WO2007071020A1 - Process for recovering iron as hematite from a base metal containing ore material - Google Patents
Process for recovering iron as hematite from a base metal containing ore material Download PDFInfo
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- WO2007071020A1 WO2007071020A1 PCT/CA2006/002038 CA2006002038W WO2007071020A1 WO 2007071020 A1 WO2007071020 A1 WO 2007071020A1 CA 2006002038 W CA2006002038 W CA 2006002038W WO 2007071020 A1 WO2007071020 A1 WO 2007071020A1
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- leachate
- base metal
- chloride
- lixiviant
- acid
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Classifications
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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
- 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
- C22B7/006—Wet processes
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0423—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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present invention relates generally to processes for mineral extraction and ore processing and more specifically, to processes for recovering iron as hematite from a base metal containing ore material and to processes for recovering base metals from base metal containing materials.
- the process involves leaching a base metal sulfide ore at atmospheric pressure with a lixiviant containing a relatively low concentration of hydrochloric acid and a high chloride concentration. More specifically, the lixiviant used in this process comprises hydrochloric acid, a chloride and an oxidant.
- the chloride may be an alkali metal chloride, magnesium chloride, calcium chloride and mixtures thereof.
- the oxidant may be an alkali metal peroxide, an alkali metal perchlorate, magnesium perchlorate, alkali metal chlorate, earth metal perchlorate, chlorine, alkali metal hypochlorite, hydrogen peroxide and peroxysulfuric acid, and mixtures thereof.
- the leaching step yields a solid residue and a base metal-rich leachate which contains dissolved iron therein.
- the sulfur from the leachate and solid residue may be removed by forming and stripping hydrogen sulfide during the leaching step. Some or all of the hydrogen sulfide may then be converted to elemental sulfur. A by-product of this conversion reaction is energy.
- the base-metal rich leachate may be subjected to base metal recovery steps (which may include an additional leaching step) and/or value metal recovery steps to extract the nickel, copper, zinc and cobalt and any dissolved platinum group metals, gold and silver.
- iron is first removed from the pregnant leachate by precipitating an iron oxide (hematite or spinel) using a magnesium oxide additive and effecting a solid/liquid separation step.
- the magnesium oxide is obtained from a pyrohydrolysis reaction of spent magnesium chloride, which also recovers hydrochloric acid for recycle.
- the process only contemplates the recovery of hydrochloric acid formed as a by-product of the pyrohydrolysis, for reuse in the leach circuit.
- 0005 Iron is and has always been considered a major problem in hydrometallurgical processes. In atmospheric processes, the iron is usually precipitated as an oxy-hydroxide, and in higher temperature autoclave processes, as an impure hematite.
- WPL waste hydrochloric acid steel mill pickle liquors
- WPL typically contains water, 18 to 25% weight of ferrous chloride (FeCl 2 ), less than 1% weight ferric chloride (FeCl 3 ), small amounts of free hydrochloric acid and small amounts of organic inhibitors.
- the process of Kovacs includes two steps namely, a first oxidation step and a second thermal decomposition step.
- the ferrous chloride in the WPL is oxidized using free oxygen to obtain ferric oxide and an aqueous solution containing ferric chloride. No hydrochloric acid is liberated at this stage.
- the first oxidation step is carried out under pressure (preferably, 100 p.s.i.g.) and at an elevated temperature (preferably, 149°C).
- the resultant ferric chloride solution is thermally decomposed to obtain ferric oxide and HCl gas, which is recovered as hydrochloric acid. More specifically, the resultant solution is heated up to 175-180 0 C at atmospheric pressure. The HCl is stripped off at a concentration of 30% with >99% recovery and good quality hematite is produced. While recovery of hydrochloric acid and hematite may be achieved using this process, its application tends to be limited to liquors containing only ferrous/ferric chlorides. When other chlorides are present in the solution, for instance, magnesium chloride, the activity of the chloride ions and protons tends to be too high to permit any reaction to take place simply by heating the solution to the desired temperature. Accordingly, this process
- DM TOR/264119-00003/2103883.1 tends not to be well adapted for use in leaching processes involving chlorides other than ferric chloride.
- Lalancette describes performing chloridation by leaching a base metal mixture containing substantial amounts of iron with hydrochloric acid at a temperature of 100 0 C, in the presence of an oxidant. This chloridation transforms part of the iron into ferric chloride which, in sulfide ores, can only be achieved in the presence of an oxidant.
- the ferric chloride solution is then heated to evaporation while in the presence of moisture. Thereafter, the resultant ferric chloride is subjected to hydrolysis to thereby transform it into ferric oxide and hydrochloric acid.
- the metal chlorides remaining in the final solid mixture are not affected by this mild hydrolysis and can be separated from the ferric oxide solids by leaching with water.
- Efficient iron removal also tends to pose significant challenges in the recovery of base metals from laterite ores using chloride-based leaching processes.
- United States Patent Publication No. 2004/0228783 of Harris et al. describes a process for the recovery of value metals from material containing base metal oxides in which iron is simultaneously leached and precipitated from the laterite ore along with base metals.
- the lixiviant used in the leaching step may comprise magnesium chloride and hydrochloric acid.
- the lixiviant may further include an oxidant.
- the leachate contains solubilised base metals, such as nickel, cobalt, manganese, copper, aluminum, zinc and chromium and a solid residue that contains iron.
- the leach is conducted under conditions at which at least some, and preferably all or substantially all, of the iron that is leached from the ore is immediately hydrolyzed and precipitated as hematite and/or magnetic iron oxide.
- the resultant leachate may contain only residual amounts of iron.
- DM_TOR/264119-00003/2103883.1 2005 Ni/Co 10, Perth, W. Australia, May 16-18, 2005 a process was described wherein the limonite fraction of a laterite ore is leached by hydrochloric acid in a solution of calcium and sodium chlorides.
- the process can be operated in either one or two stages, the first stage being at 100-110 0 C, and the second, or if a single-stage process, at 150-220 0 C.
- both dissolved iron and magnesium are precipitated via the use of lime (CaO), iron as hematite and magnesium as MgO.
- the process requires the substantial addition of sulfuric acid to regenerate the hydrochloric acid, with the sulfate being controlled by the further addition of lime.
- the acid saturated and partly reacted ore is heated to approximately 90-100 0 C and leaching is performed with hydrochloric acid to obtain a lixiviate containing water soluble nickel, cobalt, iron, chromium and magnesium chlorides and an insoluble residue.
- the lixiviate is then filtered from the insoluble residue to produce a head solution.
- Lalancette describes two processes by which the nickel and cobalt can be recovered along with hydrochloric acid and iron oxide.
- One process involves recovering the nickel and cobalt from the head solution using techniques such as electrowinning and solvent extraction, specific-ion exchange resins and sulfide precipitation.
- the leftover solution containing ferrous chloride, magnesium chloride and chromium chloride along with excess acid can be evaporated in the presence of a potassium chloride solution to yield a solid residue of the chlorides.
- This residue may be roasted in the presence of air and steam at temperatures ranging from 450 to 475°C to oxidize the ferrous chloride to iron oxide and produce gaseous hydrochloric acid.
- the foregoing circuit is complex, and may
- DM TOR/264119-00003/2103883.1 5 not yield a hematite product of high purity. This is because some of the magnesium will form its oxychloride, otherwise known as "Sorel Cement," and as a result it will not be possible to wash this magnesium out of the hematite, since the oxychloride is markedly insoluble.
- a process for recovering iron material from a base metal containing material includes providing the base metal containing material and providing a lixiviant comprising an acid and a chloride.
- the acid may be selected from the group consisting of an organic acid, sulfurous acid, sulfuric acid and hydrochloric acid.
- the chloride may be selected from the group consisting of magnesium chloride, calcium chloride, sodium chloride, potassium chloride, ferrous chloride and lithium chloride.
- the process further includes performing a leaching step on the base metal containing material at atmospheric pressure in the absence of an oxidant, using the lixiviant to obtain a solid residue and a leachate containing dissolved iron therein, and separating the leachate from the solid residue.
- the leachate is then treated to recover therefrom at least some of the iron as a hematite product of high purity.
- the base metal containing material is selected from the group consisting of an ore, a concentrate and an intermediate material.
- the base metal containing material is sulfide ore material. The sulfide ore material contains at least one
- DM_TOR/264119-00003/2103883.1 6 base metal selected from the group consisting of nickel, copper, zinc and cobalt.
- the sulfide ore material contains at least one of gold, silver and a platinum group metal.
- the sulfide ore material may be selected from the group consisting of pyrrhotite, pentlandite, chalcopyrite, pyrite, arsenopyrite, galena and sphalerite.
- the base metal containing material is an oxidic ore material.
- the oxidic ore material is a laterite ore material.
- the laterite ore material may be one of a limonite ore material, a saprolite ore material, a hematitic clay material and a serpentinite material.
- the laterite ore material contains at least one base metal selected from the group consisting of nickel, manganese, magnesium, copper and cobalt.
- the concentration of the chloride in the lixiviant is adjusted to obtain a solubility of between about 75% and about 95% of its saturation point.
- magnesium chloride is selected as the chloride.
- the acid in the lixiviant is an organic acid.
- the organic acid may be selected from the group consisting of acetic acid, tartaric acid and citric acid.
- the acid is hydrochloric acid and the chloride is magnesium chloride.
- the concentration of magnesium chloride in the lixiviant is adjusted to at least about 300g/L. In an additional feature, the concentration of magnesium chloride in the lixiviant is adjusted to between about 340g/L and 420 g/L.
- the leaching step is performed at a temperature between about 2O 0 C and about the boiling point of the lixiviant. In still another feature, the leaching step is performed at a temperature between about 105 0 C and about 110 0 C.
- the step of treating the leachate to recover therefrom at least some of the iron as a hematite product of high purity includes heating the leachate to distill the hydrochloric acid therefrom, and simultaneously subjecting the leachate to a precipitation step to promote the formation of the hematite product.
- the leachate is heated to a temperature of between about 190 0 C and about 250 0 C and most preferably, between about 220 0 C and about 250 0 C.
- the leachate is heated to a temperature of at least about 18O 0 C and the precipitation step includes of one of adding water and adding steam to the leachate.
- the precipitation step includes of one of adding water and
- the process further includes separating the precipitate from the remaining leachate and drying the precipitate.
- the process further includes recovering the chloride from the remaining leachate.
- the base metal containing material is a sulfide ore material and the process further includes removing hydrogen sulfide gas formed during the leaching step.
- the hydrogen sulfide is stripped in a continuous manner.
- the base metal containing material is a sulfide ore material and the solid residue is an upgraded base metal concentrate.
- the base metal containing material is a laterite ore material and the leachate is a base metal-rich leachate.
- a process for recovering a base metal from a base metal containing material includes providing the base metal containing material and providing a lixiviant.
- the lixiviant includes an acid and a chloride.
- the acid is selected from the group consisting of an organic acid, sulfurous acid, sulfuric acid and hydrochloric acid.
- the chloride is selected from the group consisting of magnesium chloride, calcium chloride, sodium chloride, potassium chloride, ferrous chloride and lithium chloride.
- the process further includes performing a leaching step on the base metal containing material at atmospheric pressure in the absence of an oxidant, using the lixiviant to obtain a solid residue and a leachate containing dissolved iron therein and then separating the leachate from the solid residue.
- the leachate is then treated to recover therefrom at least some of the iron as a hematite product of high purity, prior to one of the leachate and the solid residue being subjected to a series of base metal recovery steps.
- the base metal containing material is a sulfide ore material
- the process further includes removing hydrogen sulfide gas formed during the leaching step.
- the hydrogen sulfide is stripped in a continuous manner and reacted with sulfur dioxide gas in a Claus reaction to obtain elemental sulfur and steam.
- the base metal containing material is a sulfide ore material and the solid residue is an upgraded base metal concentrate.
- the upgraded base metal concentrate is
- DM TOR/264119-00003/2103883.1 subjected to a series of base metal recovery steps that includes providing a second lixiviant comprising an acid and a chloride.
- the acid may be selected from the group consisting of an organic acid, sulfurous acid, sulfuric acid and hydrochloric acid.
- the chloride may be selected from the group consisting of magnesium chloride, calcium chloride, sodium chloride, potassium chloride, ferrous chloride and lithium chloride.
- the process further includes performing a second leaching step on the upgraded base metal concentrate at atmospheric pressure, using the second lixiviant to obtain second solid residue and a second leachate containing at least one base metal dissolved therein. The second leachate is then separated from the second solid residue and treated to recover therefrom the at least one base metal.
- the base metal containing material contains at least one of gold, silver and a platinum group metal and the second solid residue is an upgraded value metal concentrate.
- the upgraded value metal concentrate is subjected to at least one value metal recovery step.
- the base metal containing material contains at least one of gold, silver and a platinum group metal and the second leachate is a value metal-rich leachate. The value metal-rich leachate is subjected to at least one value metal recovery step.
- the base metal containing material is a laterite ore material and the leachate is a base metal-rich leachate.
- the base metal-rich leachate is subjected to a series of base metal recovery steps.
- FIG. 1 is a schematic representation of a process according to an embodiment of the invention involving the removal of iron material from a sulfide ore material using a lixiviant in a leaching step to obtain a solid residue in the nature of an upgraded base metal concentrate and a leachate containing dissolved iron therein;
- FIG. 2 is a schematic representation of a process for recovering base metals and value metals from the upgraded base metal concentrate obtained by the process shown in FIG. 1 ;
- FIG. 3 is a schematic representation of a process according to another embodiment of the invention involving the removal of iron material from a laterite ore material using a lixiviant in a leaching step to obtain a solid residue and a base metal-rich leachate.
- ore material means an ore and any material derived from the processing of an ore, including without limiting the foregoing, any metal processing by-product (i.e. flue dust and furnace baghouse dust), any intermediate material produced during the treatment of an ore (i.e. slags, calcines, impurity residues, dross and anode slimes), any concentrate, any matte such as a converter matte, or any tailings from the processing of an ore.
- any metal processing by-product i.e. flue dust and furnace baghouse dust
- any intermediate material produced during the treatment of an ore i.e. slags, calcines, impurity residues, dross and anode slimes
- any concentrate i.e. slags, calcines, impurity residues, dross and anode slimes
- any concentrate i.e. slags, calcines, impurity residues, dross and anode slimes
- FIG. 1 there is shown a schematic representation of a process in accordance with an embodiment of the invention, designated generally with reference numeral 20.
- the process 20 involves the removal of iron material from a base metal containing ore material using a lixiviant during a leaching step.
- the process 20 includes the following steps: providing a base metal containing material in the nature of a sulfide ore material (step 30); providing a lixiviant (step 40); performing a leaching step on the sulfide ore material at atmospheric pressure, using the lixiviant to obtain a solid residue and a leachate containing dissolved iron therein (step 50); separating the leachate from the solid residue (step 60); and treating the leachate to recover therefrom at least some of the iron as a hematite product of high purity (step 65).
- the sulfide ore material contains relatively substantial amounts of sulfur and iron, as well as one or more base metals, such as, nickel, copper, zinc and cobalt.
- the sulfide ore material may further contain one or more value metals such as gold, silver or a platinum group metal (PGM).
- PGM platinum group metal
- Suitable sulfide ore materials for use in process 20 include pyrrhotite, pentlandite, chalcopyrite, pyrite, arsenopyrite, galena, sphalerite and any aggregates and/or mixtures thereof.
- the sulfide ore material does not require substantial treatment (i.e. roasting or flotation) prior to being subjected to the process shown in FIG. 1.
- the sulfide ore material may be subjected to beneficiation or may be crushed and/or ground (at step 70) as shown in FIG. 1.
- the performance of such conditioning steps tends to improve the overall efficiency of the process by reducing the residence time of the lixiviant in the sulfide ore material and by encouraging the dissolution of iron in the leachate thereby leading to a reduction in the volume of solid residue obtained from the leaching step 50.
- the lixiviant used in the leaching step 50 includes an acid and a chloride. Contrary to other known hydrometallurgical processes applicable to sulfide ore materials, the lixiviant does not contain an oxidant and the leaching step is carried out under predominantly reducing conditions.
- the acid in the lixiviant may be an organic acid, sulfurous acid, sulfuric acid or hydrochloric acid.
- the preferred acid is hydrochloric acid. Examples of an organic acid that may be used in performing the leaching step 50, include acetic acid, tartaric acid and citric acid.
- the lixiviant employs relatively low concentrations of acid.
- the amount of acid to be used in the lixiviant tends to depend on the chemical composition of the sulfide ore material. Different sulfide ore materials require different amounts of acid in the lixiviant.
- hydrochloric acid it has been found that between about 500 kg to about 1000 kg (100% dry basis) of hydrochloric acid may be needed for each tonne of sulfide ore material to be leached.
- the amount of acid in the lixiviant is substantially stoichiometric.
- DM TOR/264119-00003/2103883.1 1 1 between about 100% and about 110% of the stoichiometric amount of acid may be used. It is believed that the high activity of H + ions in the high strength chloride solution may make the use of close to stoichiometric concentrations of acid in the lixiviant possible.
- the chloride constituent in the lixiviant may be magnesium chloride, calcium chloride, sodium chloride, potassium chloride, lithium chloride, ferrous chloride or mixtures thereof.
- the preferred chloride for use in the lixiviant is magnesium chloride as it tends to be more readily recycled than the other specified chlorides.
- Magnesium chloride is most preferred where the acid employed in the lixiviant is hydrochloric acid. As will be explained in greater detail below, where the lixiviant includes hydrochloric acid, it will be possible to precipitate more of the iron in the leachate as hematite or magnetite during a hydrolytic distillation stage. The hematite or magnetite thus formed is of high purity and may be easily recovered.
- magnesium chloride is used in the lixiviant with hydrochloric acid, there exists the possibility that magnesium oxychloride may be formed during the hydrolytic distillation stage, the formation of which would contaminate the hematite and result in a loss of chloride from the system.
- the risk of this occurrence tends to be relatively small.
- magnesium chloride tends not to suffer from some of the drawbacks associated with some of the other above-identified chlorides. For instance, sodium chloride and potassium chlorides are prone to crystallisation and calcium chloride tends to form a stable sulfide, which on oxidation causes insoluble calcium sulfate (gypsum) to precipitate, resulting in significant scaling problems in the reactors and piping.
- the chloride concentration of the lixiviant prior to leaching is adjusted to obtain a solubility in the range of 75-95% of its saturation. This adjustment will yield different amounts of chloride ion initially in solution given that the solubility of the specified chlorides varies considerably.
- the chloride concentration may also be adjusted to take into account the concentration of iron in the sulfide ore material. In the preferred embodiment, the chloride concentration will be adjusted so as to yield between about 30g/L and about 50g/L of ferrous chloride at the end of the leaching step 50. It should be appreciated that the concentration of chloride ions and acid in the lixiviant is selected to maximize dissolution of iron in the lixiviant.
- the concentration of magnesium chloride in the lixiviant should be at least 300 g/L.
- the optimum concentration of magnesium chloride has been determined to be between about 340g/L and about 420 g/L.
- the concentration of chloride has been determined to be important in the kinetics of the leaching reactions, and on the vapour pressure of both water and hydrochloric acid above the reaction slurry. Higher total chloride concentrations lead to increased kinetics and lower vapour pressures of water but higher in hydrochloric acid.
- the leaching step 50 the sulfide ore material is contacted and leached with the lixiviant to obtain a solid residue and a leachate containing dissolved iron therein.
- a majority of the leachable iron in the source sulfide ore material will be in solution.
- at least 70% of the iron will be dissolved in the leachate and more preferably, the leachate will contain over 90% of the iron.
- the leaching step 50 may be conducted in a single reactor, or in a plurality or reactors arranged either in series or in parallel. In the preferred embodiment, the leaching step 50 is carried out in three or more leaching reactors. These leaching reactors may be pressurized or unpressurized vessels. Preferably, the leaching step 50 is carried out in an unpressurized vessel (i.e. at atmospheric or ambient pressure). The use of an unpressurized vessel tends to be less cost intensive. In contrast to certain known prior art processes which require elevated pressures and temperatures to obtain reaction kinetics sufficiently rapid to enable a viable commercial process, the leaching step 50 tends to achieve satisfactory reaction kinetics at atmospheric pressure.
- the leaching step 50 may be conducted as a continuous process or a batch process. If conducted as a continuous process, the leaching may be performed co-currently, countercurrently, or in any other suitable manner known in the art. The leaching step 50 may also be conducted in a pachuca.
- the leaching step 50 may carried out at a temperature that lies in the range of about 20 0 C to about the boiling point of the lixiviant at ambient pressure, (which is about 12O 0 C).
- the filterability of the leach residue has been found to be greatly enhanced at temperatures greater than about 105 0 C due to the dehydrating effects of the chloride lixiviant.
- the temperature at which the leaching step 50 may be conducted is preferably between 105 0 C and about 110 0 C.
- the pH is usually an important parameter in hydrometallurgical processes, the pH tends not to have an important role in the leaching step 50. It may however be used as an indicator of the reaction progress or as a control mechanism.
- the redox (or oxidation-reduction) potential (Eh) tends not be a significant parameter of the leaching step 50.
- the leaching conditions are maintained at the natural oxidation-reduction potential of the system, which tends to be reducing.
- leaching of the sulfide ore material is controlled to permit the dissolution of iron only - no substantial amounts of base metals or value metals are dissolved within the leachate.
- the base metals and any value metals in the sulfide ore material remain in the solid residue.
- the solid residue obtained from the leaching step 50 is an upgraded base metal concentrate upon which may be further processed to recover the base metals and any value metals contained therein.
- Hydrogen sulfide gas is formed during the leaching step 50 as the sulfur in the sulfide ore material is converted to hydrogen sulfide under reducing conditions.
- the hydrogen sulfide thus formed is removed from the lixiviant at step 70.
- the hydrogen sulfide gas is stripped from the lixiviant in a continuous manner to ensure the concentration of hydrogen sulfide in the lixiviant is kept relatively low.
- An inert (non-oxidizing) carrier gas for instance, argon or nitrogen
- the leaching step 50 may be conducted under a relatively small negative pressure (vacuum) to remove the hydrogen sulfide gas formed.
- DM_TOR/264119-00003/2103883.1 14 0057 At least one portion of the hydrogen sulfide gas is reacted (at step 80) with sulfur dioxide gas, in a Claus reaction to recover an elemental sulfur product and steam, according to the following chemical reaction:
- the Claus reaction may be carried out in one or more stages, using one or more catalysts. High rates of recovery in the order of 94% to 97% of elemental sulfur may be achieved. It will thus be appreciated that reacting the sulfur dioxide gas in a Claus reaction allows for the recovery of the intrinsic energy in the sulfide ore material.
- the high-pressure steam produced by this reaction may be used to supply and/or sustain the energy requirements of the processing and refining operations, thereby potentially resulting in substantial savings in operating costs.
- the hydrogen gas so liberated may be collected for use as a clean energy source. For instance, it could be employed as clean fuel to power the oxy-fuel burners of a pyrohydrolysis reactor used for further refining the upgraded base metal concentrate obtained.
- a fuel cell i.e. a solid oxide fuel cell
- a co-generation plant to produce electric power and high-pressure steam. The electric power thus generated could be used to supply some or all of the energy requirements of the plant and associated township.
- a typical sulfide ore containing about 30% sulfur at a treatment rate of 5000 to 10,000 tonnes ore/day would generate at least 10 MW of electric power using existing solid oxide fuel cell technology.
- recovering the useful energy from a sulfide ore in this manner alleviates the requirement for the generation of on-site power and heat energy from the burning of fossil fuels such as coal, oil or natural
- DM TOR/264119-00003/2103883.1 15 gas and furthermore, eliminates the production of the greenhouse gases associated with the burning of these fuels. Moreover, substantial savings in energy costs may be achieved.
- the cuprous sulfide formed at step 90 is exposed to oxygen (i.e. "blown") at step 100 as in any typical copper converter to re-form the elemental molten copper and liberate sulfur dioxide gas. Since both of the reactions with the molten copper (steps 90 and 100) are kinetically fast, only a relatively small amount of copper need be employed to perform step 90. As a result, the reactor may be run on a continuous basis. Alternatively, the cuprous sulfide may be sold to a copper smelter if desired and fresh copper may be supplied to carry out step 90.
- a portion of the sulfur dioxide gas formed at step 90 may be used as an oxidant in a lixiviant in an additional leaching step carried out to further refine the upgraded base metal concentrate (as further explained below). The remaining portion may be employed in the Claus reaction carried out at step 80.
- the sulfur dioxide may be converted to sulfuric acid, or collected as liquid sulfur dioxide for sale or re-use.
- the hydrogen sulfide stripped from the lixiviant is reacted to molten copper at step 80 to obtain cuprous sulfide and hydrogen gas
- the hydrogen sulfide may be contacted with a solution of a metal or metalloid to thereby form a sulfide, in particular a solution of a copper salt or one containing arsenic - which sulfide may be used in further base metal refining steps.
- the hydrogen sulfide could be burned directly in air to generate steam and a high-strength stream of sulfur dioxide which may be recovered separately as liquid sulfur dioxide.
- DM TOR/264119-00003/2103883.1 16 obtained following the leaching step 50.
- the solid residue and leachate are subjected to a solid/liquid separation step 110, following which the upgraded base metal concentrate is subjected to a series of base metal recovery steps and the leachate is treated for the recovery of an iron product and recycled hydrochloric acid.
- the leachate may be necessary to heat the leachate to at least about 19O 0 C to precipitate the iron as hematite.
- the leachate will be heated to a temperature between about 19O 0 C and about 25O 0 C, and most preferably, between about 22O 0 C and about 250 0 C.
- the precipitation step 130 involves air/oxygen sparging (although, other suitable oxidants may be used) and adding sufficient moisture/water to hydrolyse the iron to thereby promote the formation of a hematite precipitate.
- the precipitate thus obtained is a high-purity, easily filterable, crystalline hematite product.
- the water required for the reaction may be most conveniently added as steam, the latter also providing the heat necessary for distilling the hydrochloric acid from the leachate.
- the iron may be oxidized by air and hydrolysed by water to form hematite according to following chemical reactions:
- magnesium chloride used in the lixiviant is magnesium chloride, or if appreciable quantities of magnesium have been dissolved in the leaching step, then magnesium sulfate, which has a much lower solubility than magnesium chloride, will precipitate and will form instead of jarosite.
- the iron is precipitated out of the remaining leachate as hematite, this need not be the case in all applications, hi an alternative embodiments, other iron product precipitates could be obtained. More specifically, if only a limited quantity of air is added during the precipitation step, magnetite will be formed according to following chemical reactions:
- the iron will precipitate as ferrous oxide according to the following chemical reaction:
- the remaining leachate (now an iron-depleted, magnesium chloride liquor) and the hematite product are then subjected to a solid/liquid separation step 140.
- the hematite product thus recovered may be dried and sold, or simply disposed of.
- the magnesium chloride liquor is regenerated and recycled for use in the process 20.
- the recycled magnesium chloride liquor and the recycled hydrochloric acid may be combined to form some of the lixiviant used in leaching step 50.
- the recycled magnesium chloride liquor, the recycled hydrochloric acid and the sulfide ore material may be combined in any particular order prior to being introduced into the reactor(s) in which leaching step 50 is conducted. However, it is preferred that sulfide ore material and the recycled magnesium chloride liquor be combined prior to the recycled hydrochloric acid being added.
- the upgraded base metal concentrate is subjected to a series of base metal recovery steps that include performing a second leaching step 150. This, however, need not be the case in every application.
- the upgraded base metal concentrate may be subjected to flotation to obtain separate base metal concentrates and a precious metal concentrate.
- the second leaching step 150 is carried out substantially as set out in United States Patent Application Publication No. 2005/0118081 of Harris et al., the disclosure of which is hereby incorporated by reference. To facilitate understanding, the second leaching step 50 is briefly described below.
- the upgraded base metal concentrate is contacted and leached with a second lixiviant to obtain a solid residue in the nature of a value metal concentrate and a leachate containing predominantly all of the base metals and any iron remaining from the primary leach circuit, in solution.
- the value metal concentrate and the base metal rich-leachate are subjected to a solid/liquid separation step 160, following which the value metal concentrate is treated to extract one or more value metals therefrom and the base metal rich-leachate is subjected to a series of base metal recovery steps as explained in greater detail below.
- the solid/liquid separation step 160 may employ any known technique for effecting such separation including pressure or vacuum filtration, countercurrent decantation or centrifuge.
- the second leaching step 150 may be carried out a temperature that lies in the range of about 20 0 C to about the boiling point of the lixiviant at ambient pressure, (which is about 120 0 C).
- the leaching conditions in particular, the lixiviant, redox potential (Eh) and pH, may be controlled to dissolve predominantly all of the base metals and remaining iron from the upgraded base metal concentrate.
- the value metals such as, the platinum group metals (PGMs), gold and silver are not substantially leached - these remain in the solid residue to be recovered by any means known in the art.
- the value metal concentrate may be subjected to a leaching step to dissolve the PGMs, gold and silver.
- the lixiviant used for this leaching step could be the same as that employed in the first and second leach circuits, except that the redox potential for the system would be increased preferably to greater than about
- Known PGM separation steps could then be performed to recover the PGMs, gold and silver present.
- value metal recovery could be effected by cementation with metallic copper, zinc or organic or inorganic reductants.
- the lixiviant used in the second leaching step 150 includes an acid, an oxidant, and a chloride.
- the lixiviant includes the remaining leachate from the precipitation step 130 (that is, a solution of ferric chloride and magnesium chloride).
- a lixiviant similar or substantially similar to that used in the primary leach that is, a lixiviant comprising an acid and a chloride, but no oxidant
- a lixiviant comprising an acid and a chloride, but no oxidant
- certain base metals i.e. nickel and cobalt
- the leachate (containing ferrous chloride and magnesium chloride) obtained following the first leaching step 50 could be employed in the second leaching step 150.
- the acid may be an organic acid, sulfurous acid, sulfuric acid or hydrochloric acid - with hydrochloric acid being the preferred acid.
- the oxidant may be a mixture of sulfur dioxide and oxygen and/or air. The sulfur dioxide formed during the "blowing" of cuprous sulfide at step 100 could be used as a constituent of the second lixiviant.
- other oxidants taken alone or in combination, may be used to similar advantage.
- any of the following compounds could be suitable oxidants for the second lixiviant: alkali metal peroxides, alkaline earth metal peroxides, alkali metal perchlorates, alkaline earth metal perchlorates, ammonium perchlorate, magnesium perchlorate, alkali metal chlorates, alkaline earth metal chlorates, alkali metal hypochlorites, alkaline earth metal hypochlorite, chlorine, hydrogen peroxide and peroxysulfuric acid.
- the chloride may be magnesium chloride, calcium chloride, sodium chloride, potassium chloride, lithium chloride, ferrous chloride or mixtures thereof and moreover, may be the same chloride as the one used in the primary leach circuit.
- the use of magnesium chloride in the second lixiviant is particularly favoured, since it is amenable to a pyrohydrolysis step (if necessary), as further described below.
- hydrogen sulfide gas may be formed during the leaching step 150 as the remaining sulfur in the upgraded base metal concentrate material is converted to hydrogen sulfide under reducing conditions.
- the hydrogen sulfide thus formed may be stripped from the lixiviant in a continuous manner.
- the stripping of hydrogen sulfide may be facilitated by adding an inert (non-oxidizing) carrier gas to the lixiviant solution.
- any remaining iron in solution occurs at step 170. Accordingly, where hydrogen sulfide is formed during the leaching step 150, it will be possible to distil the hydrochloric acid and precipitate hematite from the leachate by heating the leachate to a temperature of at least 18O 0 C in the presence of additional moisture/water and simultaneously subjecting the remaining leachate to a precipitation step, as in the primary leach circuit. As mentioned above, where no additional moisture/water is supplied, it may be necessary to heat the leachate to at least about 190 0 C to precipitate the iron as hematite. Preferably, the leachate will be heated to a temperature between about 19O 0 C and about 25O 0 C, and most preferably, between about 220 0 C and about 250 0 C.
- hydrolytic distillation may be carried out to precipitate jarosite. If there is insufficient iron present for this purpose, then some may be added from the primary leach circuit. The jarosite thus obtained tends to be very pure and
- DM_TOR/264U9-00003/2103883.1 21 may be easily filtered.
- a solid/liquid separation step 175 is then carried out to separate the hematite or jarosite precipitate from the leachate.
- the base metal-rich leachate may be subjected to a series of base metal recovery steps. These steps may be carried out in accordance with any known base metal extraction process including ion exchange, solvent extraction, electrowinning or sulfide precipitation. The use of electrowinning may be particularly advantageous, since power generated from process 20 either in the form high- pressure steam or hydrogen gas may be used. IQ accordance with the foregoing process, high rates of base metal extraction may be obtained. For instance, using this process, recovery rates of greater than 95% have been achieved for nickel and cobalt, and greater than 85% for copper.
- Hydrochloric acid may be recovered and recycled after each metal removal step in a manner analogous to that carried out in the primary leach circuit, thereby obviating the need to neutralize the acid with a base.
- the value metal-depleted leachates may also be treated to regenerate the chloride and acid constituents of the lixiviant.
- magnesium oxide (magnesia) and hydrochloric acid may be obtained by subjecting the base metal-depleted leachate to a pyrohydrolysis step.
- the oxy-fuel burners of the pyrohydrolysis reactor could be fuelled by the hydrogen gas generated at step 90.
- the magnesium oxide thus produced may be used in the recovery of base metals - more specifically, to effect neutralization and precipitation of certain metal products (e.g. cobalt and nickel oxide).
- the use of magnesium oxide for neutralization and precipitation is advantageous because the required amount of magnesium oxide may be produced by the system.
- the addition of magnesium oxide does not add any further ions in the leachate, which would otherwise require the use of additional treatment steps.
- the hydrochloric acid content of the condensate was in the range 0.5-3.0 g/L.
- concentration of the hydrochloric acid was as high as 3.0-3.5M.
- FIG. 3 there is shown a schematic representation of a process designated with reference numeral 200 in accordance with another embodiment of the invention, which involves the removal of iron material from an oxidic ore material.
- the oxidic ore material to be treated contains nickel oxide, cobalt oxide, zinc oxide and/or copper oxide.
- the oxidic ore material is a laterite ore material.
- the laterite ore material may be a limonite ore material, a saprolite ore material, a hematitic clay material or a serpentinite material.
- the laterite ore material may contain various profiles of the afore-mentioned materials.
- the laterite ore material may comprise a low-magnesium, high-iron limonite and high-magnesium, low-iron saprolite.
- Process 200 is generally similar to process 20 used to treat the sulfide ore material, in that it includes the steps of: providing a base metal containing material (in this case, a laterite ore material) 210; providing a lixiviant 220; performing a leaching step on the laterite ore material at atmospheric pressure, using the lixiviant to obtain a solid residue and a base metal-rich leachate containing dissolved iron therein 230; separating the leachate from the solid residue 240; and treating the leachate to recover therefrom iron as a hematite product of high purity (step 245).
- a base metal containing material in this case, a laterite ore material
- a lixiviant 220 performing a leaching step on the laterite ore material at atmospheric pressure, using the lixiviant to obtain a solid residue and a base metal-rich leachate containing dissolved iron therein 230
- separating the leachate from the solid residue 240 and treating the leachate to recover there
- the laterite ore material does not require substantial treatment (i.e. roasting or flotation) prior to being subjected to the leaching step 230.
- DM TOR/264119-00003/2103883.1 26 it may be advantageous to perform certain well-known physical conditioning steps (i.e. benef ⁇ ciation, crushing and/or grinding) on the laterite ore material to improve the overall efficiency of the process.
- certain well-known physical conditioning steps i.e. benef ⁇ ciation, crushing and/or grinding
- the lixiviant used in the leaching step 230 is similar to that used in the leaching step 50. It includes an acid and a chloride.
- the acid in the lixiviant may be an organic acid (such as, acetic acid, tartaric acid and citric acid), sulfiirous acid, sulfuric acid or hydrochloric acid. Although, hydrochloric acid is preferred.
- the amount of acid to be used in the lixiviant tends to depend on the iron content in the laterite ore material. Generally speaking, the higher the content of icon in the laterite ore material, the more acid will be required needed to put the iron in solution.
- the chloride constituent in the lixiviant may be magnesium chloride, calcium chloride, sodium chloride, potassium chloride, lithium chloride, ferrous chloride or mixtures thereof.
- Magnesium chloride is the preferred chloride, particularly where the acid employed in the lixiviant is hydrochloric acid.
- the chloride concentration in the lixiviant prior to leaching is adjusted to obtain a solubility in the range of about 75% to about 95% of its natural solubility and more preferably, between about 85% to 95%. This adjustment will yield different amounts of chloride ion in solution given that the solubility of the specified chlorides varies considerably. For instance, calcium is more soluble than magnesium, which in turn is more soluble than sodium.
- the chloride concentration may also be adjusted to take into account the concentration of iron in the laterite ore material. It should be appreciated that the concentration of chloride ions and acid in the lixiviant is selected to maximize dissolution of iron and the base metals in the lixiviant and to ultimately, to effect recovery of at least 90% of the base metals.
- the concentration of magnesium chloride in the lixiviant will be in the range of about 300g/L to about 420 g/L.
- a magnesium chloride concentration of about 360g/L has been found to be suitable.
- a higher concentration of magnesium chloride is preferred, more specifically, in the range of about 380 g/L to 400g/L.
- the laterite ore material is contacted and leached with the lixiviant to obtain a solid residue and a base metal-rich leachate containing dissolved iron therein.
- a majority of the iron in the laterite ore material will be in solution.
- at least 70% of the iron will be dissolved in the leachate and more preferably, the leachate will contain over 90% of the iron found in the laterite ore material.
- the iron thus dissolved may be either ferrous or ferric.
- the greater the amount of iron dissolved in the leachate the greater the amount of base metals will be put into solution. This is because when the iron dissolves, the base metals previously held in the iron matrix (most commonly nickel, cobalt and manganese) are released into the leachate.
- iron which is largely present as goethite in laterite nickel ores, may be solubilized according to the following reaction:
- the leaching step 230 may be carried out under conditions that tend to control the leaching of magnesium.
- magnesium leaching could be inhibited by using a relatively high initial magnesium chloride concentration in the lixiviant.
- the lixiviant may be prepared with an initial magnesium chloride concentration that is greater than about 380 g/L, and more preferably, greater than about 400 g/L.
- an organic acid which has a sparingly soluble magnesium salt could be used as the constituent acid in the lixiviant.
- Tartaric acid and citric acid have been found to be effective for the control of dissolved magnesium in such instances.
- the leaching of magnesium may be inhibited by using a lixiviant with a chloride other than magnesium chloride and ensuring the lixiviant is saturated by the alkaline earth metal cation selected.
- the leaching step 230 may be conducted in a single reactor, or in a plurality or reactors arranged either in series or in parallel. These leaching reactors may be pressurized or unpressurized vessels. Preferably, the leaching step 230 is carried out in an unpressurized vessel (i.e. at atmospheric or ambient pressure). The use of an unpressurized vessel tends to be less cost intensive.
- the leaching step 230 may be conducted as a continuous process or a batch process. If conducted as a continuous process, the leaching may be performed co-currently, countercurrently, or in any other suitable manner known in the art. The leaching step 230 may also be conducted in a pachuca or as a heap leach.
- the leaching step 230 may carried out at a temperature that lies in the range of about 20 0 C to about the boiling point of the lixiviant at ambient pressure, (which is about 120 0 C).
- the temperature at which the leaching step 50 may be conducted is between about 105 0 C and about 110 0 C.
- the pH is an important parameter in hydrometallurgical processes, the pH tends not to have an important role in the leaching step 230.
- the redox potential (Eh) tends not be a significant parameter of the leaching step 230. While it is preferred that the leaching conditions be maintained at the natural oxidation-reduction potential of the system, unlike most leach circuits, there is no requirement in the present embodiment to control the redox potential.
- a solid residue in the nature of a solid residue and a leachate containing the initial chloride salt (in this case magnesium chloride), ferrous chloride and ferric chloride is
- DM TOR/264119-00003/2103883 1 29 obtained following the leaching step 230.
- the solid residue and leachate are subjected to a solid/liquid separation step 250, following which the leachate is treated for the recovery of at least some of the iron as a hematite product of high purity and recycled hydrochloric acid, and further subjected to a series of base metal recovery steps.
- the leachate obtained also contains aluminum chloride, it will be possible to recover therefrom aluminum as an alumina product.
- the iron could be precipitated as hematite and the hydrochloric acid could be distilled from the leachate, by heating the leachate to a temperature of at least 180 0 C in the presence of additional moisture/water (step 260) and simultaneously subjecting the remaining leachate to a precipitation (step 270).
- additional moisture/water it may be necessary to heat the leachate to at least about 19O 0 C to precipitate the iron as hematite.
- the leachate will be heated to a temperature between about 190 0 C and about 25O 0 C, and most preferably, between about 220 0 C and about 250 0 C.
- the precipitation step 270 is generally similar to precipitation step 130 described earlier, in that it involves air sparging and adding sufficient moisture/water to hydrolyse the iron to thereby promote the formation a hematite precipitate.
- the precipitate thus obtained is a high-purity, easily filterable, crystalline hematite product.
- the water required for the reaction may be most conveniently added as steam, the latter also providing the heat necessary for distilling the hydrochloric acid from the leachate.
- a catalyst preferably oxalic acid
- Such a catalyst has the advantage of significantly improving the reaction kinetics, enhancing the yield of hematite and increasing the concentration of the hydrochloric acid distilled off.
- the iron is advantageously removed as hematite without co- precipitating any of the base metals.
- the high chloride brine environment allows for extremely selective precipitation due to the highly crystalline nature of the precipitates.
- the leachate may be heated to a temperature of between about 16O 0 C and about 19O 0 C (preferably, between about 175°C and about 185°C) and simultaneously subjected to a precipitation step similar to precipitation step 270.
- the remaining leachate (now iron-and-aluminum-depleted) and the hematite and alumina products are then subjected to a solid/liquid separation step 280 which may be performed using any known technique including vacuum filtration. Once recovered, the hematite and alumina may be dried and sold, or simply discarded.
- the remaining (base metal-rich) leachate is subjected to a first and second series of base metal recovery steps 290.
- the first series of base metal recovery steps are carried out to extract from the leachate, base metals other than nickel and cobalt.
- the first series of steps may be carried in accordance with any known base metal extraction process including ion exchange, solvent extraction, electrowinning or precipitation.
- the remaining leachate may further be treated with chemical additives to precipitate manganese, copper, zinc, manganese and cobalt as well as any trace amounts of iron, aluminum and/or chromium that may be present. While the first series of the base metal recovery steps are performed, the nickel and cobalt are maintained in solution.
- a second series of base metal recovery steps may be performed on the remaining leachate to recover the nickel using hydrolytic distillation in a manner analogous to hematite described above. More specifically, nickel may be recovered from the leachate as nickel oxide by adding seed of the said nickel oxide, raising the temperature close to the
- the steam itself may be used to raise the temperature.
- the nickel oxide so produced is coarse and crystalline, and may be separated by any manner known in the art. It will be thus be appreciated that in accordance with the foregoing process high rates of base metal extraction may be obtained. For instance, using this process, recovery rates of greater than 90% have been achieved for nickel and cobalt.
- the leachate may also be treated to regenerate the chloride and acid constituents of the lixiviant. More specifically, hydrochloric acid may be recovered and recycled after each metal removal step in a manner analogous to that carried out in the primary leach circuit of process 20, thereby obviating the need to neutralize the acid with a base.
- the magnesium chloride solution may be recycled as well.
- One portion of the recycled magnesium chloride may be returned to the leach circuit whereas as another portion may be used in a pyrohydrolysis reaction to form magnesium oxide (magnesia) and hydrochloric acid.
- the magnesium oxide thus produced may be sold or used in the recovery of base metals - more specifically, to effect neutralization and precipitation of certain metal products (e.g. cobalt and nickel hydroxides).
- the use of magnesium oxide for neutralization and precipitation is advantageous because the required amount of magnesium oxide may be produced by the system.
- the addition of magnesium oxide does not add any further ions in the leachate, which would otherwise require the use of additional treatment steps.
- Example 14 The experiment of Example 14 was repeated but with aluminum chloride instead of ferric chloride, and with the temperature maintained between 180 0 C and 21O 0 C. hi this case, 60% of the aluminum was precipitated as alumina (shown to be Al 2 O 3 by X-Ray diffraction)
- Example 13 The experiment of Example 13 was repeated, except that the temperature was maintained at 18O 0 C for four hours and neither water nor fresh feed solution was added. No reactions of any kind were observed. The solution remained liquid. This example demonstrates that no solids were formed from a magnesium chloride-ferric chloride mixture at 180 0 C.
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Abstract
Description
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Priority Applications (2)
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CA 2639796 CA2639796A1 (en) | 2005-12-23 | 2006-12-13 | Process for recovering iron as hematite from a base metal containing ore material |
AU2006326812A AU2006326812A1 (en) | 2005-12-23 | 2006-12-13 | Process for recovering iron as hematite from a base metal containing ore material |
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US75287705P | 2005-12-23 | 2005-12-23 | |
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