AU2003273610B2 - Reducing cyanide consumption in gold recovery from finely ground sulphide ores and concentrates - Google Patents
Reducing cyanide consumption in gold recovery from finely ground sulphide ores and concentrates Download PDFInfo
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- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 title claims description 84
- 239000010931 gold Substances 0.000 title claims description 61
- 229910052737 gold Inorganic materials 0.000 title claims description 59
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims description 58
- 239000012141 concentrate Substances 0.000 title claims description 51
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims description 44
- 238000011084 recovery Methods 0.000 title description 20
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 49
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 49
- 239000004571 lime Substances 0.000 claims description 49
- 230000003647 oxidation Effects 0.000 claims description 44
- 238000007254 oxidation reaction Methods 0.000 claims description 44
- 238000002386 leaching Methods 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 32
- 230000008569 process Effects 0.000 claims description 28
- 235000019738 Limestone Nutrition 0.000 claims description 18
- 239000006028 limestone Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 12
- 229910052683 pyrite Inorganic materials 0.000 claims description 12
- 239000011028 pyrite Substances 0.000 claims description 12
- 239000011819 refractory material Substances 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 5
- MJLGNAGLHAQFHV-UHFFFAOYSA-N arsenopyrite Chemical compound [S-2].[Fe+3].[As-] MJLGNAGLHAQFHV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052964 arsenopyrite Inorganic materials 0.000 claims description 3
- 229910052959 stibnite Inorganic materials 0.000 claims description 3
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims 4
- 229910052751 metal Inorganic materials 0.000 claims 4
- 239000003513 alkali Substances 0.000 description 26
- 239000000203 mixture Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 19
- 229910052500 inorganic mineral Inorganic materials 0.000 description 17
- 239000011707 mineral Substances 0.000 description 17
- 235000010755 mineral Nutrition 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- 230000001590 oxidative effect Effects 0.000 description 13
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- MNWBNISUBARLIT-UHFFFAOYSA-N sodium cyanide Chemical compound [Na+].N#[C-] MNWBNISUBARLIT-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 239000002562 thickening agent Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 150000004763 sulfides Chemical class 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910001919 chlorite Inorganic materials 0.000 description 3
- 229910052619 chlorite group Inorganic materials 0.000 description 3
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 3
- 229910052598 goethite Inorganic materials 0.000 description 3
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 3
- 239000010909 process residue Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910000512 ankerite Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 2
- 229910001254 electrum Inorganic materials 0.000 description 2
- XXOYNJXVWVNOOJ-UHFFFAOYSA-N fenuron Chemical compound CN(C)C(=O)NC1=CC=CC=C1 XXOYNJXVWVNOOJ-UHFFFAOYSA-N 0.000 description 2
- 150000002344 gold compounds Chemical class 0.000 description 2
- -1 gold tellurides Chemical class 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- 229910052627 muscovite Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 2
- 229910021653 sulphate ion Inorganic materials 0.000 description 2
- 150000004772 tellurides Chemical class 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 150000003567 thiocyanates Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 1
- 229910021532 Calcite Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- MOAOBEKGMNGXJG-UHFFFAOYSA-N [Te].[Te].[Te].[Au].[Au] Chemical compound [Te].[Te].[Te].[Au].[Au] MOAOBEKGMNGXJG-UHFFFAOYSA-N 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- NPEWZDADCAZMNF-UHFFFAOYSA-N gold iron Chemical compound [Fe].[Au] NPEWZDADCAZMNF-UHFFFAOYSA-N 0.000 description 1
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229910052935 jarosite Inorganic materials 0.000 description 1
- 239000012633 leachable Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000003260 vortexing Methods 0.000 description 1
Classifications
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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
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- Manufacture And Refinement Of Metals (AREA)
Description
WO 2004/042094 PCT/AU20031001400 1 REDUCING CYANIDE CONSUMPTION IN GOLD RECOVERY FROM FINELY GROUND SULPHIDE ORES AND CONCENTRATES FIELD OF THE INVENTION This invention is directed to a process by which gold, silver and other precious minerals can be recovered from a refractory material such as an ore/concentrate/residue in such a manner that the amount of cyanide consumption is reduced.
BACKGROUND ART Extraction of precious minerals such as gold from an ore or concentrate using cyanide leaching is well-known. The cyanide leaching must be conducted under alkaline conditions.
Gold in sulphide mineralisation can occur in several forms: S free gold and electrum and fine inclusions of these particles in sulphide minerals S gold compounds (tellurides and selenides) gold locked in the lattice of pyrite, arsenopyrite, stibnite etc (invisible gold) In free milling ores, particulate free gold and electrum can be recovered by conventional gravity and cyanidation methods. When these particles are present as fine inclusions in sulphide minerals, fine grinding is used to liberate the particles prior to cyanide leaching.
Fine gold particles locked in other minerals can be liberated by fine grinding from p80 w 70p to p80 12p. This liberation of fine gold particles from sulphides and quartz gange particles by fine grinding and cyanide leaching is well known.
It has been found that fine grinding to circa 10 microns and leaching with sodium cyanide can recover the majority of the free gold and the gold present as gold compounds. High pH (-11 12) high cyanide concentration (2 5000 ppm NaCN vs 200 300 ppm used conventionally) and long leach times are required, (48 72 hours vs 18 24 hours required conventionally). Under these conditions, recoveries of 80 90% for gold can be achieved with consumptions of lime of 5 -15 kg/t and 12 20 kg/t of sodium cyanide. Normal commercial operation results in consumption of SUBSTITUTE SHEET (RULE 26) WO 2004/042094 PCTAU20031001400 2 5 kg/t of lime and 1.5 2.5 kg/t of sodium cyanide.
During the fine grinding process, the sulphide minerals are also finely ground and a large surface area of fresh unoxidised sulphide mineralisation is exposed. It is this sulphide surface which reacts with cyanide during cyanide leaching for gold extraction to form thiocyanates and other thio species. This results in the high cyanide consumption observed during cyanide leaching of finely ground sulphidic gold ores.
It has been reported that fine grinding of pyrite concentrates by stirred ball mills, the LURGI centrifugal ball mill and the Sweco vibrating mill produced significant recoveries in gold extraction by cyanide leaching. The grind sizes achieved were p50 of 2 8p. During leaching, the cyanide consumption was double that observed at a coarser grind.
Some types of ores are not able to be leached using cyanide, as the precious minerals are locked in the ore in such a manner that extraction using cyanide does not work. These types of ores can be called refractory ores. A typical refractory ore comprises a sulphide ore and a carbonaceous ore.
In order to release the precious minerals from refractory ores (thereby allowing cyanide leaching to be carried out) it is known to initially pretreat the ore by roasting, by bacterial leaching, and to use chemical leaching at elevated temperatures and pressures all of which increases the cost of recovering the precious minerals from the ore/concentrates.
Most pre-treating leaching processes use oxygen and acidic conditions. Once the ore/concentrate has been treated, the acid must be neutralised prior to cyanide leaching which requires less acid or more alkaline conditions. This increases the cost of extraction of the precious minerals.
Alkaline leaching is known but alkaline leaching is not very efficient with refractory materials.
International patent application PCT/AU99/00795 describes an alkaline leaching process to extract precious metals such as gold. The alkaline leaching process requires fine grinding of the ore and lime and/or limestone is used as the alkaline reagent. Oxygen is used as the oxidising agent and the process is continued until approximately 90% of sulphide WO 2004/042094 PCTAU20031001400 3 oxidation had taken place. The resultant product is subjected to cyanide leaching to remove gold and other precious minerals.
A disadvantage with the above alkaline leaching process is that the amount of cyanide consumed during the extraction process is rather high which adds to the cost of the overall process. Also, the reaction time is quite long.
During the fine grinding process, the sulphide minerals are finely ground and a large surface area of fresh unoxidised sulphide mineralisation is exposed. It is this sulphide surface which reacts with cyanide during cyanide leaching for gold extraction to form thiocyanates and other thio species. This results in the high cyanide consumption observed during cyanide leaching of finely ground sulphidic gold ores. In our previous process described in the above International patent application, the sulphide was almost totally oxidised but even so, there was still a large consumption of cyanide.
OBJECT OF THE INVENTION The present invention is directed to the discovery that the amount of cyanide consumed during an alkaline extraction process can be remarkably reduced (for instance by up to 66%) by only partially oxidising the ore/concentrate in a pretreatment step prior to extraction with cyanide.
In one form, the invention resides in a process for extracting gold and other precious metals from a refractory material (such as an ore/concentrate such as a sulphide ore), the method comprising fine grinding the ore, subjecting the ground ore to an leaching step in the presence of an alkaline material (which may be lime and limestone) and oxygen as the oxidising agent, adjusting the leaching step such that the amount of oxidation is between 9%-20% and subjecting the partially oxidated ore/concentrates to a cyanide extraction step.
The refractory ore/concentrate may comprise a sulphide ore a carbonaceous ore, pyrites, arsenopyrite, stibnite and may contain other compounds such as selenium and tellurium.
The ore/concentrate is typically finely ground to a p80 of microns. Various devices are commercially available to grind a solid to this particle size.
WO 2004/042094 PCTAU20031001400 4 The alkaline leaching step is preferably conducted at a temperature of between 60-95' as this can provide a further reduction in the consumption of cyanide during the extraction process. For instance, the amount of cyanide consumed at 70-85' is approximately half of that consumed at between room temperature-50 by solids partially oxidised.
The leaching step can be conducted to provide a sulphide oxidation of between 8-15% by solids partially oxidized. The oxidation is typically carried out using oxygen introduced into a leach reactor. When the desired level of sulphide oxidation had occurred, oxygen is no longer added to the reactor.
The alkaline conditions (more correctly conditions which are less acidic than the very well-known acid leaching in sulphuric acid) can be maintained using limestone and lime. The amount of lime can be between The pH of the leach is typically maintained between 5-7.
The leached solution is then typically subjected to a cyanide extraction step to extract the gold and other precious minerals from the ore/concentrate.
Initial oxidation of the finely ground ore/concentrates to about 12% as opposed to almost fully oxidising the ore/concentrate allows a gold extraction of approximately 90% and a sodium cyanide consumption of approximately 2 kg per tonne ore.
As a comparison, leaching a finely ground ore/concentrate without partial oxidation consumed approximately 16-20 kilograms of sodium cyanide per tonne of ore.
The best conditions seem to be to fine grind the initial ore/concentrate, only partially oxidise the finely ground material to @12%, keep the temperature to between 60-85 degrees C, and use a lime/limestone mixture to keep the pH level alkaline.
Fine grinding already results in an increase of cyanide consumption relative to unground product. Partial oxidation provided a further reduction in cyanide consumption relative to unoxidised material. Maintaining the temperature at between 60-85 provided a further reduction in the cyanide consumption.
WO 2004/042094 PCT/AU2003/001400 Using the process according to the invention, leaching of the ore/concentrate was completed within 8-24 hours as opposed to 54-72 hours for the un oxidised material.
BEST MODE In seeking to treat gold ores and concentrates which contain a mixture of cyanide leachable gold and refractory gold, tests were carried out on a material with these properties in which the gold concentrates containing circa 40 g/t gold in the form of free gold, gold telluride, fine gold locked in sulphide and gangue minerals and invisible gold. The method of fine grinding followed by the limestone/lime/oxygen method of sulphide oxidisation was chosen for these tests. Only small amounts of these reagents were added with the aim of partially oxidising sulphides to provide incremental recovery of invisible gold. The concentrate was finely ground to p80 sizings between 9 and 16 microns and leached with oxygen and an 85%:15% mixture of limestone and lime at 80 0 C. The pre-treated oxidised residues from these oxidative leach tests were then leached at pH 10.5 with 500 ppm free cyanide. The gold recovery from the oxidised residue ranged from 86.4% to 94.1%.
A surprising and unexpected result was that the cyanide consumption decreased with increasing oxidation from 6.2 kg/t to 2.4 kg/t for the final residue. The cyanide consumption appeared to undergo a step change for samples ground finer than p80 11.4 and averaged 2.5 kg/t.
Further tests were carried out to clarify this result. Unoxidised pyrite concentrates were leached under the conditions shown in Table 1 below.
First, unground concentrate with p 8 0 70p was leached, then concentrate finely ground to a p80 of 9.1 and 10.9p respectively was leached with 500 ppm free cyanide and finally 2000 ppm free cyanide and 20 kg/t lime. These show a 2 4 times increase in sodium cyanide consumption for leaching finely ground concentrate compared with leaching unground concentrate.
Table 1: Results on Unoxidised Concentrates Cyanide Leach Tests WO 2004/042094 PCT/AU2003/001400 Concentrate Test Ultrafine CYANIDATION Sample Description Grind Free Au Ag NaCN Lime Cyanide Rec- Rec Cons- Conslevel kg/tonne kg/tonne ppm 1 As As 500 57.5 53.3 2.55 2.18 received received -500 ppm free cyanide 2 As As 500 55.6 41 3.78 3.68 received received -500 ppm free cyanide 1 UFG 9.1 500 71.6 50 7.09 13.69 500 ppm free cyanide 2 UFG 10.9 500 71.71 48 9.54 11.2 500 ppm free cyanide 1 UFG 9.1 2000 86.0 71 10.4 2000 ppm free cyanide, kg/t lime UFG 2000 ppm free 10.9 2000 87.6 79 11.5 cyanide, kg/t lime WO 2004/042094 PCT/AU2003/001400 7 Two pyrite concentrates containing 33 and 34 g/t gold, with the gold in the form of free gold, gold tellurides, invisible gold in pyrite and fine gold particles locked in sulphide and gangue minerals was ground in a horizontal bead mill to a p80 of circa 10u. The concentrate was oxidatively leached with oxygen and 130 kg/t of limestone/lime mixture in the ratio 110%/20% at 80 0 C for 24 hours. The aim of the tests was to oxidise less than 10% of the sulphide sulphur. The partly oxidised concentrate was cyanide leached under the conditions shown in Table 2 below.
The results show that when the ground concentrate was oxidised by only 9 11% of its sulphide sulphur content, and cyanide leached for gold recovery that the cyanide consumption was reduced by more than two thirds compared to the finely ground, unoxidised material.
Table 2: Results of Cyanide Leach Tests on Oxidised Residues Concentrate Ultrafine Grind Sulphur CYANIDATION Sample p80 Oxidation Free Au REC Ag REC NaCN Lime Cyanide CONS CONSlevel- kg/tonne kg/tonne ppm 1 9.1 0 500 71.6 50 7.09 13.7 1 9.1 0 2000 86.0 71 10.4 1 16.14 12.7 500 86.40 54.55 6.2 4.4 1 11.1 9.8 500 85.4 58.4 2.1 1 11.1 9.8 5000 86.4 58 3.7 1 11.1 13.4 500 86.8 68 2.63 2 10.9 0 500 71.7 48 9.54 11.2 2 10.9 0 2000 87.6 79 11.5 2 10.9 8.7 2000 87.8 91.7 4.09 2 10.9 16.9 2000 89.6 90 4.67 2 10.9 9.8 2000 84.9 75 9.11 2 10.9 10.4 2000 86.7 82 6.78 2 10.9 10.6 2000 88.5 80 4.55 2 10.9 12 2000 90.1 80 5.55 WO 2004/042094 PCT/AU2003/001400 8 2 10.9 11.4 2000 90.9 82 4.48 Effect of Temperature To further test the effectiveness of alkaline oxidation for reducing cyanide consumption, oxidation tests using 85% lime, oxygen and 20% w/w solids were carried out for 24 hours at 50, 60, and 80°C. The oxidised pulps were leached with sodium cyanide at pH 10.5 as described in Table 3 below and cyanide consumption measured. These results show that the greatest reduction in cyanide consumption occurred at and 80 0
C.
Table 3: Effect of Oxidative Leach Temperature on Cyanide Consumption Concentrate Ultrafine Leach Leach Gold Cyanide Lime Sample Grind p80 Time Sulphur Temperature Recovery Consumption Addition (hrs) Oxidation (kglt) (kg/t) 2 10.9 0 71.7 9.5 2 10.9 24 9.8 50 84.9 9.11 2 10.9 24 10.4 60 86.7 6.78 2 10.9 24 10.6 70 88.5 4.55 2 10.9 24 11.4 70 90.9 4.48 2 10.9 24 8.7 85 87.8 4.09 Continuous Leach Testing Trials were carried out to test the cyanide consumption of materials oxidised in a flow system.
The principle variables trialled were the level of sulphide oxidation, vessel temperature, which was varied in the range 60 70 degrees, and the blend of limestone and lime components in the alkali added to the leach.
A single concentrate sample was used in all of the continuous testing, and an analysis of this sample is listed below in Table 4.
WO 2004/042094 PCT/AU2003/001400 9 Table 4: Head Analysis Concentrate Sample Element Sample 2 Fe w/w 32.8 Cu ppm 2450 Ag ppm 16 Te ppm 213 Au ppm 38. 1 (39.4 repeat) S w/w 39.6 The concentrate sample consisted predominantly of pyrite, with silica, sericite, muscovite and chlorite making up the major gangue components. The sample contained 213 ppm tellurium; however no tellurides were visible under optical microscope. The sample contained a minor amount of calcite, and had an 80% passing size of 91.5 microns.
The continuous leach run was carried out as follows: 100 kg of concentrate was finely ground as feed to a continuous reactor and split into representative 20 kg sub samples. The slurry was ground to 80% passing 12 microns, and sent for head analysis.
A three stage continuous oxidative leach reactor was set up and commissioned. The reactor was designed to operate for 24 hours per day with continuous feed of both concentrate and alkali slurry at measured rates. Discharge from the leach was to be gravitated to a thickener for thickening, with the thickener overflow stream used as makeup water to the feed and alkali circuits.
The continuous leach reactor was operated under the following conditions: Run No. 1 Operating Parameter Target level Slurry Density in Oxidative leach Operating Temperature 700 C Residence Time 12 hrs Alkali Blend 20% lime/80% limestone WO 2004/042094 PCTiAU2003/001400 Target Sulphide Oxidation Level Alkali addition kg/tonne Run No. 2 Operating Parameter Slurry Density in Oxidative leach Target Sulphide Oxidation Level Operating Temperature Residence Time Alkali Blend Alkali addition kg/tonne Start at 8% wlw and progressively increase to 14% w/w by control of exit pH and alkali addition 90 110 kg/tonne, adjusted to match targeted level of sulphide oxidation Target level 12- 14% (aim 12.5%) 60 0
C
12 hrs 20% limestone 100 Run No. 3 Operating Parameter Slurry Density in Oxidative leach Target Sulphide Oxidation Level Operating Temperature Residence Time Alkali Blend Alkali addition kg/tonne Target level 12 -14% (aim 12.5 70 C 12 hrs 8% lime/92% limestone 100 Ultrafine Grinding WO 2004/042094 PCTiAU20031001400 11 Fine grinding of the pyrite concentrate was carried out in a four litre Netzsch horizontally stirred bead mill. The mill was fitted with a 4 litre chamber and disc style agitator. The grinding media was screened 1 3 mm river sand. The mill was fitted with an AC inverter for accurate determination of the mill power draw and operating rpm. The feed slurry was sampled initially for particle size determination by a Lasersizer. The entire feed sample was ground to a size of p80 12 microns Continuous Stirred Reactor The continuous leach reactor consisted of three stainless steel vessels connected in series using overflow ports. Each reactor had a live voluie of 5 litres and an aspect ratio of 1. Each reactor was baffled to prevent solution vortexing, and agitated by a 100 mm diameter radial impeller.
Oxygen was introduced into each reactor by air spear, which terminated directly below the impeller. Oxygen flow was controlled off a pressure cylinder using rotameters.
Each vessel was jacketed, with hot water continuously circulated through the jacket to maintain the temperatures within the leach at the desired level. The outside of the jacket was insulated to minimise heat loss.
The overflow port was located at the top of each reactor, with the inlet port located below the impeller line. This facilitated slurry transport between the vessels.
Discharge from the leach overflowed from the final leach reactor into a 300 mm diameter thickener. Underflow was withdrawn from the thickener regularly and filtered. These filtered samples were used in subsequent cyanidation leaching. Thickener overflow was used to dilute ground slurry and alkali prior to addition to the leach, and also to makeup for evaporative loss across the leach train.
Cyanide Leaching The partially oxidised leach residues collected during the leaching program were tested for gold and silver recovery by cyanidation in a bottle roll apparatus. Approximately 1000 grams of residue at 35 w/w solids was be added to a 5 HDPE bottle, and the bottle rotated at 30 rpm on a set of WO 2004/042094 PCT/AU2003/001400 12 rollers. Cyanide and hydrated lime were added to the bottle prior to starting the test.
The Effect of Sulphide Oxidation on Gold Recovery The main operating parameter that required optimising in the continuous leach run was the level of sulphide oxidation required. The batch testwork had narrowed the target range to 8 14 w/w, however the aim of the continuous test was to reduce the target range to within 1 This was examined in the first oxidative leach run, with the level of sulphide oxidation varied in the first 250 hours of operation.
Data outlining the effect of the level of sulphide oxidation on the amount of gold recovered from the oxidised residue is shown in Table 5. The cyanide and lime consumption in the cyanide leach is also listed. The level of sulphide oxidation listed in Table 5.4 refers to feed concentrate.
Table 5: Effect of Sulphide Oxidation on Gold Recovery from Concentrate Sample Sulphide mass Gold NaCN Lime Consumption Oxidation increase Recovery Consumption kg/tonne of feed across leach kg/tonne of feed concentrate concentrate As received 71.5 8.3 12.4 12.5 14 92 2.4 1.8 11.5 12.6 91 2.6 2.2 11.4 88 2.4 9.8 10.9 87 2.8 1.6 9.2 9.9 86 2.4 8.4 9.4 85 2.5 1.4 6.8 7.5 84 3.4 2 The sodium cyanide consumption observed for the residue oxidised to a sulphide oxidation of 12.5% was 2.4 kg/tonne of oxidised residue (2.6 kg/tonne of feed), at a lime consumption of 1.65 kg/tonne of WO 2004/042094 PCTiAU2003/001400 13 oxidised residue (1.8 kg/tonne of feed).
The level of sulphide oxidation in the range given in table 5 i.e.
between 8-14%) did not appear to have much impact on the cyanide consumption, with a cyanide consumption in the range 2.2 2.5 kg/tonne of residue noted at sulphide oxidation levels in the range 8 14%. All of the cyanide leach tests were carried out at a free cyanide level of 500 ppm, and at pH 10.5. Lime was added to the tests to hold the pH at this level, rather than as a single addition and the pH was stable throughout the cyanide leach tests, with low lime consumption observed. The cyanide level was stable throughout the cyanide leach tests, and was easy to control at the target level of 500 ppm.
The Effect of Temperature on Gold Recovery Leach Run No 1 was carried out at a temperature of 70 degrees, whereas for leach Run No 2 the temperature was lowered to 60 degrees.
The average gold recovery from oxidised residues produced in Leach run No 1, with temperature maintained at 700C, was 87%, with the gold recovery ranging from 85 90%. The average sodium cyanide consumption was 2.8 kg/tonne, at an average lime consumption of 1 1.5 kg/tonne. The average sulphide oxidation achieved at 70 degrees was 11.5% w/w, with approximately 90 95% of the limestone/lime blend added to the leach consumed in the oxidation.
The data for the second leach run, carried out at 60 degrees, was very similar to Leach Run No 1. The average gold recovery from the oxidised residue was 88%, at an average sodium cyanide consumption of kg/tonne, and a lime consumption of 1.4 kg/tonne. The level of sulphide oxidation achieved at 60 degrees was 10.8% w/w on average. The amount of limestone/lime blend consumed in the oxidation was again over The potential drawback of lower temperature operation is formation of other iron precipitates, rather than goethite. The colour of the iron precipitate formed at 600C was slightly darker than the precipitate formed at 70'C, however there was no detrimental effect on the cyanide consumption of the residue. The settling rates observed for the lower temperature precipitates WO 2004/042094 PCTiAU2003/001400 14 were slightly lower than noted for the leach residues produced at 70 0
C,
however this effect was only marginal.
The Effect of Alkali Blend The final variable tested in Leach run No 3 was the amount of lime in the blend, which was decreased from 20% down to Leach Run No 1 was carried out at a temperature of 70 degrees, with 20% lime present in the alkali blend. Leach Run No 3 was carried out at a temperature of degrees, with the amount of lime in the alkali blend reduced to 8%.
The average gold recovery from oxidised residues produced in Leach run No 1, with 20% lime present in the alkali blend, was 87%, with the gold recovery ranging from 85 90%. The average sodium cyanide consumption was 2.8 kg/tonne, at an average lime consumption of 1 kg/tonne. The average sulphide oxidation achieved at 70 degrees was 11.5% w/w, with approximately 90% of the limestone/lime blend added to the leach consumed in the oxidation. The sulphide oxidation ranged from 7.5 The data for the third leach run, carried out with only 8% lime present in the alkali blend, was similar to Leach Run No 1. The average gold recovery from the oxidised residue was 88%, at an average sodium cyanide consumption of 2.6 kg/tonne, and a lime consumption of 1.9 kg/tonne. The lime consumption in the cyanide leach stage was slightly elevated with 8% lime in the alkali blend, compared to residues produced with 20% lime in the alkali blend.
The average level of sulphide oxidation achieved in run No 3 was 11.8% w/w. The amount of limestone/lime blend consumed in the oxidation was again 95%. There was no significant difference between the results of the leach run carried out with 20% lime in the alkali blend relative to run No 3, carried out at 8% lime in the alkali blend.
Elemental and Mineralogical Analysis of the Oxidative Leach A summary of data collected during Leach Run 3, outlining the varying elemental and mineralogical analysis of the solids phase in each leach reactor is presented in Table 6. Leach Run No 3 was carried out at 0 C, with a lime level of 8% w/w in the alkali blend. The discharge pH from WO 2004/042094 PCT/AU2003/001400 the leach was above 5 throughout the run, and so there was little driving force for the formation of sulphated iron precipitates. The data was collected by chemical analysis and XRD analysis of samples taken from each tank when the leach was operating at steady state.
By the end of the oxidative leach, less than 1% of the mass of the leach residue was made up of limestone, indicating that more than 95% of the alkali added to the leach was consumed in the leach reaction. The amount of alkali consumed, and the amount of pyrite oxidised confirm the anticipated general pyrite leach reaction: FeS 2 2CaO 15/402 5/2H 2 0 FeO.OH CaSO 4 .2H 2 0 Table 6: Analysis of Oxidative Leach Tank Discharge for Run No 3 Composition Feed Tank 3 discharge Fe 32.8 27.5 %S 34.1 30.4 Si 6.3 5.4 Ca 0.15 2.4 FeS 2 63 48 FeS 2 Oxidation 0.0 13.2 FeO.OH 0 8 SiO2 6.2 5.6 Muscovite 15 16 Chlorite 5.4 3.45 Ankerite 6.6 1.4 CaS04.2H 2 0 0 9 CaCO 3 0.4 0.7 MASS 100 114 The mass increase across the oxidative leach was approximately 14%, with the bulk of the increased mass present as goethite and gypsum. Approximately 10% of the final leach residue was made up of WO 2004/042094 PCT/AU20031001400 16 gypsum.
Some of the gangue minerals present in the concentrate sample, in particular chlorite and ankerite, were consumed in the oxidative leach. The most likely by products from reaction of these gangue minerals would magnesium and aluminium oxides, which would not be resolved clearly in the XRD analysis, as they tend to be amorphous.
The only iron reaction product identified in the XRD was goethite, FeO.OH. No sulphated iron precipitates were identified by XRD. The leach residues were relatively simple, with few reaction products, which confirmed that the majority of the reacted pyrite leached according to the leach reaction specified above. This simple reaction system greatly simplifies the heat and material balance for the process.
The Effect of Leach Discharge pH on Reagent Consumption in the Cyanide Leach During the early stages of the continuous run, the leach discharge pH varied, as the amount of alkali added to the leach was varied.
The exit pH increased gradually across the first 200 hours of operation, varying from 2 5, before settling down in the range 5 6 once the alkali blend addition was optimised.
The impact of operating the final stage of the leach at lower pH is that the amount of sulphate incorporated into the iron precipitate increases, due to formation of jarosite and iron hydroxy-sulphate phases. Residual iron levels in the solution phase also increase at lower pH. Both of these effects impact on the cyanide consumption in the cyanidation stage.
The effect of leach discharge pH on cyanide and lime consumption in the cyanide leach is outlined in Table 7.
WO 2004/042094 PCT/AU2003/001400 17 Table 7: The Effect of Discharge pH on Reagent Consumption in the Cyanide Leach Discharge Residual Iron Gold Recovery NaCN Lime pH Tenor in consumption consumption solution ppm kg/tonne kg/tonne 81 86 8.9 4 12 88 6.4 2 4.6 <5 88 4.1 2 <1 90 2.4 1 6 <1 90 2.6 1 Discharge pH had a significant effect on reagent consumption levels in the cyanide leach. The recommended discharge pH for the leach would be in the range 5 6, to achieve a cyanide consumption of 3 kg/tonne or less.
To achieve this discharge pH and still achieve the desired level of sulphide oxidation, the alkali stream will need to be added to the leach at a slight excess over stoichiometric, and a 10% excess is recommended.
Gold Leach Kinetics in the Cyanide Leach Table 8, outlines the relative cyanide leach kinetics for a preferred process residue, oxidised to 12 wlw sulphide oxidation, relative to a sample of finely ground concentrate leached under similar conditions.
Table 8: Leach Kinetics in the Cyanide Leach Stage Time hrs Process Residue 12 oxidation Finely ground concentrate 25 kg/tonne lime addition Tails Gold NaCN Tails Gold NaCN grade g/t Extraction Consumption grade Extraction Consumption w/w kg/tonne g/t wlw kg/tonne 0.00 29.8 0.00 0.00 36.1 0.00 0.00 1.00 8.9 69.9 0.20 30.2 16.2 1.9 3.00 4.9 83.4 0.15 26.3 27.1 3.9 WO 2004/042094 PCT/AU2003/001400 7.00 91.0 0.61 14.3 60.3 6.1 24.00 2.7 90.7 1.13 10.6 70.4 12.2 30.00 2.6 91.0 1.88 48.00 2.7 90.9 1.61 8.2 77.2 16.5 54.00 2.7 90.9 1.69 72.00 2.7 90.9 2.20 5.8 83.9 18.4 The process oxidative pretreatment of the pyrite concentrate results in a significant increase in the cyanide leach kinetics. Leaching of the process residue is essentially complete within 8 24 hours of leaching, compared to 54 72 hours for the un-oxidised finely ground concentrate.
Figure 1 Comparative CIL Kinetics Process Oxidised Residue vs Finely Ground Concentrate II 1 ach Ie g/t GORe Residi 0 10 20 30 40 Time hrs 50 60 70 It should be appreciated that various changes and modifications can be made to the invention without departing from the spirit and scope of the invention.
Claims (11)
1. A process for extracting a metal from a refractory material containing the metal, the process comprising fine grinding the material, subjecting the ground material to a leaching step in the presence of an alkaline material and an oxidizing agent, adjusting the leaching step such that the amount of oxidation is between and subjecting the partially oxidized material to a cyanide extraction step to recover the metal.
2. The process of claim 1, wherein the refractory material comprises a sulphide, a carbonaceous, a pyrite, an arsenopyrite, or a stibnite ore or concentrate.
3. The process of claim 1, wherein the material is ground to a of 20 microns.
4. The process of claim 1, wherein the alkaline material is selected from lime and limestone.
The process of claim 4, wherein the pH of the leaching step is between 5-7.
6. The process of claim 1, wherein the amount of oxidation is between about 9% to about 12%.
7. The process of claim 1, wherein the oxidizing agent is oxygen.
8. The process of claim 1, wherein the leaching step is conducted at a temperature of between 60-95".
9. The process of claim 1, wherein the leaching step is carried out at 1 atmosphere or less.
The process of claim 1, wherein the metal is gold or silver.
11. A process for extracting gold or silver from a refractory material containing gold or silver, the process comprising fine grinding the material to a p80 of 20 microns, subjecting the ground material to a leaching step in the presence of an alkaline material which comprises lime andlor limestone and an oxidizing agent which comprises oxygen, maintaining the pH of the leaching step between 5-7, maintaining the temperature between 60-85 degrees C, adjusting the leaching step such that the amount of oxidation is between about 9%-about 12%, and subjecting the partially oxidized material to a cyanide extraction step to recover the gold or silver.
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