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WO2010105292A1 - Élimination d'impuretés à partir de minéraux hydratés - Google Patents

Élimination d'impuretés à partir de minéraux hydratés Download PDF

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Publication number
WO2010105292A1
WO2010105292A1 PCT/AU2010/000302 AU2010000302W WO2010105292A1 WO 2010105292 A1 WO2010105292 A1 WO 2010105292A1 AU 2010000302 W AU2010000302 W AU 2010000302W WO 2010105292 A1 WO2010105292 A1 WO 2010105292A1
Authority
WO
WIPO (PCT)
Prior art keywords
temperature
leach
heating
hour
period
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/AU2010/000302
Other languages
English (en)
Inventor
Graham Jeffery Sparrow
Michael John Fisher-White
Roy Randall Lovel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Commonwealth Scientific and Industrial Research Organization CSIRO
Original Assignee
Commonwealth Scientific and Industrial Research Organization CSIRO
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AU2009901092A external-priority patent/AU2009901092A0/en
Application filed by Commonwealth Scientific and Industrial Research Organization CSIRO filed Critical Commonwealth Scientific and Industrial Research Organization CSIRO
Priority to CN2010800171912A priority Critical patent/CN102395692A/zh
Priority to AU2010225450A priority patent/AU2010225450C1/en
Publication of WO2010105292A1 publication Critical patent/WO2010105292A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • C22B3/08—Sulfuric acid, other sulfurated 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
    • 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
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • 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
    • C22B1/04—Blast roasting
    • 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 present invention relates to the removal of impurities from mineral resources and in particular, the invention relates to the removal of phosphorous from oxidic iron ores.
  • iron oxide bearing materials generally referred to herein as iron ore for simplicity
  • iron ore used in certain industrial processes to meet strict specifications with respect to impurities.
  • iron ore used as a feedstock for blast furnace smelting to produce iron is often desired to have a low phosphorous content.
  • methods for removing phosphorous from molten iron exist, a number of factors such as financial penalties and market access make it attractive to ensure that phosphorous is removed from the iron ore prior to its use in smelting.
  • phosphorous reduction to 0.1 weight % may be commercially acceptable, but a reduction to less than 0.08 weight % is more desirable. Most desirable is a reduction to less than 0.07 weight %.
  • an iron ore and a roasting additive such as an alkali earth metal halide
  • a roasting step of from 500-1200 0 C, prior to a leaching step conducted with an inorganic acid (such as hydrochloric acid), in order to remove phosphorous from the iron ore.
  • an inorganic acid such as hydrochloric acid
  • the object of the invention is to increase the economic viability of the process for removing elements, particularly phosphorous, from mineral ores, particularly hydrated oxidic iron ores.
  • the inventors have discovered that the heating step of the prior art is unduly complex.
  • the high temperatures and additives used during the heating step are not necessary in order to remove impurities to the requisite degree.
  • This invention removes impurity elements from iron ores by heating the ore without any additives, followed by a leaching step to remove impurity elements.
  • a method for the removal of elements from an iron ore including the steps of heating the ore to a temperature not exceeding about 500 0 C and subsequently contacting the ore with an acid or alkaline leach solution to remove the impurity elements from the ore.
  • the step of heating the ore is conducted without the presence of roasting additives or leaching solutions. That is, the iron ore is heated in air or in an atmosphere that may be varied as discussed below.
  • the step of heating the iron ore may be conducted at a temperature above about 225 0 C.
  • the step of heating the iron ore is conducted at a temperature of above about 250 0 C.
  • the step of heating the iron ore may be conducted at a temperature as high as about 500 0 C.
  • the step of heating the iron ore is conducted at a temperature of below about 350 0 C in air. More preferably, the step of heating the iron ore is conducted at a temperature of about 300 0 C.
  • the step of heating the iron ore may be carried out with conventional furnaces (eg a rotary furnace, a fluidized bed furnace, a travelling grate furnace or a flash furnace) with direct or indirect heating in an appropriate gas atmosphere.
  • furnaces eg a rotary furnace, a fluidized bed furnace, a travelling grate furnace or a flash furnace
  • the atmosphere is air, but heating in atmospheres other than air (eg combustion gases) is also effective.
  • the element requiring removal (the impurity element) from an iron ore may be, for instance, phosphorous, silica, or alumina. Other sample specific elements (eg sulphur) may also be removed. In one specific case, the element requiring removal is phosphorous. In these embodiments, the phosphorous that is removed from the iron ore may be present in a goethitic and/or limonitic phase in the iron ore, but may also be present in any non-oxidic apatitic phase of the ore.
  • the leach solution may be an acidic or alkaline aqueous solution.
  • the acidic leaching solution may be an inorganic or organic acid. Examples of acidic leach solutions include HCI, HNO 3 , H 2 SO 4 , and citric acid.
  • the leach solution is alkaline.
  • alkaline leach solutions include NaOH, KOH and NH 4 OH. More preferably, the leach solution is NaOH.
  • the step of contacting the iron ore with a leach solution may be conducted at ambient temperature or at an elevated temperature up to the boiling point of the leaching solution.
  • the step of contacting the iron ore with a leach solution is conducted at an elevated temperature.
  • the inventors also believe that during the heating, dehydroxylation of the goethite to a deformed hematite (as opposed to a dense hematite phase) occurs.
  • impurity elements in the goethite originally
  • these impurity elements are able to be leached from the mineral.
  • Apatite (Ca 5 (P ⁇ 4) 3 OH) is a common, familiar accessory mineral in iron ores that is known to be soluble in acid. It is not possible to remove phosphorous associated with goethite under the conditions used to remove phosphorous associated with apatite because untreated high phosphorous goethitic ores are not greatly affected by acid leaching. Apatite (and its phosphorous) in ores treated by the process of the invention is expected to be leached along with the more difficult phosphorous associated with goethite.
  • the temperature and time of heating, the time of leaching, and the concentration of the leachant depend on the iron ore and on the final desired product specification.
  • the step of heating the iron ore can be conducted for a time as little as 0.25 hr or less. Heating times of up to about 24 hrs are not detrimental but may not be cost efficient. Preferably, the heating time is from about 0.25 hr to about 4 hours. More preferably, the heating time is about 1 hour.
  • the step of contacting the iron ore with a leach solution may be conducted for a time of up to about 5 hours. Longer leaching times are not detrimental but are not as cost efficient. Preferably, the leaching time is about 3 hr. More preferably, the leaching time is about 0.25 to 1 hr.
  • the concentration of the leach solution may be from about 0.001 M to about 5.0 M. Higher concentrations are not detrimental but are not likely to be as cost efficient or safe.
  • the step of contacting the iron ore with a leach solution may be carried out in a reaction vessel with suitable agitation to ensure good contact between the iron ore and the leaching solution.
  • Single or multiple stages of leaching may be carried out as required to achieve a satisfactory impurity element removal.
  • the heated ore could be contacted with the leach solution under conditions used in heap leaching operations.
  • Examples 1 to 11 illustrate the method of the present invention on two Australian Brockman high phosphorous iron ores. Both samples were crushed to less than 1.2 mm to improve sample homogeneity. Phosphorous removal from coarse samples is more favourable in industrial applications but difficult to demonstrate in a reproducible manner.
  • iron ore sample 1 contained 62.0 wt% Fe, 0.146 wt% P, 3.07 wt% SiO 2 , and 2.27 wt% AI 2 O 3 while iron ore sample 2 contained 62.1 wt% Fe, 0.123 wt% P, 3.22 wt% SiO 2 , and 2.18 wt% AI 2 O 3 ,
  • the leach solids were collected by filtration, washed with water and dried at 60 C C. The leach solutions were collected as required. The amount of the elements removed by the various test conditions was assessed using the
  • ICP-OES Inductively Coupled Plasma-Optical Emission Spectroscopy
  • Leaching either ore sample directly with boiling water resulted in the removal of virtually no impurity elements.
  • Leaching iron ore sample 1 with sodium hydroxide solution did remove a small amount of phosphorous, along with some alumina and silica.
  • leaching with sodium hydroxide also resulted in removal of phosphorous, silica and alumina with the amounts removed increasing with higher concentrations of sodium hydroxide in the leaching solution.
  • Leaching iron ore sample 2 with sulphuric acid resulted in dissolution of some phosphorous but virtually none of the silica or alumina. There was a 1.2% weight loss in the leach.
  • a heating temperature of 250 0 C is sufficient to obtain removal of some of the impurities with a sodium hydroxide leach. However, better impurity element removal is achieved with higher heating temperatures of 275-350 0 C. Heating above 350 °C does not significantly improve the removal of the impurities.
  • the heat treatment causes the goethite to undergo phase changes that then makes the impurities available for removal in the sodium hydroxide leach. Consequently the heating temperature should be chosen to achieve the required impurity element removal.
  • a heating time as short as 15 minutes has been shown to be sufficient to achieve appreciable impurity element removal with a sodium hydroxide leach and a heating time of more than 1 hour does not have any further significant beneficial effects. It is anticipated that a flash heating treatment of less than 15 minutes may be a practical embodiment of this invention.
  • the heat treatment causes the goethite to undergo phase changes that then makes the impurities available for removal in the sodium hydroxide leach. Consequently the heating temperature, and the time at temperature, should be chosen to achieve the required impurity element removal.
  • the effect of the concentration of sodium hydroxide in the leach on the amount of phosphorous removed after a heat treatment is shown when the iron ore sample 1 is either: 1. subjected to a heating step of 300 0 C for a period of 1 hour in air, followed by being contacted with a boiling water leach solution;
  • Leaching with boiling water after a heat treatment at 300 0 C for 1 hour removes little of the impurities, but significantly greater levels of impurity element removal can be achieved in a leach with boiling 0.001 M NaOH after a heat treatment at 300 0 C for 1 hour. Greater amounts of impurity element removal are achieved when higher concentrations of sodium hydroxide are used in the leach.
  • Test Heating Heating Leaching Leaching XRF assay data (wt%) condition temp. time solution temp.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne un procédé d'élimination d'un élément d'impureté à partir d'un minerai de fer. Le procédé comprend les étapes de chauffage du minerai à une température ne dépassant pas environ 500°C, puis de mise en contact du minerai avec une solution de lixiviation acide ou alcaline pour éliminer par lixiviation l'élément d'impureté du minerai.
PCT/AU2010/000302 2009-03-16 2010-03-15 Élimination d'impuretés à partir de minéraux hydratés Ceased WO2010105292A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN2010800171912A CN102395692A (zh) 2009-03-16 2010-03-15 从水化矿物中去除杂质
AU2010225450A AU2010225450C1 (en) 2009-03-16 2010-03-15 Impurity removal from hydrated minerals

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2009901092A AU2009901092A0 (en) 2009-03-16 Impurity removal from hydrated minerals
AU2009901092 2009-03-16

Publications (1)

Publication Number Publication Date
WO2010105292A1 true WO2010105292A1 (fr) 2010-09-23

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PCT/AU2010/000302 Ceased WO2010105292A1 (fr) 2009-03-16 2010-03-15 Élimination d'impuretés à partir de minéraux hydratés

Country Status (3)

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CN (1) CN102395692A (fr)
AU (1) AU2010225450C1 (fr)
WO (1) WO2010105292A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103882225A (zh) * 2014-04-04 2014-06-25 北京科技大学 一种酸浸脱除高磷铁矿中的磷及酸液循环利用的方法
WO2025097163A1 (fr) * 2023-11-03 2025-05-08 Allonnia, Llc Élimination sélective d'impuretés à partir de minerai à l'aide de combinaisons de biobroth et de biosolvants ajustés en ph

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102616797B (zh) * 2012-05-02 2013-10-09 厦门大学 一种云母的提纯方法
CN109913638A (zh) * 2019-04-01 2019-06-21 中钢集团南京新材料研究院有限公司 一种降低超级铁精矿中硅、铝含量的方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1367102A (en) * 1970-11-11 1974-09-18 Australian Mineral Dev Lab Process for the reduction of the phosphorus content of iron ores
US4154608A (en) * 1978-07-19 1979-05-15 Uop Inc. Production of high purity iron powder
WO1993010271A2 (fr) * 1991-11-14 1993-05-27 S.A. Mineração Da Trindade - Samitri Amelioration d'un processus permettant de reduire la teneur en phosphore et autres gangues du minerai de fer et de ses agglomerats
WO2010015019A1 (fr) * 2008-08-05 2010-02-11 Technological Resources Pty. Limited Traitement de minerai de fer

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5767136A (en) * 1980-10-09 1982-04-23 Sumitomo Metal Ind Ltd Dephosphorizing method for ore
BRPI0401372B1 (pt) * 2004-03-09 2015-08-18 Universidade Federal De Ouro Preto Processo para remoção de fósforo em minérios de ferro
CN100413982C (zh) * 2007-04-28 2008-08-27 中南大学 一种高铝褐铁矿石铁铝分离工艺
CN101338361A (zh) * 2008-08-11 2009-01-07 昆明晶石矿冶有限公司 一种高磷赤铁矿赤褐铁矿磁化焙烧—浸出降磷方法
CN201560225U (zh) * 2009-03-04 2010-08-25 解能 一种高磷铁矿超声波脱磷装置

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1367102A (en) * 1970-11-11 1974-09-18 Australian Mineral Dev Lab Process for the reduction of the phosphorus content of iron ores
US4154608A (en) * 1978-07-19 1979-05-15 Uop Inc. Production of high purity iron powder
WO1993010271A2 (fr) * 1991-11-14 1993-05-27 S.A. Mineração Da Trindade - Samitri Amelioration d'un processus permettant de reduire la teneur en phosphore et autres gangues du minerai de fer et de ses agglomerats
WO2010015019A1 (fr) * 2008-08-05 2010-02-11 Technological Resources Pty. Limited Traitement de minerai de fer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103882225A (zh) * 2014-04-04 2014-06-25 北京科技大学 一种酸浸脱除高磷铁矿中的磷及酸液循环利用的方法
WO2025097163A1 (fr) * 2023-11-03 2025-05-08 Allonnia, Llc Élimination sélective d'impuretés à partir de minerai à l'aide de combinaisons de biobroth et de biosolvants ajustés en ph

Also Published As

Publication number Publication date
AU2010225450C1 (en) 2013-11-21
CN102395692A (zh) 2012-03-28
AU2010225450A1 (en) 2011-10-06
AU2010225450B2 (en) 2013-05-30

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