WO2017190393A1 - 一种以钛铁复合矿为原料提取铁、钛的方法及过滤设备 - Google Patents

一种以钛铁复合矿为原料提取铁、钛的方法及过滤设备 Download PDF

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WO2017190393A1
WO2017190393A1 PCT/CN2016/083966 CN2016083966W WO2017190393A1 WO 2017190393 A1 WO2017190393 A1 WO 2017190393A1 CN 2016083966 W CN2016083966 W CN 2016083966W WO 2017190393 A1 WO2017190393 A1 WO 2017190393A1
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titanium
raw material
iron
ferrotitanium
ore
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French (fr)
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朱鸿民
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朱鸿民
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/10Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1204Obtaining 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
    • C22B34/1209Obtaining 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1218Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C22B9/023By filtering
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Definitions

  • the invention mainly belongs to the field of non-ferrous metallurgy, and particularly relates to a method and a filtering device for extracting iron and titanium by using titanium-iron composite ore as raw material.
  • Titanium-iron composite ore such as vanadium-titanium magnetite in Panxi area of Hebei province and Chengde area of Hebei province, has wide distribution, abundant reserves and huge resources, and titanium resources in ilmenite composite ore account for more than 91% of national titanium resources. High comprehensive utilization value.
  • most of the smelting of titanium-iron composite ore in the industry adopts the traditional "blast furnace-converter" process.
  • the iron and vanadium oxides in the mineral are reduced to vanadium-containing molten iron, while the titanium component mainly enters the slag in the form of low-oxide.
  • the slag-iron ratio is relatively high, and a large amount of titanium slag is difficult to be effectively treated, and most of it is processed into water slag, slag crushed stone, expanded slag and slag beads and other low economic value building materials.
  • the use of titanium, which is about 25% in terms of TiO 2 cannot be effectively utilized, which is a huge waste of China's abundant titanium resources.
  • Zhu Hongmin proposed a new metallurgical process for ferrotitanium composite ore based on the USTB molten salt electrolysis process.
  • the composite process ilmenite ore is first controlled by way of selective reduction of the carbon into the hot molten iron, titanium carbon (TiC x O z) and a slag phase components (Al 2 O 3, MgO, CaO, SiO 2) of The mixture is then subjected to a wet acid leaching process to remove the slag phase components, thereby enriching the titanium oxycarbide.
  • the titanium oxide having a purity of more than 90% can be used as a raw material for the USTB titanium electrolysis process, and can also be used for the production of titanium tetrachloride and titanium dioxide.
  • the process controls the degree of reduction in the state in which titanium oxide is reduced to titanium oxide (TiC x O z ), which realizes the docking with the USTB titanium electrolysis process and improves the subsequent acid leaching process.
  • TiC x O z titanium oxide
  • the efficiency of separation greatly improves the utilization rate of titanium in the ferrotitanium composite ore while effectively reducing the cost of the USTB titanium electrolysis process.
  • the present invention discloses a method and an apparatus for extracting iron and titanium from a ferrotitanium composite ore.
  • the method for extracting iron and titanium by using the ferrotitanium composite ore as a raw material adopts a “high temperature controllable method”.
  • a new complete process flow of carbothermal reduction - slag phase mixing - high temperature filtration separation to achieve separation and enrichment of titanium components in ferrotitanium composite ore; for the above new process flow, the invention also discloses a specific use for The high temperature filtration separation apparatus of the above new process flow effectively realizes the separation of the mixture in the new process flow at a high temperature.
  • a method for extracting iron and titanium from a ferrotitanium composite ore comprising the steps of:
  • the titanium-rich phase material with a purity higher than 95% means that the preparation is obtained.
  • the mass percentage of carbonitride, and/or titanium oxynitride in the titanium-rich phase material obtained is higher than 95%.
  • the amount of the carbon-containing reducing agent formulated in the step (2) is capable of reducing all the iron oxide in the crushed pretreated ferrotitanium ore to metal iron and capable of pretreating the crushing
  • the titanium oxide in the later ilmenite composite ore is all reduced to one or both of titanium oxycarbide and titanium oxycarbonitride; that is, the amount of the carbonaceous reducing agent formulated in the step (2) is not less than
  • the amount of the carbonaceous reducing agent required for reduction of iron oxide in the ferrotitanium composite ore after the crushing pretreatment and the titanium oxide in the ferrotitanium ore after the crushing pretreatment is reduced to the The sum of the amounts of the carbon-containing reducing agent required for the titanium-rich phase material (one or two of titanium oxide and titanium oxycarbonitride).
  • the mass of the carbon-containing reducing agent formulated in the step (2) is 20% to 30% of the mass of the ferrotitanium ore after the crushing pretreatment.
  • the composition of the slag phase in the preliminary product is controlled to be: at 1300 to 2000 ° C, the slag phase blending material is blended into the preliminary product to make the initial preparation In the product, the melting point of the slag phase is lower than the melting point of the titanium-rich phase material.
  • the slag phase compounding material is any one or a combination of two or more of MgO, Al 2 O 3 , CaO, and SiO 2 .
  • the form of the slag phase compounding material is granular or powdery.
  • the filtering raw material is filtered through a filter, specifically: one of two ways of using the filtering on the filtering part and the lower part in the lower part of the filtering net. Combination or two ways.
  • the filtered raw material is filtered through a filter at a temperature of 800 to 1800 °C.
  • the sieve uses a layered porous material.
  • the layered porous material has a melting point higher than 1800 ° C, the layered porous material does not react with the filtering raw material, and the layered porous material is any one of a metal, a non-metal, and a composite material. .
  • the metal is any one of molybdenum, titanium and zirconium
  • the non-metal is any one of carbon, silicon nitride and zirconium dioxide
  • the composite material adopts the above-mentioned metal and non-metal The material is compositely prepared.
  • the atmosphere is an argon atmosphere, a nitrogen atmosphere or an air atmosphere.
  • the mixture is heated to carry out a reduction reaction, and the temperature is raised to 1300 to 2000 ° C, followed by heat preservation.
  • the temperature increase rate is 3-7 ° C/min.
  • the temperature is raised to 1300 to 2000 ° C, and the heat is kept for 2 to 10 hours.
  • the mixture is ball milled and uniformly mixed.
  • the mixture is ball-milled and uniformly mixed, and the powdery mixture is press-formed.
  • the ilmenite composite ore is any one of ilmenite, vanadium titano-magnetite, titanium concentrate, and iron concentrate, or a combination of any two or more thereof.
  • the carbon-containing reducing agent is any one of activated carbon, graphite powder, charcoal, petroleum coke, and pitch, or a combination of any two or more thereof.
  • a filtering device for the method for extracting iron and titanium from a ferrotitanium composite ore the filtering device being specifically used in the step (6) to make the liquid slag phase from a solid state
  • the titanium-rich phase material particles are separated, and the main portion of the filtration apparatus includes a raw material carrying container, a filtration layer, and a slag phase recovery device from top to bottom.
  • the raw material carrying container is provided with a piston which is in close contact with the inner wall of the container, and the piston is free to move up and down.
  • the side of the slag phase recovery device has an air outlet, and the air outlet is connected to a vacuum system for reducing the air pressure of the slag phase recovery device to achieve the filtering effect of the filter layer.
  • the raw material carrying container, the filter layer and the slag phase recovery device of the filtering device can be detached and sealed and assembled to each other.
  • the process flow is simple and compact, the process parameters are stable, and the production cost is low;
  • titanium enrichment efficiency is high, and can be widely applied to various grades of ilmenite composite ore.
  • 1 is a flow chart of a method for extracting iron and titanium from a ferrotitanium composite ore
  • FIG. 2 is a schematic structural view of a filtering device
  • Example 3 is an X-ray diffraction pattern of a lower partial reduction product obtained under an argon atmosphere in Example 1 of the present invention
  • Example 4 is an X-ray diffraction pattern of an upper partial reduction product obtained under an argon atmosphere in Example 1 of the present invention
  • Figure 5 is an X-ray diffraction spectrum of a portion of the product on the filter screen after filtration under reduced pressure in Example 1 of the present invention
  • Example 6 is an X-ray diffraction spectrum of a portion of a product under the filter after separation and filtration under reduced pressure in Example 1 of the present invention
  • Figure 7 is an X-ray diffraction spectrum of the upper partial reduction product obtained under a nitrogen atmosphere in Example 2 of the present invention.
  • Example 8 is an X-ray diffraction spectrum of a part of a product on a filter screen after pressure filtration separation in Example 2 of the present invention.
  • Figure 9 is an X-ray diffraction spectrum of a portion of the product on the filter screen after filtration under reduced pressure in Comparative Example 1 of the present invention.
  • Figure 10 is an X-ray diffraction spectrum of a portion of the product on the filter after separation by atmospheric filtration in Comparative Example 2 of the present invention.
  • the ilmenite composite ore is a general term for a class of ores, including various kinds of ore and titanium-rich ores such as vanadium-titanium magnetite in the Panxi area and Chengde area of China, including ilmenite. At least one of vanadium titano-magnetite, titanium concentrate, iron concentrate and the like.
  • the ferrotitanium composite ore can be pretreated in a crushing device such as a vibration mill, which can increase the surface area of the ore and facilitate subsequent sufficient reaction;
  • the ball mill After the carbonaceous reducing agent is added to the raw material, the ball mill can be uniformly mixed and the powder can be press-formed;
  • the carbonaceous reducing agent is used to provide a carbon component that is reduced in the reaction, and specifically includes at least one of activated carbon, graphite powder, charcoal, petroleum coke, asphalt, and the like;
  • the amount of carbon-containing reducing agent is calculated according to the chemical reaction dose ratio, and the carbothermal reduction process is controlled to a suitable degree, so that the iron oxides in the raw materials are all reduced to metallic iron, and the titanium oxide is all reduced to carbon. Titanium oxide, titanium oxynitride or a mixture of the two;
  • the mixture is heated and subjected to a reduction reaction in a furnace such as a blast furnace or an electric furnace having a certain atmosphere, and the certain atmosphere may be argon gas, nitrogen gas, air or a mixture thereof;
  • the temperature After reaching the set temperature, the temperature is kept for a period of time, and the holding time varies from 1 to 15 hours depending on the situation, more preferably 2 to 10 hours;
  • the iron oxides in the ferrotitanium composite ore material are all reduced to metal iron, and the titanium oxide is all reduced to titanium oxycarbonate, titanium oxynitride or a mixture thereof;
  • the reduced product molten iron is directly discharged at a high temperature due to a relatively high specific gravity, and an initial product in which a titanium-rich phase substance and a slag phase substance are dispersed is obtained; further, it may also be used.
  • the reduction product is pretreated by cooling, crushing, pulverizing, wet grinding, refining, etc.
  • the wet powder is placed in a magnetic separation device for magnetic separation to fully remove the iron phase components therein, wherein the magnetic separation device It can be used to process circulating raw materials;
  • a certain amount of slag phase matching material is blended in the preliminary product, and the material comprises at least one of MgO, Al 2 O 3 , CaO, and SiO 2 , for example, MgO, Al 2 O may be blended into the initial product.
  • MgO, Al 2 O may be blended into the initial product.
  • CaO, SiO 2 or a combination of any two of MgO, Al 2 O 3 , CaO, SiO 2 in the initial product, or MgO, Al 2 O in the initial product 3.
  • the amount of the slag phase compounding material to be blended is controlled so that the titanium-rich phase material and the slag phase material in the preliminary product have a melting point difference, and the melting point of the slag phase component after the blending is lower than the melting point of the titanium-rich phase material.
  • the slag phase mixing step can be carried out directly at high temperatures
  • the prepared mixture that is, the filtered raw material is placed in a filtering device, and filtered at a certain temperature, which ensures that the titanium-rich phase material is solid while maintaining the slag phase component in a liquid state and having a certain fluidity.
  • the above certain temperature range is 600 to 2000 ° C, more preferably 800 to 1800 ° C;
  • a certain pressure difference can be constructed and maintained in the filtering device to make the filtering process proceed more quickly and thoroughly, such as by pressurizing the upper part of the filtering device, decompressing the lower part, or a combination of the two;
  • the filter device body includes the raw material carrier from top to bottom.
  • the container, the filter layer and the slag phase recovery device are three parts which can be freely disassembled and sealed and assembled.
  • the upper material carrying container is provided with a piston which is closely attached to the inner wall of the container, and the piston can move up and down for pressurization; the lower slag phase recovery device side Connected to the vacuum system to reduce the pressure in the lower part of the filter.
  • the reaction materials, metal materials such as molybdenum, titanium, zirconium, etc., non-metal materials such as carbon, silicon nitride, zirconium dioxide, etc., and composite materials of the above two types of materials can be used for the construction of filtration equipment.
  • the choice of layer materials, in addition to meet the same requirements as the filter equipment materials, should also ensure that the material is a layered porous structure, which plays
  • the ferrotitanium composite ore is subjected to high-temperature carbothermal reduction, initial separation of iron and slag phase distribution, and the filtered raw material is placed in a raw material carrying container of the filtering device.
  • the upper and lower portions of the filtering layer can be constructed in the following three ways. The pressure difference between them enables effective filtering:
  • the filtration equipment is cooled to room temperature and then disassembled into upper, middle, and lower portions, and an enriched titanium-rich phase material can be obtained in the upper portion of the filtration layer, and a slag phase material can be obtained in the lower portion of the filtration layer to realize recovery and secondary utilization.
  • the upper part of the reduced product is crushed and ground to below 200 mesh, and Al 2 O 3 , MgO, CaO and SiO 2 powders are dispensed, and separated by filtration under reduced pressure at 1800 ° C, and finally solid particles are obtained on the filter line.
  • the structure was analyzed by X-ray diffraction, as shown in Figure 5 of the specification, the main phase was titanium oxide (TiC 0.5 O 0.5 ), the composition analysis showed that the purity of the titanium component was 95.3%; the white block was obtained in the lower part of the filter. After crushing and grinding into powder, the structure was analyzed by X-ray diffraction. As shown in Fig. 6 of the specification, the main phase was CaAl 2 Si 2 O 8 -CaMgSi 2 O 6 , and the composition analysis showed that the titanium component mass fraction was 4.9%. .
  • TiC x N y O z titanium oxynitride
  • unreduced components TiC x N y O z
  • the upper part of the reduced product is crushed and ground to below 200 mesh, and Al 2 O 3 , MgO, CaO and SiO 2 powders are dispensed, separated by pressure filtration at 1500 ° C, and finally solid particles are obtained on the filter line.
  • the structure was analyzed by X-ray diffraction.
  • the main phase was titanium oxycarbonitride (TiC x N y O z ), and the composition analysis showed that the purity of the titanium component was 97.2%;
  • the white block was crushed and ground into powder and analyzed by X-ray diffraction.
  • the results showed that the main phase was CaAl 2 Si 2 O 8 -CaMgSi 2 O 6 , and the composition analysis showed that the mass fraction of the titanium component was 3.6%.
  • the X-ray diffraction analysis results of the reduced products show After selective thermal reduction by carbon, the iron oxide in the ilmenite composite ore is reduced to metallic iron, the titanium oxide is reduced to titanium oxynitride (TiC x N y O z ), and the other components are not reduced. .
  • the reduced product is crushed and ground to below 200 mesh, and is mixed with Al 2 O 3 , MgO, CaO and SiO 2 powders, and separated by pressure filtration at 800 ° C, and finally solid particles are obtained in the upper portion of the filtration layer, and X is obtained.
  • the structure was analyzed by ray diffraction, and the main phase was titanium oxycarbonitride (TiC x N y O z ), and the composition analysis showed that the purity of the titanium component was 96.8%.
  • the iron oxide in the ilmenite complex is reduced to metal iron deposited in the lower part
  • the titanium oxide is reduced to titanium oxide (TiC 0.5 O 0.5 ) and other unreduced components (Al 2 O 3 -MgO-CaO-SiO 2 ) is in the upper part.
  • the upper part of the reduced product was crushed and ground to below 200 mesh, and then separated by filtration under reduced pressure at 1800 ° C. Finally, no white solid was obtained in the lower portion of the filter, and a powder was obtained in the upper portion, and the result of X-ray diffraction analysis was as described in the specification.
  • the iron oxide in the ilmenite complex is reduced to metal iron deposited in the lower part
  • the titanium oxide is reduced to titanium oxide (TiC 0.5 O 0.5 ) and other unreduced components (Al 2 O 3 -MgO-CaO-SiO 2 ) is in the upper part.
  • the upper part of the reduced product was crushed and ground to below 200 mesh, and Al 2 O 3 , MgO, CaO and SiO 2 powders were added, and the mixture was separated by atmospheric filtration at 1800 ° C, and finally no white solid was obtained in the lower portion of the filter.
  • the powder is obtained in the upper part, and the X-ray diffraction analysis result is as shown in FIG. 10 of the specification, indicating that the titanium component in the ilmenite composite ore cannot be separated by high-temperature filtration to obtain an effective richness without using a vacuum or pressurized filtration method. set.
  • the invention not only solves the problems of material consumption and environmental pollution caused by the acid leaching process, but also avoids the pretreatment process such as crushing, wet grinding and ultrasonic treatment in the flotation process, and completes the ferrotitanium through equipment such as blast furnace and electric furnace.
  • the anode material of the process can also be used for the production of titanium tetrachloride and titanium dioxide, and it is expected to greatly improve the technical and economic indicators of the titanium product refining process.
  • the special nature of the filter material makes the requirements of the filter material more stringent, which leads to the failure of the existing filtration equipment to complete the high-temperature filtration separation process in the new process.
  • the present invention constructs a set of high-temperature filtering equipment matched with it, which can effectively realize the liquid slag phase and solid carbon (nitrogen) titanium oxide (TiC x (N y ) O at high temperature).
  • TiC x (N y ) O liquid slag phase and solid carbon (nitrogen) titanium oxide (TiC x (N y ) O at high temperature).
  • the invention can significantly improve the utilization rate of the titanium component in the ferrotitanium composite ore, and the existing large amount of ferrotitanium composite ore resources can be recycled and enriched by high efficiency and environmental protection, which can not only alleviate the current situation of the shortage of titanium resources, but also more important. Is expected to significantly reduce the current titanium smelting process The cost of the economy and the large-scale continuous production of titanium products provide a new way for the innovation and development of titanium metallurgy technology.

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Abstract

一种以钛铁复合矿为原料提取铁、钛的方法及过滤设备。所述方法将钛铁复合矿原料中配入含碳还原剂,均匀混合后,在氩气或空气气氛下升至高温还原,使其中的铁组分还原成金属铁,钛组分则转化为碳氧化钛和碳氮氧化钛中一种或两种。铁水由于比重较高沉积于下方可直接分离,弥散分布着碳氧化钛、碳氮氧化钛颗粒的渣相经调配组成后,在高温下经过滤网过滤分离,最终获得品位高于95%的碳(氮)氧化钛产品。同时还提供了适用于上述方法的过滤装置,该设备具有高熔点低活性的多孔层状过滤材料。

Description

一种以钛铁复合矿为原料提取铁、钛的方法及过滤设备 技术领域
本发明主要属于有色金属冶金领域,具体涉及一种以钛铁复合矿为原料提取铁、钛的方法及过滤设备。
背景技术
钛铁复合矿,如我国攀西地区、河北承德地区的钒钛磁铁矿,其分布广泛、储量丰富、资源巨大,并且钛铁复合矿中钛资源占全国钛资源的91%以上,具有极高的综合利用价值。目前工业上钛铁复合矿的冶炼大多采用传统的“高炉—转炉”工艺,矿物中的铁、钒氧化物被还原成含钒铁水,而钛组分则主要以低价氧化物的形式进入渣中,由于炉料和冶炼技术水平的差异,渣铁比相对较高,大量的钛渣难以有效处理,大部分被加工成水渣、矿渣碎石、膨胀矿渣和矿渣珠等经济价值较低的建材用料,其中的钛组分(以TiO2计约为25%)无法得到有效利用,这对我国丰富的钛资源造成了巨大的浪费。
近年来研究者提出用“转底炉直接还原—电炉熔分—细磨磁选—酸洗”工艺来处理钒钛磁铁矿,实现了渣中钛组分的回收。相较于“高炉—转炉”冶炼工艺,该工艺路线在降低了吨铁成本和流程能耗的同时,由于没有破坏矿相结构和酸溶性,降低了后续酸洗工艺中酸的用量,从而提高了后期酸溶去除高钛渣中钙镁氧化物的效率。
对于钛渣的处理,近年提出的氯化法、硫酸法虽然是较具工业开发价值的工艺路线,但是由于原料中脉石成分居多,导致大量消耗原辅材料,相应经济成本较高。同时,这些工艺都还存在回收利用率不 高、工艺流程较长、环境污染等问题。
针对现行钛铁复合矿工艺流程存在的问题,朱鸿民等在USTB熔盐电解制备金属钛工艺的基础上,提出了钛铁复合矿冶金新流程。该流程首先通过可控碳热选择性还原的方式使钛铁复合矿转变成铁水、碳氧化钛(TiCxOz)和渣相组分(Al2O3、MgO、CaO、SiO2)的混合物,然后采用湿法酸浸工艺去除渣相组分,从而实现碳氧化钛的富集。最终得到纯度90%以上的碳氧化钛既可作为USTB钛电解工艺原料,又可用于生产四氯化钛和钛白粉。与前几种工艺相比,该流程将还原程度控制在钛氧化物被还原成碳氧化钛(TiCxOz)的状态,实现了与USTB钛电解工艺的对接,并且提高了后续酸浸工艺分离的效率,在有效降低USTB钛电解工艺成本的同时,大大提高了钛铁复合矿中钛的利用率。朱鸿民等基于该新流程,又提出了通过浮选工艺替换酸浸工艺实现碳氧化钛和渣相组分的有效分离,成功避开了湿法酸浸工艺存在物料消耗大和环境污染的问题,降低了整个流程的经济和环境成本,实现了钛铁复合矿冶金新流程的进一步优化。然而,浮选工艺本身也存在预处理工序较多、流程冗长等缺点。
同时,上述各工艺从工艺流程、资源消耗、环境污染以及对钛的提取利用率上,都存在进一步改进的空间,导致了一定程度的流程冗长、处理过程中资源消耗较大、不够环保等不足之处,反映在产业上则体现为钛的提取相对困难、价格较高,不利于钛的大规模产业应用,因此,亟待提出更为先进和优化的工艺流程以及与之相匹配的设备。
发明内容
针对上述问题,本发明公开了一种以钛铁复合矿为原料提取铁、钛的方法及设备,本发明所公开的以钛铁复合矿为原料提取铁、钛的方法采用了“高温可控碳热还原—渣相调配—高温过滤分离”的新的成套工艺流程来实现钛铁复合矿中钛成分的分离和富集;针对上述新工艺流程,本发明还公开了一种特定的用于上述新工艺流程的高温过滤分离设备,以有效地实现对该新工艺流程中的混合物在高温下的分离。
本发明是通过以下技术方案实现的:
一种以钛铁复合矿为原料提取铁、钛的方法,所述方法包括以下步骤:
(1)以钛铁复合矿为原料,将原料进行破碎预处理;
(2)往破碎预处理后的钛铁复合矿中配入含碳还原剂,均匀混合,得到包含钛铁复合矿和含碳还原剂的混合物;
(3)在一定气氛下,对步骤(2)获得的所述混合物升温进行还原反应,得到包含富钛相物质、铁和渣相的还原产物;
(4)将所述还原产物中的铁排出分离,得到包含富钛相物质和渣相的初分产物,并收集排出分离的铁,完成铁的提取;
(5)调控所述初分产物中渣相的组成,得到过滤原料,在所述过滤原料中,渣相和富钛相物质具有熔点差;
(6)在高温下,将所述过滤原料经过滤网进行过滤,使液态的渣相从固态的富钛相物质颗粒中分离,制备得到纯度高于95%的富钛相物质,完成钛的提取。其中,纯度高于95%的富钛相物质是指制备获 得的富钛相物质中碳氧化钛、和/或碳氮氧化钛的质量百分数高于95%。
进一步地,所述富钛相物质包含TiCmOn和TiCxNyOz中的至少一种,其中m+n=1,x+y+z=1,且0<m,n,x,y,z<1。
进一步地,步骤(2)中配入的所述含碳还原剂的量能够将所述破碎预处理后的钛铁复合矿中的铁氧化物全部还原成金属铁并且能够将所述破碎预处理后的钛铁复合矿中的钛氧化物全部还原成碳氧化钛和碳氮氧化钛中一种或两种;即步骤(2)中配入的所述含碳还原剂的量不少于将所述破碎预处理后的钛铁复合矿中的铁氧化物还原成铁所需的含碳还原剂的量与将所述破碎预处理后的钛铁复合矿中的钛氧化物还原成所述富钛相物质(碳氧化钛和碳氮氧化钛中一种或两种)所需的含碳还原剂的量之和。
进一步地,步骤(2)中配入的所述含碳还原剂的质量为所述破碎预处理后钛铁复合矿质量的20%-30%。
进一步地,步骤(5)中,调控所述初分产物中渣相的组成具体为:在1300~2000℃下,往所述初分产物中配入渣相调配材料,以使得调配后的初分产物中,渣相的熔点低于富钛相物质的熔点。
进一步地,所述渣相调配材料为MgO、Al2O3、CaO和SiO2中的任意一种或任意两种以上组合。
进一步地,所述渣相调配材料的形态为颗粒状或粉末状。
进一步地,步骤(6)中,将所述过滤原料经过滤网进行过滤,具体为:采用过滤网上部加压和过滤网下部减压两种方式中的一种方 式或两种方式结合。
进一步地,在步骤(6)中,在800~1800℃的温度下,将所述过滤原料经过滤网进行过滤。
进一步地,在步骤(6)中,所述滤网采用层状多孔材料。
进一步地,所述层状多孔材料的熔点高于1800℃,所述层状多孔材料不与所述过滤原料反应,并且所述层状多孔材料为金属、非金属和复合材料中的任意一种。
进一步地,所述金属为钼、钛和锆中的任意一种,所述非金属为碳、氮化硅和二氧化锆中的任意一种,所述复合材料采用上述金属和非金属两类材料复合制备而成。
进一步地,步骤(3)中,所述气氛为氩气气氛、氮气气氛或空气气氛。
进一步地,步骤(3)中,对所述混合物升温进行还原反应,升温至1300~2000℃后进行保温。
进一步地,步骤(3)中,控制升温进行还原反应的过程中,升温速率为:3-7℃/min。
进一步地,步骤(3)中,升温至1300~2000℃后进行保温,保温时间为2-10小时。
进一步地,在步骤(2)之后和步骤(3)之前,将所述混合物球磨并混合均匀。
进一步地,在步骤(2)之后和步骤(3)之前,将所述混合物球磨并混合均匀后,将粉末状的混合物压制成型。
进一步地,所述钛铁复合矿为钛铁矿、钒钛磁铁矿、钛精矿和铁精矿中的任意一种或者任意两种以上的组合。
进一步地,所述含碳还原剂为活性炭、石墨粉、木炭、石油焦和沥青中的任意一种或者任意两种以上的组合。
一种过滤设备,所述过滤设备用于所述一种以钛铁复合矿为原料提取铁、钛的方法,所述过滤设备具体用于步骤(6)中,使液态的渣相从固态的富钛相物质颗粒中分离,所述过滤设备的主体部分从上至下包括原料承载容器、过滤层和渣相回收装置。
进一步地,所述原料承载容器配有一个紧贴于容器内壁的活塞,活塞可自由上下移动。
进一步地,所述渣相回收装置的侧面具有出气孔,所述出气孔与真空系统连接,真空系统用于降低渣相回收装置的气压,以实现过滤层的过滤作用。
进一步地,所述过滤设备的原料承载容器、过滤层和渣相回收装置能够相互拆卸和密封组装。
本发明的有益技术效果:
1、工艺流程简单紧凑、工艺参数稳定、生产成本低;
2、无毒、污染小、环境友好;
3、钛的富集效率高,而且可广泛适用于各种品位的钛铁复合矿。
附图说明
图1为以钛铁复合矿为原料提取铁、钛的方法流程图;
图2为过滤设备的结构示意图;
图3为本发明实施例1中在氩气气氛下获得的下部分还原产物的X射线衍射图谱;
图4为本发明实施例1中在氩气气氛下获得的上部分还原产物的X射线衍射图谱;
图5为本发明实施例1中减压过滤分离后,过滤网上部分产物的X射线衍射图谱;
图6为本发明实施例1中减压过滤分离后,过滤网下部分产物的X射线衍射图谱;
图7为本发明实施例2中在氮气气氛下下获得的上部分还原产物的X射线衍射图谱;
图8为本发明实施例2中加压过滤分离后,过滤网上部分产物的X射线衍射图谱;
图9为本发明比较例1中减压过滤分离后,过滤网上部分产物的X射线衍射图谱;
图10为本发明比较例2中常压过滤分离后,过滤网上部分产物的X射线衍射图谱;
附图标记:1.原料承载容器、2.过滤层、3.渣相回收装置、4.活塞、5、过滤原料、6.富钛相物质、7.渣相。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细描述。应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
相反,本发明涵盖任何由权利要求定义的在本发明的精髓和范围上做的替代、修改、等效方法以及方案。进一步,为了使公众对本发明有更好的了解,在下文对本发明的细节描述中,详尽描述了一些特定的细节部分。对本领域技术人员来说没有这些细节部分的描述也可以完全理解本发明。
在本发明中,所述钛铁复合矿是一类矿石的统称,包含了如我国攀西地区、承德地区的钒钛磁铁矿等各种富含钛和铁的矿石,具体包括钛铁矿、钒钛磁铁矿、钛精矿、铁精矿等矿石中的至少一种。
在工艺开始时可在振动磨等破碎设备中对钛铁复合矿进行破碎等预处理,这样可增加矿石的表面积,利于后续充分反应;
在原料中配入含碳还原剂后可进行球磨混合均匀并将粉末压制成型;
含碳还原剂用于提供反应中还原的碳成分,具体包括活性炭、石墨粉、木炭、石油焦、沥青等中的至少一种;
含碳还原剂配入量按照化学反应剂量比计算得出,将碳热还原过程控制在合适的进行程度,使得原料中的铁氧化物全部被还原成金属铁,钛氧化物全部被还原成碳氧化钛、碳氮氧化钛或二者的混合物;
在具有一定气氛的高炉或电炉等设备中对所述混合物升温进行还原反应,一定气氛可以是氩气、氮气、空气或者其混合物;
缓慢升温到约1200~2200℃,更优选为1300~2000℃;
在到达设定温度后保温一段时间,根据情况保温时间在1~15小时不等,更优选为2~10小时;
经过高温还原反应,钛铁复合矿原料中的铁氧化物全部被还原成金属铁,钛氧化物全部被还原成碳氧化钛、碳氮氧化钛或二者的混合物;
还原反应进行完毕后,还原产物铁水由于比重相对较高沉于底部,可在高温下直接排出,得到弥散分布着富钛相物质和渣相物质的初分产物;更进一步地,也可以采用如冷却、破碎、粉碎、湿磨、细化等工艺对还原产物预处理后,将湿化粉料置于磁选设备中进行磁选分离,以充分除去其中的铁相组分,其中磁选设备可采用能处理环形循环流动原料的;
在初分产物中配入一定量的渣相调配材料,这些材料包含MgO、Al2O3、CaO、SiO2中的至少一种,譬如:可以往初分产物中配入MgO、Al2O3、CaO、SiO2中任意一种,或者往初分产物中配入MgO、Al2O3、CaO、SiO2中任意两种的组合,或者往初分产物中配入MgO、Al2O3、CaO、SiO2中任意三种的组合,或者往初分产物中配入MgO、Al2O3、CaO、SiO2四种材料。配入的渣相调配材料的量控制在能够使初分产物中的富钛相物质和渣相物质具有熔点差即可,调配后渣相组分的熔点低于富钛相物质的熔点。
为了使得流程紧凑优化,渣相调配步骤可直接在高温下进行;
将调配完毕的混合物即过滤原料置于过滤设备中,在一定的温度下进行过滤,该温度保证了富钛相物质为固态的同时,使渣相组分保持为液态并具有一定的流动性,从而实现二者的有效分离;具体而言,上述一定的温度范围为600~2000℃,更优选为800~1800℃;
过滤设备中可构造出并保持住一定的压力差,以使过滤工序进行得更为迅速和彻底,如通过过滤设备上部加压、下部减压或者二者结合的方式;
更进一步地,为了上述工艺流程中高温过滤工序的顺利进行,针对过滤工序的特点,设计了与之相匹配的过滤设备,如说明书附图2所示,过滤设备主体从上至下包括原料承载容器、过滤层、渣相回收装置,三部分可自由拆卸和密封组装,上部原料承载容器配有一个紧贴于容器内壁的活塞,活塞可自由上下移动用于加压;下部渣相回收装置侧面与真空系统连接,用于降低过滤层下部气压。由于整个过滤过程在高温(800~1800℃)下进行,并且整个过滤设备与过滤原料(包括渣相(Al2O3、MgO、CaO、SiO2)及富钛相物质(TiCx(Ny)Oz,x+y+z=1)在高温下长时间接触,因而过滤设备的构造必须选择熔点高并且在室温到高温下均不与所述过滤原料(包括渣相及富钛相物质)反应的材料,金属类材料如钼、钛、锆等,非金属材料如碳、氮化硅、二氧化锆等,以及以上述两类材料的复合材料均可用于过滤设备的构建。对于过滤层材料的选择,在满足与过滤设备材料相同的要求外,还应当保证材料为层状多孔结构,从而起到较好的过滤作用。
钛铁复合矿经高温碳热还原、初分除铁和渣相调配后得到过滤原料置于过滤设备的原料承载容器中,在一定的温度下,可采用如下三种方式构造过滤层上部和下部之间的压力差,从而实现有效过滤:
1、上部加压:使与原料承载容器连接的加压活塞向下运动,渣相在压力的作用下穿过过滤层流入渣相回收装置,富钛相物质则富集 在过滤层上部;
2、下部减压:利用与渣相回收装置连接的真空系统,使过滤层下部处于相对较低的气压状态,上部渣相在大气压作用下穿过过滤层流入渣相回收装置,富钛相物质则富集在过滤层上部;
3、上部加压与下部减压相结合:使与原料承载连接的加压活塞向下运动的同时,利用与渣相回收装置连接的真空系统给过滤层下部减压,构造过滤层上部和下部之间的压力差。
待过滤工序完成,将过滤设备冷却至室温后拆卸成上中下三部分,在过滤层上部可以得到富集的富钛相物质,过滤层下部可以得到渣相物质,实现回收和二次利用。
以下详细实施例及比较例是为了更好地显示以上公开的本发明技术的特殊功效或特征,按照众所共知的约定,本发明专利要保护的核心内容范围并不仅仅限于以下实施例所提供的工艺技术参数和条件。
实施例1
称取200.0g经振动磨破碎成细小颗粒的钛铁矿(FeO:42.7%,TiO2:47.5%),配入42.9g石墨粉(碳含量99.9%),然后置于行星式球磨机中混合均匀,球磨后粉末压制成型并置于高温炉内,控制炉内为氩气气氛并缓慢升温至2000℃,保温3小时后冷却至室温,得到分为上下两个部分的还原产物,下部分的还原产物经X射线衍射分析其结构,如说明书附图3所示,为还原产物铁;上部分的还原产物经X射线衍射分析其结构,如说明书附图4所示,为碳氧化钛(TiC0.5O0.5) 与未被还原组分的混合物。可以看出经碳热选择性还原后,钛铁复合矿中的铁氧化物被还原成金属铁沉积在下部,钛氧化物被还原成碳氧化钛(TiC0.5O0.5,x+y+z=1)和其它未被还原的组分(Al2O3-MgO-CaO-SiO2)处于上部。将还原产物上部块体破碎并研磨至200目以下,配入Al2O3、MgO、CaO和SiO2粉末,在1800℃下以减压过滤的方式进行分离,最终在过滤网上部得到固体颗粒,经X射线衍射分析其结构,如说明书附图5所示,其主相为碳氧化钛(TiC0.5O0.5),成分分析显示钛组分纯度为95.3%;在过滤网下部得到白色块体,破碎研磨成粉末后经X射线衍射分析其结构,如说明书附图6所示,其主相为CaAl2Si2O8-CaMgSi2O6,成分分析显示其中钛组分质量分数为4.9%。
实施例2
称取200.0g经振动磨破碎成细小颗粒的高钛渣(Fe2O3:10.5%,TiO2:77.7%),配入51.5g石墨粉(碳含量99.9%),然后置于行星式球磨机中混合均匀,球磨后粉末压制成型并置于高温炉内,控制炉内为氮气气氛并缓慢升温至1300℃,保温7小时后冷却至室温,得到分为上下两个部分的还原产物,还原产物铁沉积在下部,上部经X射线衍射分析其结构,如说明书附图7所示,为碳氮氧化钛(TiCxNyOz)与未被还原组分的混合物。将还原产物上部块体破碎并研磨至200目以下,配入Al2O3、MgO、CaO和SiO2粉末,在1500℃下以加压过滤的方式进行分离,最终在过滤网上部得到固体颗粒,经X射线衍射分析其结构,如说明书附图8所示,其主相为碳氮氧化钛(TiCxNyOz),成分分析显示钛组分纯度为97.2%;在过滤网下部得到白色块体,破碎 研磨成粉末后经X射线衍射分析其结构,结果显示其主相为CaAl2Si2O8-CaMgSi2O6,成分分析显示其中钛组分质量分数为3.6%。
实施例3
称取200.0g经振动磨破碎成细小颗粒的铁精矿(Fe2O3:47.3%,FeO:29.2%,TiO2:12.4%),配入38.6g石墨粉(碳含量99.9%),然后置于行星式球磨机中混合均匀,球磨后粉末压制成型后置于高温炉内,在半开放系统中缓慢升温至1700℃,保温5小时后冷却至室温,对还原产物的X射线衍射分析结果显示,经碳热选择性还原后,钛铁复合矿中的铁氧化物被还原成金属铁,钛氧化物被还原成碳氮氧化钛(TiCxNyOz),其它组分则没有被还原。将还原产物破碎并研磨至200目以下,配入Al2O3、MgO、CaO和SiO2粉末,在800℃下以加压过滤的方式进行分离,最终在过滤层上部得到固体颗粒,经X射线衍射分析其结构,其主相为碳氮氧化钛(TiCxNyOz),成分分析显示钛组分纯度为96.8%。
比较例1
称取200.0g经振动磨破碎成细小颗粒的钛铁矿(FeO:42.7%,TiO2:47.5%),配入42.9g石墨粉(碳含量99.9%),然后置于行星式球磨机中混合均匀,球磨后粉末压制成型后置于高温炉内,控制炉内为氩气气氛并缓慢升温至2000℃,保温3小时后冷却至室温,对还原产物的X射线衍射分析结果显示,经碳热选择性还原后,钛铁复合矿中的铁氧化物被还原成金属铁沉积在下部,钛氧化物被还原成碳氧化钛(TiC0.5O0.5)和其它未被还原的组分(Al2O3-MgO-CaO-SiO2)处于 上部。将还原产物上部破碎并研磨至200目以下,然后在1800℃下以减压过滤的方式进行分离,最终在过滤网下部并未得到白色固体,而在上部得到粉末,X射线衍射分析结果如说明书附图9所示,与说明书附图4对比可知上部固体与还原产物成分一致,说明如果不调配渣相组成形成碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)与渣相的熔点差异,高温过滤分离工序无法实施,钛铁复合矿中的钛组分无法有效富集。
比较例2
称取200.0g经振动磨破碎成细小颗粒的钛铁矿(FeO:42.7%,TiO2:47.5%),配入42.9g石墨粉(碳含量99.9%),然后置于行星式球磨机中混合均匀,球磨后粉末压制成型后置于高温炉内,控制炉内为氩气气氛并缓慢升温至2000℃,保温3小时后冷却至室温,对还原产物的X射线衍射分析结果显示,经碳热选择性还原后,钛铁复合矿中的铁氧化物被还原成金属铁沉积在下部,钛氧化物被还原成碳氧化钛(TiC0.5O0.5)和其它未被还原的组分(Al2O3-MgO-CaO-SiO2)处于上部。将还原产物上部破碎并研磨至200目以下,配入Al2O3、MgO、CaO和SiO2粉末,在1800℃下以常压过滤的方式进行分离,最终在过滤网下部并未得到白色固体,而在上部得到粉末,X射线衍射分析结果如说明书附图10所示,说明如果不采用减压或加压的过滤方式,钛铁复合矿中的钛组分无法经高温过滤分离得到有效富集。
本发明不仅解决了酸浸工艺带来的物料消耗巨大和环境污染的问题,而且避开了浮选工艺中破碎、湿磨、超声处理等预处理工序, 在通过高炉、电炉等设备完成钛铁复合矿中铁、钛组分的还原和铁水的排出后,创造性地在高温下直接配入配入Al2O3、MgO、CaO或SiO2粉末调整渣相组成,形成碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)与渣相组分的熔点差,然后在高温下经过滤分离设备过滤分离为液态渣相和富集的固态碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)颗粒。整套工艺流程紧凑高效,最终得到的碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)品位高达95%以上,不仅可以直接作为USTB熔盐电解制备金属钛工艺的阳极原料,同样可用于四氯化钛和钛白粉的生产,有望大大提高钛产品精制工艺的技术经济指标。
本发明的核心在于在高温下采用过滤分离的方式实现液态渣相与碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)颗粒的分离,然而现有的过滤设备大多在常温下使用,无法耐受高温;并且液态渣相与碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)颗粒在高温环境下的物理化学性质较为特殊,使得对过滤材料的要求更为严格,这就导致了现有过滤设备无法完成新工艺流程中的高温过滤分离工序。因此本发明在提出新工艺流程的基础上,构建了一套与之相匹配的高温过滤设备,可以有效地实现高温下液态渣相和固态碳(氮)氧化钛(TiCx(Ny)Oz,x+y+z=1)颗粒的分离,解决了现有过滤设备无法胜任高温过滤分离工序的问题,从而为本发明提出的新工艺流程的有效实施提供了保证。
本发明可以显著地提高钛铁复合矿中钛组分的利用率,使现有的大量钛铁复合矿资源得到高效环保的回收富集,这不仅可以缓解钛资源日益缺失的现状,更为重要的是有望大幅降低现行钛冶炼工艺的经 济成本,实现钛产品的大规模连续化生产,为钛冶金技术的革新发展提供一条新的途径。

Claims (24)

  1. 一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述方法包括以下步骤:
    (1)以钛铁复合矿为原料,将原料进行破碎预处理;
    (2)往破碎预处理后的钛铁复合矿中配入含碳还原剂,均匀混合,得到包含钛铁复合矿和含碳还原剂的混合物;
    (3)在一定气氛下,对步骤(2)获得的所述混合物升温进行还原反应,得到包含富钛相物质、铁和渣相的还原产物;
    (4)将所述还原产物中的铁排出分离,得到包含富钛相物质和渣相的初分产物,并收集排出分离的铁,完成铁的提取;
    (5)调控所述初分产物中渣相的组成,得到过滤原料,在所述过滤原料中,渣相和富钛相物质具有熔点差;
    (6)在高温下,将所述过滤原料经过滤网进行过滤,使液态的渣相从固态的富钛相物质颗粒中分离,制备得到纯度高于95%的富钛相物质,完成钛的提取。
  2. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述富钛相物质包含TiCmOn和TiCxNyOz中的至少一种,其中m+n=1,x+y+z=1。
  3. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(2)中配入的所述含碳还原剂的量能够将所述破碎预处理后的钛铁复合矿中的铁氧化物全部还原成金属铁并且能够将所述破碎预处理后的钛铁复合矿中的钛氧化物全部还原成碳氧化钛和碳氮氧化钛中一种或两种。
  4. 根据权利要求3所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(2)中配入的所述含碳还原剂的质量为所述破碎预处理后钛铁复合矿质量的20%-30%。
  5. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(5)中,调控所述初分产物中渣相的组成具体为:在1300~2000℃下,往所述初分产物中配入渣相调配材料,以使得调配后的初分产物中,渣相的熔点低于富钛相物质的熔点。
  6. 根据权利要求5所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述渣相调配材料为MgO、Al2O3、CaO和SiO2中的任意一种或任意两种以上组合。
  7. 根据权利要求6所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述渣相调配材料的形态为颗粒状或粉末状。
  8. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(6)中,将所述过滤原料经过滤网进行过滤,具体为:采用过滤网上部加压和过滤网下部减压两种方式中的一种方式或两种方式结合。
  9. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,在步骤(6)中,在800~1800℃的温度下,将所述过滤原料经过滤网进行过滤。
  10. 根据权利要求8所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,在步骤(6)中,所述滤网采用层状多孔材料。
  11. 根据权利要求10所述一种以钛铁复合矿为原料提取铁、钛的 方法,其特征在于,所述层状多孔材料的熔点高于1800℃,所述层状多孔材料不与所述过滤原料反应,并且所述层状多孔材料为金属、非金属和复合材料中的任意一种。
  12. 根据权利要求11所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述金属为钼、钛和锆中的任意一种,所述非金属为碳、氮化硅和二氧化锆中的任意一种,所述复合材料采用上述金属和非金属两类材料复合制备而成。
  13. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(3)中,所述气氛为氩气气氛、氮气气氛或空气气氛。
  14. 根据权利要求13所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(3)中,对所述混合物升温进行还原反应,升温至1300~2000℃后进行保温。
  15. 根据权利要求14所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(3)中,控制升温进行还原反应的过程中,升温速率为:3-7℃/min。
  16. 根据权利要求14所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,步骤(3)中,升温至1300~2000℃后进行保温,保温时间为2-10小时。
  17. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,在步骤(2)之后和步骤(3)之前,将所述混合物球磨并混合均匀。
  18. 根据权利要求17所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,在步骤(2)之后和步骤(3)之前,将所述混合物球磨并混合均匀后,将粉末状的混合物压制成型。
  19. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述钛铁复合矿为钛铁矿、钒钛磁铁矿、钛精矿和铁精矿中的任意一种或者任意两种以上的组合。
  20. 根据权利要求1所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述含碳还原剂为活性炭、石墨粉、木炭、石油焦和沥青中的任意一种或者任意两种以上的组合。
  21. 一种过滤设备,所述过滤设备用于权利要求1-20之一所述一种以钛铁复合矿为原料提取铁、钛的方法,其特征在于,所述过滤设备具体用于步骤(6)中,使液态的渣相从固态的富钛相物质颗粒中分离,所述过滤设备的主体部分从上至下包括原料承载容器、过滤层和渣相回收装置。
  22. 根据权利要求21所述一种过滤设备,其特征在于,所述原料承载容器配有一个紧贴于容器内壁的活塞,活塞可自由上下移动。
  23. 根据权利要求22所述一种过滤设备,其特征在于,所述渣相回收装置的侧面具有出气孔,所述出气孔与真空系统连接,真空系统用于降低渣相回收装置的气压,以实现过滤层的过滤作用。
  24. 根据权利要求22所述一种过滤设备,其特征在于,所述过滤设备的原料承载容器、过滤层和渣相回收装置能够相互拆卸和密封组装。
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