, so that the titanium in the melt slag is beneficial to extracting the titanium, if the high-grade titanium slag can be directly used for titanium white by a sulfuric acid method or a molten salt chlorination method, the subsequent alkali melting, acid leaching and other treatments are not needed, the resources are effectively saved, and if the titanium content in the melt slag is lower, the titanium slag smelting is carried out, so that the grade of the titanium slag is reduced, the economy is not realized, and the alkali melting impurity removal is directly carried out, so that the titanium in the low-grade melt slag is effectively utilized;
(5) According to the method, the obtained titanium slag is treated according to the grade of titanium, if the grade of titanium slag is higher, the titanium slag is directly used for titanium white by a sulfuric acid method or a molten salt chlorination method, so that complex impurity reduction treatments such as subsequent alkali melting and acid leaching are reduced, and if the grade of titanium slag is low, alkali melting treatment is carried out again, so that resources are effectively saved;
(6) The product obtained through the alkali fusion and acid leaching processes can be used for fused salt chlorination, the requirement of fused salt chlorination on the impurity content in the raw materials is low, the requirement on the titanium grade of the intermediate product can be reduced, the complex impurity removal procedure is not needed, the flow is simple, and the cost is saved.
Drawings
FIG. 1 is a process flow chart of the method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite.
Detailed Description
A method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite is shown in figure 1, and comprises the following steps:
s1, extracting vanadium: concentrating the vanadium titano-magnetite to obtain vanadium titano-magnetite concentrate and titanium concentrate; carrying out wet vanadium extraction on the vanadium-titanium magnetite concentrate, and separating to obtain leaching solution and leaching material, wherein the leaching solution can be used for the subsequent vanadium precipitation process after being collected, and the leaching material is dried at normal temperature or under heating;
s2, smelting reduction: mixing the vanadium-titanium magnetite concentrate subjected to vanadium extraction with a reducing agent in a smelting reduction furnace for reduction smelting to obtain semisteel and melt slag, wherein the semisteel can be used for steelmaking; and (3) detecting the titanium content of the molten slag, if the titanium content in the molten slag is more than 35%, carrying out the step (S3) on the molten slag and the titanium concentrate together, and if the titanium content in the molten slag is less than or equal to 35%, directly carrying out the step (S4) on the molten slag.
S3, smelting titanium slag: combining titanium concentrate or molten slag (titanium grade is more than 35%) with the titanium concentrate, mixing with a reducing agent, carrying out reduction smelting to obtain semisteel and titanium slag, wherein the semisteel can be used for steelmaking, if the grade of the obtained titanium slag is higher than 75%, the semisteel can be directly used for titanium white by a sulfuric acid method or a molten salt chlorination method, and if the grade of the titanium slag is lower than 75%, continuing to carry out step S4;
s4, alkali fusion: taking titanium slag (the titanium content is less than 75%), or melting slag (the titanium grade is less than or equal to 35%), or combining the titanium slag and the melting slag (the titanium content of the titanium slag is less than 75% and the titanium grade of the melting slag is less than or equal to 35%), adding alkali metal hydroxide and water, and performing alkali melting treatment for 0.5-2 h at 450-750 ℃; wherein the mass ratio of the alkaline slag is (0.6-1.3) 1, and the addition amount of water is 7-15% of the mass of the slag to obtain alkaline slag; the added water can dissolve the alkali metal hydroxide and mix with the titanium slag and/or the melt slag more uniformly; the alkali metal hydroxide can be sodium hydroxide and/or potassium hydroxide with stronger activity;
s5, soaking in water: leaching the alkali slag at 20-60 ℃ to obtain leached slag;
s6, acid leaching: and mixing the water leaching slag with acid, and performing acid leaching treatment to obtain titanium-rich slag.
The application firstly carries out ore dressing on vanadium titano-magnetite, separates the vanadium titano-magnetite into vanadium titano-magnetite concentrate and titanium concentrate, respectively processes the vanadium titano-magnetite concentrate and the vanadium titano-magnetite concentrate, firstly carries out wet vanadium extraction on the vanadium titano-magnetite concentrate, then adopts a HIsmolt smelting reduction technology (SRV furnace) to carry out reduction smelting on the vanadium titano-magnetite concentrate with complex components and lower titanium content, has strong adaptability to raw materials, can directly use pulverized coal without coke, has short flow, less emission of harmful substances, can directly use powdery iron concentrate without pelletizing,the cost is saved, and the molten slag generated after the iron concentrate passes through the SRV furnace contains part of TiO 2 (TiO 2 The content is 10-40 percent); the method for reducing and smelting the titanium concentrate with high titanium content by adopting a titanium slag furnace, wherein the titanium slag furnace is common equipment for producing titanium slag, and can be directly used for titanium white by a sulfuric acid method or a molten salt chlorination method if high-grade titanium slag can be obtained; if the grade of the obtained titanium slag is not high, enriching titanium, and further enriching titanium by alkali fusion treatment; because the titanium content in the molten slag is greatly changed according to the raw material components, in order to fully and efficiently utilize the titanium in the molten slag, the method firstly detects the titanium content in the molten slag, if the titanium content is more than 35 percent, the molten slag and the titanium concentrate are jointly introduced into a titanium slag furnace for smelting, thereby being beneficial to obtaining higher titanium slag grade, facilitating the further titanium enrichment treatment, and particularly when the titanium slag grade is more than or equal to 75 percent, the method can be directly used for titanium white by a sulfuric acid method or a molten salt chlorination method, if the obtained titanium slag grade is less than or equal to 35 percent, the obtained titanium slag is jointly smelted with the titanium concentrate, the obtained titanium slag grade is seriously influenced, the low-grade titanium slag cannot be used as a titanium white raw material by a sulfuric acid method or a molten salt chlorination method, therefore, the method directly carries out alkali smelting, and then carries out water leaching, and the titanium content in water leaching slag obtained after water leaching is more than 40 percent. And leaching the water leaching slag to obtain the titanium-rich slag with the titanium content of more than 75%.
The alkali metal oxide is exemplified by sodium hydroxide, the melting point of NaOH is 318 ℃, and when the reaction temperature is above 350 ℃, the alkali melting process can be regarded as a liquid-solid reaction between molten state NaOH and titanium slag or molten slag. NaOH is used as an ionized high-temperature solvent, has lower vapor pressure and viscosity, thus having good dissolving capacity for titanium slag or melt slag and being capable of effectively converting each phase in the titanium slag or melt slag into corresponding sodium salt thereof. In the smelting process, due to the addition of the reducing agent, part of tetravalent titanium is reduced to trivalent and sintered into a phase of black titanium stone under the high temperature condition, and the molecular formula is Ti 3 O 5 . The titanium slag or the melt slag mainly comprises TiO 2 、Ti 2 O 3 、FeO、Fe 2 O 3 、A1 2 O 3 、SiO 2 MgO, caO, mnO, etc., wherein Fe 2 O 3 MgO, caO and the like do not react with sodium hydroxide fused salt chemically, and are inert in the fused salt decomposition process. Therefore, the reaction system involved in the process of decomposing the sodium hydroxide molten salt of the titanium slag or the molten slag is as follows: naOH-TiO 2 ，NaOH-Ti 2 O 3 ，NaOH-(Fe,Mn)O， NaOH-A1 2 O 3 ，NaOH-SiO 2 And the like, respectively reacting with sodium hydroxide fused salt to generate corresponding sodium salt. The specific reaction equation is as follows:
2Ti 3 O 5 +12NaOH+O 2 →6Na 2 TiO 3 +6H 2 O (1)
2MnO 2 +4NaOH+O 2 →2Na 2 MnO 4 +2H 2 O (2)
Al 2 O 3 +2NaOH→2NaAlO 2 +H 2 O (3)
SiO 2 +2NaOH→Na 2 SiO 3 +H 2 O (4)
2Cr 2 O 3 +8NaOH+3O 2 →4Na 2 CrO 4 +4H 2 O (5)
the alkali-soluble slag generated in the alkali-melting process can lead NaAlO to be immersed in water 2 And Na (Na) 2 SiO 3 The soluble sodium salt is dissolved in water, and then the water-insoluble sodium titanate and the water-soluble NaAlO can be washed by water for a plurality of times 2 And Na (Na) 2 SiO 3 Separating to obtain water leaching slag containing sodium titanate, and then carrying out acidolysis.
During the acid leaching process, most of the sodium titanate salt can be dissolved by the acid, and the dissolved titanium ions exist in the acid liquor in the form of coordination octahedra. During boiling, these coordinated octahedra re-crystallize to form TiO 2 ·H 2 O, at the same time, a small part of sodium titanate is directly formed into meta-titanic acid in the form of ion exchange, and TiO is further formed in the drying and calcining processes 2 。
Na 2 TiO 3 +4H + →Ti(OH) 2 2+ +2Na + +H 2 O (6)
Na 2 TiO 3 +2H + →H 2 TiO 3 +2Na + (8)
H 2 TiO 3 →TiO 2 +H 2 O (9)
Preferably, the wet vanadium extraction in the step S1 adopts powdery vanadium-titanium magnetite concentrate, static leaching is carried out at normal temperature, leaching solution is 0.3-1.5 mol/L dilute acid, and leaching time is 7-30 d; specifically, the dilute acid can be 0.3-1 mol/L hydrochloric acid solution and 0.5-1.5 mol/L sulfuric acid solution.
Preferably, the reduction smelting raw material in the step S2 is powdery vanadium-titanium magnetite concentrate, the reducing agent is coal dust, coke is not needed, the cost is saved, in addition, auxiliary materials are added, the auxiliary materials are dolomite or lime, the mass ratio of the vanadium-titanium magnetite concentrate, the coal dust and the auxiliary materials is (10-15): (3-5): (0.3-1.0), the reduction smelting reaction temperature is 1200-1600 ℃, and the reaction time is 4-13 h.
Preferably, the reducing smelting reducing agent in the step S3 is one or more of anthracite, metallurgical coke and petroleum coke, and the reducing temperature is 1600-2000 ℃; anthracite, metallurgical coke, petroleum coke and the like all adopt specifications of high fixed carbon (fixed carbon is more than 70%).
Preferably, in the step S5, the alkali-soluble slag is firstly ground, screened by a 150-250 mesh sieve, and then subjected to water leaching treatment so as to improve water leaching efficiency.
Preferably, after the water leaching treatment in the step S5, water is used for washing to be neutral, water leaching residues are obtained through filtration, and the influence of pH on acid leaching is reduced through water washing.
Preferably, step S6 adopts a pressurizing or normal pressure acid leaching method;
the pressure of the pressurized acid leaching is 0.3-0.5 MPa, and the stirring is carried out under the stirring condition, the stirring speed is 500-800 r/min, the temperature of the pressurized acid leaching is 120-140 ℃, and the time is 3-5 h;
the normal pressure acid leaching step comprises the following steps: reflux reaction is carried out for 5 to 10 hours at the temperature of 100 to 110 ℃;
the leaching solution is hydrochloric acid solution with the concentration of 0.6-1.2 mol/L or sulfuric acid solution with the concentration of 0.6-1.5 mol/L, and the liquid-solid ratio is 40-70:1, ml/g.
Preferably, the titanium-rich slag obtained in the step S6 is used for producing the raw material of titanium dioxide by a molten salt chlorination method, the requirement of the molten salt chlorination on the impurity content in the raw material is low, the requirement on the titanium grade of the intermediate product can be reduced, the complex impurity removal procedure is not needed, the flow is simple, and the cost is saved.
Example 1
The specific preparation steps of the titanium-rich material product obtained by the method for fully utilizing ferrotitanium and vanadium resources in the vanadium titano-magnetite are as follows:
s1, extracting vanadium: vanadium titano-magnetite (TiO) 2 :13.4 percent) to obtain vanadium-titanium magnetite concentrate (TiO) 2 : 10.5%) and titanium concentrate (TiO 2 : 45.3%); carrying out wet vanadium extraction on the iron ore concentrate, wherein the leaching solution is 0.4mol/L hydrochloric acid solution (liquid-solid ratio is 3:1), the leaching time is 15 days, the leaching rate of vanadium is 59%, the vanadium-containing leaching solution is collected and then used for the subsequent vanadium precipitation process, and the leached material is dried at normal temperature;
s2, smelting reduction: mixing the iron ore concentrate subjected to vanadium extraction with a reducing agent in a smelting reduction furnace for reduction smelting, wherein the raw material is powdery iron ore concentrate (70-80% of mesh number-200), the reducing agent is coal dust, and the auxiliary material is lime; the mass ratio of the iron concentrate to the pulverized coal to the auxiliary materials is 11:3:0.4, the reaction temperature is 1400 ℃, the reaction time is 10 hours, semisteel and melt slag (34.5%) are obtained, and the semisteel is used for steelmaking; the titanium content in the molten slag is lower than 35%, so that the molten slag is directly subjected to alkali fusion;
s3, smelting titanium slag: mixing titanium concentrate with a reducing agent, performing reduction smelting, wherein the reducing agent is anthracite, the reduction temperature is 2000 ℃, and semisteel and titanium slag are obtained, the semisteel is used for steelmaking, and the titanium slag TiO 2 The grade is 62%;
s4, alkali fusion: mixing the molten slag obtained after crushing the S2 and the titanium slag obtained after crushing the S3, wherein the mass ratio of the molten slag to the titanium slag is 3:2, adding sodium hydroxide and water into the mixture, and performing alkali fusion treatment for 1h at 510 ℃, wherein the mass ratio of the alkali slag is 0.7:1, the addition amount of the water is 10% of the mass of the slag, and obtaining alkali slag through alkali fusion;
s5, soaking in water: grinding S4 alkali-soluble slagSieving with 200 mesh sieve, soaking undersize alkali slag in water at 45deg.C for 4 hr (liquid-solid ratio of 5:1), washing with water to neutrality, filtering, and oven drying to obtain water-soaked slag (TiO) 2 ：42.6％)；
S6, acid leaching: mixing the water leaching slag with dilute acid, carrying out acid leaching reaction in a pressurized reaction kettle for 5 hours at the pressure of 0.35MPa and the acid leaching temperature of 130 ℃ for 3.5 hours, stirring at the speed of 600r/min, wherein the dilute acid is 0.9mol/L hydrochloric acid solution, and the liquid-solid ratio is 45:1, ml/g, so as to finally obtain titanium-rich slag (TiO 2 : 85.9%) and can be used in molten salt chlorination process.
Example 2
The specific preparation steps of the titanium-rich material product obtained by the method for fully utilizing the ferrotitanium vanadium resources in the vanadium titano-magnetite by the method are as follows:
s1, extracting vanadium: vanadium titano-magnetite (TiO) 2 :13.4 percent) to obtain vanadium-titanium magnetite concentrate (TiO) 2 : 10.5%) and titanium concentrate (TiO 2 : 45.3%); carrying out wet vanadium extraction on the iron concentrate, wherein the leaching solution is 0.5mol/L hydrochloric acid solution, the leaching time is 12 days, the leaching rate of vanadium is 65%, the vanadium-containing leaching solution is collected and then used for the subsequent vanadium precipitation process, and the leached material is dried at normal temperature;
s2, smelting reduction: mixing the iron concentrate subjected to vanadium extraction with a reducing agent in a smelting reduction furnace for reduction smelting, wherein the raw material is powdery iron concentrate, the reducing agent is pulverized coal, the auxiliary material is dolomite, the mass ratio of the iron concentrate to the pulverized coal to the auxiliary material is 13:4:0.6, the reaction temperature is 1400 ℃, the reaction time is 8 hours, and semisteel and molten slag (38.6%) are obtained, wherein the semisteel is used for steelmaking; the titanium content in the molten slag is more than 35%, so that the molten slag is sent into a titanium slag furnace for titanium slag smelting;
s3, smelting titanium slag: and mixing part of the melt slag, the titanium concentrate and a reducing agent, and carrying out reduction smelting, wherein the reducing agent is anthracite, and the reduction temperature is 1800 ℃. Obtaining semisteel and titanium slag, wherein the semisteel is used for steelmaking, and the titanium slag is TiO 2 The grade is 58%;
s4, alkali fusion: adding sodium hydroxide and water into the titanium slag after crushing the S3, and performing alkali fusion treatment for 1.5 hours at 550 ℃; wherein the mass ratio of the alkaline slag is 1:1, the adding amount of water is 12% of the mass of the slag, and the alkaline slag is obtained through alkaline melting;
s5, soaking in water: grinding S4 alkali-soluble slag, sieving with 180 mesh sieve, soaking undersize alkali-soluble slag in water at 50deg.C for 3.5 hr, washing with water to neutrality, filtering, and oven drying to obtain water-soaked slag (TiO) 2 ：55.02％)；
S6, acid leaching: mixing the water leaching slag with dilute acid, reacting for 10 hours in a reflux device, wherein the dilute acid is hydrochloric acid solution with the mol/L of 1.0, the liquid-solid ratio is 50:1, and the ml/g, and finally obtaining titanium-rich slag (TiO 2 : 82.3%) and can be used in molten salt chlorination process.
Example 3
The specific preparation steps of the titanium-rich material product obtained by the method for fully utilizing the ferrotitanium vanadium resources in the vanadium titano-magnetite by the method are as follows:
s1, extracting vanadium: vanadium titano-magnetite (TiO) 2 :13.6 percent) to obtain vanadium-titanium magnetite concentrate (TiO) 2 : 9.8%) and titanium concentrate (TiO 2 : 45.9%); carrying out wet vanadium extraction on the iron concentrate, wherein the leaching solution is a sulfuric acid solution with the concentration of 1.1mol/L, the leaching time is 12 days, the leaching rate of vanadium is 70%, the vanadium-containing leaching solution is collected and then used for the subsequent vanadium precipitation process, and the leached material is dried at normal temperature;
s2, smelting reduction: mixing the iron concentrate subjected to vanadium extraction with a reducing agent in a smelting reduction furnace for reduction smelting, wherein the raw material is powdery iron concentrate, the reducing agent is pulverized coal, the auxiliary material is dolomite, the mass ratio of the iron concentrate to the pulverized coal to the auxiliary material is 13:4:0.5, the reaction temperature is 1400 ℃, the reaction time is 9 hours, and semisteel and molten slag (32.9%) are obtained, wherein semisteel is used for steelmaking; the titanium content in the molten slag is lower than 35%, so that the molten slag is directly subjected to alkali fusion;
s3, smelting titanium slag: mixing titanium concentrate and a reducing agent, and carrying out reduction smelting, wherein the reducing agent is anthracite, and the reduction temperature is 1800 ℃. Semi-steel and titanium slag are obtained, the semi-steel is used for steelmaking, and TiO is obtained 2 The grade is 76% titanium-containing slag, and the titanium slag can be directly used for sulfuric acid process titanium white;
s4, alkali fusion: taking molten slag crushed in the step S2, adding sodium hydroxide and water, and performing alkali fusion treatment for 2 hours at 600 ℃; wherein the mass ratio of the alkaline slag is 1.2:1, the adding amount of water is 13% of the mass of the slag, and the alkaline slag is obtained through alkaline melting;
s5, soaking in water: grinding and screening the S4 alkali-soluble slag, sieving with a 200-mesh sieve, soaking the undersize alkali-soluble slag in water at 55 ℃ for 4 hours, washing with water to be neutral, filtering and drying to obtain water-soaked slag (TiO) 2 ：40.7％)；
S6, acid leaching: mixing water leaching slag with dilute acid, carrying out acid leaching reaction in a pressurized reaction kettle for 6 hours, wherein the pressure is 0.4MPa, the stirring speed is 600r/min, the dilute acid is 0.95mol/L hydrochloric acid solution, and the liquid-solid ratio is 48:1 ml/g, and finally obtaining titanium-rich slag (TiO 2 : 87.8%) and can be used in molten salt chlorination process.
Example 4
The specific preparation steps of the titanium-rich material product obtained by the method for fully utilizing the ferrotitanium vanadium resources in the vanadium titano-magnetite by the method are as follows:
s1, extracting vanadium: (TiO) 2 :13.6 percent) to obtain vanadium-titanium magnetite concentrate (TiO) 2 : 9.8%) and titanium concentrate (TiO 2 : 45.9%); carrying out wet vanadium extraction on the iron concentrate, wherein the leaching solution is a sulfuric acid solution with the concentration of 1.0mol/L, the leaching time is 15 days, the leaching rate of vanadium is 67%, the vanadium-containing leaching solution is collected and then used for the subsequent vanadium precipitation process, and the leached material is dried at normal temperature;
s2, smelting reduction: mixing the iron ore concentrate subjected to vanadium extraction with a reducing agent in a smelting reduction furnace for reduction smelting, wherein the raw material is powdery iron ore concentrate, the reducing agent is pulverized coal, the auxiliary material is lime, the mass ratio of the iron ore concentrate to the pulverized coal to the auxiliary material is 12:3:0.5, and the reaction temperature is 1200 ℃ and the reaction time is 11h. Semi-steel and molten slag (25.5%) are obtained, and the semi-steel is used for steelmaking; s3, smelting titanium slag: mixing titanium concentrate and a reducing agent, and carrying out reduction smelting, wherein the reducing agent is anthracite, and the reduction temperature is 1600 ℃. Obtaining semisteel and titanium slag, wherein the semisteel is used for steelmaking, and the titanium slag is TiO 2 The grade was 68.6%.
S4, alkali fusion: mixing the molten slag after S2 crushing with the titanium slag after S3 crushing, wherein the mass ratio of the molten slag to the titanium slag is 3:7, adding sodium hydroxide and water into the mixture, and performing alkali fusion treatment for 2 hours at 580 ℃; wherein the mass ratio of the alkaline slag is 1.2:1, the adding amount of the water is 12% of the mass of the slag, and the alkaline slag is obtained through alkaline melting;
s5, soaking in water: grinding S4 alkali-soluble slag, sieving with 200 mesh sieve, soaking undersize alkali-soluble slag in water at 50deg.C for 4 hr, washing with water to neutrality, filtering, and oven drying to obtain water-soaked slag (TiO) 2 ：64.5％)；
S6, acid leaching: mixing the water leaching slag with dilute acid, carrying out acid leaching reaction in a pressurized reaction kettle for 5 hours under the pressure of 0.35MPa, stirring at the speed of 500r/min, and obtaining a sulfuric acid solution with the dilute acid of 1.2mol/L, wherein the liquid-solid ratio is 60:1, ml/g, so as to finally obtain titanium-rich slag (TiO 2 : 79.6%) and can be used in molten salt chlorination process.
In order to compare with the conventional method for recovering titanium from the blast furnace slag, the leaching experiment is carried out by selecting the melt slag in S2 in examples 1-4, wherein the leaching conditions are pressurized or normal pressure leaching, and the leaching conditions are consistent with the leaching conditions in each example S6, and the TiO of the solid slag obtained after direct leaching 2 The contents of the titanium-rich slag TiO obtained in examples 1-4 are 51.9%, 40.6%, 65.2%, 53.3%, respectively 2 The contents are 85.9%, 82.3%, 87.8% and 79.6% respectively. The direct acid leaching method can not effectively recycle the titanium in the blast furnace slag or the molten slag, but the method can effectively recycle the titanium in the blast furnace slag and the molten slag, and the recycling rate of the titanium reaches 90 percent.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application. It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. A method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite is characterized by comprising the following steps:
s1, extracting vanadium: concentrating the vanadium titano-magnetite to obtain vanadium titano-magnetite concentrate and titanium concentrate; carrying out wet vanadium extraction on the vanadium-titanium magnetite concentrate, and carrying out solid-liquid separation to obtain a leaching material; the wet vanadium extraction in the step S1 adopts powdery vanadium-titanium magnetite concentrate, static leaching is carried out at normal temperature, leaching liquor is 0.3-1.5 mol/L dilute acid, and leaching time is 7-30 d;
s2, smelting reduction: mixing the leaching material with a reducing agent in a smelting reduction furnace for reduction smelting to obtain semisteel and molten slag; detecting the titanium content of the melt slag, if the titanium content in the melt slag is more than 35%, carrying out a step S3 on the melt slag and the titanium concentrate together, and if the titanium content in the melt slag is less than or equal to 35%, directly carrying out a step S4 on the melt slag;
s3, smelting titanium slag: mixing the titanium concentrate or the melt slag with the titanium concentrate, and mixing with a reducing agent to perform reduction smelting in a titanium slag furnace to obtain semisteel and titanium slag, and if the grade of the obtained titanium slag is less than 75%, continuing to perform step S4; if the grade is more than or equal to 75%, the method is used for producing raw materials of titanium dioxide by a sulfuric acid method or raw materials by a molten salt chlorination method;
s4, alkali fusion: taking the titanium slag, or the molten slag, or the combination of the titanium slag and the molten slag, adding alkali metal hydroxide and water, and performing alkali fusion treatment for 0.5-2 h at 450-750 ℃; wherein the mass ratio of the alkaline slag is (0.6-1.3) 1, and the addition amount of the water is 7-15% of the mass of the slag to obtain alkaline slag;
s5, soaking in water: soaking the alkali slag in water at 20-60 ℃ to obtain water soaked slag;
s6, acid leaching: and mixing the water leaching slag with acid, and performing acid leaching treatment to obtain titanium-rich slag.
2. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
the reduction smelting raw material in the step S2 is powdery vanadium-titanium magnetite concentrate, the reducing agent is pulverized coal, and in addition, auxiliary materials are added, wherein the auxiliary materials are dolomite or lime, the mass ratio of the vanadium-titanium magnetite concentrate, the pulverized coal and the auxiliary materials is (10-15): (3-5): (0.3-1.0), the reduction smelting reaction temperature is 1200-1600 ℃ and the reaction time is 4-13 h.
3. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
and step S3, the reduction smelting reducing agent is one or more of anthracite, metallurgical coke and petroleum coke, and the reduction temperature is 1600-2000 ℃.
4. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
the alkali metal hydroxide in the step S4 is sodium hydroxide and/or potassium hydroxide.
5. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
and S5, grinding and screening the alkali-soluble residues, screening the alkali-soluble residues through a 150-250 mesh screen, and carrying out water leaching treatment.
6. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
and (5) after the water leaching treatment, washing with water to be neutral, and filtering to obtain the water leaching slag.
7. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
step S6, acid leaching adopts a pressurizing or normal pressure acid leaching method;
the pressure of the pressurized acid leaching is 0.3-0.5 MPa, and the stirring is carried out under the stirring condition, the stirring speed is 500-800 r/min, the temperature of the pressurized acid leaching is 120-140 ℃, and the time is 3-5 h;
the normal pressure acid leaching step comprises the following steps: reflux reaction is carried out for 5 to 10 hours at the temperature of 100 to 110 ℃;
the leaching acid liquid is hydrochloric acid solution with the concentration of 0.6-1.2 mol/L or sulfuric acid solution with the concentration of 0.6-1.5 mol/L, and the liquid-solid ratio is 40-70:1, ml/g.
8. The method for fully utilizing ferrotitanium vanadium resources in vanadium titano-magnetite according to claim 1, which is characterized in that,
and (3) using the titanium-rich slag obtained in the step (S6) to produce raw materials for titanium dioxide by a molten salt chlorination method.
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