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WO2015081775A1 - Procédé pour utiliser complètement un concentré de magnétite de vanadium-titane à teneur élevée en chrome - Google Patents

Procédé pour utiliser complètement un concentré de magnétite de vanadium-titane à teneur élevée en chrome Download PDF

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Publication number
WO2015081775A1
WO2015081775A1 PCT/CN2014/089728 CN2014089728W WO2015081775A1 WO 2015081775 A1 WO2015081775 A1 WO 2015081775A1 CN 2014089728 W CN2014089728 W CN 2014089728W WO 2015081775 A1 WO2015081775 A1 WO 2015081775A1
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titanium
vanadium
chromium
slag
mass
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Chinese (zh)
Inventor
齐涛
王丽娜
赵龙胜
陈德胜
赵宏欣
于宏东
刘亚辉
曲景奎
薛天艳
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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Priority claimed from CN201310653270.8A external-priority patent/CN103757426B/zh
Priority claimed from CN201310654831.6A external-priority patent/CN103757199B/zh
Application filed by Institute of Process Engineering of CAS filed Critical Institute of Process Engineering of CAS
Publication of WO2015081775A1 publication Critical patent/WO2015081775A1/fr
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • B03C1/005—Pretreatment specially adapted for magnetic separation
    • B03C1/015—Pretreatment specially adapted for magnetic separation by chemical treatment imparting magnetic properties to the material to be separated, e.g. roasting, reduction, oxidation
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • 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

Definitions

  • the invention belongs to the field of hydrometallurgy, and in particular, the invention relates to a method for comprehensively utilizing a high chromium type vanadium titanium magnet concentrate.
  • Panxi, Sichuan is the largest vanadium-titanium magnetite base in China. Its TiO 2 reserves account for more than 35% of the world's titanium reserves, accounting for more than 90% of the proven reserves in China, mainly concentrated in Panzhihua, Baima, and Hongge. Hehe and four mining areas. The vanadium-titanium magnetite in the Hongge mining area is currently the largest vanadium-titanium magnetite deposit in China with a reserve of 3.545 billion tons.
  • the red, high-chromium vanadium-titanium magnetite concentrate Compared with the Panzhihua vanadium-titanium magnetite concentrate, the red, high-chromium vanadium-titanium magnetite concentrate has the same content of iron, titanium and vanadium, and the associated chromium content is higher.
  • the grade of chromium (Cr 2 O 3 0.5% to 2%) is 8 to 10 times that of Panzhihua vanadium-titanium magnetite concentrate.
  • blast furnace route there are two main methods for comprehensive utilization of high-chromium vanadium-titanium magnetite concentrates: blast furnace route and direct reduction route.
  • blast furnace route see Chinese patent CN101020970A
  • high-chromium vanadium-titanium magnetite concentrate is smelted in a blast furnace or an electric furnace to obtain molten iron containing chromium and vanadium.
  • the titanium-containing slag obtained by the method is difficult to recycle, which not only causes waste of resources, but also has the risk of causing environmental deterioration due to the presence of chromium.
  • the direct reduction route can be further divided into the “first vanadium after iron” method (see Chinese patent CN102061397A) and the “first iron after vanadium” method (see Chinese patent CN101082068A, CN101294242A).
  • the high chromium vanadium-titanium magnetite concentrate is mixed with the sodium salt and oxidized and calcined at a high temperature, and then the vanadium and chromium are leached with water, and the residue after the water immersion is mixed with the pulverized coal to make a ball. After that, direct reduction is carried out in a rotary hearth furnace or an electric furnace.
  • the method has long process flow, high energy consumption, and the added sodium salt decomposes at high temperature to release harmful gases and pollute the environment.
  • the high-chromium vanadium-titanium magnet concentrate is dried by the batching ball, and then directly reduced in a rotary kiln or a rotary hearth furnace, and then the obtained metallized pellet is charged into an electric furnace for melting. Separation.
  • the Chinese patent CN101082068A does not describe the process conditions of direct reduction and melting separation, and the Chinese patent CN101294242A adopts a three-step high-temperature process of rotary hearth furnace reduction-electric furnace melting separation-electric furnace oxygen smelting, which has complicated process and high energy consumption.
  • the existing patent literature on high chromium (Cr 2 O 3 0.5% to 2%) vanadium-titanium magnet concentrate is basically a method of high temperature reduction and vanadium chrome hot metal blowing, and the general direct reduction-melting process is The iron and titanium are completely separated, and the deep reduction method is generally adopted.
  • the existing titanium-rich slag preparation technology generally uses titanium concentrate as a raw material and directly smelts in an electric furnace to obtain a titanium-rich slag having a TiO 2 mass content of about 75%.
  • the technology is relatively mature, but it is not suitable for the smelting of direct reduction-electric furnace melting of titanium slag, which is mainly because the content of impurities in the titanium slag of the electric furnace is relatively high.
  • the method for preparing titanium-rich slag by using electric furnace melting titanium slag as raw material generally adopts hydrochloric acid leaching to improve the raw material after activation.
  • Common activation methods include sodium roasting, mechanical activation, and microwave strengthening. This is because the phase of the titanium slag in the electric furnace is very stable, and it is very difficult to extract directly using hydrochloric acid.
  • the object of the present invention is to provide a kind of industrial operation and low energy consumption for the shortcomings of low utilization rate of titanium, vanadium and chromium, high energy consumption and serious environmental pollution in the conventional blast furnace iron-converter steelmaking process.
  • the invention provides a method for preparing vanadium chromium titanium slag by using high chromium type vanadium titanium magnet concentrate, comprising the following steps:
  • step 2) partially reducing the mixture of step 1), the reduction temperature is 1000-1300 ° C, and the reduction time is 1-10 h to obtain a metallized material;
  • the metallized material obtained in the step 2) is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed to obtain iron fine powder and vanadium chromium titanium slag.
  • the high chromium type vanadium titanium magnet concentrate has a TFe mass content of more than 40%, a TiO 2 mass content of more than 9%, and a V 2 O 5 mass content. More than 0.4%, the mass content of Cr 2 O 3 is more than 0.5%; and the carbon-containing reducing agent in step 1) is preferably one or more of anthracite, bituminous coal, lignite, and coke.
  • the additive of the step 1) is any one or more of sodium carbonate, potassium carbonate, sodium tetraborate, sodium fluoride, and alkali metal sodium silicate.
  • the metallization ratio of the metallized material in the step 2) is 30% to 80%.
  • the magnetic separation strength of the magnetic separation in step 3) is 200 to 2000 Oersted.
  • the recovery rates of titanium, vanadium and chromium in the vanadium chromium titanium slag after magnetic separation are respectively greater than 93%; the mass content of TFe in the iron fine powder is greater than 90%; the TFe in the vanadium chromium titanium slag The mass content is less than 35%; the phase of the vanadium chromium titanium slag is more unstable, and the titanium slag obtained by melting at a high temperature Compared with, it is more conducive to efficient extraction of titanium resources.
  • the existing direct reduction-electric furnace melting process uses high-temperature melting process, high energy consumption, and the obtained titanium slag phase is very stable, and it is usually necessary to extract titanium resources after activation.
  • Common activation methods include sodium roasting, mechanical activation, and microwave strengthening. This not only greatly increases equipment investment, but also greatly increases the energy consumption of the process.
  • the present invention adopts a partial reduction-magnetic separation technique, which not only avoids the high-temperature melting process, but also controls the orientation of vanadium and chromium to be consistent with titanium, and the phase of the obtained vanadium-chromium-titanium slag is relatively unstable, which is easy to follow.
  • the treatment extracts titanium, vanadium and chromium.
  • the method for comprehensively utilizing a high chromium type vanadium titanium magnet concentrate of the present invention comprises the following steps:
  • step 2) partially reducing the mixture of step 1), the reduction temperature is 1000-1300 ° C, and the reduction time is 1-10 h to obtain a metallized material;
  • the metallized material obtained in the step 2) is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed to obtain iron fine powder and vanadium chromium titanium slag;
  • step 4) The intermediate slurry obtained in step 4) is subjected to solid-liquid separation to obtain leach residue and a leachate containing vanadium and chromium;
  • the leaching residue obtained in the step 5) is washed and desiliconized, and then dried at 100 to 200 ° C to obtain a titanium-rich slag.
  • the steps 1) to 3) are both specific steps of the above method for preparing vanadium chromium titanium slag, and further specifically, the high chromium type of the step 1)
  • the content of TFe of the vanadium-titanium magnetite concentrate is more than 40%, the mass content of TiO 2 is more than 9%, the mass content of V 2 O 5 is more than 0.4%, and the mass content of Cr 2 O 3 is more than 0.5%;
  • the carbonaceous reducing agent is preferably one or more of anthracite, bituminous coal, lignite, and coke.
  • the additive of the step 1) is any one or more of sodium carbonate, potassium carbonate, sodium tetraborate, sodium fluoride, and alkali metal sodium silicate.
  • the metallization material has a metallization ratio of 30% to 80%.
  • Step 3) The magnetic separation strength of the magnetic separation is 200 to 2000 Oersted.
  • the recovery rates of titanium, vanadium and chromium in the vanadium chromium titanium slag after magnetic separation are respectively greater than 93%; the mass content of TFe in the iron fine powder is greater than 90%; the TFe in the vanadium chromium titanium slag The mass content is less than 35%; the phase of the vanadium chromium titanium slag is more unstable, and is more favorable for the efficient extraction of titanium resources than the titanium slag obtained by high temperature melting.
  • the mass percentage concentration of the hydrochloric acid solution in the step 4) is 10% to 30%, and the leaching time is 1 to 10 hours.
  • the mass concentration of TFe in the vanadium-containing and chromium-containing acid leaching solution in step 5) is 10 to 50 g/L, and the mass concentration of V 2 O 5 is 1.0. ⁇ 4.5 g/L, the mass concentration of Cr 2 O 3 is 1.5 to 6.0 g/L, and the mass concentrations of TiO 2 and SiO 2 are both less than 1.5 g/L.
  • the titanium-rich slag of the step 6) has a mass content of TiO 2 of more than 75%.
  • the recovery of titanium in the method is greater than 98%, and the recovery rates of vanadium and chromium are both greater than 90%.
  • the invention also provides a method for preparing titanium-rich slag by using vanadium chromium titanium slag, comprising the following steps:
  • step 2) The intermediate slurry obtained in step 1) is subjected to solid-liquid separation to obtain leach residue and a leachate containing vanadium and chromium;
  • the method for preparing titanium-rich slag by using vanadium chromium titanium slag according to the invention wherein the vanadium chromium titanium slag has a TFe mass content of less than 35%, the TiO 2 mass content is 15% to 30%, and the V 2 O 5 mass content. It is 0.5% to 3.0%, and the mass content of Cr 2 O 3 is 0.5% to 3.0%.
  • the vanadium chromium titanium slag can be prepared by the method for preparing vanadium chromium titanium slag using the high chromium type vanadium titanium magnet concentrate provided by the above invention.
  • the mass percentage concentration of the hydrochloric acid solution in the step 1) is 10% to 30%; and the leaching time in the step 1) is preferably 1 to 10 hours.
  • the mass concentration of TFe in the vanadium-containing and chromium-containing acid leaching solution is 10 to 50 g/L, and the mass concentration of V 2 O 5 is 1.0. ⁇ 4.5 g/L, the mass concentration of Cr 2 O 3 is 1.5 to 6.0 g/L, and the mass concentrations of TiO 2 and SiO 2 are both less than 1.5 g/L.
  • the titanium-rich slag of the step 3) has a mass content of TiO 2 of more than 75%.
  • the recovery rate of titanium in the method for preparing titanium-rich slag by using vanadium-chromium-titanium slag is greater than 98%, and the recovery rates of vanadium and chromium are both greater than 90%.
  • the existing direct reduction-electric furnace melting process has high energy consumption due to the high-temperature melting process, and the obtained titanium
  • the slag phase is very stable and usually requires titanium resources for activation.
  • Common activation methods include sodium roasting, mechanical activation, and microwave strengthening. This not only greatly increases equipment investment, but also greatly increases the energy consumption of the process.
  • the present invention employs a partial reduction-magnetic separation-hydrochloric acid leaching technique, which not only avoids the high-temperature melting process, but also controls the orientation of vanadium and chromium to be consistent with titanium.
  • the phase of the obtained vanadium-chromium-titanium slag is relatively unstable, and is directly acid-immersed with hydrochloric acid. The extraction rate of vanadium and chromium is high, and the impurity removal rate is high.
  • the present invention first proposes a partial reduction technique, that is, a method of controlling the degree of reduction, which can realize the separation of iron from titanium, vanadium and chromium, and provides an effective way for comprehensive utilization of high chromium vanadium-titanium magnetite.
  • the recovery rates of titanium, vanadium and chromium are both higher than 93%, and the resource utilization rate is high.
  • the iron content of the iron fine powder of the present invention is more than 90%, and is a high-quality steelmaking raw material.
  • the vanadium chromium titanium slag of the present invention is obtained by magnetic separation. Compared with the titanium slag obtained by electric furnace melting, the mineral phase structure of vanadium chrome-titanium slag is more unstable. The acid leaching of vanadium chrome-titanium slag can not only greatly improve the grade of titanium slag, but also realize the separation of titanium and vanadium and chromium. Efficient separation greatly increases the recovery of titanium, vanadium and chromium.
  • the titanium-rich slag obtained by the invention has a TiO 2 content of more than 75%, and can be used as a sulfuric acid-based titanium white raw material, and a titanium-rich slag having a TiO 2 mass content of more than 88% can also be obtained as a chlorinated titanium white raw material.
  • the process for comprehensively utilizing high-chromium vanadium-titanium magnetite concentrate of the invention has mild reaction conditions and greatly improves resource utilization rate, wherein the recovery rate of titanium is greater than 98%, and the recovery rates of vanadium and chromium are greater than 90 %.
  • Embodiments 1 to 6 of the present invention are a process flow diagram of Embodiments 1 to 6 of the present invention.
  • Embodiments 7 to 12 of the present invention are a process flow diagram of Embodiments 7 to 12 of the present invention.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 55%, TiO 2 mass content is 12.1%, V 2 O 5 mass content is 0.53%, Cr 2 O 3 mass content is 1.10%)
  • the mixture of anthracite and sodium carbonate is mixed, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and sodium carbonate is 100:8:2.5; the obtained mixture is partially reduced at 1200 ° C, and the reduction time is 2 hours.
  • Metallization material with a metallization rate of 70% is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 600 Oe to obtain a TFe mass content of 93.5.
  • % iron fines and TFe, TiO 2 , V 2 O 5 and Cr 2 O 3 are 21.5%, 27.5%, 1.10% and 2.10% vanadium chromium titanium slag, respectively; the recovery of titanium in this process 96.5%, the recovery rate of vanadium is 94.2%, and the recovery rate of chromium is 93.8%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 55%, TiO 2 mass content is 12.1%, V 2 O 5 mass content is 0.53%, Cr 2 O 3 mass content is 1.10%)
  • the mixture of bituminous coal and sodium tetraborate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, bituminous coal and sodium tetraborate is 100:20:3; the obtained mixture is partially reduced at 1300 ° C, and the reduction time is 1 hour.
  • the metallization material having a metallization rate of 80% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed under a magnetic field strength of 1000 Oersted to obtain a mass content of TFe.
  • 95.5% of iron fines and TFA, TiO 2 , V 2 O 5 and Cr 2 O 3 are respectively 18.6%, 29.5%, 1.03% and 1.75% of vanadium chromium titanium slag; titanium recovery in this process The rate was 95.7%, the recovery of vanadium was 93.9%, and the recovery of chromium was 93.1%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 47.2%, TiO 2 mass content is 10.5%, V 2 O 5 mass content is 1.20%, Cr 2 O 3 mass content is 0.58%)
  • the lignite is mixed to prepare a mixed material, wherein the weight ratio of the vanadium-titanium magnet concentrate to the coke is 100 : 2; the obtained mixed material is partially reduced at 1000 ° C for a reduction time of 10 hours to obtain a metal having a metallization ratio of 30%.
  • the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed under a magnetic field strength of 2000 Oersted to obtain iron fine powder and TFe having a TFe mass content of 90.1%.
  • the content of TiO 2 , V 2 O 5 and Cr 2 O 3 was 34.8%, 15.5%, 1.52% and 0.80%, respectively.
  • the recovery of titanium in this process was 94.3%, and the recovery of vanadium was 94.3%. 92.1%, the recovery rate of chromium is 91.8%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe has a mass content of 40.5%, TiO 2 has a mass content of 9.2%, V 2 O 5 has a mass content of 0.86%, and Cr 2 O 3 has a mass content of 0.75%).
  • the mixture of anthracite and sodium silicate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and sodium silicate is 100:10:1; the obtained mixture is partially reduced at 1150 ° C, and the reduction time is 4 hours.
  • a metallization material having a metallization ratio of 62% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 200 Oersted to obtain a mass content of TFe.
  • 97.5% of iron fines and TFA, TiO 2 , V 2 O 5 and Cr 2 O 3 are respectively 18.8%, 20.5%, 1.21% and 1.07% of vanadium chromium titanium slag; titanium recovery in this process The rate was 93.2%, the recovery of vanadium was 91.5%, and the recovery of chromium was 90.9%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 47.2%, TiO 2 mass content is 10.5%, V 2 O 5 mass content is 1.20%, Cr 2 O 3 mass content is 0.58%)
  • the mixture is prepared by mixing coke and sodium silicate, wherein the weight ratio of vanadium-titanium magnetite concentrate, coke and sodium silicate is 100:6.5:4; the obtained mixture is partially reduced at 1200 ° C, and the reduction time is 2 hours.
  • the metallization material having a metallization rate of 76% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 800 Oersted to obtain a mass content of TFe.
  • 94.7% of iron fines and Tef, TiO 2 , V 2 O 5 and Cr 2 O 3 were respectively 17.8%, 25.4%, 2.04% and 1.17% of vanadium chromium titanium slag; titanium recovery in this process The rate was 92.8%, the recovery of vanadium was 90.6%, and the recovery of chromium was 90.3%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe has a mass content of 40.5%, TiO 2 has a mass content of 9.2%, V 2 O 5 has a mass content of 0.86%, and Cr 2 O 3 has a mass content of 0.75%).
  • the mixture of anthracite and sodium tetraborate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and additive is 100:4:10; the obtained mixture is partially reduced at 1000 ° C, and the reduction time is 10 hours.
  • Metallization material with a metallization rate of 45% is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 1600 Oersted to obtain a mass content of TFe of 92.1. % iron fines and TFe, TiO 2 , V 2 O 5 and Cr 2 O 3 have a mass content of 24.3%, 17.5%, 1.41% and 1.27% vanadium chromium titanium slag; the recovery of titanium in this process 95.8%, the recovery rate of vanadium is 93.9%, and the recovery rate of chromium is 93.5%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 55%, TiO 2 mass content is 12.1%, V 2 O 5 mass content is 0.53%, Cr 2 O 3 mass content is 1.10%)
  • the mixture of anthracite and sodium carbonate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and sodium carbonate is 100:8:2.5; the obtained mixture is partially reduced at 1200 ° C, and the reduction time is 2 hours.
  • Metallization material with a metallization rate of 70% is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 600 Oe to obtain a TFe mass content of 93.5.
  • the mass content of % iron fines and TFe, TiO 2 , V 2 O 5 and Cr 2 O 3 were 21.5%, 27.5%, 1.10% and 2.10% of vanadium chromium titanium slag, respectively.
  • the content of TFA, TiO 2 , V 2 O 5 and Cr 2 O 3 was 21.5%, 27.5%, 1.10% and 2.10% of vanadium chromium titanium slag mixed with 25% hydrochloric acid solution, and leached at 150 ° C.
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 4.5:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 36.5.
  • the mass concentration of g/L, V 2 O 5 is 2.5 g/L, the mass concentration of Cr 2 O 3 is 6.0 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 1.5 g/L; the obtained leaching residue is washed.
  • a titanium-rich slag having a TiO 2 mass content of 92.6% was obtained; in this process, the recovery of titanium was 98.6%, the recovery of vanadium was 94.5%, and the recovery of chromium was 95.4%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 55%, TiO 2 mass content is 12.1%, V 2 O 5 mass content is 0.53%, Cr 2 O 3 mass content is 1.10%)
  • the mixture of bituminous coal and sodium tetraborate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, bituminous coal and sodium tetraborate is 100:20:3; the obtained mixture is partially reduced at 1300 ° C, and the reduction time is 1 hour.
  • the metallization material having a metallization rate of 80% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed under a magnetic field strength of 1000 Oersted to obtain a mass content of TFe.
  • 95.5% of iron fine powder and Tef, TiO 2 , V 2 O 5 and Cr 2 O 3 have a mass content of 18.6%, 29.5%, 1.03% and 1.75% of vanadium chromium titanium slag;
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 10:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 16.7.
  • the mass concentration of g/L, V 2 O 5 is 1.2 g/L, the mass concentration of Cr 2 O 3 is 2.0 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 0.8 g/L; the obtained leaching residue is washed.
  • a titanium-rich slag having a TiO 2 mass content of 76% is obtained; in this process, the recovery of titanium is 98.1%, the recovery of vanadium is 90.5%, and the recovery of chromium is 90.2%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 47.2%, TiO 2 mass content is 10.5%, V 2 O 5 mass content is 1.20%, Cr 2 O 3 mass content is 0.58%)
  • the lignite is mixed to prepare a mixed material, wherein the weight ratio of the vanadium-titanium magnet concentrate to the coke is 100:2; the obtained mixed material is partially reduced at 1000 ° C for a reduction time of 10 hours to obtain a metal having a metallization ratio of 30%.
  • the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed under a magnetic field strength of 2000 Oersted to obtain iron fine powder and TFe having a TFe mass content of 90.1%.
  • the content of TiO 2 , V 2 O 5 and Cr 2 O 3 was 34.8%, 15.5%, 1.52% and 0.80% of vanadium chromium titanium slag, respectively.
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 3:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 46.2.
  • the mass concentration of g/L, V 2 O 5 is 4.1 g/L, the mass concentration of Cr 2 O 3 is 2.3 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 1.0 g/L; the obtained leaching residue is washed.
  • titanium-rich slag having a TiO 2 mass content of 80% is obtained; in this process, the recovery of titanium is 98.4%, the recovery of vanadium is 91.1%, and the recovery of chromium is 92.8%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe has a mass content of 40.5%, TiO 2 has a mass content of 9.2%, V 2 O 5 has a mass content of 0.86%, and Cr 2 O 3 has a mass content of 0.75%).
  • the mixture of anthracite and sodium silicate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and sodium silicate is 100:10:1; the obtained mixture is partially reduced at 1150 ° C, and the reduction time is 4 hours.
  • a metallization material having a metallization ratio of 62% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 200 Oersted to obtain a mass content of TFe.
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 7:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 14.8.
  • the mass concentration of g/L, V 2 O 5 is 1.9 g/L, the mass concentration of Cr 2 O 3 is 1.7 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 1.0 g/L; the obtained leaching residue is washed.
  • a titanium-rich slag having a mass content of TiO 2 of 89.7% was obtained; in this process, the recovery of titanium was 98.2%, the recovery of vanadium was 92.4%, and the recovery of chromium was 93.7%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe mass content is 47.2%, TiO 2 mass content is 10.5%, V 2 O 5 mass content is 1.20%, Cr 2 O 3 mass content is 0.58%)
  • the mixture is prepared by mixing coke and sodium silicate, wherein the weight ratio of vanadium-titanium magnetite concentrate, coke and sodium silicate is 100:6.5:4; the obtained mixture is partially reduced at 1200 ° C, and the reduction time is 2 hours.
  • the metallization material having a metallization rate of 76% is obtained; the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 800 Oersted to obtain a mass content of TFe.
  • the vanadium chromium titanium slag having a mass content of 94.7% of iron fines and TFe, TiO 2 , V 2 O 5 and Cr 2 O 3 was 17.8%, 25.4%, 2.04% and 1.17%, respectively.
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 5.5:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 21.5.
  • the mass concentration of g/L, V 2 O 5 is 3.9 g/L, the mass concentration of Cr 2 O 3 is 2.0 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 0.8 g/L; the obtained leaching residue is washed.
  • titanium-rich slag having a TiO 2 mass content of 90.3% is obtained; in this process, the recovery of titanium is 98.9%, the recovery of vanadium is 94.2%, and the recovery of chromium is 93.6%.
  • High chromium type vanadium-titanium magnetite concentrate (TFe has a mass content of 40.5%, TiO 2 has a mass content of 9.2%, V 2 O 5 has a mass content of 0.86%, and Cr 2 O 3 has a mass content of 0.75%).
  • the mixture of anthracite and sodium tetraborate is prepared, wherein the weight ratio of vanadium-titanium magnetite concentrate, anthracite and additive is 100:4:10; the obtained mixture is partially reduced at 1000 ° C, and the reduction time is 10 hours.
  • Metallization material with a metallization rate of 45% the obtained metallized material is crushed and ground to a particle size of 90% less than 0.074 mm, and magnetic separation is performed at a magnetic field strength of 1600 Oersted to obtain a mass content of TFe of 92.1.
  • the content of iron fines and TFe, TiO 2 , V 2 O 5 and Cr 2 O 3 was 24.3%, 17.5%, 1.41% and 1.27% of vanadium chromium titanium slag, respectively.
  • an intermediate slurry is obtained, wherein the liquid-solid mass ratio of the dilute hydrochloric acid to the leaching slag is 4:1; the intermediate slurry is subjected to solid-liquid separation to obtain a leaching slag and a leaching solution containing vanadium and chromium, and the mass concentration of TFe in the leaching solution is 29.2.
  • the mass concentration of g/L, V 2 O 5 is 2.8 g/L, the mass concentration of Cr 2 O 3 is 2.2 g/L, and the mass concentration of TiO 2 and SiO 2 are both less than 1.2 g/L; the obtained leaching residue is washed.
  • a titanium-rich slag having a TiO 2 mass content of 93.5% was obtained; in this process, the recovery of titanium was 98.6%, the recovery of vanadium was 92.6%, and the recovery of chromium was 91.8%.

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Abstract

L'invention concerne un procédé qui permet d'utiliser complètement un concentré de magnétite de vanadium-titane à teneur élevée en chrome et qui comprend les étapes suivantes : 1) le mélange d'un concentré de magnétite de vanadium-titane à teneur élevée en chrome avec un agent réducteur carboné et des additifs afin de préparer des matières mélangées ; 2) la réduction d'une partie des matières mélangées afin d'obtenir des matières métallisées ; 3) l'exécution d'une séparation magnétique sur les matières métallisées afin d'obtenir du fer pulvérulent et des laitiers de vanadium-chrome-titane ; 4) le mélange des laitiers de vanadium-chrome-titane avec une solution d'acide chlorhydrique et l'exécution d'une lixiviation afin d'obtenir une suspension épaisse intermédiaire ; 5) l'exécution d'une séparation solide-liquide sur la suspension épaisse intermédiaire obtenue dans l'étape 4) afin d'obtenir des résidus de lixiviation et une liqueur de lixiviation qui contient du vanadium et du chrome ; 6) l'exécution d'un lavage et une désilication sur les résidus de lixiviation obtenu dans l'étape 5) afin d'obtenir des laitiers riches en titane. Le procédé, pour la première fois, fournit une technologie d'utilisation à la fois de la réduction partielle et de la lixiviation par de l'acide chlorhydrique, permettant ainsi non seulement de mettre en œuvre la séparation entre le fer et le titane, le vanadium et le chrome, mais également de mettre en œuvre une séparation efficace entre le titane et le vanadium et le chrome. Dans le procédé, les conditions de réaction sont légère, et le taux d'utilisation des ressources élevé, et du fer pulvérulent de qualité élevée et des laitiers riches en titane peuvent être obtenus.
PCT/CN2014/089728 2013-12-05 2014-10-28 Procédé pour utiliser complètement un concentré de magnétite de vanadium-titane à teneur élevée en chrome Ceased WO2015081775A1 (fr)

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CN201310654831.6 2013-12-05
CN201310653270.8A CN103757426B (zh) 2013-12-05 2013-12-05 一种利用钒铬钛渣制备富钛渣的方法
CN201310653270.8 2013-12-05
CN201310654831.6A CN103757199B (zh) 2013-12-05 2013-12-05 一种利用高铬型钒钛磁铁精矿制备钒铬钛渣的方法

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CN115710632B (zh) * 2022-11-22 2024-06-11 东北大学 一种高碳石煤分步微波焙烧—超声微泡酸浸提钒的方法
CN115747488A (zh) * 2022-11-22 2023-03-07 东北大学 一种钒页岩微波悬浮焙烧—拌碱熟化提钒系统及其提钒方法
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CN117327898A (zh) * 2023-09-28 2024-01-02 吉林金钢钢铁股份有限公司 一种低碳钢水、硅钒合金和富钛渣的生产系统及方法
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