WO2002042503A1 - Extraction de metaux precieux de minerais refractaires carbones - Google Patents

Extraction de metaux precieux de minerais refractaires carbones Download PDF

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Publication number
WO2002042503A1
WO2002042503A1 PCT/US2001/043408 US0143408W WO0242503A1 WO 2002042503 A1 WO2002042503 A1 WO 2002042503A1 US 0143408 W US0143408 W US 0143408W WO 0242503 A1 WO0242503 A1 WO 0242503A1
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WO
WIPO (PCT)
Prior art keywords
acid
slurry
hypochlorite
ozone
pregnant leach
Prior art date
Application number
PCT/US2001/043408
Other languages
English (en)
Inventor
John J. Lee
Original Assignee
Orthotech Industrial Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Orthotech Industrial Corporation filed Critical Orthotech Industrial Corporation
Priority to AU2002216679A priority Critical patent/AU2002216679A1/en
Publication of WO2002042503A1 publication Critical patent/WO2002042503A1/fr

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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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • 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 generally to processes for recovering precious metals from carbonaceous refractory ores and specifically to leaching processes for recovering precious metals from carbonaceous refractory ores.
  • the process for recovering precious metals from carbonaceous refractory materials generally includes the following steps:
  • the relatively simple and low cost process can recover precious metal, including gold, silver, platinum, and palladium, at relatively high rates.
  • the process is more simplified and cost-effective than processes presently in use for the recovery of gold and other precious metals from carbonaceous ores, concentrates containing the same, or carbonaceous tailings. Consequently, the process can effectively treat precious metal- containing materials that are too poor in recoverable metal values to be economically treated by conventional processes.
  • the feed slurry can contain a variety of acids, such as mineral acids. More preferably, the acid is selected from the group consisting of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, hydrofluoric acid, hydrobromic acid, oxalic acid, and mixtures thereof, with mineral acids such as sulfuric acid, hydrochloric acid, and nitric acid being most preferred. Because the process uses such acids to dissolve precious metal values, it can avoid or minimize the environmental pollution often associated with conventional hydrometallurgical processes, which utilize environmentally harmful chemical compounds such as cyanide and thiourea in precious metal recovery.
  • acids such as mineral acids. More preferably, the acid is selected from the group consisting of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, hydrofluoric acid, hydrobromic acid, oxalic acid, and mixtures thereof, with mineral acids such as sulfuric acid, hydrochloric acid, and nitric acid being most preferred.
  • the carbonaceous material can be oxidized by a number of different oxidizing agents, such as ozone, molecular oxygen, chlorine gas, sulfuric acid, and alkaline hypochlorite, with ozone being most preferred.
  • the slurry conditions are important to the effective oxidation of the carbonaceous material in the feed slurry.
  • the feed slurry in the contacting step (b) has a temperature ranging from about 40 to about 65 C, and the pH in the contacting step (b) ranges from about pH 1 to about pH3.
  • the oxidizing agent is ozone
  • the ozone is preferably contacted with the feed slurry at a rate ranging from about 0.25 to about 0.60 g/hr.
  • the oxidized slurry is contacted with a hypohalite under acidic conditions to dissolve the precious metal.
  • the hypohalite is a hypohalite of alkali or alkaline earth metals.
  • the most preferred hypohalites include sodium hypochlorite, potassium hypobromite, calcium hypochlorite, potassium hypochlorite, calcium hypobromite, barium hypochlorite, barium hypobromite, and mixtures thereof.
  • the effectiveness of the hypohalite and acid in dissolving the precious metal values largely depend upon the concentration of the hypohalite and the pH of the slu ⁇ y.
  • concentration of the hypohalite in the pregnant leach slurry ranges from about 0.04 to about 0.4% by weight and the pH of the slurry ranges from about pH 2.2 to about pH 6.8.
  • the synergistic combination of the hypohalite and the acid provide an economical process by which gold-bearing sulfide ores that have been pretreated with such conventional techniques as autoclave oxidation and bio-oxidation can be subjected to direct application for the extraction of gold from the oxidized slurry. This would eliminate the expensive practice whereby gold-bearing sulfide ores pretreated in acidic solution by those oxidation techniques are washed and the pH adjusted to a high alkaline condition prior to applying conventional cyanidation.
  • the present invention relates to a process whereby improved recovery of gold is made from gold-bearing carbonaceous ores and other materials containing the same.
  • an acidified brine slu ⁇ y of carbonaceous ores is treated with an effective quantity of ozone at ambient temperature which will convert the carbonaceous matter to an oxidized form that will enable gold and other metal values associated with the ore matrix to be solubilized in subsequent hydrometallurgical extraction step without interference by the carbonaceous impurities.
  • the aqueous slurry of carbonaceous ores mixed with a calculated amount of halide of alkali metals or alkali earth metals is acidified with any of the mineral acids such as sulfuric, hydrochloric, or nitric acid to a pH range between 1.0 and 3.0, with a prefe ⁇ ed embodiment being 1.2 and 2.5. While the acidic ore slurry is thoroughly agitated by mechanical means and heated to a temperature in the range between 40° and
  • UV ozone from a commercial ozone generation source is dispersed into the slurry by a sparging action.
  • the slurry in the reaction vessel is cooled to room temperature upon completion of oxidation by the ozone treatment and the hydrometallurgical gold extraction follows. While agitation is still continued throughout the process, the oxidized ore slurry is mixed with an adequate amount of hypohalite of alkali metals or alkali earth metals such as sodium hypochlorite, potassium hypobromite, or calcium hypochlorite. At this time, the acidity of the slurry is measured and adjusted to an optimum pH range between 2.2 and 6.8, with the same acid initially used for the acidification in the ozone treatment step.
  • CIL carbon-in-leach
  • Gold-bearing carbonaceous refractory ore 10 used for treatment pursuant to the present invention is crushed and pulverized 14 to produce a comminuted ore 18 having particle sizes to a maximum 100 mesh or particle diameter of less than 150 micrometers.
  • pulverized (or comminuted) ore 14 of known weight is initially mixed in an open vessel containing an acidified brine solution and slowly, yet thoroughly agitated by means of an impeller system at speeds ranging from 100 to 500 rotations per minute to form an aqueous slurry 24.
  • the density of aqueous slurry 24 normally comprises from 20 to 50 weight percent solids.
  • the aqueous slu ⁇ y 24 is oxidized 28 with ozone to form an oxidized slu ⁇ y 32 in which the carbonaceous compounds are oxidized.
  • the aqueous slurry 24 is continuously agitated at ambient temperature, while UV ozone from a commercial ozone generation source is sparged into the slurry at flow rates ranging from 0.25g to 0.60g per hour until completion of the oxidation reaction.
  • ozone This will take a total consumption of ozone in the range between 2.4g and 4.0g for the particular carbonaceous ore used in the present invention.
  • quantity of ozone necessary for the complete oxidation will vary depending on the magnitude of carbonaceous impurities loaded in the ore matrix given the chemical reaction condition applied.
  • the pH of the slurry during the ozone treatment will be maintained at about 1.0 to 3.0.
  • the cooled slurry 40 is leached 44 to form a pregnant leach slurry 48 including dissolved precious metals.
  • the agitation is continued for the next period of time ranging from 2 to 10 hours, and gold is extracted from the oxidized ore slurry by adding a selected hypohalite such as sodium hypochlorite as a leaching chemical in the concentration range of about 0.04 to 0.4%.
  • the acidity of the cooled slurry 40 in the processing vessel is adjusted to a pH range between 2.2 and 6.8, and in general practice, the working pH range will be between 2.5 and 5.5, with a prefe ⁇ ed embodiment being between 2.8 and 3.6. In most cases, however, the pH adjustment at this step is unnecessary because the acidity maintained during the ozone pretreatment will give a desirable pH range for leaching out the metal values in the subsequent step.
  • the recoverability of gold from carbonaceous refractory ores can be substantially improved by the acid-ozone pretreatment followed by conventional cyanidation techniques that involve filtering the oxidized slurry after the ozone treatment, adjusting the pH with lime, and leaching the metal out of the slu ⁇ y with sodium cyanide for 24 hours.
  • the ozone treatment has also considerably improved the recovery of precious metals including gold and silver from refractory ores.
  • the ore slurry is acidified to a pH level of 3.0 or below using preferably acetic acid is subjected to UV ozone treatment.
  • the pH level of the slurry is raised to pH 11.0 or higher using lime and caustic soda in order to leach out the precious metals.
  • the highly alkaline ore slu ⁇ y is then
  • the precious metals are leached out of the suitably basic slu ⁇ y using leach chemicals such as cyanide and hypochlorite.
  • the acidic leaching process of the present invention is not only highly potent for the efficient recovery of gold as shown in the following examples, but it is also effective in recovering some members of platinum group metals such platinum and palladium. I have also found that there is no noticeable decrease in the leaching efficiency even at a temperature range as low as a few degrees above the freezing point by the present acidic leaching process.
  • hypohalite ions such as those from sodium hypochlorite are good oxidizing agents, especially in acid solution, and the halite ions have the ability to function as
  • the metal complexes formed in the oxidation-reduction reaction in acid solution appear to be stable for an extended period of time.
  • sodium hypochlorite was used as a leach chemical for the extraction of gold from the slurry.
  • the clean pregnant liquid containing the chloro-auric complex was separated from the spent slurry by filtration, and the liquid was analyzed daily for gold for a period of two weeks. The results showed that the metal complex was stable for more than a week without a noticeable degree of decomposition.
  • the hypohalite ions have the tendency to undergo disproportionation reaction, resulting in the production of halite ions as:
  • hypohalite ions will considerably lose the oxidizing power as well as the ability to complex with the precious metals.
  • the recovery of gold and other precious metals from the resulting pregnant liquid is made by performing a liquid/solid separation 52 to form a residue 56 and a pregnant leach solution 60 which is then subjected to precious metal recovery 64 to form a precious metal product 68.
  • Precious metal recovery 64 can be performed by applying such techniques as carbon adsorption and Merrill-Crowe precipitation. It is also found that the metals can be recovered effectively in the acidic solution by precipitating them with aluminum. For instance, in one embodiment of the present invention, a series of 500 ml Erlenmeyer flasks are filled with clean pregnant liquid which has been produced from the leaching process. After adding aliquots of aluminum dust, the flasks are then magnetically agitated for 4 to 24 hours.
  • the pH of the leachate in the flasks ranges between 3.0 and 6.0.
  • the clean spent solution from each flask is sampled for a quantitative determination of soluble gold still remaining in solution.
  • This quantitative analysis is made by atomic absorption spectrometry equipped with an electro-thermal atomization system. The results show that aluminum dust is able to precipitate gold greater than 99.9% in all replicate tests.
  • Example 1 For a purpose of comparing the extractability of gold, the ore used in Example 1 was subjected to a cyanide treatment. Three replicate vessels, each charged with 100 grams of the oxide ore, were slurried with 300 ml of 0.1% sodium cyanide solution at a pH of about 11.5. The processing vessels were agitated for 24 hours and the slurries were filtered. Gold values were determined in the clean leachate as well as in the tailings. The data showed that an average of 90.2% total gold was extracted by cyanidation, as compared to 94.3% extraction by the method of this invention (see Example 1). EXAMPLE 3
  • a carbonaceous ore containing 0.32°7 gold, and 3.4% by weight total carbon including 0.25% organic carbon was processed for the extraction of gold by the process of the present . invention in parallel with standard cyanide leaching technique for comparison.

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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

L'invention comporte un procédé consistant à soumettre un minerai (10) réfractaire carboné à une oxydation (32) acide afin de détruire les composés carbonés, puis à une extraction (44) par lixiviation acide des métaux précieux.
PCT/US2001/043408 2000-11-21 2001-11-21 Extraction de metaux precieux de minerais refractaires carbones WO2002042503A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2002216679A AU2002216679A1 (en) 2000-11-21 2001-11-21 Recovery of precious metals from carbonaceous refractory ores

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US25227100P 2000-11-21 2000-11-21
US60/252,271 2000-11-21

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003095687A1 (fr) * 2002-05-10 2003-11-20 Australian Nuclear Science & Technology Organisation Procede d'oxydation
WO2004059018A1 (fr) * 2002-12-31 2004-07-15 Intec Ltd Recuperation de metaux a partir de materiaux sulfures
WO2004087970A1 (fr) * 2003-04-02 2004-10-14 Shapovalov Viatcheslav Dmitrie Procede de recuperation de metaux non ferreux, rares et precieux dans des minerais robustes
CN100344775C (zh) * 2002-12-31 2007-10-24 英泰克有限公司 从硫化物原料中回收金属的方法
US20120148461A1 (en) * 2009-08-24 2012-06-14 Metal Tech Ltd. Process for multi metal separation from raw materials and system for use
WO2013044380A1 (fr) * 2011-09-27 2013-04-04 Nichromet Extraction Inc. Procédé et système permettant l'extraction de l'or avec des halogènes
US9206492B2 (en) 2014-03-12 2015-12-08 Dundee Sustainable Technologies Inc. Closed loop method for gold and silver extraction by halogens
US20160032420A1 (en) * 2013-02-11 2016-02-04 Richard Neylon Methods for treating carbon materials including carbonaceous ores
CN113430393A (zh) * 2021-06-25 2021-09-24 甘肃省地质矿产勘查开发局第三地质矿产勘查院 一种环保浸金剂及其制备方法和应用
US11136681B2 (en) * 2015-06-24 2021-10-05 Greene Lyon Group, Inc. Selective removal of noble metals using acidic fluids, including fluids containing nitrate ions
US11193214B2 (en) 2013-12-20 2021-12-07 Greene Lyon Group, Inc. Method and apparatus for recovery of noble metals, including recovery of noble metals from plated and/or filled scrap

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4979986A (en) * 1988-02-22 1990-12-25 Newmont Gold Company And Outomec U.S.A., Inc. Rapid oxidation process of carbonaceous and pyritic gold-bearing ores by chlorination
CS669690A3 (en) * 1990-12-27 1992-07-15 Vyzk Ustav Chem Tech Process for dissolving a waste sludges from deactivated catalyst used inthe palladium regeneration process
US5147617A (en) * 1991-05-21 1992-09-15 Freeport-Mcmoran Inc. Process for recovery of gold from gold ores using a complexing pretreatment and sulfurous acid leaching
US5169503A (en) * 1988-06-24 1992-12-08 Baughman David R Process for extracting metal values from ores
JPH06136465A (ja) * 1992-10-26 1994-05-17 Nissan Motor Co Ltd 使用済み触媒からの白金族金属回収方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4979986A (en) * 1988-02-22 1990-12-25 Newmont Gold Company And Outomec U.S.A., Inc. Rapid oxidation process of carbonaceous and pyritic gold-bearing ores by chlorination
US5169503A (en) * 1988-06-24 1992-12-08 Baughman David R Process for extracting metal values from ores
CS669690A3 (en) * 1990-12-27 1992-07-15 Vyzk Ustav Chem Tech Process for dissolving a waste sludges from deactivated catalyst used inthe palladium regeneration process
US5147617A (en) * 1991-05-21 1992-09-15 Freeport-Mcmoran Inc. Process for recovery of gold from gold ores using a complexing pretreatment and sulfurous acid leaching
JPH06136465A (ja) * 1992-10-26 1994-05-17 Nissan Motor Co Ltd 使用済み触媒からの白金族金属回収方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Derwent World Patents Index; AN 1993-000460 *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003095687A1 (fr) * 2002-05-10 2003-11-20 Australian Nuclear Science & Technology Organisation Procede d'oxydation
WO2004059018A1 (fr) * 2002-12-31 2004-07-15 Intec Ltd Recuperation de metaux a partir de materiaux sulfures
CN100344775C (zh) * 2002-12-31 2007-10-24 英泰克有限公司 从硫化物原料中回收金属的方法
US7858056B2 (en) 2002-12-31 2010-12-28 Intec, Ltd. Recovering metals from sulfidic materials
WO2004087970A1 (fr) * 2003-04-02 2004-10-14 Shapovalov Viatcheslav Dmitrie Procede de recuperation de metaux non ferreux, rares et precieux dans des minerais robustes
GB2414740A (en) * 2003-04-02 2005-12-07 Viatcheslav Dmitrie Shapovalov Method for recovery of nonferrous, rare and precious metals from robust minerals
GB2414740B (en) * 2003-04-02 2006-07-19 Viatcheslav Dmitrie Shapovalov Method for recovery of nonferrous, rare and precious metals from robust minerals
US20120148461A1 (en) * 2009-08-24 2012-06-14 Metal Tech Ltd. Process for multi metal separation from raw materials and system for use
WO2013044380A1 (fr) * 2011-09-27 2013-04-04 Nichromet Extraction Inc. Procédé et système permettant l'extraction de l'or avec des halogènes
US9051626B2 (en) 2011-09-27 2015-06-09 Dundee, Technologies Durables Inc. Method and a system for gold extraction with halogens
US20160032420A1 (en) * 2013-02-11 2016-02-04 Richard Neylon Methods for treating carbon materials including carbonaceous ores
US11193214B2 (en) 2013-12-20 2021-12-07 Greene Lyon Group, Inc. Method and apparatus for recovery of noble metals, including recovery of noble metals from plated and/or filled scrap
US9206492B2 (en) 2014-03-12 2015-12-08 Dundee Sustainable Technologies Inc. Closed loop method for gold and silver extraction by halogens
US11136681B2 (en) * 2015-06-24 2021-10-05 Greene Lyon Group, Inc. Selective removal of noble metals using acidic fluids, including fluids containing nitrate ions
US11566334B2 (en) 2015-06-24 2023-01-31 Greene Lyon Group, Inc. Selective removal of noble metals using acidic fluids, including fluids containing nitrate ions
CN113430393A (zh) * 2021-06-25 2021-09-24 甘肃省地质矿产勘查开发局第三地质矿产勘查院 一种环保浸金剂及其制备方法和应用

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