US us United States c2) Patent Application Publica oy os) 03) ey @y (86) (60 BUTLER EXTRACTION OF GOLD FROM CAT ASSOCIATED GOLD CONCENTRAT Inveator: Dean R. BUTLER, Hahindor?(AU) Assignee: PRECIOUS METALS RECOVERY PTY LID, “Melbourne, Victoria (AU) Appl. No, 137266,001 PCT Filed Ape. 23,2010) PCT No, PCTIAU2010/000461 $371 M0), (2).(4) Date Now. 24, 2011 Provisional application No, 61/172,273, filed on Apr 24, 2009, provisional application No. 61/213,672, 1200671 20 IAI (10) Pub. No.: US 2012/0067170 Al (43) Pub, Date Mar. 22, 2012 filed on Jul. 1, 2009, provisional application No. 61/213,673, filed on Jul. 1, 2009, provisional applica sion No, 61/244,309, filed on Sep. 21, 2008 ication Classification (1) Ine 5 1100 2005.01), (2) US.CL 751428 on ABSTRACT The invention involves a method for recovering gold from a gold concentrate comprising: dissolving gold from the con- ‘entre in an aqueous liquot to provide a god liquor, sub- iecting the gold liquoeto electrolysisinanelectrowinaingeell to provide cathode-asociated gold material; leaching the cathode associated gold material in an aqueous Hiquor under reducing conditions to provide a tated solid residue; and smelling the treated solid residue wo reeover gold.US 2012/0067170 AI EXTRACTION OF GOLD FROM CATHODE, "ASSOCIATED GOLD CONCENTRATES FIELD 10001}, ‘The invention relates to a method! and system for ‘exiicton of gold from gold concentrates involving dissoly= jing the gold in an aqueous liquor, eleetrowinning to provide ‘cathode associated gold eoncentratesand processing the con- BACKGROUND {0002} In many gold processing operations a sequence of ‘nit opertions is sed hat lead to Une disoltion of gold ina liguoe ‘The components of the liguor are. substantially soluble, ie the ytd values tel in a soluble liguo sueam, Fnhemor, insoluble motos associate withthe source materials are present in oly very Tew conceatraton. Thus, forexample, gold fom an ore may be taken up ina cyanide Tiuor (he fist soluble iguor steam, absorbed onto carbo an then faken up (or sirippe) fom carbon ito a secon more concentrated soluble gokdTiquor stream (he stip liguoe. Altematively gol from a gravity gold concentrate nay be taken up drely into a concentrated soluble gold Figo stoum [0003] The concentrated soluble gol liquor steam is typi tally fed to an electrolysis ell, where the action of electric ‘eurrent leas othe deposition of gold on or under the cathe ‘ole This deposited yold is herein elered (oa eathode- associated gold concentrate. 11004} Cathode-asociated pold in general does not contin ‘aluble amounts of platinum group meals (PGMs)—this may be because lite of these materials ae present inthe source materi, or because some of thexe materiale poorly Soluble and donot travel in soluble liquor steams (ypiclly ‘yanidebased) hat are used osoubilise gold ales Cathe ‘odesassocated gold concentrates are usually funer pro- ‘essed by smneling, wherein Mux i added © da euhode- sociated gold concentrate and the mintre is beted a temperate tient to mel fax snd gold. Base metal and base metal associated contaminants present inthe eathode- sociated gold concentrate pss ito the molten ux to fon a slag phase hich afer eoling canbe physically separated from the precious metal (bullion) phase. characteristic of the smelting operation is thatthe precious metals are consol data ina molten button orbar which basa significa lower surface arc thn the surice are ofthe eathade associated concentrate 10005) _Altrmatve clases of gold eeovery operations are used in he recovery of gold asa byproduct ia the mining of bese metals suchas copper and nickel. When gold in the Source material is found in small quantities in sociation th valuable quantities of copper or other bese metals, impure base metal is cast (by meting) to form an anode for tse in anelectolysis cel, andthe aetion ofeurentinthiseel leads tothe dissolution of copper (ith deposition of purified oppr on thecathode)-Un-dissolved resides fom he anode Getuting any wace amounts of gold) accumulate under the anode, and comprise the anode mid. Components of anode mndareinsoluble nthe eid eletrolysis igor) and donot travel inasolble liquor stream. Those insoluble components tay frequently incide valueble amounts of platinum group tcals(POMs) sells goldandsiver Thecontaminantsin Mar. 22, 2012 contaminants ina cathode-ssociated gold concentrate ‘becatse (a the source material is dlleren;(b) many process- ing steps are different, and in particular contaminants in ‘anode-tssociated conocalrate have not travelled ina soluble Tiquor stream while contaminants in a eathode-associated concentrate have generally tnvelled in a soluble liquor stream on two separate occasions: and (c) anode-associated gol concentrates have in steps prior ta clectrolysis, been part ‘fa molten-metal enviroament (for example when the ante is cast) whereas cathode-associated gold concentrates have ‘ever, prior to electrolysis, been pat of a molten-metal env ronmeat, Anode mid concentrates are typically provessed ‘sing a suocession of specialised leaching steps to recover various valuable components in various leach liquors. The smelting of anode muds comprising valuable levels of PGMs as well as gold is counter productive because smelting leads ‘oa consolidation of gokd, silver and PGMs ina molten mass vith a significantly reduced surlace area (relative to anode ‘mud, and the selective leaching of valuable components ‘rom this low surface area molten mass is much more difficult than selective leaching ofthe original high surface area anode aud. [0006] ‘The current methods of refining eathode associated gold trom electrolysis of aqueous gold liquor generally fnvolve smelting of the cathode associated) gold without leaching prior to hea treatment. 0007} ‘The discussion of documents, sets, materials, ‘devices, atieles and the lke is inehided in tis specification Solely forthe purpose of providing a context fr the present invention. Tis not suggested or represented that any oral of these matters formed part of the prior art base or were com- ‘mon general knowledge in the fleld relevant to the present inventionas it existed before the priority date ofeach claim of this application, SUMMARY, [0008] The inventor has found that the recovery of gold Irom cathode associated gold formed inthe electowinning process can be enfianced by leaching of cathode assoeiated gold with an aqueous reducing liquor [0009] Accordingly, there is provided a method for recov ring gold from a gold concentrate comprising: [0010] dissolving gold from the concentrate in an aqueous liquor, [0011] subjecting the gold tguor o electrolysis in an elee- Acowinning cell to provide cahode-associted gold materi [0012] Ieaching the cathode associated gold material in an ‘aqucous iguor under reducing conditions lo provilea treated solid reside; and [0013] smelting the treated solid residue to recover gold [014] In one set of embodiments the gold containing Jiquoris derived fom stripping of gol fromearbon on which the gold is sorbed, In another embodiment the liquor is oxale aid [0026] Examples of suitable non-metal containing redue- ing agenis may be selected from the group consisting of suites, oxalic neid,formie acid, hydrazine, acetates includ- ing acetic acid, citraes including citric acid sulfite and ihionite and preferably sulfies and other onganie acids COrganie acids are particularly suitable. [0027] The leaching ofthe cathode associated gold concen- trate under redcing conditions may use an aqueous leach ‘composition selected from the group consisting of aqueous base, aqueous acid, aqueous chelating agent and mixtures oF aqueous chelating agent with acd or base. For example, the aqueous reducing liquor may bean aeidie aqueous reducing liquor. Altematively, the aqueous reducing liquor is an alka- Tine aqueous reducing liquor. [0028] Preferably thereducing Hiquorinat feast one contact between with source material is scidic, preferably the pl is Jess than about 1.5, more preferably less than about 1.0, Preferably the acid is # nomaxidising acid. Preferably the acid is hydrochloric acid [0029] In a preferred embodiment the reducing agent is 2 regencrable reducing agent, for example, a reducing agent ‘whieh canbe regenerated from the oxidised form producedas 4 resul of the process by clectolyic regeneration of the reducing agent, [0030] The method may further comprise leaching the ‘deposited gold concentrate, prior to sad reducing leach sep, ‘nan aqueous liquor comprising one or more agents selected from the group consisting of hydrochloric sci, nitric acid, alkali, chelating agens, carboxy ie acids and their salts, chlo- rates, perchlorates, chlorides, luorsilicates, phesol sullate and peroxydivuliate [0031] Inone set of embodiments the method further com- prises subjecting the solid residue from leaching in aqueous ducing liquor to atleast ane leaching step in an aqueous liquors comprising agens selected fom the proup consisting ofhydrochloricaeid, nitric acid, alkali, lead acetate chelating ‘agents, carboxylic acids and thei sais, chlorates, perchlor ates, chlorides, forosiliates, phenol sulfate and peroxyd ulate, [0032] Examples of carboxylic acid which may be used in Jeaching prio to, with the reducing leach or afterthe reducing leach include Forme acid, soetie acid, lactic acid, cite aid, jsobutyric acid and salts thereof such as the alkali metal and alkaline earth metal salts. Examples of chlorides which may be used in leaching prior to, with the reducing leach or after the reducing leach inde ammonium chloride, sodium chlo- fide, potassium chloride, calcium chloride and strontinm chloride [0033] The method may comprise «plurality of steps involving contacto theeathode associated gold material with ‘an aqueous reducing liquor,US 2012/0067170 AI 10034) Preferably the contact between the source material tnd the aqueous reducing liquor is caried out at negative fist Eh, ala subsequent contactbetween the source material ‘and an aqueous reducing liquor i carried out at a more nega tive second Eh, 10035] Preferably the Fh remains negative throughout the ‘contact period between aqueous reducing liquor and the source material and reside derived therefrom, 10036] Ina prefered embodiment of the invention the con- tact between the source material or residue and aqueous Tiquor is carried outin conditions that encourage the dslodge- mnt of refractory material from the surface ofthe slid, Sch ‘conditions may include ultrasonic agitation, 10037] Inone set of embodiments the leaching is conducted ava temperature of atleast 60" C. 10038] Preferably the process ofthe invention leads to the recavery ofa greater quantity of gol fom the source material than is apparent ina standard bullion asay test of the source material. Preferably the excess gold recovery over bllion assay’ grade is at least 1%, preferably atleast 29%, preferably atleast 5%, [0039] |The process preferably comprises removing the Tiquor from the source material which takes place ater con- tacting the source material with the agueous reducing liquor AA wide range of methods aod apparatus are known in the industry for soli-lquid separation. For example, te liquor may be percolated through the source materia ins batch tank ‘and collected as run of, the source material may be filtered froma slury using suitable filtration equipment known inthe minerals procesting industry orallemaively the source mate rial solids may submit to gravity separation from liquor, for ‘example, in stitablebatch or continuous sting tanks knows inthe industry. In one embodiment the sep of contacting the source material with an aqueous liquor under reducing ditions is carried out by agitating (eg. stirring, siding oF ‘ihenvise agitating) an aqueous slury ofthe source material ‘with a reducing agent and the aqueous slurry liquor is removed from the source material by iration. Oder met- ‘ods such as centrifugal separation may’ be used if desied but may be less practical on an industrial scale, Sueh methods may, however, be suitable in use of the process for assay of precious metals, [0040] The process of gold recovery frequently involves & Jeaching step and adsompion of gold and other precious met- ‘als oto an adsorbent such as carboa or a suitable syatheic resin, Improvements in the adsorption process such as the ‘carbon in column (CIC), carbon in leach (CIL) and earbon in pulp(CIP) processes have led efficient gold recovery which In some cases have even justified reprocessing of mine tail- ings, Previous metals are stripped from the adsorbent by ‘elution using suitable iquor comprising lxiviant and oxidant, [0041] _Inone embodiment the gole-tich source material is preferably cathodic material or eathadic shige from ele teo-winning of a strip liquor such as may be used to remove precious metals from sorption onto carbon. Preferably said ‘eathodie material has been tated to remove steel wool 0042] In another embodiment the gold-rich source mate- rial comprises gold sorbed onto carbon, [0043] Ina prefered embodiment the reducing iguorin at Teast one contaet with source material comprises at least one chelating agent, preferably selected from the group consist ing of beta-diketones, amino polycarboxylic acids, sats of amino polyearhoxylie acids, carboxylic acids, salts of care boxslie acids, and polyphospbonats. Mar. 22, 2012 [044] In a prefered embodiment the material subject 19 Jeaching in an aqueous reducing liquor is ily divided, [0045] For example, the material subject to leaching in aqueous liquor may be finely divided providing on wet siev~ Jngat east 0% by weight passing through 100 micron sieve and more preferably atleast 80% by weight passing through 130 micron sieve. [0046] In one embodiment of the invention the method ‘optionally comprises treatment either prior (© lesehing in ‘aqueous reducing liquor, after leaching in aqueous reducing Tiquor of both before and after leaching in aqueous reducing liquor. The optional testinent may inl at east one leach- ing stepin an aqueous liquor comprising agents selected fr the group consisting of hydrochloric aid, nitric acid alll, Jead acetate, ammonium chloride, calcium ehlorde, stron. tium chloride, acetic acid and citric acid. The optional real ‘meat step preferably comprises leehing in an aqueous alkali ‘metal hydroxide, an aqueous nitric aid, aqueous hydrochle- Fic acid or mixtures ofthe acids, The optional treatment step ‘may he conducted at elevated tempertire sch as at fom 40 C10 90°C. and more preferably from 60° C. to 89°C. Iemay bbe advantageous inthis embodiment to eondict the option treatment with application of agitation such as ultrasonic jon, The optional treatment may if desired comprise plurality ofleaches using the same of different aqueous leach liquors before andlor aller the reducing leach, [0047] Inge embodiment, the solid reside fom the ague- ‘us reducing liquors treated with an aqueous alkaline liquor ‘whieh has a pH greater than 13, more preferably greater than 14. Inone embodiment, the alkaline liquor comprises at least 5% sodium hydroxide, [0048] Ina prefered embodiment at least one step selected {rom contact with the aqueous reducing liquor and leaching prior or alter said contact with the aqueous reducing liquor is ‘carried out in conditions that encourage the dislodgement of reffactory material from the surface of the source material or sold esidve, Examples of seh conditions inelude ultrasonic agitation, [0049] The use of ultrasonic agitation is prefered and in particular frequency inthe range 10-60 Kitz, more prefer fhly 20-15 KE is preferred. Inne set of embovtimens ulin sonics ate applied to-a hot leach liquor, for example at a temperature of atleast 60°C. [0050] In one preferred set of embodiments the method ‘comprises said reducing leach and a subsequent acid leach ‘wherein the liquor used in the reducing Teach comprises hydrochloric seid (preferably 0.5 to $M hydrochlorie acid) And stannous chloride (preferably trom $ 10 150 grams per lite of stannous chloride dihydrate, moce preferably 10 10 100 and even more preferably 30 to 50 grams perlite of stannous chloride dihydrate) and the liquor used inthe sub- sequent aid leach comprises nitric acid (preferably about St0 about 70%, more preferably 20% to 6% and even more preferably about 50% nitric acid) in water Theweightatio of liquid to solid material in the subsequent acid leach step is sreferably in the range of 10:1 10 100:1 (preferably 20:1 to 0:1, more preferably about 40:1). [0081] Themethod may comprise weatment prior or after Teaching with the aqueous redicing liquor The soli residue ‘which has been treated in accordance with the inveation may be further refined to provide preciows metal by: methods known in the art such as by smelting. In one preferred cmbodinientof the invention the refining step comprises add- ing Said residue fo a crucible, and heating the contents toUS 2012/0067170 AI smelting temperature. The smelting process may include the use of a flux, such as a ux comprising borax, or may be fux-less. 10082] Ina prefered embodiment as an intial step the ux Js placed in the erucible and melt prior t addition of the treated solid residue, or the solid residue plus metal. In @ further preferred embodiment there is no flux mixed with the treated solid residue or sold residue mixed plus metal 10053] Daring the process of smelting gold the present Jventor bas found! that signiieamt amount of gold, re- ‘quently ofthe order of from I t0 3% or even more is lost t0 slag. Even when the sig is ground and reintroduced into an carler part of the gold recovery circuit this slag associnted told may be substantially unrecoverable, 10084] In one set of embodiments of the heating step the cathode associated gold concentrate is added to a previously melted pool of metal comprising a material comprising & metal selected from copper, silver, gold and platinum group metals. Ina preferred set of embadiments the ssid material has a concentration of at least $0% by weight (preferably at least 90% and more preferably at least 95% aad sll more preferably atleast 9% by weight) of one of eopper, silver. fold and platinum group metals 1005) In one preference the molten pool has a melting point in excess of 900°C. Preferably the pool metal has one ‘tal selected from the group consisting of gol, silver and ‘copper. In one set of prefered embodiments the metal come ponents are placed in proximity to the treated solid residive ‘andthe melting step causes the metal components (preferably Selected from god, silver, copper) to melt 10056] |The smelting may, in one et af embodiments,com- prise: [0087] smelting the reduced solid residue by forming @ molten pool comprising at least one metal selected from ‘copper, silver, gold and platinum group metals; and 10058] adding the redvced solid residue into the pool of ‘molten metal 10059] Ina particularly prefered set of embodiments the ‘molten pool i formed frm a solid particulate mixture com- prising particles of treated solid residue and particles of at Feast one metal selected from copper, silver. gold and plat ‘num group metals. In this set of embodiments the pool metal preferably comprises silver, copper or mixtures thereo!: The Particulate mixture of the residue and at least one metal ‘clcted from copper silver and gold is preferably gradually added to a heated ervcble such that a molten pool is Formed ‘during addition and further particulate mixture is added 10 nd becomes partof the molten pool. The particulate mixture ‘of the residue and at least one metal selected from copper silver, gold and platinum group metals are, in one set of nboiments, gradually added ta preformed molten pool of orax. Inanotber set of embodiments the particulate mixture ‘does not comprise particles of borax or other uxing agents 10060] In ove set of embodiments the smelting method ‘comprises adding the treated solid residue to a previously ‘melted pool comprising at least one meal selected fom cop- per siher, gold and platinum group metals, {0061} Ina farther st ofembodimentsthe smelting method ‘comprises enclosing the treated solid reside is ia @ metal sheet or foil, preferably selected from atleast one of copper. silver, gold and platinum group metals. The process ean be ‘conducted to avoid or minimize contact of the treated solid residue with the crucible Mar. 22, 2012 10062] ‘The erucible used in the smelting may comprise 2 ‘ceramic material (preferably ceramic material at is rela- tively inert to corosion when contacted by molten borax) [0063] The smelting is preferably conducted in a crucible ‘whieh comprises less than 10% by weight (preferably less ‘than 5%) carbon and less than 10% by weight (preferably less than 5%) of earbides. [0064] Inone set of embodiments the reduced solid residue Js added (0 the molten pool through a conduit such as & ‘ceramic pipe that guides said material into the bulk pase of the molten pool. It is prefered that the residue does not encounter the walls of th enveible that eontains the molten pool [0065] Attheconclusionof the smeling process the molten ool may be poured into a mold t form an ingot, bullion bar ‘or dore bat [0066] In a farther aspect there is provided a system for recovery of gold from a concentrate that inchides gold, the system comprising: [0067] (@) means for contacting the concentrate with an ‘aqueous liquor to dissolve gold, 10068] Gi) anelectrowinning cell forsubjecting the prod- uct of step () to electrolysis to provide a cathode 2ss0- ciated mateeal, 10069] Gi) a crocible for contacting cathode-associated ‘meri from step (i) with an agucous Teacant under rediacing conditions, and [0070] Civ) means for smelting the produet of step ii) 10 recover gold [0071] ‘Tae system in one set of embodiments further com- prives « means for applying thermal or ultasonic eneryy {ring anyone of steps (i), (i) oF (i) [0072] In a preferred embodiment of the system the ert cible comprises less than 10% by weight carbon and less than 10% by weight of carbides [0073] ‘The invention will now be deseribed with reference {o the following examples. It is to be understood that the ‘examples are provided by way o illustration of te iavention fand that they are in no way fimiting 10 the scope of the EXAMPLES Example 1 [0074] Silver Lake Gold Gravity Conceatrate (SLGGC) Sovurse material [0075] Gold gravity concentrate fom the gold processing circuit at Silver Lake's Lakewood Gold production facility (near Kalgoorlie Ausiralia) was stripped in caustic cyanide ‘andthe strip liquor processed in an elecirossinning cel, Cath- ‘de material an cathode sludge from te cell was aggregated ‘and soaked in 25% HCI for2 hrs to leach out stel Woo! ro the sample. ‘The residual material was rinsed and dried 10 provide 12.5 kg of source material, Grab lots ofthis material ‘were taken and aggregated to procure @ 500 g sample of source material [0076] The source material was homogenised by crushing And chopping. and multiple 10 gub-samples were riffle spit. of these sub-samples were submited for bullion analysis to the Penh Mint at lay St East Perth, Western Australis, The bullion assay results were:US 2012/0067170 AI Mar. 22, 2012 Goivaie Shere Wewirofnb ——Goltwness Sharan ve Weigtofeiewnle __Galonsy) __ (lao ae) ol Scie) lions Tors oa Tae Tons Tee 7a foal some lem mee xB ve ones wos ri aon an aa ee Examples Reducing Leach Step on SLGGC 10077] One of thel0 g subsamples of SLGGC described above Was added toa beaker with liquor comprising 200 mlof 50% HCI and 8 g stannous chloride, The contents of the beaker were heated to 80deg C. andar S minutes thebeaker ‘vas placed in # Soniclean 160T ultrasonic bath (bah water at 60 degC. frequency 40kF17, maximum power 250 W, power setting 60% of 250 W=150 W), After S minute of ultrasonic agitation the beaker was re-heated and the cycle repeated 2 times. The residue was obtained by filtration, rinsed in water and dried. The (un-smelted) residue was found to have a Tighter cofour than the initial 10g sub-sample, and was sent t0 the Perth Mint for bullion analysis, and the gold content (expresied as apercentof 10g starting material) was found to be 61.77%, an increase from 60.42% inthe starting materi Alalne Leach Step After Reducing Leach on SLGGC 10078] A 10 gsub-sample of SLGGC source material was provided with a reducing leach as described above, Residue from the reducing leach step was added vo 200 mal of «10% sodium hydroxide liquor, and taken to 80 deg C. for § min- utes, followed by 3 eycles of ultrasonic agitation as in the above example. The resultant residue was obtained by ilkm- tion, rinsed in water and dried, The (nnsmelted) resultant residue was sent othe Perth Mint for bullion analysis, and the gold content expressed asa percent of 10g stating material) ‘was found to be 61.94%, an increase from 60.4% in the starting material. Example 3 Silver Lake Gold Carbon-in-Pulp Concentrate (SLGCIP) 10079] | Gold-loaded carbon derived from the CIP gold pro- ‘cessing cieuitat Silver Lake's Lakewood Gold production facility (near Kalgoorlie Australia) was stripped in caustic ‘eyanide and the strip liquor procested in an electrowinaing ‘ell. Cathode material and cathode sludge from the eel was aaregated and soaked in 25% HCI for brs to leach out steel ‘woo from the sample, The residual material was rinsed and ried to provide 12-5 kg of source material. The source mato rial was homogenised ina kitchen blender, and multiple 10 8 sub-samples wore riffle split. 6 of these sub-samples were submitted for bullion analysisto the Perth Mintat Fay St East Perth, Western Australi, The bullion asay results were ‘Reducing Leach Step on SLGCIP Source Material [0080] One of the10 g sub-samples was added ton beaker ‘with liquor comprising 200 ml of 30% HCl and 8g stannous chloride. The contents ofthe beaker were cated to 80 deg C and alter $ minutes the beaker was placed in a “Sonilean 1607" ultrasonic bath (bath water at 60 dex C. frequency 40 KHz, maximum power 250 W, power setting 6% of 250 W-150W)-After Sminutes of Wasonie gitation the beaker was reheated and the eyele repeated 2 times, The reside was joblained by filtration, rinsed in water and dried, Alkaline Leach Step on SLGCIP Source Material [0081] Residue from the reducing leach step (described above)was axed to 200 ml of a 10% sodium hydroxide Tiquor, and taken to 80 deg C. for § minutes, followed by 3 cycles of ultrasonic agitation as described above, The result fant residue was obtained by filtration, rinsed in water a ‘ried, The (un-smelted) esultat residue wes sent tothe Perth ‘Mint for bullion analysis, and the gold conten! (expressed as ‘a percent of 10 g stating material) was found to be 37.52%, fan increase om 36.4% in the starting material. The silver ‘eantent Was found tobe 7.58%, an increase fom 7.46% inthe Sart material, Smelting [0082] A 10 g sub-sample of SLGCIP source material was ‘akon theough a reducing leach step andl an alkaline leah step cording to the above protocols, and the dry residue from the alkaline leach stop was aided to 30 fire assay erncible. The Toaded enieible Was placed inside an electric fmace pre- hated to 1220-degC. and kept al this temperature for 1.Shis. ‘When the crucible was withirawa from the furnace, it con tained. fluid phase comprising molten gold, an dark sid phase that adhered to the base of the ervible. The liguid ‘hase was poured into a button mould, anda clean separation achieved from the dark sold phase. After cooling the button ‘vas removed from the mould and sent for bullion assay, The ark sold pase weighed 1.5 g. portion ofthe dark solid ‘phase (0.41 g) was added t 250 mi of freshly prepared aqua repa (I part cone nite acid and 4 parts cone hydrochloric seid) na beaker at 80 deg C. After 5 minutes the besker was placed ina Soniclean 1607 ultrasonie bath (bath water at 60 og. frequency 20 KH, hath setting a intensity 250 W). After $ minutes of wrasonie agitation the beaker was re heated and the eycle repeated 2 times, Then 50 ml cone hydrochloric acd wasadded tothe Beaker and the beaker was ‘cheated and given ane further Smite period of ultrasonic ‘agitation at 60 dey C. Thereafer the liquor in the beaker wasUS 2012/0067170 AI Jmmediately filtered and sent for gold assay by flame AAS. ‘The gold content ofthe button was found tobe 264 g, andthe Jeaelt-assay gold content of the dark solid residue was found tw be 109 g. The total amouat of recovered gol from the 10 subsample was thus 3.73 g, an increase from 3.68 g in the Sarin material Example 5 10083] Silver Lake Gold Gravity Concentrate (SLGGC) Source materi Reducing Leach Step on SLGGC {0084} | 10.gsub-samples of Silver Lake Gold Gravity Con- centrate (SLGGC) were prepared as previously described, “The gold value (by bullion asssy) in each subesample was 60.4°%, 10085] A 1006 g sub-sample (particle size sub 250 microns) was aed To 2 500 al beaker. Liquor comprising 8 8 stannous chloride dihydrate (dissolved), 100 ml eoncen- trated FICL and 100 ml water vas added tothe beaker, and the beaker was placed in a heated ultrasonic bath (Soniclean, ‘maximum power-250 W) at 60° C, for § hours. Ultrasonic agitation (60% max soting) was applied according to the following schedule: 10 minutes initial sonication, 80 minutes pause, 10 minutes sonication, 80 minutes pause and soon to the end of the 8 hour period. No mechanical agitation was sed, 10086] After 8 hours. the contents of the beaker were fll terod (Whatasan 40ashles filter paper equivalent ination speed to Whatman 2) and the residue on the filter paper ‘washed with water. The residue was then washed from the paper into another 500 mi beaker, and care was taken fo use Jess than 100 mal of water to achive tis transfer. The water level in the Beaker was made up to 100ml, and 100 als oF 8% aqueous sodium hydroxide iguor was added to provide 4% ‘inal eaustic leach iquor forthe second leach, The beaker Was placed ina heated ultrasonic bath and teated according to the above protocol. After filtrationand water washing, the residue ‘vas dred in an oven at 80" C. overnight. The residuceake was readily disrupted io make fine powder by simple mechanical stimulus with a spatula, 10087] 100 g of “ine silver” granules (plus 99.9% silver) ‘was purchased from PW Bock & Co silver merchants of Adelaide, Australia. The granules were approximately 2 mm in diameter. Sheet silver (ine silver grate) of diameter 0.3 ‘mm, with each sheet weighing 10 was aso purchased from PW Beck & Co. [0088] The granules were placed in a 250 ml fire assay ‘erucible purchased fom Furnace Industries, of Perth Aust lia, The loaded crucible was placed inside an electric Furnace ‘and brought to 1220° C, Moen silver derived fom the gran tles formed a small pool on the bottom ofthe crucible. 10089] Dried residue derived from the caustic leach step described above was folded ino 10 g piece of sheet silver The hot erueible containing the silver pool was withdraws from the Furnace, and the silver shoot envelope was droppe Jno the crucible directly onto the molten silver pool. The sheet silver melted quickly andthe contents ofthe silver shoot ‘envelope became immersed in the silver pool without making, ‘contact with the sides ofthe crucible. The crucible was imme= “ately returned tothe Tumace, brought back to 1220° C. and retained at that temperature for 15 mints. The men con- of the hot erucible were poured into a hemispherical Mar. 22, 2012 button mould, and allowed cool The button was dislodged from the mould and quenched in water, then allowed to dry ‘The approximate dimensions of the hemispherical bution were: diameter 4em, ax height 3 em. The button was delled ‘out © obtain approx 6 g of shavings and burrs, which were ‘sent for bullion assay Umpire Astay Laboratories, in Perth Australia, 0090} ‘Te inti 10.06 g sub-sample comprised gold at {60.49% (autiple bullion assay results on replicate samples). The gold recovered from the Button described above wis 6.16. sgand 0.14 g gold (total) was assayed onthe filter papers used Jn the acid and alkaline leaching seps prio o smelting. This corresponds on total of 6.3 g gold recovered from the initial subsample, compared to 10.06%0.604-6076 2 gold expected from the bullion assay on the initial sub-sample. The (0.368 g gold increment represents the benefit obtained by sing the method ofthe invention, Example 6 Silver Lake Gold Gravity Concentrate (SLGGC)Source Material (a) [0091] Gold loaded carbon from the gravity gold cireit at Silver Lake's Lakewood Gold production facility (near Kale oorlie Ausralia) was sipped ineausticeyanide and the strip Jiquor processed in an electowinning cell Cathode materia ‘and cathode sludge from the eell was aggregated and soaked 25% {1Cl for 2h, to leach out steel woo frm the sample The residual material was rinsed and dred to provide 12.3 kg ‘of source material. This source material was homogenised by ‘rushing and chopping, ad auliple 10g sub-samples were fille split, Apart fom the 10g sub-samples the remainder of the material Was smelted using the standard Silver Lake pro- cess, and the commercially recoverable gold was found 0 be 77.06% gold Silver Lake Gold Carbon in Pulp (CIP) Concentrate—Source Material () 0092] Gold loaded carbon from the C-L circuit at Silver Lake's Lakewood Gold production facility (near Kalgoorie Ausra) Was stripped in caustic eyanide and the srip liquor processed in an cleciinning cell. Cathode material and tathode sludge from the cell was aggregated and soaked 25% HCI for 2 hr, to Teach out steel woo! from the sample ‘The residual material was rinsed and dried to provide 12.5 ka ‘ofsouree material. This souree material was homogenised by ‘rushing and chopping, aad multiple 10 g sub-samples were fille split. Apart fom the 10g sub-samples the remainder of the material was smelted using the standard Silver Lake pro- cess, and the commercially recoverable gold was found (0 be 35.08% pol. Reducing Leach Step [0093] Take 10 g sub-sample and add to reducing liquor. ‘The leaching processas deseribedin the fst par of Fxample 4 (*Rediucing Leach Step on SUGCIP source material”), [094] Nove: Ifthe reducing leach is not the fist leaching ‘ep, use leach residue from the previous leaching step. Note {hat the 10g sub-samples were used as source material inthe inital leaching sep. Alkaline Leach Step [0098] Take 10 subsample and odd alkane Hiquor. The alkaline leach is as described in the second part of Example 4 (Alkaline leach step on SLGCIP source material”)US 2012/0067170 AI 10096] Note: IF the aikaline leach is not the first leaching step, use lech reside from the previous leaching step. Note thatthe 10g sub-samples were used as source material in the inital leaching sep Leaching in 50% Nitec Acid [0097] Take 10 g subsample and add to 200 ml of 50% ric aid liquor. Perform ultrasonic agitation, filtering rins- and drying as deseribed in the first part of Example 4 (Reducing Leach Step oa SLGCIP source materia [0098] Note: Ifthe acid leach isnot the first leaching step, tse leach residue from the previous leaching step. Note that the 10 g sub-samples were used as source material in the inl lesehing sep Borax Smelting [0099] Fitter and dry leached concentrate; ‘material with 20 g borax and add to a crucible and eat the ‘encible to 1220? C- inside an electric furnace for 1.5 hours Pour molten material from the erucble into the mold and allow to cool. Remove the contents ofthe mold and remove slag from the precious metal bution, Weigh the button and send a supe ofthe button fo the Perth Mint to establish the ‘concentration of old in the button. 10100] Calculate the gold content of the source material (the initial cathode assorted pold concentrate usedin the leach sequence), Silver Pool Smelting [0101] Take 100 gof fine silver granules, add to a crucible and heat to 1220° C. in an electric fumace. Take shoot silver ‘of diameter 0.3 mm (fine silver grade, 10 g per sheet) and wrap the sheet around the finely divided material to be smelted, (his material is theres remaining afte previous leaching steps on 10 of sub-sample) to form a silver eave- Jope, Remove the hot crucible containing molten silver from the farace and drop the silver envelope into it, Immediately return theerucible othe furnaceand reheat to 1220°C. for 1S ‘minutes, Pour the mten contents ofthe hot crucible into-@ button mold and allow to cool, Remove slag and dil out the button to obtain shavings and burs for bullion assay Residual goldon filter papers andin leach solutions aresdded to aqua regia and gold found in this way is added to gold bullion numbers. TABLI Commesaty ‘malo gol Mar. 22, 2012 TABLE 2 Get ern neal "pols Leschsogene eh seese Example 7 [0102] Silver Lakes$00.97 g of wire gold (referred to 2 (C1P-2) was received fom Silver City Mining Company this was described as described as being Silver Lake Resources CP plant material from Lakewood Gold Processing Facil ‘This sample was taken by representative sampling from a ‘Wire gold production un after hydrochloric acid treatment 10 remove the calhode wire and the gold grade of the sample (calculated by commercial smelting ofthe production sample ‘with gold determination of the bullion bar by bullion assay from the Perth mint). The gold content was found to be 35.08% by weight PreSmelt Treatment [0103] 10 gofCIP-2(representativesubsampleobtained by ‘ile spliting) was added to 200 ml of $0% by volume nitric ‘acid in water in a 600 onl beaker. The beaker was placed in a Iheated wltasonic bath at 60° C. ('Soniclean” brand, ma im power-250 W) and agitated at maximum power for one hour The liquor was filtered off and he residue washed with water, [0104] The water washed residue was added to iquor ‘comprising 8 g stannous chloride dehydrate (dissolved) 100 fal cone. hydrochloric acid aid 100 ml water in a 600 ml beaker. The beaker was placed ina heated wliasonic bath at 60" C. (*Soniclean” brand, maximum power-250 W) and agitated at maximum power for one hour, The liquor was likered off and the residue washes! with water [0105] The water washed residue from the previous step ‘was added to 200 ml of 0? by volume nitric acid in water ia 1600 ml beaker. The beaker was placed in aheated ultrasonic bath at 6° C.("Soniclean” brand, maximum power-250 W) and agitated at maximum power for one hour. The Tiquor was filtered off and the residue washed with water, and dried. [0106] All iter papers and liquors produced in the above ‘operations were assayed lor gold by standard techniques. same Nenbr Pas Cosi CHE SLCPANY tqinaatntue pina em Cy ied ak suetavao Fgura 2m Chy ‘epee ps 20 gD 1 hs ih pep ee 0 ep ie on {tide Te bon ea dda mt ed an Rectan Sento apeUS 2012/0067170 AI Upwase Simple olitesnesstign “Gold com Init Stns esi messi Newberg) Sot paper TOTAL S00) 1. A method for recovering gold from a gold concentrate ‘comprising: dissolving gold from the concentrate in an aqueous liquor to prsiden gold liquor, subjecting the gold liquor to electrolysis in an electrowin= ning eel to provide cathode-assocated gold material; leaching the eathode associated gold material in an ce ‘vs liquor under reducing conditions to provide treated solid residue: and smelting the treated soli residue to recover gold. 2. The method according to claim I wherein the gol con= ‘cenirate comprises earboa sorbed with gold and the method Jurkier comprises stripping gold from the carbon by contact with an aqueous iquor to provide sid pold iquor. 3. The method according to claim 1 wherein te gold con- ‘entrate comprises a gravity concentrate andthe method fur- ther comprises dissolving gold from the gravity concentrate to provide said gol liquor 4. The method secording claim 1 wherein leaching the ‘cathode associated gold material under reducing conditions jnvolves wse of an aqueous leech composition selected from the group consisting of aqueous base, aqueous acid, aqueous ‘cholating agent, and mixtures ofaqueous chelating agent with id or hase, 5, The method according to claim 1 wherein the aqueous reducing liquor is an acidie aqueous reducing liquor of pH Jess than about 1.5. 6. The method according to claim 1 wherein the aqueous reducing liquor is an alkaline aqueous reducing liquor. 7. The method according to claim 1 wherein the method further comprises leaching the deposited gold concentrate prior to said reducing leach step, in an aqueous fiquor com- Prising oncor more agents selected from the roup consisting Dfhydrochlorieacid, nitric acid alkali, ead acetate, chelating ‘agents, carhonylie acids anc their salts, erates, perehlor- ales, chlorides, luorosilicate, phenol sulfonate, and peroxy- ddisulfate, 8, The method according to claim 1 wherein the method Jurther comprises subjecting the sold residue from leaching jn aqueous reducing quot to atleast one leaching step ina ‘aqueous liquor comprising agents selected from the group, consisting of hydmehloric acid, nitric acid, alkali, leat acetate, chelating agents, carboxylic acids and their salts, chlorate, perchlorates, chlorides fuorsilicate, phenol sul- Jonate, and peroxydisulfate 9, (canceled) 10, The method of claim 8 wherein the contact beeen at Jeastone ofthe gold concentrate and residue and the aqueous fiquor is caried out under conditions of ultrasonic agitation, Mar. 22, 2012 11, The method for recovering gold aeconding to claim 10 ‘wherin'a mixturof the eathode-associated gold concentrate and reducing liquor is subject to ulirisonie radiation at Trequency in the range 10-60 kHz, 12, The method for recovering gold according to claim 1 wherein the cathode comprises steel wool and the method ‘comprises testing the cathose having deposited gold mate- fal to remove the steel woo 13. The method of claim I comprising 2 plurality of steps involving contacto theeathode associated gold material with ‘an aqueous reducing liquor 14, The method according o claim 1 wherein the reducing conditions are provided by a reducing agen. 15, The method according o claim 1 wherein the reducing conditions are provided by a least one reducing agent com- rising metal species selected from the group consisting of ‘chromium (Cr, tin(Sa 1), copper (Cu and titanium (TT, 1 I) and non-metal containing reducing agents selected from sulfites, organic aids with sulfites and oxalic acid 16, The method aocording to claim 1 wherein the aqueous recng liquor comprises stannous ion. 17. The method acconling to claim 1 comprising said redcing leach anda subsequent acid each wherein the liquor used inthe reducing leach comprises hydrochloric acid and stannous chloride and the liquor used inthe subsequent acid Teach comprises nite acid in water. 18, The method according to clan 17 wherein the weight ‘ito of liga to solid material inthe subsequent acid leach sep is in the range of 10:1 {0 100:1 19. The method according to claims 14 further comprising subjecting the solid residue fom leaching in aqueous redne- ing liquor to leaching with an alkaline liquoz. 20, The method according to claim 19 wherein the aqueous alkaline iquor has a pH greater than 13. 21. The method for recovering gold acconting to claim 19 wherit the alkaline liquor comprises atleast 5% sodium hydroxide 22, The method secordingw claim 1 wherein the reducing liquor comprises atleast one agent selected from organic acids and thee sal, 23, The method according wo claim 1 wherein the reducing Jiquor comprises at least one base metal chelating agent selected from the group consisting of betr-diketones, amino polyearboxylic acids, salts of amino polyearboxylic acids carboxslic acids, salts of eatboxylie acids, and polyphospho- 24, The method according to claim 1 wherein the material subject to leaching in an aqueous redocing liquor is finely divided 25. The method according to claim 1 whersin the material subjeetto leaching inaqueous liquors finely divided provid- ‘ng’on wet sieving at least 80% by weight passing theou TWO micron sieve, 26, The method according to claim 1 wherein the smelting of aid residue ina crucible is conducted without addition oF aaflux, 27. The method according to claim 1 wherein the smelting ‘of said residue is conducted in the presence ofa borax ux 28, The method aeconing to claim 1 wherein the step of pracessing the residue to recover gold comprises forming @ ‘molten pool comprising at least one metal selected from copper, silver gold and platinum group metals 29. The method according to claim 28 wherein the molten pool is formed from a solid particulate mixture comprisingUS 2012/0067170 AI particles of twated solid residue and particles of a least one ‘metal Selected from copper, silver, gold and platinum group metals '30, The method according to claim 28 wherein the molten pools poured intoa mold form an ingot, bullion bar or dre bar ‘3. The method according to claim 28 wherein the molten pool has a melting point in excess of 900°C. 32, The method according to claim 28 wherein the pool tal comprises silver, epper or mixtures there: 33. Themethodaccording i claim28 wherein apanicuate mixture of the residue and atleast one metal selected Irom ‘copper, silver gold and platinum group metals is graklly ‘added tow heated crucible such that molten pool is formed ‘during alton and further particulate mixture is added t0 ‘and becomes part of the molten poo. 34. Themethodaccording to claim28 whereina paticulate mixture of the residue and atleast one metal selected Irom ‘copper silver, gold and platinum group metals are gradually ‘added tou preformed molten pool af borax Mar. 22, 2012 shod aeconting to claim 34 wherein the particw- ‘docs not comprise particles of borax or other dTuxing agents 136, The method aoordng wo claim 28 wherein the meting step comprises adding te treated sold residue toa previously ‘melted pool comprising at least one metal selected fom op- pet silver, pod and platinum group metas, 37. The mithod according io claim 28 whercin at least part ofthe treated solid residues enclosed ina metal sheet orf preferably selected from atleast one of copper, silver, go and platinum group metal. ‘38. The method aoconling to claim 27 whercin smelling is cconccted ina enaible comprising s ceramic material, inet tomolten borax, 39, The method according 1 claim 38 whercin smelting is conducted in a erueible which comprises less than 10% by ‘weight carbon and less than 10% by weight of carbides. 40-43. (canesled)