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EP3374531B1 - Procédé et appareil pour la déphosphoration du minerai de fer - Google Patents

Procédé et appareil pour la déphosphoration du minerai de fer Download PDF

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Publication number
EP3374531B1
EP3374531B1 EP16820328.9A EP16820328A EP3374531B1 EP 3374531 B1 EP3374531 B1 EP 3374531B1 EP 16820328 A EP16820328 A EP 16820328A EP 3374531 B1 EP3374531 B1 EP 3374531B1
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unit
iron ore
roasting
grinding
conditioning
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German (de)
English (en)
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EP3374531A1 (fr
Inventor
Luca TOMMASI
Florina Liliana ARSENE
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Danieli and C Officine Meccaniche SpA
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Danieli and C Officine Meccaniche SpA
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Priority claimed from PCT/IB2016/056794 external-priority patent/WO2017081646A1/fr
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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
    • C22B1/00—Preliminary treatment of ores or scrap
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting

Definitions

  • Embodiments described here concern a method and an apparatus for the dephosphorization of iron ore.
  • the iron ore is extracted from mines, typically open or subterranean.
  • mines typically open or subterranean.
  • contaminating compounds such as phosphorus, sulfur and arsenic.
  • compounds based on phosphorus, sulfur, arsenic, zinc, copper, lead and mercury which are the main contaminating compounds that are frequently found in ferrous mines.
  • the content of phosphorus-based compounds can also be more than 1% in weight, which greatly limits the use thereof.
  • the iron ore in particular consists to a large extent of small particles, with a diameter generally less than 0.1 mm, of an oolite form, that is, ovoid morphological structures that have generated through enucleation, very compact and very difficult to treat with the conventional technique of grinding and magnetic separation, and also by leaching.
  • the minerals containing phosphorus typically apatite minerals, Ca 5 (PO 4 )(F, Cl, OH), can be dispersed very finely in the ferrous matrix, which greatly limits the impact that grinding and also leaching can have.
  • a purpose of the present invention is to perfect a method for the dephosphorization of iron ore that makes available a final concentrate of iron ore with a content of phosphorus that is at least acceptable for the metallurgy industry.
  • US 3,402,041 discloses a known process for removing phosphorus from iron oxide-bearing materials such as iron ores and iron ore concentrates.
  • the Applicant has devised, tested and embodied the present invention to overcome the shortcomings of the state of the art and to obtain these and other purposes and advantages.
  • Embodiments described here concern a method for the dephosphorization of iron ore with a phosphorous content greater than 0.5% of magnetite, hematite or mixed type.
  • the method comprises: a pre-conditioning of the iron ore by means of a pre-conditioning compound solid or in solution, with a content less than 5% in weight of the total ferrous mixture, said pre-conditioning compound being able to induce, by subsequent heating, a stress inside the material; an oxidizing roasting of the iron ore; a subsequent leaching, to obtain a final concentrate with a reduced phosphorus content, with a reduction higher than 85%.
  • the pre-conditioning is preferably performed upstream of the oxidizing roasting.
  • the apparatus comprises a pre-conditioning unit of the iron ore operating through a pre-conditioning compound that generates gas when it is heated, an oxidizing roasting unit of the iron ore fed and a leaching unit from which a concentrate of iron ore is obtained with a reduced phosphorous content.
  • the present description also includes the intervals that derive from uniting or overlapping two or more intervals described, unless otherwise indicated.
  • the present description also includes the intervals that can derive from the combination of two or more values taken at different points, unless otherwise indicated.
  • Embodiments described here concern a method for the dephosphorization of iron ore.
  • Embodiments described here also concern the iron ore obtainable using the method for the dephosphorization of iron ore described here.
  • the dephosphorized iron ore obtainable according to the method described here can be used to produce steel.
  • embodiments described here concern an iron ore with an oolite ore structure.
  • a possible example of iron ore can provide a total content of iron of about 50-65% w/w and a mean content of phosphorus of about 0.8% w/w.
  • a big part of the phosphorus content is in the mineralogical form of apatite, or multiple inclusions of fine ferrous oxides carrying apatite.
  • Other minerals containing phosphorus in minimum parts or traces are also present, such as calcium-apatite.
  • Fig. 1 is used to describe embodiments of the method according to the present description, which include a pre-conditioning of the iron ore, with a phosphorus content greater than 0.5%, using a granulate or solution containing a pre-conditioning compound which, through subsequent heating, induces a stress inside the material, particularly the apatite, for example by developing a gas or a chemical attack on the phosphorus.
  • the pre-conditioning compound can be solid or in solution and with a content of less than 5% in weight of the total ferrous mix.
  • the pre-conditioning can be performed upstream of the oxidizing roasting.
  • the method then provides the oxidizing roasting of the iron ore and subsequent leaching, to obtain a final concentrate with a reduced phosphorus content, with a reduction of more than 85%.
  • the pre-conditioning of the iron ore using a granulate or solution containing a pre-conditioning compound which, through heating, generates a gas can provide to use a solution of calcium chloride (CaCl 2 ), or calcium carbonate (CaCO 3 ) or manganese chloride (MnCl 2 ), or iron chloride (FeCl 3 ).
  • the pre-conditioning of the iron ore due to a mechanism that not only generates stress on the level of the mineral matrix, also attacks the apatite, making it more soluble in the solution of the acid or base leaching agent and therefore improves the removal of the phosphorus in the subsequent leaching step, after the oxidizing roasting of the pre-conditioned ore.
  • a possible secondary grinding and a possible magnetic separation ( fig. 5 ) it is provided to immerse it in the solution or it is mixed with the granulate containing the pre-conditioning compound.
  • the pre-conditioning time can be as much as 3 hours, for example, but not restrictively, from 1 to 3 hours, in particular from 1.5 to 2.5 hours, for example 2 hours.
  • the material can be filtered and subjected to heating through drying, for example in a kiln or analogous drying device, or loaded directly into the roasting kiln.
  • a high concentration solution is used during immersion, for example up to about 30%, in particular from about 15% to about 30%, more particularly from about 20% to about 25%.
  • the pre-conditioning compound is CaCl 2 and that the solution has a high concentration, about 20-22%.
  • the operating conditions of the pre-conditioning of the iron ore can be:
  • the method can provide a mixing and homogenization of the granulate with the material, for example in a vertical or horizontal mixer.
  • the pre-conditioning time can be reduced to 1 hour, for example but not restrictively, it can go from 5 min to 1 hour, in particular from 10 min to 45 min, for example 30 min.
  • the material can be loaded directly into the roasting kiln.
  • a granulate of CaCl 2 is used with a mass percentage added to the iron ore, for example up to about 5%.
  • the operating conditions of the pre-conditioning of the iron ore can be:
  • the cracking effect of the oolite structures is increased, creating further new channels for the leaching agent to penetrate.
  • the pre-conditioning also contributes to creating new mineral phases which involve the phosphorus, such as for example phospho-chlorates, calcium phosphates (substitution by means of solid diffusion during the oxidizing roasting), allowing a better overall leaching of these mineral phases created ex novo.
  • the oxidizing roasting of the iron ore can be performed in an oxidizing atmosphere, in particular using air as high-temperature comburent, in particular for example at a temperature between about 800°C and 1050°C, in particular between 850° and 1000°C.
  • oxidizing roasting can not only modify the mineral phases present, it also has a cracking effect on the particles with oolite structure, creating micro-channels that promote the penetration of the leaching agent during leaching.
  • the operating conditions of the oxidizing roasting can be:
  • leaching can be performed with an acid leaching agent, or a base leaching agent.
  • acid leaching agent can be sulfuric acid (H 2 SO 4 ), nitric acid (HNO 3 ) or hydrochloric acid (HCl).
  • An example of a base leaching agent can be sodium hydroxide (NaOH). Applicant has found that the leaching agent, acid or base, reduces the content of apatite in the final concentrate thanks to the phenomenon of phosphorus leaching. The leaching phenomenon is facilitated and made operative by the cracking of the oolite structures obtained during oxidizing roasting, which exposes the phosphorus to the attack of the leaching agent. This effect is further increased, if combined with the pre-conditioning of the iron ore before oxidizing roasting, for the presumed chlorination of the apatite itself, as explained in more detail hereafter.
  • Leaching can be performed by immersing the material in a solution of leaching agent, which is kept stirred to guarantee an adequate mass transfer and to promote contact between the ore and the leaching agent, limiting the phenomenon of surface passivation. At the end of leaching, a filtration is provided, followed by washing and rinsing in water, to remove the leached phosphorus, preventing it from remaining in the final concentrate. Leaching can be performed, for example at a temperature between about 20°C and 60°C, and taking into account the influence of the temperature on the kinetics of the process and, at the same time, the variation in the solubility of the compounds present in solution as a function of the temperature: low temperatures allow to obtain better results.
  • leaching of a large part of the phosphorus can occur generally in about 15-30 minutes, or in order to reduce the content of other acid components such as silica and alumina, this period of time can be increased to 6 hours.
  • the leaching agent selected is H 2 SO 4 .
  • the concentration of H 2 SO 4 can reach 15%, in particular from 1% to 15%, more particularly from 3% to 5%.
  • the mass percentage of immersed solid of the iron ore subjected to leaching goes from about 10% to 65%.
  • the operating conditions of leaching with H 2 SO 4 can be:
  • the leaching agent selected is HCl.
  • the concentration of HCl can go for example up to 10%, in particular from 1% to 10%, more particularly from 1% to 4%.
  • the mass percentage of immersed solid of the ore subjected to leaching goes from about 10% to 65%.
  • the operating conditions of leaching with HCl can be:
  • Two-phase leaching consists in treating the iron ore by the acid or base leaching agent with a very high concentration in solution and with a higher percentage of solid at the beginning, so as to maximize the solubilized reaction speed of the phosphorus-based compounds.
  • the treatment is followed by a dilution of the concentration of the leaching agent and solid, so as to prevent a regression of the reaction equilibrium, optimizing the ratio between the quantity of leaching agent with respect to the removal of phosphorus and minimizing the leaching times.
  • Fig. 2 is used to describe embodiments, combinable with all the embodiments described here, of the method according to the present description which include a floatation of the iron ore.
  • the floatation can be performed, in particular, between the oxidizing roasting of the iron ore and subsequent leaching, to obtain a final concentrate with a reduced phosphorus content.
  • the embodiments described using fig. 2 are combinable with the embodiments described using fig. 1 , so that the method can include not only floatation but also pre-conditioning upstream of the oxidizing roasting.
  • floatation can be an inverse floatation, configured to separate at least the apatite or part of it from the remaining iron ore after oxidizing roasting and before leaching. In this way, floatation can allow to reduce the quantity of leaching agent needed later, to obtain the same reduction of phosphorus in the final concentrate.
  • Fig. 3 is used to describe embodiments, combinable with all the embodiments described here, of the method according to the present description that include, as a preliminary operation, a primary crushing/grinding of the iron ore.
  • the primary crushing/grinding as described with reference to fig. 3 , can be performed upstream of the pre-conditioning, for example in the embodiments described using figs. 1 and 2 . If the embodiments described using fig. 3 are combined with the embodiments described using fig. 2 , in possible embodiments the method can therefore include primary crushing/grinding of the iron ore, pre-conditioning, oxidizing roasting and leaching.
  • the primary crushing/grinding can be performed for example either dry or wet, so as to reduce the ore to a sufficiently small nominal size, for example less than 1 mm, so as to be able to be processed in the concentration plant.
  • the iron ore can initially be crushed to 90-100% less than 3.35 mm.
  • the ore can be ground with a ball mill in an open or closed circuit with dimensional classifiers such as for example hydrocyclones or dynamic air classifiers to obtain the desired dimensional distribution, for example 80% under 45 micrometers of nominal diameter (P 80 of 45 micrometers).
  • a high pressure grinding roll (HPGR) apparatus for the primary crushing/grinding a high pressure grinding roll (HPGR) apparatus can be used, which can be advantageous in terms of electricity consumption and to facilitate subsequent grinding, considering that the liberation size of the apatite material can be very fine.
  • HPGR high pressure grinding roll
  • Fig. 4 is used to describe embodiments, combinable with all the embodiments described here, of the method according to the present description which include, as preliminary operation, a dry or wet treatment of the iron ore.
  • the dry treatment can include primary crushing/grinding, magnetic separation obtained precisely dry, pre-conditioning of the iron ore using a granulate containing a pre-conditioning compound, to be performed before the oxidizing roasting, followed by a subsequent secondary grinding before leaching.
  • the embodiments described are particularly advantageous economically if performed dry, given no intermediate filtration is necessary and given the reduced risk of depositing of the wet ore.
  • a magnetic separation can follow, performed dry with low intensity, for example with an intensity of the magnetic field between 1000 - 2000 Gauss.
  • the decision to adopt, for example, a LIMS technique can be made according to the results of the LIMS test performed dry.
  • the non-magnetic material is separated with losses that depend on the nature of the iron oxides, in particular between 10-20%, for example 13%.
  • Fig. 5 is used to describe embodiments, combinable with all the embodiments described here, of the method according to the present description that can include a reducing roasting. In possible implementations, a possible subsequent magnetic separation can also be provided.
  • the possible reducing roasting and/or possible subsequent magnetic separation can, in particular, be performed before the oxidizing roasting and, if pre-conditioning is provided as described with reference to figs. 1, 2 and 3 , also before the pre-conditioning.
  • the possible reducing roasting and/or possible subsequent magnetic separation can be performed after the primary crushing/grinding of the iron ore.
  • the reducing roasting can be performed to convert the non-magnetic minerals, such as hematite or goethite, to synthetic magnetite, operating in a reducing atmosphere.
  • non-magnetic minerals such as hematite or goethite
  • maghemite can also be converted into magnetite.
  • An example of reducing atmosphere can be a mixture of CO, CO 2 , N 2 and possibly H 2 and/or H 2 O. Possible quantities of the reducing mixture are for example about 10% CO, 30% CO 2 , 60% N 2 .
  • other compounds with a base of hydrogen, nitrogen, oxygen and carbon can be contained in the gas, depending on the process used to obtain it.
  • Reducing roasting is performed similarly to oxidizing roasting, only the atmosphere is reducing and the temperatures are lower.
  • Reducing roasting can, in particular, be performed at a controlled high temperature under 900°C, in particular between 600°C and 800°C, to prevent the formation of wustite and metal iron.
  • a rotary kiln can be used for example for the reducing roasting. The time spent in the rotary kiln can go from 1 to 2 hours.
  • the magnetically roasted material is discharged and cooled, preferably in water, so that it can be ground.
  • the operating conditions of the reducing roasting can be:
  • a time spent in the kiln of about 1.5 hours can ensure that all the material reacts and is suitably magnetized in these operating conditions.
  • a secondary grinding, or regrinding, of the iron ore can be provided.
  • a secondary wet or dry grinding, or regrinding, of the iron ore can be provided.
  • the secondary grinding or regrinding can be performed to obtain, for example, a dimensional distribution of P 80 of 45 micrometers.
  • the specific choice of the secondary grinding parameters has for example been defined and tested experimentally by Applicant using a wet or dry grinding mill on a laboratory scale with a load of graduated grinding balls and by carrying out the Davis tube test to select the grinding size P 80 .
  • the magnetic separation which can be performed for example after the primary crushing/grinding, and/or after the reducing roasting and/or after the secondary grinding when provided, can be a low-intensity magnetic separation (LIMS) performed wet or dry, for example with an intensity of the magnetic field between about 1000 and 2000 Gauss.
  • LIMS low-intensity magnetic separation
  • a mass recovery can be obtained of more than 90%, thanks to the magnetic separation performed wet, with a removal between 30 and 35% of phosphorus in the magnetic concentrate.
  • the starting ore contains 0.8% phosphorus, this can be reduced to 0.53% phosphorus.
  • a mass recovery can be obtained of more than 85%, thanks to the magnetic separation performed dry, without any prior reducing roasting, with a removal between 35 and 40% of phosphorus in the magnetic concentrate.
  • the ore introduced contains 0.8% phosphorus, this can be taken to a concentration of 0.61%.
  • a pre-concentration of the iron ore can be provided using magnetic separation.
  • a non-magnetic material is separated, which is subjected to reducing roasting, from a magnetic material which is subjected to secondary roasting if provided, and then to the possible magnetic separation, or, if secondary grinding is not provided, sent directly to the possible magnetic separation subsequent to the reducing roasting.
  • the pre-concentration of the iron ore by magnetic separation can be a low-intensity magnetic separation (LIMS), for example with an intensity of the magnetic field of about 1000-2000 Gauss, or a medium intensity magnetic separation (MIMS).
  • LIMS low-intensity magnetic separation
  • MIMS medium intensity magnetic separation
  • this separation can be performed by a belt-type magnetic separator drum, also called a dry cobber.
  • more than 90% of the material can be concentrated with pre-concentration, obtaining:
  • floatation can also be provided as in the cases described using figs. 3 and 4 , between oxidizing roasting and leaching, or, in other variants, floatation may not be performed.
  • the magnetic separation after primary crushing/grinding, and/or after reducing roasting, and/or possibly after secondary grinding can be provided, or not.
  • Embodiments described here also concern an apparatus 10 for the dephosphorization of iron ore.
  • the embodiments of the apparatus 10 described with reference to fig. 5 can also include a secondary grinding unit 19, between the reducing roasting unit 17 and the possible magnetic separation unit 18, and a pre-concentration unit using magnetic separation 20 of the iron ore, between the primary crushing/grinding unit 16 and the reducing roasting unit 17.
  • Embodiments described here allow to considerably reduce the phosphorus content in the final concentrate, for example a reduction of up to about 0.12-0.13% w/w in the case of the embodiments described here without pre-conditioning, or even up to about 0.02-0.03% w/w in the case of the embodiments with pre-conditioning, with for example a total content of iron of about 60-64%.
  • the reducing roasting was performed under the following conditions:
  • the secondary grinding was performed with a feed size P 80 of about 1 mm, a percentage of solid of 50%.
  • the magnetic separation was performed under the following conditions:
  • the pre-conditioning where provided wet (1 st and 4 th test) was performed with a solution of CaCl 2 with a concentration of 20-22%, percentage of solid 30%, rotor speed 350 rpm, immersion time 2 hours, immersion temperature 25°C.
  • the pre-conditioning was performed with a granulate of CaCl 2 in a mass percentage of about 4%, with a mixing and homogenization time of 1 hour, environmental temperature (i.e. 25°C).
  • Oxidizing roasting was performed under the following conditions:
  • the total iron content is assessed using XRF, that is, expressed as Fe 2 O 3 % measured with XRF (X-ray fluorescence) x 0.6994.
  • the total phosphorus content is assessed using XRF, expressed as P 2 O 5 % measured with XRF (X-ray fluorescence) x 0.4364.

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Claims (19)

  1. Procédé de déphosphoration de minerai de fer ayant une teneur en phosphore supérieure à 0,5%, avec une magnétite, une hématite ou une nature mixte, ledit procédé comprenant :
    un préconditionnement du minerai de fer au moyen d'un composé de préconditionnement solide ou en solution, avec une teneur inférieure à 5% en poids du mélange ferreux total ;
    un grillage oxydant du minerai de fer ;
    une lixiviation ultérieure, afin d'obtenir un concentré final à teneur
    réduite en phosphore, avec une réduction supérieure à 85% où ledit procédé comprend un grillage réducteur avant au moins le grillage oxydant.
  2. Procédé selon la revendication 1, caractérisé en ce que ledit préconditionnement est effectué en amont du grillage oxydant.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'il comprend une lixiviation biphasique avec une concentration en acide inférieure à 3%.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'il comprend un concassage/un broyage primaire préliminaire du minerai de fer, effectué soit humide soit sec, avant au moins le grillage oxydant.
  5. Procédé selon la revendication 1, caractérisé en ce qu'il comprend une séparation magnétique, avant au moins le grillage oxydant et après le grillage réducteur, ou après le concassage/broyage primaire.
  6. Procédé selon les revendications 4 ou 4 et 5, caractérisé en ce que ledit concassage/broyage primaire est avant le grillage réducteur ou avant au moins la séparation magnétique.
  7. Procédé selon la revendication 4, 5 ou 6, caractérisé en ce que ledit procédé comprend un broyage secondaire après le grillage réducteur possible ou après le grillage oxydant.
  8. Procédé selon la revendication 7, caractérisé en ce que ledit broyage secondaire est prévu entre le grillage réducteur et la séparation magnétique.
  9. Procédé selon la revendication 7, caractérisé en ce que ledit broyage secondaire est prévu entre le grillage oxydant et la lixiviation.
  10. Procédé selon la revendication 7 ou 8, caractérisé en ce qu'il comprend, après le concassage/broyage primaire et avant le grillage réducteur, une préconcentration du minerai de fer au moyen d'une séparation magnétique.
  11. Appareil pour la déphosphoration de minerai de fer, ledit appareil comprenant :
    une unité de préconditionnement (14), une unité de grillage oxydant (12) de minerai de fer alimenté (F), et une unité de lixiviation (13) à partir de laquelle un concentré (C) de minerai de fer avec une teneur réduite en phosphore est obtenu, où ledit appareil comprend, avant au moins l'unité de préconditionnement (14), une unité de grillage réducteur (17).
  12. Appareil selon la revendication 11, caractérisé en ce qu'il comprend, avant l'unité de grillage oxydant (12), ladite unité de préconditionnement (14) du minerai de fer dans laquelle est utilisé un composé granulaire de préconditionnement ou en solution qui, par chauffage, génère un gaz.
  13. Appareil selon la revendication 11 ou 12, caractérisé en ce qu'il comprend une unité de concassage/broyage primaire (16) du minerai de fer, positionnée avant au moins l'unité de préconditionnement (14).
  14. Appareil selon l'une quelconque des revendications 11 à 13, caractérisé en ce qu'il comprend une unité de séparation magnétique (18) après l'unité de grillage réducteur (17).
  15. Appareil selon la revendication 13, caractérisé en ce que l'unité de concassage/broyage primaire (16) est positionnée avant l'unité de grillage réducteur (17).
  16. Appareil selon la revendication 14, où l'unité de concassage/broyage primaire (16) est positionnée avant l'unité de séparation magnétique (18).
  17. Appareil selon la revendication 14, caractérisé en ce qu'il comprend une unité de broyage secondaire (19), positionnée entre l'unité de grillage réducteur (17) et l'unité de séparation magnétique (18).
  18. Appareil selon l'une quelconque des revendications 11 à 17, caractérisé en ce qu'il comprend une unité de broyage secondaire (19), positionnée entre l'unité de grillage oxydant (12) et l'unité de lixiviation (13).
  19. Appareil selon l'une quelconque des revendications 13 à 18, caractérisé en ce qu'il comprend une unité de préconcentration au moyen d'une séparation magnétique (20) du minerai de fer, entre l'unité de concassage/broyage primaire (16) et l'unité de grillage réducteur (17).
EP16820328.9A 2015-11-13 2016-11-11 Procédé et appareil pour la déphosphoration du minerai de fer Active EP3374531B1 (fr)

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PCT/IB2016/056794 WO2017081646A1 (fr) 2015-11-13 2016-11-11 Procédé et appareil pour la déphosphoration du minerai de fer

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CN113403471B (zh) * 2021-06-23 2023-03-10 中钢设备有限公司 一种高磷鲕状铁矿的处理方法
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