CN106566906B - Carbon thermal sodium salt reduction melting comprehensive recovery method of vanadium titano-magnetite iron ore concentrate - Google Patents
Carbon thermal sodium salt reduction melting comprehensive recovery method of vanadium titano-magnetite iron ore concentrate Download PDFInfo
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- CN106566906B CN106566906B CN201610999665.7A CN201610999665A CN106566906B CN 106566906 B CN106566906 B CN 106566906B CN 201610999665 A CN201610999665 A CN 201610999665A CN 106566906 B CN106566906 B CN 106566906B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0006—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state
- C21B13/0013—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state introduction of iron oxide into a bath of molten iron containing a carbon reductant
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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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
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- 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
Abstract
The invention relates to a carbon-thermal sodium salt reduction melting comprehensive recovery method of vanadium titano-magnetite iron ore concentrate. In order to synchronously recover the vanadium titano-magnetite iron concentrateThe iron, vanadium and titanium are treated by a carbon-thermal sodium reduction melting separation process, and the separation process of titanium and other components is researched by combining means such as high-pressure hydrolysis, ultrasonic oscillation, filtration and the like, so that the recovery condition of iron and titanium is discussed. The results show that the compounds are expressed as Na2CO3Is a sodiumizing agent and graphite powder as a carbonaceous reducing agent, the carbon-containing pellets react for 120min at 1250-1350 ℃, then slag and iron are separated, the yield of iron is higher than 90%, the content of titanium in molten iron is lower than 0.1%, the content of vanadium is 0.49-0.52%, and the yield of vanadium is higher than 80%. Carrying out high-pressure hydrolysis on the molten slag at 100-250 ℃, then carrying out ultrasonic oscillation and filter pressing to obtain a titanium-containing suspension, and finally calcining the crystallized and separated solid to obtain TiO2The content of the titanium-rich slag is 60 to 82 percent.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of metallurgical resources, in particular to a carbon-thermal sodium salt reduction melting comprehensive recovery method of vanadium-titanium magnetite iron ore concentrate.
Background
Titanium is an important strategic resource, and metal titanium and titanium alloy are widely applied to aerospace, industrial production and civil products. The Chinese titanium resource accounts for 40 percent of the world reserves, wherein more than 90 percent of the Chinese titanium resource is distributed in the Panxi area and exists in the form of vanadium titano-magnetite, and the reserve capacity is kept to be more than 100 hundred million tons. The vanadium titano-magnetite is a composite ore with various valuable elements such as iron, vanadium, titanium and the like, the reserves of natural rutile and ilmenite are low in China, and the vanadium titano-magnetite is a main source of titanium resources. About 50% of titanium in the vanadium-titanium magnetite is distributed in iron ore concentrate, at present, the vanadium-titanium magnetite ore concentrate mainly recovers iron and vanadium through a blast furnace process or a rotary kiln-electric furnace process, and titanium is not effectively utilized due to the limitation of grade and smelting economy, so that a great amount of titanium resource is lost. According to statistics, the quantity of the climbing steel titanium-containing blast furnace slag is close to 7000 ten thousand tons, and the increase amount is about 300 ten thousand tons every year. Therefore, the recovery efficiency of titanium in the vanadium titano-magnetite concentrate is extremely urgent.
The process for preparing the titanium white by the alkaline method greatly reduces the use and discharge amount of acid, is more environment-friendly compared with the traditional acid method, and mainly comprises the steps of converting titanium in high-titanium slag into sodium metatitanate by melting and roasting sodium hydroxide, obtaining metatitanic acid precipitate by a hydrolysis process, and removing water-soluble impurities such as Si, Al and the like to realize the preliminary separation of the titanium and the impurities; and removing impurities such as Fe, Ca, Mg and the like from the washing residues through acidolysis, and further improving the grade of titanium. Based on the principle, the research on the alkali method for melting and processing the titanium-containing blast furnace slag is developed in laboratories, and finally the titanium slag with higher purity is obtained. However, in the existing alkaline process, the iron is removed by acid, vanadium titano-magnetite iron concentrate cannot be used as a raw material, so that the process flow is long, titanium in the titanium-containing blast furnace slag exists in a perovskite form, the process is extremely stable, the alkaline treatment temperature is high, and the recovery rate of the titanium is low. In addition, NaOH is used as a separating agent in the prior alkali method melting, and the energy consumption of recycling is high.
Disclosure of Invention
In view of the analysis, the invention aims to provide a carbon-thermal sodium salt reduction melting separation comprehensive recovery method for vanadium-titanium magnetite iron ore concentrate, which is used for solving the problems of longer process flow, high alkali treatment temperature, lower titanium recovery rate and higher energy consumption for recycling the separating agent.
The purpose of the invention is mainly realized by the following technical scheme:
a carbon-thermal sodium salt reduction melting comprehensive recovery method of vanadium titano-magnetite iron ore concentrate comprises the following steps:
a) mixing the vanadium titano-magnetite iron ore concentrate, a carbonaceous reducing agent and a sodium treatment agent to prepare a carbonaceous pellet;
b) the carbon-containing pellets are subjected to reduction of iron oxide and sodium treatment of titanium, silicon and aluminic acid oxides at high temperature, slag and iron separation is completed, vanadium is enriched in molten iron, and titanium is converted into sodium salt and enriched in melt separation slag;
c) mixing the molten slag and water according to a certain solid-liquid mass ratio, carrying out high-pressure hydrolysis for multiple times, allowing NaOH obtained by hydrolysis and soluble silicon and aluminum sodium salt to enter an aqueous solution, allowing metatitanic acid obtained by hydrolysis to remain in filter residues, and separating titanium from soluble impurities of silicon and aluminum by a filter pressing device;
d) mixing the filter residue with water according to a certain solid-liquid mass ratio, continuously oscillating in an ultrasonic oscillator, and filtering by a filter pressing device to obtain titanium-containing suspension and residue;
e) and (3) after the titanium-containing suspension is subjected to evaporative crystallization and filtration, calcining at high temperature to obtain titanium-rich slag.
Preferably, the sodium reagent is NaHCO3Or Na2CO3The carbonaceous reducing agent is graphite powder or carbon powder.
Preferably, in the carbon-containing pellets, the sodiumizing agent and TiO in the iron ore concentrate2、SiO2、Al2O3The ratio of the total mole number sum is (1-1.5):1, and the ratio of the carbonaceous reducing agent to the mole number sum of the oxygen and sodium reducing agents in the iron ore concentrate is (0.8-1.2): 1.
Preferably, the temperature for the reduction and sodium treatment of the carbon-containing pellets in the step b) is 1200-1400 ℃, and the time is 100-160 min.
Preferably, the temperature for high-pressure hydrolysis of the molten slag in the step c) is 100-250 ℃, the times are 3-5 times, each time is 60min, and the solid-liquid mass ratio is 30: 1-50: 1.
Preferably, the oscillation time of the filter residue and the water in the ultrasonic oscillator in the step d) is 50-100min, and the liquid-solid mass ratio of the mixture of the water and the filter residue is 30: 1-50: 1.
Preferably, the temperature of the high-temperature calcination in the step e) is 700-900 ℃, and the time is 40-80 min.
The invention has the following beneficial effects:
the process provided by the research simplifies the treatment process of the vanadium titano-magnetite iron concentrate, reduces the melting temperature, and can efficiently recover iron, vanadium and titanium resources. The concrete aspects are as follows:
1. the sodium agent is used as an alkaline flux to perform a sodium treatment reaction with the oxide of silicon, so that the formation of fayalite is avoided, the reduction of iron oxide is promoted, the melting point of sodium titanate is low, the melting temperature of molten slag can be obviously reduced, the separation of slag and iron and the dissolution of vanadium in molten iron are promoted, and the synchronous recovery of iron, vanadium and titanium is realized.
2. The sodium treatment agent can be recycled, and the characteristic of low solubility of the sodium treatment agent in water is utilized to circularly enrich and separate out, so that the evaporation and crystallization steps of the sodium treatment agent are saved, and the energy consumption of the sodium treatment agent in recycling is greatly reduced.
3. The hydrolysis is carried out under high temperature and high pressure, so that the use of acid can be avoided. Meanwhile, the polymerization degree of metatitanic acid is controlled by ultrasonic oscillation, and titanium is enriched in slag in the filter pressing process before oscillation, so that the separation of titanium and soluble salt can be realized; after oscillation, metatitanic acid particles are reduced, titanium is enriched in water to form a suspension, separation of titanium and solid impurities is realized, and the grade of titanium is further improved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a flow chart of carbon-thermal sodium reduction treatment process of vanadium titano-magnetite iron ore concentrate
Detailed Description
The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form a part hereof, and which together with the embodiments of the invention serve to explain the principles of the invention.
Example 1
Iron ore concentrate of vanadium titano-magnetite of Sichuan Wei, TFe content 55%, TiO2Content 11.86%, V2O50.54% of SiO25.73% of Al2O3The content is 2.65%. Mixing iron ore concentrate and Na2CO3Mixing with graphite powder at a certain proportion, wherein Na is2CO3As a sodiumizing agent, with TiO in iron ore concentrate2、SiO2、Al2O3The total sum of the moles of carbon and Na is 1.22CO3The ratio of the sum of the moles was 1.0.
Pressing the uniformly mixed sample on a vertical jack into a cylinder small block, drying, then preserving the heat in a graphite crucible at 1250 ℃ for 120min to perform carbothermic sodium reduction reaction, taking out the crucible after reaching the heat preservation time, and cooling. The slag and iron melting phenomena of the sample after the carbon thermal sodium reduction occur, the yield of iron reaches 90%, the titanium content in molten iron is less than 0.1%, the titanium content can be ignored, the vanadium content is 0.49-0.52%, and the yield is higher than 80%. Preparing a powder sample from the melt slag on a vibration crushing sampling machine, mixing the powder sample with water according to the solid-liquid mass ratio of 50:1, hydrolyzing the mixture in a high-pressure reaction kettle at 100 ℃ for 60min, performing filter pressing for solid-liquid separation, repeating the step for 5 times, and finally reducing the pH value of the aqueous solution to 7-8. Mixing the filtered residue with water according to a solid-liquid mass ratio of 50:1, continuously oscillating in an ultrasonic oscillator for 60min, filtering to obtain a titanium-containing suspension and residue, and determining the titanium content in the residue to be 4.87% by chemical titration analysis.
The titanium-containing suspension liquid is subjected to boiling hydrolysis, crystallization and growth to generate precipitation, solid precipitate is calcined at 700 ℃ for 60min to obtain titanium-rich slag, and the titanium dioxide grade and the total iron content in the titanium slag are respectively 60% and 1.7% through chemical titration analysis.
Example 2
The source of the iron concentrate, the contents of the components and the preparation method of the sample were the same as in example 1.
Crushing and grinding the slag subjected to carbon thermal sodium reduction at 1250 ℃ and iron removal into powder samples, stirring and hydrolyzing the powder samples in a high-pressure reaction kettle at 250 ℃ for 60min, performing solid-liquid separation, repeating the process for 5 times, removing a solution containing soluble salts such as sodium hydroxide, sodium metasilicate, sodium metaaluminate and the like, mixing the residue with water, performing ultrasonic oscillation for 60min, performing solid-liquid separation, drying the residue at 120 ℃, and determining the titanium content by chemical titration, wherein the result shows that the titanium content in the residue is reduced to 2.82%. The titanium-containing suspension is crystallized, grown and precipitated, then solid-liquid separation is carried out, the obtained solid slag is roasted for 60min at 700 ℃, and the grade of the titanium dioxide is improved to 79 percent by chemical analysis.
Comparing the cases 1 and 2, it can be known that the high-temperature hydrolysis temperature has a great influence on the grade of the titanium slag, and increasing the hydrolysis temperature is beneficial to increasing the hydrolysis degree of sodium metatitanate and reducing the sodium content of the titanium slag.
Example 3
The source of the iron concentrate, the contents of the components and the preparation method of the sample were the same as in example 1.
And drying the sodium-modified carbon-containing pellets, preserving the heat in a 1300 ℃ graphite crucible for 120min to perform carbon-heat sodium-modification reduction reaction, taking out the graphite crucible after reaching the heat preservation time, and cooling the graphite crucible, wherein the yield of iron after slag and iron are separated reaches 94%. Crushing and grinding the molten slag on a sampling machine into powder, mixing the powder with water according to the solid-liquid mass ratio of 50:1, hydrolyzing for 60min in a high-pressure reaction kettle at 100 ℃, carrying out filter pressing for solid-liquid separation, mixing the residue obtained after 5 times of hydrolysis and filtration with water according to the solid-liquid mass ratio of 50:1, continuously oscillating for 60min in an ultrasonic oscillator, and then filtering to obtain a titanium-containing suspension and residue, wherein the titanium content in the residue is determined to be 4.31% by chemical titration analysis.
The titanium-containing suspension grows up through boiling hydrolysis crystallization, solid-liquid separation is carried out to obtain solid residue containing metatitanic acid, the solid residue is calcined at 900 ℃ for 60min to obtain titanium slag, and the grade of titanium dioxide in the titanium slag is 64% through chemical titration analysis.
Comparing examples 1 and 3, it is found that an increase in the carbothermic sodium treatment temperature is advantageous for reducing the titanium content in the residue and for improving the grade of the titanium slag, but the effect is not as great as the effect of the hydrolysis temperature.
Example 4
The source of the iron concentrate, the contents of the components and the preparation method of the sample were the same as in example 1.
And drying the sodiumized carbon-containing pellets, and then preserving heat in a graphite crucible at 1350 ℃ for 120min for carbothermic sodiumized reduction reaction, taking out the graphite crucible after reaching the heat preservation time and cooling, wherein the yield of iron after slag and iron separation reaches 96%. Crushing and grinding the molten slag on a sampling machine into powder, mixing the powder with water according to the solid-liquid mass ratio of 50:1, hydrolyzing for 60min at 250 ℃ in a high-pressure reaction kettle, carrying out pressure filtration for carrying out solid-liquid separation, mixing the residue obtained after 5 times of hydrolysis filtration with water according to the solid-liquid mass ratio of 50:1, continuously oscillating for 60min in an ultrasonic oscillator, and then filtering to obtain a titanium-containing suspension and residue, wherein the titanium content in the residue is determined to be 2.27% by chemical titration analysis.
The titanium-containing suspension grows up through boiling hydrolysis crystallization, solid-liquid separation is carried out to obtain solid residue containing metatitanic acid, the solid residue is calcined at 900 ℃ for 60min to obtain titanium slag, and the grade of titanium dioxide in the titanium slag is 82% through chemical titration analysis.
Comparing cases 1 and 4, it can be known that the effect superposition effect can be achieved by simultaneously increasing the carbon thermal sodium modification temperature and the hydrolysis temperature, the titanium content in the residue can be simultaneously reduced, the hydrolysis degree of sodium metatitanate can be increased, and the optimal titanium dioxide grade can be finally obtained.
In summary, the embodiment of the invention provides a carbon-thermal sodium-reduction melting-separation comprehensive recovery method for vanadium-titanium magnetite iron ore concentrate, which simplifies the treatment process of the vanadium-titanium magnetite iron ore concentrate, reduces the melting-separation temperature, and can efficiently recover iron, vanadium and titanium resources. Properly controlling the carbon thermal sodium treatment temperature and the hydrolysis temperature, respectively reducing the titanium content in the residue, and improving the hydrolysis degree of the sodium metatitanate, thereby finally obtaining the optimal titanium dioxide grade.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (3)
1. A carbon-thermal sodium salt reduction melting comprehensive recovery method of vanadium titano-magnetite iron ore concentrate is characterized by comprising the following steps:
a) mixing the vanadium titano-magnetite iron ore concentrate, a carbonaceous reducing agent and a sodium treatment agent to prepare a carbonaceous pellet;
b) the carbon-containing pellets are subjected to reduction of iron oxide and sodium treatment of titanium, silicon and aluminic acid oxides at high temperature, slag and iron separation is completed, vanadium is enriched in molten iron, and titanium is converted into sodium salt and enriched in melt separation slag;
c) mixing the molten slag and water according to a certain solid-liquid mass ratio, carrying out high-pressure hydrolysis for multiple times, allowing NaOH obtained by hydrolysis and soluble silicon and aluminum sodium salt to enter an aqueous solution, allowing metatitanic acid obtained by hydrolysis to remain in filter residues, and separating titanium from soluble impurities of silicon and aluminum by a filter pressing device;
d) mixing the filter residue with water according to a certain solid-liquid mass ratio, continuously oscillating in an ultrasonic oscillator, and filtering by a filter pressing device to obtain titanium-containing suspension and residue;
e) after the titanium-containing suspension is subjected to evaporative crystallization and filtration, high-temperature calcination is carried out to obtain titanium-rich slag;
the temperature for the reduction and sodium treatment reaction of the carbon-containing pellets in the step b) is 1200-1400 ℃, and the time is 100-160 min;
the temperature for carrying out high-pressure hydrolysis on the medium-melting slag in c) is 100-250 ℃, the times are 3-5 times, each time is 60min, and the solid-liquid mass ratio is 30: 1-50: 1;
in the d), the oscillation time of the filter residue and water in the ultrasonic oscillator is 50-100min, and the liquid-solid mass ratio of the mixture of the water and the filter residue is 30: 1-50: 1;
the temperature of the high-temperature calcination in e) is 700-900 ℃, and the time is 40-80 min.
2. The method of claim 1, wherein the sodium reagent is NaHCO3Or Na2CO3The carbonaceous reducing agent is graphite powder or carbon powder.
3. The method as claimed in claim 2, wherein the carbon-thermal sodium salt reduction melting separation comprehensive recovery method for vanadium titano-magnetite iron ore concentrate is characterized in that in the carbon-containing pellets, a sodium agent and TiO in iron ore concentrate2、SiO2、Al2O3The ratio of the total mole number sum is (1-1.5):1, and the ratio of the carbonaceous reducing agent to the mole number sum of the oxygen and sodium reducing agents in the iron ore concentrate is (0.8-1.2): 1.
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| CN108018437B (en) * | 2017-10-24 | 2020-04-24 | 钢研晟华科技股份有限公司 | Low-temperature comprehensive recovery process for iron, vanadium and titanium in vanadium-titanium magnetite |
| CN107935033B (en) * | 2017-10-24 | 2019-09-27 | 钢研晟华科技股份有限公司 | A kind of technique that titanium-containing blast furnace slag prepares titanium white raw material |
| CN108018426B (en) * | 2017-12-12 | 2020-03-20 | 钢研晟华科技股份有限公司 | Copper slag low-temperature comprehensive utilization process based on sodium reduction |
| CN110735032B (en) * | 2019-09-03 | 2021-04-06 | 昆明禾丰环境研究所 | Vanadium-titanium-iron paragenetic ore treatment process |
| CN113072150B (en) * | 2021-04-22 | 2022-06-17 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary inorganic polymeric flocculant based on sulfuric acid acidolysis vanadium-titanium magnetite two-step method |
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