WO2005113845A1 - Recovery of nickel - Google Patents
Recovery of nickel Download PDFInfo
- Publication number
- WO2005113845A1 WO2005113845A1 PCT/AU2005/000724 AU2005000724W WO2005113845A1 WO 2005113845 A1 WO2005113845 A1 WO 2005113845A1 AU 2005000724 W AU2005000724 W AU 2005000724W WO 2005113845 A1 WO2005113845 A1 WO 2005113845A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- slurry
- process defined
- nickel
- feed material
- range
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
-
- 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present invention relates to a process for recovering nickel from an ore or concentrate via a hydrometallurgical route .
- the present invention relates particularly to recovering nickel from an ore or concentrate that contains nickel in the form of millerite (NiS) .
- the present invention relates more particularly, although by no means exclusively, to recovering nickel and cobalt from an ore or concentrate that contains nickel in the form of millerite (NiS) .
- the ore or concentrate may include other sulphide minerals in addition to millerite. There may be nickel in one or more than one of the other sulphide minerals .
- the ore or concentrate may include oxide minerals. There may be nickel in one or more than one of the oxide minerals .
- the ore or concentrate may include other sulphide minerals in addition to millerite and oxide minerals.
- nickel in one or more than one of the other sulphide minerals and the oxide minerals .
- the ore or concentrate may include other valuable metals, such as copper .
- the concentrate may be derived from a specific ore body that contains millerite and other sulphide minerals and/or oxide minerals.
- the concentrate may be derived from a blend of a number of different ore bodies and contain different minerals , including millerite .
- Materials of interest to the applicant contain millerite, heazlewoodite (Ni 3 S 2 ) , godlevskite (Ni 8 FeS 8 ) , pentlandite ((Ni,Fe) 9 S 8 ) and violarite (Ni 2 FeS 4 ) .
- the present invention was made during the course of a research program that was carried out by the applicant to investigate unexpectedly poor leachability of slurries of ores and concentrates containing blends of the minerals millerite, pentlandite, and in some instances other minerals such as violarite under acidic conditions .
- the poor leachability was obtained using a hydrometallurgical process that included pressure oxidation acid leaching under conditions that the applicant expected would achieve reasonable recoveries of nickel from the ores and concentrates .
- the research program found that the chloride concentration in process solutions used in the hydrometallurgical process had a significant impact on the leachability of nickel from millerite under acidic conditions. Specifically, the research program found that the leachability of nickel from millerite in pressure oxidation under acidic conditions decreased as the chloride concentration in process solutions increased above a specific threshold.
- the present invention is based on the realisation that, in situations in which a leach under acid conditions is required and the available process solutions for a hydrometallurgical process have chloride concentrations that are sufficient to impact adversely on leachability of nickel from millerite under acid conditions, the process should include a treatment step in which millerite is converted at least in part to an acid leachable form prior to a subsequent pressure oxidation acid leach step.
- a process for recovering nickel from a solid feed material containing nickel in the form of millerite which includes the steps of:
- the feed material includes an ore or a concentrate .
- the feed material may contain other nickel-containing minerals .
- the minerals may be sulphide and/or oxide minerals.
- the feed material may also contain other valuable metals such as cobalt and/or copper.
- the experimental program on which the present invention is based was carried out on ores and concentrates containing blends of millerite and pentlandite and in some instances other sulphide minerals .
- the process is not dependent on the nickel grade and is applicable to feed materials of any nickel grade subject to economic viability.
- the current view of the applicant is that the process is a viable option economically in situations in which at least 10% by weight of the nickel in the ore or concentrate for the process is in the form of millerite.
- the feed material may range between low grade nickel ores and concentrates, such as ores and concentrates having 2-3 wt% nickel and high grade concentrates, such as concentrates containing more than 20 wt% nickel .
- the feed material is in a particulate form having a grain size in the range of 10-40 microns.
- the preferred grain size is a function of the mineralogy of the feed material .
- the process solution contains at least 5g/l chlorides .
- the process solution contains at least 20g/l chlorides.
- step (a) includes treating the slurry of the feed material and the process solution under non- acidic conditions .
- non-acidic conditions is understood herein to mean that the pH of the slurry is above a pH of 5.5.
- step (a) includes treating the slurry of the feed material and the process solution at a pH in the range of 5.5 - 7.
- the slurry may be at a different pH, for example a higher pH, prior to step (a) .
- step (a) includes adjusting the pH of the slurry to be within the range of 5.5 - 7 and maintaining the pH within the range during step (a) by the presence of acid soluble alkaline gangue minerals in the feed material or by adding an alkaline agent to the slurry.
- step (a) includes treating the slurry of the feed material and the process solution at an elevated temperature .
- the elevated temperature is in a range of 80-160°C.
- the elevated temperature is at least 110°C. More preferably the elevated temperature is at least 130°C.
- the elevated temperature is no more than 155°C.
- Step (a) may be carried out under atmospheric or pressure conditions .
- step (a) includes treating the slurry of the feed material and the process solution under oxidation conditions.
- step (a) includes treating the slurry under pressure oxidation conditions .
- step (a) includes treating the slurry of the feed material and the process solution under pressure oxidation conditions with an 0 2 partial pressure that is sufficient to oxidise at least substantially all of the sulphide in the millerite to sulphate .
- step (a) One issue that should be considered in relation to step (a) is that the conditions of the step should be selected to minimise oxidation of minerals other than millerite that can cause undesirable acid generation.
- step (a) also includes treating the slurry of the feed material and the process solution under pressure oxidation conditions with an 0 2 partial pressure that is sufficient to oxidise other sulphide minerals in the feed material that can be oxidised without causing undesirable acid generation.
- other sulphide minerals may include heazlewoodite and godlevskite .
- step (a) includes treating the slurry of the feed material and the process solution under pressure oxidation conditions with an 0 2 partial pressure in a range of 250-1000 kPa(g) .
- the 0 2 partial pressure is in a range of 500-1000 kPa(g) in step (a).
- step (a) is in a range of 15-90 minutes.
- the slurry includes (a) soluble nickel in the process solution, (b) precipitated nickel hydroxide and/or basic nickel sulphate from the millerite, and (c) un-reacted, or partially reacted nickel-containing minerals of the type pentlandite, violarite etc.
- step (b) includes acid leaching the treated slurry from step (a) at a pH of 3 or less.
- step (b) includes pressure acid leaching the treated slurry from step (a) at a pH of 2 or less.
- step (b) includes pressure acid leaching the treated slurry from step (a) in sulphuric acid.
- step (b) includes pressure acid leaching the treated slurry from step (a) under oxidation conditions .
- step (b) includes pressure acid leaching the treated slurry from step (a) under pressure oxidation conditions with an 0 2 partial pressure in a range of 800-1200 kPa(g) .
- step (b) includes pressure acid leaching the treated slurry from step (a) at an elevated temperature.
- the elevated temperature is in a range of 100-160°C.
- the elevated temperature is at least 130°C.
- the elevated temperature is no more than 155°C.
- the elevated temperature is no more than 150°C.
- step (b) is in a range of 30-120 minutes.
- the process may include adding a separate slurry of a solid feed material and a process solution to the treated slurry from step (a) prior to or as part of step (b) .
- the process extends to situations where there are different feed materials, some of which require treatment in steps (a) and (b) (for example, feed materials containing millerite) and others of which require treatment in step (b) only (for example, feed materials that are predominantly pentlandite) .
- Steps (a) and (b) may be carried out in the same or different vessels .
- a slurry is formed from:
- the thickened slurry is supplied to an autoclave .
- the slurry is treated in the autoclave at a temperature of 150°C and 800-1000 kPa(g) 0 2 partial pressure for 30-60 minutes.
- the slurry pH is maintained in a range of 5.5-7.
- the millerite, (and heazlewoodite, and godlevskite, if present) fraction of the concentrate is oxidised with the nickel being taken into solution, a part of the nickel, typically 10-15 wt% remaining in solution, and the remainder of the nickel precipitating as an acid soluble form, typically hydroxides or basic nickel sulphates, as a consequence of hydrolysis ensuing from the presence of gangue with an alkaline potential in the concentrate.
- sulf ric acid is introduced into the autoclave and reduces the slurry pH to below 2.
- the slurry is acid leached at 150°C in the presence of oxygen for 30-120 minutes. Under these acidic conditions pentlandite, violarite and other sulphide minerals and the precipitated nickel from millerite oxidation are leached and nickel is taken into solution.
- the process solution and the remaining solids are separated, and the process solution is processed to recover nickel from solution .
- the process solution is transferred to another autoclave and is sparged with H 2 S gas, which causes precipitation of NiS from the process solution.
- the process solution containing precipitated NiS is filtered or transferred to a thickener to separate solids and liquid streams.
- the solids stream is washed, or filtered and thereafter washed to form a final NiS product.
- nickel can be recovered from the process solution as nickel hydroxide, nickel carbonate, basic nickel sulphate, or nickel metal.
- Table 1 presents nickel and cobalt recoveries for 4 sets of paired results of pressure oxidation tests completed under acidic conditions at a temperature of 150°C and an oxygen pressure of 1000 kPa(g) on millerite/pentlandite blends .
- Tests 1 and 2 slurries containing millerite/pentlandite blends containing 30-35 wt% of the nickel as millerite were leached in sulphuric acid.
- the slurry contained a relatively high chloride concentration of 28g/l, and in the case of Test 2 the slurry contained a relatively low chloride concentration of less than 0.3g/l.
- Test 1 reported a relatively low nickel recovery of 81.8% and Test 2 reported a relatively high nickel recovery of 94.5% . Similarly, Test 1 reported a relatively low cobalt recovery of 86.2% and Test 2 reported a relatively high cobalt recovery of 94.6%.
- Table 2 summarises the results of a series of tests on the two step process of the present invention carried out under different operating conditions.
- the tests were carried out on slurries containing two different blends of millerite/pentlandite, with one blend containing 30-35 wt.% of the nickel as millerite (S:Ni ratio of 0.86) and the other blend containing a 75-80 wt.% of the nickel as millerite (S:Ni ratio of 0.6).
- the tests were carried out under a series of operating conditions summarised in the Table, including:
- the research program also included pilot plant work at a later stage in the program.
- Tables 3 and 4 summarize two pilot plant runs.
- the pilot plant run summarized in Table 3 included leaching a sulphide concentrate containing a mixture of pentlandite, millerite and violarite together with other minor sulphide minerals that was ground to 80% passing 10-15 microns in a process water containing about 28 g/L chloride.
- the concentrate slurry (pH 8.2) was fed to a two stage pressure oxidation process.
- Step (a) the slurry was leached under "non-acidic" conditions at a temperature of 143°C (Feed 1) and a total pressure of 179 psig.
- the pH of the slurry reduced from 7.4 to 6.4 and the Eh increased from 300 mV to 380 mV.
- Step (a) pH changes indicated that some acid was generated in the process but was consumed by the alkaline gangue minerals .
- Step (b) the temperature was increased to 150°C, the total pressure was 210 psi, the slurry was acidified with sulphuric acid to pH below 2 and leached for further 120 minutes under acidic oxidative conditions. All of the nickel that oxidised and re-precipitated in Step (a) was extracted into solution. After 120 minutes most of the .remaining nickel sulphide minerals dissolved resulting in an overall nickel extraction of 95.5% and cobalt extraction of 90.1%.
- Step (b) 73 O Temperature in Step (b) is always at 150°C Pressure in Step (b) is always at 1000 kPa (g) No acid is added in Step (a), all acid is added in Step (b) pH in Step (a) is 6.5-7.0 pH in Step (b) is about 1.5 All leach tests done in saline process water
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Claims
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002568144A CA2568144A1 (en) | 2004-05-21 | 2005-05-20 | Recovery of nickel |
BRPI0511336-9A BRPI0511336A (en) | 2004-05-21 | 2005-05-20 | nickel recovery process |
EP05742219A EP1769095A4 (en) | 2004-05-21 | 2005-05-20 | Recovery of nickel |
AP2006003835A AP2058A (en) | 2004-05-21 | 2005-05-20 | Recovery of nickel |
AU2005245514A AU2005245514A1 (en) | 2004-05-21 | 2005-05-20 | Recovery of nickel |
JP2007516884A JP2007538147A (en) | 2004-05-21 | 2005-05-20 | Nickel recovery |
US11/602,556 US7534407B2 (en) | 2004-05-21 | 2006-11-21 | Recovery of nickel |
NO20065552A NO20065552L (en) | 2004-05-21 | 2006-12-01 | Nickel extraction |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2004902740A AU2004902740A0 (en) | 2004-05-21 | Low pressure leach process | |
AU2004902740 | 2004-05-21 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2005113845A1 true WO2005113845A1 (en) | 2005-12-01 |
Family
ID=35428423
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/AU2005/000724 WO2005113845A1 (en) | 2004-05-21 | 2005-05-20 | Recovery of nickel |
Country Status (10)
Country | Link |
---|---|
US (1) | US7534407B2 (en) |
EP (1) | EP1769095A4 (en) |
JP (1) | JP2007538147A (en) |
CN (1) | CN100420760C (en) |
AP (1) | AP2058A (en) |
AU (1) | AU2005245514A1 (en) |
BR (1) | BRPI0511336A (en) |
CA (1) | CA2568144A1 (en) |
NO (1) | NO20065552L (en) |
WO (1) | WO2005113845A1 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104024445B (en) * | 2011-12-28 | 2016-10-26 | Posco公司 | The method reclaiming dilval from nickel ores |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4039406A (en) * | 1973-08-10 | 1977-08-02 | Noranda Mines Limited | Recovering copper from concentrates with insoluble sulfate forming leach |
WO2002024966A1 (en) * | 2000-09-18 | 2002-03-28 | Inco Limited | Recovery of nickel and cobalt values from a sulfidic flotation concentrate by chloride assisted oxidative pressure leaching in sulfuric acid |
US6383460B2 (en) * | 1993-07-29 | 2002-05-07 | Cominco Engineering Services Ltd. | Process for the recovery of nickel and/or cobalt from a concentrate |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4093526A (en) * | 1977-09-08 | 1978-06-06 | Amax Inc. | Hydrometallurgical leaching and refining of nickel-copper concentrates, and electrowinning of copper |
NO833784L (en) * | 1983-10-18 | 1985-04-19 | Thomas Thomassen | AUTOCLAV CHLORINE CLUTCH OF COPPER SULFIDE CONCENTRATES |
EP0248518B1 (en) * | 1986-04-24 | 1991-11-13 | Falconbridge Limited | Separation of nickel from copper in autoclave |
US4888053A (en) * | 1988-07-07 | 1989-12-19 | Union Oil Co. Of California | Chloride leaching of iron-based, heavy metal-containing sludges |
FI88516C (en) * | 1990-02-16 | 1993-05-25 | Outokumpu Oy | Hydrometallurgical process for the treatment of zinc sulphide |
CA2068982C (en) * | 1992-05-19 | 2000-10-03 | Derek G.E. Kerfoot | Process for the separation of cobalt from nickel |
US5431788A (en) | 1993-06-28 | 1995-07-11 | Cominco Engineering Services Ltd. | Chloride assisted hydrometallurgical copper extraction |
US5869012A (en) | 1993-07-29 | 1999-02-09 | Cominco Engineering Services Ltd. | Chloride assisted hydrometallurgical extraction of metal |
US5902474A (en) | 1993-07-29 | 1999-05-11 | Cominco Engineering Services Ltd. | Chloride assisted hydrometallurgical extraction of metal |
US5650057A (en) | 1993-07-29 | 1997-07-22 | Cominco Engineering Services Ltd. | Chloride assisted hydrometallurgical extraction of metal |
US5874055A (en) | 1993-07-29 | 1999-02-23 | Cominco Engineering Services Ltd. | Chloride assisted hydrometallurgical extraction of metal |
CA2137124C (en) * | 1994-12-01 | 1999-03-16 | Tao Xue | Pressure leaching of nickel and cobalt sulphides with chlorine under controlled redox potential conditions |
FI105926B (en) * | 1998-03-16 | 2000-10-31 | Outokumpu Oy | Process for dissolving nickel out of nickel stone |
US7033480B2 (en) * | 2002-09-06 | 2006-04-25 | Placer Dome Technical Services Limited | Process for recovering platinum group metals from material containing base metals |
-
2005
- 2005-05-20 CN CNB2005800234893A patent/CN100420760C/en not_active Expired - Fee Related
- 2005-05-20 AU AU2005245514A patent/AU2005245514A1/en not_active Abandoned
- 2005-05-20 AP AP2006003835A patent/AP2058A/en active
- 2005-05-20 EP EP05742219A patent/EP1769095A4/en not_active Withdrawn
- 2005-05-20 JP JP2007516884A patent/JP2007538147A/en active Pending
- 2005-05-20 WO PCT/AU2005/000724 patent/WO2005113845A1/en active Application Filing
- 2005-05-20 CA CA002568144A patent/CA2568144A1/en not_active Abandoned
- 2005-05-20 BR BRPI0511336-9A patent/BRPI0511336A/en not_active IP Right Cessation
-
2006
- 2006-11-21 US US11/602,556 patent/US7534407B2/en not_active Expired - Fee Related
- 2006-12-01 NO NO20065552A patent/NO20065552L/en not_active Application Discontinuation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4039406A (en) * | 1973-08-10 | 1977-08-02 | Noranda Mines Limited | Recovering copper from concentrates with insoluble sulfate forming leach |
US6383460B2 (en) * | 1993-07-29 | 2002-05-07 | Cominco Engineering Services Ltd. | Process for the recovery of nickel and/or cobalt from a concentrate |
WO2002024966A1 (en) * | 2000-09-18 | 2002-03-28 | Inco Limited | Recovery of nickel and cobalt values from a sulfidic flotation concentrate by chloride assisted oxidative pressure leaching in sulfuric acid |
Non-Patent Citations (1)
Title |
---|
See also references of EP1769095A4 * |
Also Published As
Publication number | Publication date |
---|---|
CN100420760C (en) | 2008-09-24 |
CA2568144A1 (en) | 2005-12-01 |
US20070131059A1 (en) | 2007-06-14 |
US7534407B2 (en) | 2009-05-19 |
NO20065552L (en) | 2007-02-19 |
JP2007538147A (en) | 2007-12-27 |
EP1769095A1 (en) | 2007-04-04 |
AU2005245514A1 (en) | 2005-12-01 |
BRPI0511336A (en) | 2007-12-04 |
AP2058A (en) | 2009-10-21 |
CN101014724A (en) | 2007-08-08 |
AP2006003835A0 (en) | 2006-12-31 |
EP1769095A4 (en) | 2009-02-25 |
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