AU2009200714B2 - Wet process for smelting nickel oxide ore - Google Patents
Wet process for smelting nickel oxide ore Download PDFInfo
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- AU2009200714B2 AU2009200714B2 AU2009200714A AU2009200714A AU2009200714B2 AU 2009200714 B2 AU2009200714 B2 AU 2009200714B2 AU 2009200714 A AU2009200714 A AU 2009200714A AU 2009200714 A AU2009200714 A AU 2009200714A AU 2009200714 B2 AU2009200714 B2 AU 2009200714B2
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- ore
- nickel oxide
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- amount
- leachate
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- 238000000034 method Methods 0.000 title claims abstract description 73
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 61
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000003723 Smelting Methods 0.000 title claims abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 141
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000002002 slurry Substances 0.000 claims abstract description 81
- 229910052742 iron Inorganic materials 0.000 claims abstract description 64
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 41
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000002386 leaching Methods 0.000 claims abstract description 34
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 30
- 239000010941 cobalt Substances 0.000 claims abstract description 30
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000033116 oxidation-reduction process Effects 0.000 claims abstract description 30
- 239000007787 solid Substances 0.000 claims abstract description 26
- 230000003647 oxidation Effects 0.000 claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 25
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 15
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000007664 blowing Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 abstract description 8
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 230000001965 increasing effect Effects 0.000 description 11
- 229910052595 hematite Inorganic materials 0.000 description 10
- 239000011019 hematite Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 10
- 229910052804 chromium Inorganic materials 0.000 description 7
- 239000011651 chromium Substances 0.000 description 7
- 238000006386 neutralization reaction Methods 0.000 description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- -1 iron ions Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 150000001722 carbon compounds Chemical class 0.000 description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 150000003464 sulfur compounds Chemical class 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 241001131796 Botaurus stellaris Species 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002816 nickel compounds Chemical class 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000009283 thermal hydrolysis Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
A process for smelting that can attain a high leaching ratio of nickel and cobalt and a high oxidation ratio of iron 5 to trivalent iron, and, at the same time, can reduce energy cost by suppressing the amount of high-pressure air to be used as an oxidant and the amount of high-pressure steam to be used for maintaining temperature. In a smelting method comprising a first step for slurrying 10 nickel oxide ore and a second step for adding sulfuric acid to the ore slurry and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein, characterized by adjusting the carbon grade in a solid content of ore slurry so as to be 0.1 to 0.5% by mass depending on the 15 blending ratio of the nickel oxide ore that constitutes the ore slurry in the first step and controlling oxidation-reduction potential (Ag/AgCl basis) of the leachate to 400 to 600 mV by adjusting the amount of the high-pressure air to be blown so as to be 700 to 800 Nm3 per ton of carbon in a solid content 20 of ore slurry in the second step.
Description
Reguision 3.2 AUSTRALIA Patents Act 1990 COMPLETE SPECIFICATION STANDARD PATENT Invention Title: Wet process for smelting nickel oxide ore The following statement is a full description of this invention, including the best method of performing it known to us: 1A SPECIFICATION WET PROCESS FOR SMELTING NICKEL OXIDE ORE 5 BACKGROUND OF THE INVENTION FIELD OF THE INVENTION The present invention relates to a wet process for smelting nickel oxide ore, in more detail, relates to a wet process for smelting nickel oxide ore using a high pressure acid leach 10 method including a first step for preparing an ore slurry by slurrying nickel oxide ore and a second step for producing a leachate containing nickel and cobalt by adding sulfuric acid to the ore slurry transferred from the first step and leaching the ore slurry while blowing high-pressure air and 15 high-pressure steam therein (hereinafter, may be referred to as high pressure acid leach method for simplicity), wherein a high leaching ratio of nickel and cobalt is attained; a high oxidation ratio of iron to trivalent iron is attained because most of iron which is a main impurity is fixed to a leached 20 residue in the form of hematite (Fe 2 0 3 ); and at the same time the amounts of high-pressure air to be used as an oxidant and high-pressure steam to be used for maintaining temperature in the high pressure acid leach method can be suppressed leading to energy cost reduction. 25 DESCRIPTION OF THE PRIOR ART As a smelting process for separating/recovering nickel and cobalt from iron, from nickel oxide ore containing iron as a main component and nickel of 1 to 2% by mass, for example, 2 a dry smelting process in which a matte containing a nickel sulfide is produced by roasting nickel oxide ore, reducing and sulfurizing nickel compounds followed by smelting, or a reduction roast-leach process in which nickel oxide ore is 5 subjected to reduction roasting and then nickel and cobalt are selectively leached while forming an ammonium complex ion has been conventionally conducted. These smelting processes, however, have a problem that 10 these processes waste much energy and cost because these processes include a dry-treatment step for drying and roasting raw ore accompanied by much adhesive moisture and it is impossible to selectively reduce nickel and cobalt alone. A process that can be conducted easily and at a low cost instead 15 of these smelting processes, therefore, has been desired to be developed. The high pressure acid leach method using sulfuric acid has been lately paid attention to as a wet process for smelting nickel oxide ore. Unlike the above conventionally typical 20 smelting processes of nickel oxide ore, this method is composed of wet steps throughout without any dry-treatment step for drying and roasting, making it advantageous in view of energy and cost saving. 25 The high pressure acid leach method includes, for example, a leaching step for producing a leached slurry by adding sulfuric acid to a slurry of nickel oxide ore followed by leaching under the conditions of a high temperature of 200*C or higher and high pressure using an autoclave; a step for 3 separating the leached slurry into a leached residue and a leachate containing nickel and cobalt; a neutralization step for adjusting the pH of the leachate containing impurity elements besides nickel and cobalt to form a slurry of a 5 neutralization deposit containing the impurity elements such as iron and a purified mother liquor for recovering nickel; and a sulfurization step for supplying the mother liquor for recovering nickel with hydrogen sulfide gas to form a sulfide mixture of nickel/cobalt and a lean solution (for example, see 10 Patent Literature 1). Incidentally, the high pressure acid leach method has a great advantage that nickel and cobalt can be selectively leached against iron because the iron of a main impurity is fixed 15 to a leached residue in the form of hematite (Fe 2 0 3 ) by controlling the oxidation-reduction potential and temperature of the leachate in a pressurized leach reactor. On the other hand, the high pressure acid leach method had a problem that because nickel oxide ore having a large variability of ore 20 compositions and organic components contained therein is leached directly without being subjected to roasting, the oxidation-reduction potential (ORP) in leaching fluctuates sharply depending especially on the content of the organic components in the nickel oxide ore. 25 For example, at high oxidation/reduction potential in leaching, chromium contained in nickel oxide ore is oxidized to hexavalent chromium in leaching. It is necessary to reduce the hexavalent chromium to trivalent chromium with a reducing 4 agent in order to remove the hexavalent chromium in the subsequent neutralization step or wastewater treatment step, which causes smelting cost to increase. Without reduction treatment, the chromium is contained as an impurity in a nickel 5 or cobalt product or the problem happens that the chromium remains in a drain from a wastewater treatment unit. In contrast, at too low oxidation-reduction potential in leaching, titanium used in a autoclave as a corrosion-resisting material is degraded, and at the same time a large amount of iron remains 10 in the leachate due to suppressed high-temperature thermal hydrolysis of the iron and causes a problem of increasing the amount of chemicals to be used and the coprecipitation amount of nickel and cobalt in the subsequent neutralization step. 15 As a solution, for example, a method of conducting leaching while controlling the oxidation-reduction potential (Ag/AgC1 basis) of a leachate to 400 to 600 mV by adding one or more of sulfur compounds and carbon compounds to the ore slurry in a high pressure leach method is disclosed (for example, see Patent 20 Literature 1) . In this method, an added sulfur compound or carbon compound serves as a reducing agent and reduces the oxidation-reduction potential and controls to 600 my or lower where hexavalent chromium is not eluted. On the other hand, the oxidation-reduction potential lower than 400 mV not only 25 causes insufficient oxidation hydrolysis of iron but also impairs corrosion resistance of equipment materials and therefore the amount of the sulfur compound or carbon compound to be added is adjusted.
0116_4. DC 5 Incidentally, because leached iron is oxidized to hematite and hydrolyzed in the practical leaching step using this method, it is indispensable to usually use high-pressure air as an oxidant and keep the reactor pressurized. The 5 conditions for using the high-pressure air, however, are not disclosed. In order to cope with fluctuation of oxidation-reduction potential due to variation of the composition of ore and the content of organic components, and especially to prevent drop in oxidation ratio of iron to 10 trivalent iron and elution of chromium caused by the decline of the oxidation-reduction potential, the added sulfur and carbon compounds are used to serve as a reducing agent mainly to lower the oxidation-reduction potential. In this situation, an excess amount of high-pressure air has been blown to control 15 the oxidation-reduction potential. This results in an increase of an exhaust gas from the pressurized reactor leading to an increase of heat loss. The amount of high-pressure steam to be used for temperature control is increased to compensate the heat loss and keep the temperature in the pressurized 20 reactor, which has increased energy cost. [Patent Literature 1] JP-A-2005-350766 (Page 1, Page 2) [Patent Literature 2] JP-A-2005-281733 (Page 1, Page 2) 25 SUMMARY OF THE INVENTION Considering the above problem in conventional technologies, the present invention is directed towards providing a wet process for smelting nickel oxide ore using a high pressure acid leach method including a first step for 30 preparing an ore 6 slurry by slurrying nickel oxide ore and a second step for producing a leachate containing nickel and cobalt by adding sulfuric acid to the ore slurry transferred from the first step and leaching the ore slurry while blowing high-pressure air and 5 high-pressure steam therein (hereinafter, may be referred to as high pressure acid leach method for simplicity), wherein a high leaching ratio of nickel and cobalt is attained; a high oxidation ratio of iron to trivalent iron is attained because most of iron which is a main impurity is fixed to a leached 10 residue in the form of hematite; and at the same time the amounts of high-pressure air to be used as an oxidant and high-pressure steam to be used for maintaining temperature in the high pressure acid leach method can be suppressed leading to energy cost reduction. 15 After having intensively studied the relation among the content of organic components contained in ore, the amount of high-pressure air to be used and the oxidation-reduction potential in the wet process for smelting nickel oxide ore using 20 the above high pressure acid leach method in order to attain the above object, the present inventors have found that when the carbon grade in a solid content of the ore slurry is adjusted so as to be a specified value depending on the blending ratio of the nickel oxide ore having a different carbon grade that 25 constitutes the ore slurry in the first step and the oxidation-reduction potential (Ag/AgCl basis) of the leachate is controlled to 400 to 600 mV by adjusting the amount of high-pressure air to be blown so as to be a specified value in the second step; a high leaching ratio of nickel and cobalt is 7 attained; a high oxidation ratio of iron to trivalent iron is attained because most of iron which is a main impurity is fixed to a leached residue in the form of hematite; and at the same time the amount of high-pressure steam to be used can be 5 suppressed by adjusting the amount of high-pressure air to be used leading to energy cost reduction, and completed the present invention. That is, according to the 1st aspect of the present 10 invention, there is provided a wet process for smelting nickel oxide ore using a high pressure acid leach method comprising a first step for preparing an ore slurry by slurrying nickel oxide ore and a second step for producing a leachate containing nickel and cobalt by adding sulfuric acid to the ore slurry 15 transferred from the first step and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein, characterized by adjusting the carbon grade in a solid content of said ore slurry so as to be 0.1 to 0.5% by mass depending on the blending ratio of the nickel oxide ore having a different 20 carbon grade that constitutes the above ore slurry in the above first step and controlling oxidation-reduction potential (Ag/AgCl basis) of the above leachate to 400 to 600 mV by adjusting the amount of the above high-pressure air to be blown so as to be 700 to 800 Nm3 per ton of carbon in a solid content 25 of said ore slurry in the above second step. In addition, according to the 2nd aspect of the present invention, there is provided the wet process for smelting nickel oxide ore, characterized by further controlling the amount of 0116_4. DDC 8 the high-pressure steam to be used to 150 to 200 kg per ton of dry ore, in the first aspect 1. In addition, according to the 3rd aspect of the present 5 invention, there is provided the wet process for smelting nickel oxide ore, characterized by adjusting the carbon grade in a solid content of the above ore slurry so as to be 0.1 to 0.15% by mass, in the 1st aspect. 10 In addition, according to the 4th aspect of the present invention, there is provided the wet process for smelting nickel oxide ore, characterized in that the oxidation ratio of iron in the leachate is 80% or higher in the above second step, in the 3rd aspect. 15 The wet process for smelting nickel oxide ore of the present invention attains a high leaching ratio of nickel and cobalt as well as a high oxidation ratio of iron to trivalent iron because most of iron which is a main impurity is fixed to 20 a leached residue in the form of hematite, and at the same time can suppress the amount of high-pressure steam to be used by adjusting the amount of high-pressure air to be used leading to energy cost reduction. The process, therefore, is very valuable in industries. 25 In yet a further aspect of the invention there is provided a wet process for smelting nickel oxide ore using a high pressure acid leach method comprising a first step of preparing an ore slurry by slurrying nickel oxide ore and a second step of 0116_4 . C 8a producing a leachate containing nickel by adding sulfuric acid to the ore slurry transferred from the first step and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein, wherein the nickel oxide ore 5 comprises more than one nickel oxide ores having different carbon grades and the process further comprises adjusting the carbon grade of the solid content of the ore slurry in the first step to be 0.1 to 0.5% by mass by adjusting on the blending ratio of the nickel oxide ores having a different carbon grades that 10 constitutes the ore slurry in the first step and controlling the oxidation-reduction potential (Ag/AgCl basis) of the above leachate to 400 to 600 mV by adjusting the amount of the above high-pressure air to be blown so as to be 700 to 800 Nm 3 per ton of carbon in the solid content of the ore slurry in the second 15 step. Reference to any prior art in the specification is not, and should not be taken as, an acknowledgment, or any form of suggestion, that this prior art forms part of the common general 20 knowledge in Australia or any other jurisdiction or that this prior art could reasonably be expected to be ascertained, understood and regarded as relevant by a person skilled in the art. 25 As used herein, except where the context requires otherwise, the term "comprise" and variations of the term, such as "comprising", "comprises" and "comprised", are not intended to exclude other additives, components, integers or steps.
0116_4 .DOC 8b BRIEF DESCRIPTION OF THE DRAWINGS [Figure 1] Figure 1 shows a relation between the carbon grade in ore and the ORP of the acid leachate. (Example 1) [Figure 2] Figure 2 shows a relation between the carbon 9 grade in ore and the ratio (Fe (III) /Fe, total) representing the oxidation ratio of iron. (Example 1) [Figure 3] Figure 3 shows a relation between the amount of high-pressure air to be blown per ton of carbon in ore and 5 the ORP of the leachate. (Example 2, Comparative Example 1) (Figure 4] Figure 4 shows a relation between the amount of high-pressure air to be blown (amount of high-pressure air) and the amount of high-pressure steam to be used (amount of high-pressure steam). (Example 3) 10 DETAILED DESCRIPTION OF THE INVENTION The wet process for smelting nickel oxide ore of the present invention is described in detail hereinafter. The wet process for smelting nickel oxide ore of the 15 present invention is a wet process for smelting nickel oxide ore using a high pressure acid leach method comprising a first step for preparing an ore slurry by slurrying nickel oxide ore and a second step for producing a leachate containing nickel and cobalt by adding sulfuric acid to the ore slurry transferred 20 from the first step and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein, characterized by adjusting the carbon grade in a solid content of said ore slurry so as to be 0.1 to 0.5% by mass depending on the blending ratio of the nickel oxide ore having a different 25 carbon grade that constitutes the above ore slurry in the above first step and controlling oxidation-reduction potential (Ag/AgCl basis) of the above leachate to 400 to 600 mV by adjusting the amount of the above high-pressure air to be blown so as to be 700 to 800 Nm3 per ton of carbon in a solid content 10 of said ore slurry in the above second step. It is important in the process for smelting of the present invention to adjust the carbon grade in a solid content of an 5 ore slurry so as to be a specified value depending on the blending ratio of several kinds of nickel oxide ore, the raw material and to adjust the amount of high-pressure air to be blown in leaching to a specified value in accordance with the amount of carbon in the ore slurry. This adjustment can control the 10 oxidation-reduction potential (Ag/AgC1 basis) of a leachate to 400 to 600 mV and enables a high leaching ratio of nickel and cobalt to be attained and a high oxidation ratio of iron to trivalent iron to be attained because most of iron which is a main impurity is fixed to a leached residue in the form of 15 hematite. Further, because the amount of an exhaust gas from the pressurized reactor is reduced leading to reduction of heat loss by adjusting the amount of high-pressure air to be blown so as to be a specified value, the amount of high-pressure steam to be used in leaching can be controlled to 150 to 200 kg per 20 ton of dry ore leading to energy cost reduction in leaching. That is, in a process for smelting using a conventional high pressure acid leach method, comparatively large amount of organic components is sometimes contained in the mined nickel 25 oxide ore that, when it is treated, the oxidation-reduction potential in leaching is markedly lowered. Because oxidation of iron is not promoted in this situation, a large amount of divalent iron ions remain in a leachate making it difficult to separate iron from crude aqueous solution of sulfuric acid of 11 nickel/cobalt mixture in a subsequent step or causing cost increase of operation materials necessary for the separation. In addition, degradation in corrosion resistance of the pressurized reactor and ancillary facilities is brought about. 5 It is, therefore, important to keep the oxidation-reduction potential proper, which has led to blowing of an excessive amount of high-pressure air. Here, the oxidation/reduction potential (Ag/AgCl basis) 10 of the leach is 400 to 600 mV, preferably 550 to 600 mV. That is, the oxidation-reduction potential (Ag/AgCl basis). lower than 400 mV causes not only insufficient oxidation of iron, but also impairs the corrosion resistance of equipment materials. In contrast, the oxidation-reduction potential (Ag/AgCl basis) 15 over 600 mV causes a problem that the chromium oxidized to hexavalent is contained as an impurity in a nickel or cobalt product or remains in a drain from a wastewater treatment unit. Therefore, in the above process for smelting, because the 20 content of organic components in an ore slurry is stably adjusted to a desired value by adjusting the carbon grade in a solid content of the ore slurry so as to be a specified value depending on the blending ratio of several kinds of nickel oxide ore of the raw material, the effect on the oxidation and an 25 excessive fluctuation can be suppressed. Incidentally, adjustment of the carbon grade in a solid content of the ore slurry is conducted by periodically analyzing the carbon grades in several kinds of the ore to be treated and blending them. Further, in the above process for smelting, the 12 oxidation-reduction potential (Ag/AgCl basis) of a leachate can be controlled to 400 to 600 mV by adjusting the amount of high-pressure air to be blown to a specified value in leaching in accordance with the carbon grade in the ore slurry. As a 5 result, the oxidation ratio of iron, which indicate a ratio of the concentration of trivalent iron ions to the concentration of total iron ions in the leachate goes up to 50% or higher, and especially 80% or higher in the case of the carbon grade of 0.15% or lower. 10 The carbon grade in a solid content of the ore slurry is 0.1 to 0.5% by mass, preferably 0.1 to 0.15% by mass. That is, the carbon grade over 0.5% by mass lowers the oxidation-reduction potential of the leachate making it 15 difficult to control the oxidation-reduction potential (Ag/AgCl basis) to 600 mV or lower without blowing an excessive amount of high-pressure air. On the other hand, considering the existence amount of organic components in ore, it is difficult to make the carbon grade to be lower than 0.1% bymass. 20 The amount of high-pressure air to be blown is adjusted so as to be 700 to 800 Nm3 per ton of carbon in a solid content of the ore slurry. That is, when the ore having the above carbon grade is used, the amount of high-pressure air to be blown 25 less than 700 Nm3 lowers the oxidation-reduction potential of the leachate making it difficult to control the oxidation-reduction potential (Ag/AgCl basis) to 400 mV or higher, which not only causes insufficient oxidation hydrolysis of iron, but also may impair the corrosion resistance of 13 equipment materials. On the other hand, the amount of high-pressure air to be blown over 800 Nm 3 causes an increase of the amount of an exhaust gas leading to an increase of heat loss, which increases the amount of high-pressure steam to be 5 used for keeping the temperature, while enhancing the oxidation-reduction potential of the leachate. Here, high-pressure air is blown into a pressurized reactor in order to control the oxidation-reduction potential 10 of a leachate to a specified value. As it is possible to maintain an oxidative atmosphere by purging carbonic acid gas generated in leaching into the pressurized reactor as it is, the carbonic acid gas is preferably discharged timely together with the exhaust gas by a pressure automatic control system 15 installed to the pressurized reactor. By this method, blowing of high-pressure air prevents excessive blowing and it is adjusted to 700 to 800 Nm 3 per ton of carbon in a solid content of the ore slurry. In this time, the amount of high-pressure steam to be used can be controlled to 150 to 200 kg per ton of 20 dry ore. Here, the dry ore means the ore dried at about 100 0 C and removed adherent moisture. High-pressure air to be usually used for industry, for example, air having a pressure of 3 to 6 MPaG is used as the 25 above high-pressure air. High-pressure steam to be usually used for industry, for example, steam having a pressure of 3 to 6 MPaG is used as the above high-pressure steam.
14 The wet process for smelting nickel oxide ore using the above high pressure acid leach method is not particularly limited, as long as it includes a first step for preparing an ore slurry by slurrying nickel oxide ore and a second step for 5 producing a leachate containing nickel and cobalt by adding sulfuric acid to the ore slurry transferred from the first step and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein. The following conditions are applied in the above step so that the leaching ratio of each 10 of nickel and cobalt reaches 90% or higher and to 95%. The nickel oxide ore to be used in the above step is so-called lateritic ore such as limonite and saprolite. Nickel content in the lateritic ore is usually 0.5 to 3.0% by mass and 15 nickel is contained as a hydroxide or a silicic bittern (magnesium silicate) mineral. In addition, iron content is 10 to 50% by mass and iron is contained mainly as a trivalent hydroxide (goethite, FeOOH) . Divalent iron is partially contained in the si-licic bittern mineral. 20 As the above first step, nickel oxide ore is slurried by grinding and crushing in the water. Thereafter, it is preferable to remove redundant water in the slurry and thicken the slurry using a solid-liquid separation unit such as a 25 thickener to prepare the ore slurry of a specified concentration. In this time, the carbon grade in a solid content of the ore slurry is adjusted so as to be in a specified range depending on the blending ratio of several kinds of nickel oxide ore of the raw material.
15 The concentration of the slurry to be used in the above step is not particularly limited because it depends largely on the properties of nickel oxide ore to be treated. However, the 5 leached slurry of high concentration is preferable and usually adjusted so as to be about 25 to 45% by mass. That is, the leached slurry of a concentration lower than 25% by mass requires a large facility to obtain a same residence time in leaching, and also an addition amount of an acid increases in 10 order to adjust the residual acid concentration. In addition, the obtained leachate has a lower concentration of nickel. In contrast, the leached slurry of a concentration higher than 45% by mass makes the viscosity (yield stress) of slurry itself high, and causes a problem of difficult transfer (frequent clogging 15 of pipe, high energy requirement etc. ) while it requires smaller facilities. As the above second step, the slurry of nickel oxide ore is added with sulfuric acid and subjected to blowing of 20 high-pressure air as an oxidant and high-pressure steam as a heat source and stirring while controlled under specific conditions of pressure and temperature to form a leached slurry composed of a leached residue and a leachate. The leachate containing nickel and cobalt is thus obtained. As the operation 25 in this step is conducted under a pressure depending on a specified temperature, for example, 3 to 6 MPaG, a pressure vessel of thermal resistance (autoclave) that can bear these conditions is used.
16 In the above step, nickel and cobalt are leached to a sulfide and leached iron sulfide is fixed as hematite in the leach reaction and the high-temperature hydrolysis represented by the following formulae (1) to (5). However, as fixation of 5 iron ions does not entirely proceed, the iron ions of divalent and trivalent are usually contained besides nickel and cobalt in a liquid part of the obtained leached slurry. [leach reactionJ 10 MO + H 2
SO
4 -4 MSO 4 + H20 (1) (wherein M indicates Ni, Co, Fe, Zn, Cu, Mg, Cr, Mn or the like) 2FeOOH + 3H2S0 4 - Fe 2 (SO4) 3 + 4H 2 0 (2) FeO + H2SO4 - FeSO 4 + H 2 0 (3) 15 [high-temperature hydrolysis] 2FeSO 4 + H 2
SO
4 + 1/202 -. Fe 2 (304)3 + H20 (4) Fe 2
(SO
4
)
3 + 3H20 - Fe 2 0 3 + 3H 2
SO
4 (5) The temperature to be used in the above step is not 20 particularly limited, but is preferably 220 to 280*C, more preferably 240 to 270*C. It is because most of iron is fixed as hematite by conducting the reaction in this range of temperature. In a temperature lower than 220 0 C, iron dissolves and remains in the reaction solution due to a low rate of the 25 high-temperature hydrolysis resulting in an increase of the load in the subsequent neutralization step for removing the iron, which makes it very difficult to separate the iron from nickel. In contrast, a temperature higher than 280"C is not suitable because the selection of the material of a vessel to be used 17 for leaching at high pressure is difficult and in addition the cost of steam for raising temperature is increased, while the high-temperature hydrolysis itself is promoted. 5 The amount of sulfuric acid to be used in the above step is not particularly limited and an excessive amount is used so as to leach iron in ore. For example, an amount of 200 to 500 kg per ton of ore is used. An amount more than 500 kg per ton of ore of sulfuric acid to be added is not desirable due to high 10 cost of the sulfuric acid. Incidentally, the pH of the obtained leachate is preferably adjusted so as to be 0.1 to 1.0, considering filterability of the leach residue containing hematite generated in the solid/liquid separation step. 15 EXAMPLES Hereinafter, the present invention is described more specifically with reference to examples and comparative examples of the invention, to which, however, the present 20 invention is not limited at all. The analysis method of metals used in the examples and comparative examples is ICP emission spectroscope analysis. (Example 1) 25 Nickel oxide ore having a nickel content of 1.25% by mass and an iron content of 46% by mass that was adjusted so that the carbon grade was 0.1 to 0.3% by mass was slurried to obtain a slurry having a solid fraction of about 40% by mass, which was charged in an autoclave reactor of 1 M 3 in volume made of 18 titanium. Sulfuric acid was added so that the concentration of free sulfuric acid was about 45 g/l in the terminal reaction solution. High-pressure air of about 5 MPaG was blown into the autoclave 5 at a rate of 750 Nm 3 per ton of carbon in a solid content of the ore slurry and at the same time high-pressure steam of about 5 MPaG was blown. The slurry was kept at 245 0 C for an hour while being stirred. The concentration of iron and the ORP (Ag/AgCl electrode basis) of the obtained leached slurry were measured. 10 The amount of high-pressure steam used was 200 kg per ton of dry ore. The leached slurry was added with a slurry of calcium carbonate and deprived of a trivalent Fe ion through oxidative neutralization followed by measuring the concentration of 15 divalent Fe remaining in the liquid. The total Fe concentration in the leachate in the leached slurry and the divalent Fe concentration and amount of the liquid after neutralization were used to inversely calculate the concentration of trivalent Fe in the leachate, which was used to calculate an oxidation 20 ratio of iron ( (concentration of trivalent iron/concentration of total iron) x 100). The results are shown in Figures 1 and 2. Figure 1 shows a relation between the carbon grade in ore and the ORP of the acid leachate. Figure 2 shows a relation between the carbon 25 grade in ore and the ratio (Fe(III)/Fe, total) showing the oxidation ratio of iron. It can be understood from Figures 1 and 2 that when the carbon grade in ore is 0.10% to 0.30%, the oxidation/reduction 19 potential of the leachate is 480 to 580 mV and the oxidation ratio of iron in the leachate is 50% or higher, and that when the carbon grade in ore is 0.15% or lower, the oxidation ratio of iron in the leachate is 80% or higher. 5 (Example 2, Comparative Example 1) Nickel oxide ore having a nickel content of 1.25% by mass and an iron content of 46% by mass that was adjusted so that the carbon grade was 0.1 to G.3% by mass was slurried to obtain 10 a slurry having a solid fraction of about 40% by mass, which was charged in an autoclave reactor of 1 m 3 in volume made of titanium. Sulfuric acid was added so that the concentration of free sulfuric acid was about 45 g/l in the terminal reaction solution. 15 High-pressure air of about 5 MPaG was blown into the autoclave at the rates of 700 to 800 Nm 3 (Example 2) and 875 Nm 3 (Comparative Example 1) each per ton of carbon in ore and at the same time high-pressure steam of about 5 MPaG was blown. The slurry was kept at 245"C for an hour while being stirred. The ORP (Ag/AgCl 20 electrode basis) of the obtained leached slurry and the amount of high-pressure steam used per ton of dry ore were measured. The results are shown in Figure 3. Figure 3 shows a relation between the amount of high-pressure steam to be blown per ton of carbon in ore and the ORP of the leachate. 25 It can be understood from Figure 3 that when the amount of high-pressure air to be blown is 700 to 800 Nm 3 (Example 2) per ton of carbon in ore, the ORP is controlled to about 520 mV. When the amount of high-pressure air to be blown was 20 increased to 875 Nm 3 (Comparative Example 1), the ORP of the leachate was controlled to 600 mV or lower, but the amount of high-pressure steam, which is not shown in the figure, increased greatly to higher than 250 kg per ton of dry ore. 5 (Example 3) The amount of high-pressure air to be blown per ton of carbon in ore (amount of high-pressure air), the amount of high-pressure steam to be used per ton of dry ore (amount of 10 high-pressure steam) and each ORP of the leachate were measured in the leaching of the similar slurry as in Example 2 under similar conditions as in Example 2. The results are shown in Table 1 and Figure 4. Figure 4 shows a relation between the amount of high-pressure air to be blown (amount of high-pressure 15 air) and the amount of high-pressure steam to be used (amount of high-pressure steam). Table 1 Amount of high-pressure 721 740 757 779 air (Nm3/t--C)727475 79 Amount of high-pressure 170 164 180 189 steam (Kg/t-Solid)17161819 ORP (mV) 525 545 504 498 20 It can be understood from Table 1 that even when the amount of high-pressure air is increased, the ORP of the leachate is not increased proportionally, but limited to a certain level. It can be understood that from Figure 4 that when the amount of high-pressure air is in the range of 700 to 800 Nm 3 per ton 25 of carbon in ore, the amount of high-pressure steam can be controlled to the range of 150 to 200 kg per ton of dry ore.
21 It can be also understood that the amount of high-pressure steam is increased proportionally to the increased amount of high-pressure air. The high-pressure air of increased amount does not contribute toward enhancing the ORP of the leachate, 5 but is discharged from a vent (control valve) of the autoclave. The steam of an amount more than necessary is discharged with the air resulting in energy loss. It can be understood from the above that a high oxidation 10 ratio of iron to trivalent iron is attained and at the same time the amounts of high-pressure air and high-pressure steam to be used can be suppressed leading to energy cost reduction in Examples 1, 2 and 3 where leaching is conducted by adjusting the carbon grade in ore so as to be 0.1 to 0.5% by mass and 15 adjusting the amount of high-pressure air to be blown so as to be 700 to 800 Nm 3 per ton of carbon in ore. As apparent from the above, the wet process for smelting nickel oxide ore of the present invention can attain a high 20 leaching ratio of nickel and cobalt and a high oxidation ratio of iron to trivalent iron and at the same time can reduce energy cost by suppressing the amounts of high-pressure air and high-pressure steam to be used for maintaining an oxidative atmosphere or temperature, in the wet process for smelting 25 nickel oxide ore using the high pressure acid leach method, and therefore, is suitable as a smelting method for nickel oxide ore to be used in the high pressure acid leach method.
Claims (8)
1. A wet process for smelting nickel oxide ore using a high pressure acid leach method comprising a first step of preparing 5 an ore slurry by slurrying nickel oxide ore and a second step of producing a leachate containing nickel by adding sulfuric acid to the ore slurry of the first step and leaching the ore slurry while blowing high-pressure air and high-pressure steam therein, wherein the nickel oxide ore comprises more than one 10 nickel oxide ores having different carbon grades and the process further comprises adjusting the carbon grade of the solid content of the ore slurry in the first step to be 0.1 to 0.5% by mass by adjusting the blending ratio of the nickel oxide ores having a dif ferent carbon grades that constitutes the ore slurry 15 in the first step and controlling the oxidation-reduction potential (Ag/AgCl basis) of the above leachate to 400 to 600 mV by adjusting the amount of the above high-pressure air to be blown so as to be 700 to 800 Nm 3 per ton of carbon in the solid content of the ore slurry in the second step. 20
2. The wet process for smelting nickel oxide ore according to claim 1 wherein the amount of the high-pressure steam the second step is controlled to be 150 to 200 kg per ton of dry ore. 25
3. The wet process for smelting nickel oxide ore according to claim 1 or 2 wherein the carbon grade in a solid content of the ore slurry is adjusted to be 0.1 to 0.15% by mass. 0116_4 .DOC 23
4. The wet process for smelting nickel oxide ore according to any one of the preceding claims wherein the leachate contains iron and the oxidation ratio of iron in the leachate is 80% or higher in the above second step. 5
5. The process of any one of claims 1 to 4 wherein the oxidation-reduction potential of the slurry is from 550 to 600mV on an Ag/AgCl basis. 10
6. The process of any one of claims 1 to 5 wherein the nickel oxide ore further includes cobalt or cobalt containing compounds, and the nickel containing leachate further includes cobalt. 15
7. The process of any one of claims 1 to 6, wherein slurry has a solids content of about 25 to about 45% by mass.
8. A process according to claim 1 substantially as hereinbefore described with reference to any one of the 20 examples.
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| JP2008-042419 | 2008-02-25 | ||
| JP2008042419A JP5125597B2 (en) | 2008-02-25 | 2008-02-25 | Method for hydrometallizing nickel oxide ore |
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| AU2011232311A1 (en) * | 2010-03-24 | 2012-10-11 | Australian Nuclear Science And Technology Organisation | Process for leaching refractory uraniferous minerals |
| JP5704410B2 (en) * | 2012-03-21 | 2015-04-22 | 住友金属鉱山株式会社 | Method for producing hematite for iron making |
| JP5790726B2 (en) | 2013-03-19 | 2015-10-07 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
| CN104404248B (en) * | 2014-10-29 | 2017-09-05 | 昆明理工大学 | The leaching method and its leaching agent of lead in a kind of recovery lead oxide ore |
| JP6350634B2 (en) * | 2016-10-26 | 2018-07-04 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
| JP7354845B2 (en) * | 2020-01-15 | 2023-10-03 | 住友金属鉱山株式会社 | Method for producing nickel sulfate aqueous solution |
| JP7480528B2 (en) * | 2020-03-03 | 2024-05-10 | 住友金属鉱山株式会社 | Hydrometallurgical process for nickel oxide ore |
| JP7585894B2 (en) * | 2021-03-11 | 2024-11-19 | 住友金属鉱山株式会社 | Hydrometallurgical process for nickel oxide ore |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3761566A (en) * | 1971-09-13 | 1973-09-25 | American Metal Climax Inc | Leaching of nickel lateritic ores with waste iron sulfate solutions |
| CN1206747A (en) * | 1997-07-28 | 1999-02-03 | 中国科学院化工冶金研究所 | Process of chlorine complexing oxidation method for slective leaching nickel cobalt copper sulfurized ore |
| US20050118082A1 (en) * | 2001-12-21 | 2005-06-02 | Mohamed Buarzaiga | Chromium removal from leach liquors produced during high pressure acid leaching of lateritic ores |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS616216A (en) * | 1984-06-21 | 1986-01-11 | Mitsui Mining & Smelting Co Ltd | Wet treatment of laterite ore |
| JPS6328835A (en) * | 1986-07-22 | 1988-02-06 | Agency Of Ind Science & Technol | Method for extracting cobalt from cobalt-containing ore |
| JPS63137128A (en) * | 1986-11-27 | 1988-06-09 | Agency Of Ind Science & Technol | Acid treatment of manganese nodule |
| JP3387302B2 (en) * | 1996-01-26 | 2003-03-17 | 大平洋金属株式会社 | Method for producing high purity rare earth metal oxide |
| JP4285296B2 (en) * | 2004-03-29 | 2009-06-24 | 住友金属鉱山株式会社 | Nickel smelting method |
| JP4525428B2 (en) * | 2004-05-13 | 2010-08-18 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
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- 2008-02-25 JP JP2008042419A patent/JP5125597B2/en active Active
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3761566A (en) * | 1971-09-13 | 1973-09-25 | American Metal Climax Inc | Leaching of nickel lateritic ores with waste iron sulfate solutions |
| CN1206747A (en) * | 1997-07-28 | 1999-02-03 | 中国科学院化工冶金研究所 | Process of chlorine complexing oxidation method for slective leaching nickel cobalt copper sulfurized ore |
| US20050118082A1 (en) * | 2001-12-21 | 2005-06-02 | Mohamed Buarzaiga | Chromium removal from leach liquors produced during high pressure acid leaching of lateritic ores |
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| AU2009200714A1 (en) | 2009-09-10 |
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| CA2650372A1 (en) | 2009-08-25 |
| CA2650372C (en) | 2016-05-03 |
| JP5125597B2 (en) | 2013-01-23 |
| AU2009200714A8 (en) | 2013-03-07 |
| AU2009200714B8 (en) | 2013-03-07 |
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