EP0119685B1 - Procédé hydrométallurgique pour traiter des arsénopyrites - Google Patents
Procédé hydrométallurgique pour traiter des arsénopyrites Download PDFInfo
- Publication number
- EP0119685B1 EP0119685B1 EP84300292A EP84300292A EP0119685B1 EP 0119685 B1 EP0119685 B1 EP 0119685B1 EP 84300292 A EP84300292 A EP 84300292A EP 84300292 A EP84300292 A EP 84300292A EP 0119685 B1 EP0119685 B1 EP 0119685B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- concentrate
- species
- solution
- oxidized
- arsenic
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired
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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
- C22B11/06—Chloridising
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/08—Obtaining noble metals by cyaniding
Definitions
- This invention is directed to a novel environmentally amicable hydrometallurgical process for the recovery of gold from arsenical pyrite concentrate.
- the mineral arsenopyrite is known to contain gold which is in solution in the mineral matrix or is present as fine inclusions. This gold is not available for extraction by hydrometallurgical processes which treat only the mineral surfaces, for example, cyanidation.
- the mineral pyrite is often associated with arsenopyrite and may contain in its matrix finely dispersed gold which is difficult to extract.
- Arsenopyrite and pyrite are the main constituents of arsenical pyrite concentrates.
- the conventional means of liberating gold from arsenical pyrite concentrates is to roast the material and then treat the calcine by cyanidation. This process generates environmental pollution problems due to the airborne emission of sulphur and arsenic oxides.
- the tailings from the calcine cyanidation contain arsenic which is also a potential environmental contaminant.
- Arsenical pyrite concentrates may also be treated for gold recovery through conventional pyrometallurgical processes which include copper smelting, lead smelting and zinc roasting. These processes also produce potentially harmful airborne arsenic emissions from the treatment of these concentrates. Problems associated with the added arsenic burden in the process flows also arise.
- U.S. 3,793,429 discloses a nitric acid leaching process for extracting gold, iron and copper sulphide ores.
- U.S. 2,805,936 discloses a hydrometallurgical process for the recovery of valuable metals as Cu, Ni, Co, As, Au or the like from an arsenical sulphide concentrate, said process comprising the steps:
- An object of the present invention is to provide an environmentally amicable process for decomposing gold-bearing arsenical pyrite concentrates.
- the invention is characterised in that the arsenical sulphide concentrate is arsenical pyrite concentrate containing gold, the acidity of said acidic solution is sufficient to cause arsenic in said concentrate to be oxidized to the +5 oxidation state and to cause nitrogen of said oxidized nitrogen species to be reduced essentially to nitric oxide, gold is extracted from a solid residue formed in step a), arsenic in the precipitated arsenic species of step b) is in the +5 oxidation state and the liquid fraction treated in step b) is separated from the precipitated arsenic species and re-used in step a).
- step a) iron in said concentrate is oxidized to the +3 oxidation state and sulphide in said concentrate is oxidized to sulphate.
- said solid residue formed in step a) is separated from said acidic solution before said dissolved arsenic species is precipitated in step b).
- Arsenopyrite and pyrite are decomposed in acid solutions where the pH is less than 2 by the action of oxidized nitrogen species where the nitrogen has an oxidation state of +3 or greater. These species include nitric acid, nitrous acid and nitrogen dioxide.
- the main products from the decomposition are soluble ferric iron species, soluble arsenate species, soluble sulphate species, elemental sulphur and nitric oxide, as well as nitrogen dioxide.
- Nitrogen dioxide becomes increasingly abundant as a product in the gas phase as the nitric acid concentration increases: see Canadian Patent No. 995,468, Paul B. Queneau et al., August 24, 1976.
- the minor products are arsenic trioxide and nitrous acid.
- the gold contained in the concentrate remains in the solid residue which is composed of elemental sulphur and insoluble gangue minerals. Any silver present in the concentrate would also report to the residue.
- Figure 1 illustrates arsenic concentration as a function of time for three similar experiments with solution composition as a variable.
- the gold in the decomposition residue may be readily extracted by conventional techniques such as cyanidation, following leaching of the residue with sodium hydroxide to dissolve sulfur prior to cyanidation, or treatment with oxidizing chloride lixiviants, such as aqua regia. Silver may also be extracted by these techniques.
- the decomposition solution does not contain significant quantities of species which complex gold, for example, chloride ions. These would put the gold into solution and a separate additional process step would have to be included to extract it.
- the active nitrogen oxides are required only to decompose the minerals in the concentrate.
- the oxidizing nitrogen species should be present in sufficient concentration in the solution to provide an adequate rate of dissolution. Any suitable acid may be used to form the soluble ferric iron species. An adequate rate of dissolution is about 10 to 30 minutes.
- nitrogen dioxide is the decomposition agent for arsenopyrite with sulphuric acid present.
- the sulphuric acid is formed from the decomposition of pyrite.
- the active nitrogen oxides are reduced to nitric oxide which may then be regenerated by an oxidant.
- a useful oxidant is oxygen which reacts with nitric oxide in the presence of water to form nitrogen dioxide, nitrous acid and nitric acid as shown in the reactions set forth below.
- the regeneration of nitric oxide to the higher valence states may be done concurrently with the decomposition or as a separate operation.
- Nitrous oxide is formed by the decomposition of nitric oxide according to the side reaction shown below.
- the active nitrogen oxides can be regenerated during the decomposition step, the quantity of these oxides present at any time may be quite small.
- the criterion is that there must be sufficient acid present in solution to form the soluble ferric iron species. It must be emphasized that it is the oxidized nitrogen species rather than oxygen that are the active decomposition agent. The presence of oxidized nitrogen species with sulphuric acid differentiates the decomposition step described above from the Calera process.
- Figure 1 shows the arsenic concentration as a function of time for three similar experiments in which the only variable is the composition of the solution.
- the three compositions are 3 M acid as HN0 3 ; 2.5 M acid as H 2 SO 4 ; 0.5 M acid as HN0 3 ; and 3.0 M acid as H 2 SO 4 .
- the other conditions are given on Figure 1. It is apparent from the data that the presence of nitric acid greatly speeds the rate of reaction.
- the decomposition and regeneration steps are both exothermic.
- a solution which is three molar in nitric acid is reacted with fine arsenical pyrite concentrate at 15% solids without oxygen present for regeneration
- the temperature increase of the slurry is 40°C.
- oxygen present for generation the temperature increases is 130°C. Since the rates of the decomposition and regeneration reactions increase with temperature the overall reactions appear to accelerate as they proceed. It is possible that controlled cooling may be required to prevent the melting of elemental sulphur and to prevent the precipitation of salts.
- the decomposition step proceeds at any temperature above ambient. However, on a practical basis, the reaction is preferably carried out at temperatures of between 80° and 120°C. It is desirable that sufficient acid be present to form the soluble ferric iron species. Without this acid, compounds will precipitate from solution. If oxygen is used for regeneration, any oxygen pressure above ambient is adequate. Agitation increases the speed of the reactions and improves the quality of the final sulphur-bearing residue.
- the decomposition leach can be carried out over a wide range of solid-liquid ratios. Increasing the ratio of solids to liquids provides economic benefits, but the upper limit of this ratio is reached when the solubility limit of dissolved species is reached.
- the soluble arsenic, iron and sulphur must be removed from solution.
- Arsenic in the pentavalent state as ferric arsenate can be removed from solution with ferric iron.
- the following reaction shows the formation of ferric arsenate from ferric nitrate and arsenate.
- Ferric arsenate is produced virtually quantitatively from an equimolar solution of ferric nitrate and arsenic acid at all temperatures above ambient.
- the rate of precipitation can be controlled by temperature. At room temperature, complete precipitation requires several months; at 100°C precipitation requires one to two hours; and at 200°C precipitation occurs in less than one hour.
- Ferric arsenate can be precipitated rapidly at low temperatures by the neutralization of the acid in the solution. At 25°C the solubility of ferric arsenate between pH 3 and pH 7 is very low. The solids produced at low temperature tend to be colloidal and difficult to filter. The solids can contain ferric hydroxide which also tends to be colloidal,
- a calcium-bearing neutralizing agent such as calcium oxide or calcium carbonate, can be used to neutralize excess acid in solution and to remove sulphate in order to improve ferric arsenate precipitation.
- arsenic trioxide can precipitate when the filtered decomposition solution is cooled.
- arsenate or ferric compounds may be added to the solution.
- Sulphate is removed from solution by the addition of calcium-bearing materials to form calcium sulphate.
- the reaction between calcium carbonate and sulphuric acid is as follows.
- Gypsum CaS0 4 - 2H 2 0
- Gypsum has a low solubility which is virtually unaffected by temperature.
- the solubility ofCaS04 - 2H 2 0 is approximately 0.1 M.
- Anhydrite (CaS0 4 ) forms at temperatures above 60°C (although the crossover point from gypsum may be as high as 110°C due to supersaturation).
- the solubility of anhydrite drops rapidly with temperature. Solubility data for anhydrite in water gives a solubility of 0.02 M at 60°C and .0015 M at 160°C.
- Ferric iron can be removed from solution by the formation of insoluble iron compounds.
- ferric hydroxide Fe(OH) 3
- Fe(OH) 3 ferric hydroxide
- This material may be undesirable as it is colloidal and very difficult to filter.
- the temperature is raised to 100°C, the precipitate is transformed to goethite, a more crystalline ferric iron compound; and as the temperature is raised further to 130°C, hematite (Fe 2 0 3 ) is produced.
- the exact nature of the precipitate is dependent on neutralization history and the duration at temperature.
- a residual iron concentration of 5 g/I can be achieved in the presence of 60 g/I H 2 SO 4 at 150°C. At 200°C, the same residual can be achieved in the presence of 90 g/I H 2 SO 4 .
- hydronium jarosite (H 3 0)Fe 3 (SO Q ) 2 (OH) 6 ) and fibroferrite (Fe(OH)(S0 4 )) are expected to form.
- Hydronium jarosite is the most significant below 150°C.
- Fibroferrite is most significant above 150°C.
- jarosite may be formed by the addition of alkali salts where the alkali metal or radical is NH 4 , Na, K, Ag or Pb. Jarosites are typically formed at 90 to 150°C at a pH of 1.0 to 1.5.
- ferric-sulphate compounds precipitated is difficult to specify as many different species are possible and the factors which govern their formation are complex.
- trace elements such as bismuth or tellurium may be present in the concentrate being treated. While some of these trace elements will report to the leach residue or waste precipitation residues, some may build up in solution and have to be bled-off. When trace elements are present in sufficient concentration, their recovery may be warranted.
- Another possible process for a concentrate that is primarily arsenopyrite is a decomposition step with recycled nitric acid solution containing soluble calcium, using oxygen for regeneration. After leaching, the solution is cooled to precipitate calcium sulphate and a solid-liquid separation is made. The liquid is heated to precipitate ferric arsenate and another solid-liquid separation is made to give a solution to which calcium carbonate is added before reuse.
- one possible process is a decomposition step with a recycled solution, nitric oxide gas and oxygen being used for regeneration. This is followed by another decomposition step without oxygen to convert all the nitrogen oxides to nitric oxide, which is bled off.
- a solid-liquid separation produces a residue for gold treatment. Calcium carbonate is added to the liquid which is then heated to a high temperature to precipitate ferric arsenate, calcium sulphate and hematite. Another solids-liquid separation provides liquid for decomposition.
- the decomposition was rapid and complete.
- Example 2 A test was conducted to demonstrate the decomposition of a pyrite-rich concentrate (as in Example 2) using a ferric nitrate and sulphuric acid solution. This example simulates a decomposition using the product solution from Example 6.
- Example 1 A test was performed to demonstrate the decomposition of an arsenopyrite concentrate (as in Example 1) using nitric oxide gas. Oxygen was added to regenerate the active nitrogen oxides. The nitric oxide gas was produced by the reaction of arsenopyrite with nitric acid as in Example 1.
- a pyrite-rich concentrate can be reacted in a similar manner.
- the decomposition step was the same as for Example 2 using a nitric acid solution and oxygen for regeneration.
- the decomposition step was carried out with a nitric acid and calcium nitrate solution. After decomposition, the slurry was cooled to reduce the solubility of calcium sulphate.
- the decomposition step was as Example 6 using nitric acid solution and oxygen for regeneration.
- a second decomposition step was conducted as in Example 7 using the filtrate from above. Oxygen was not used.
- the solution from the precipitation stage could be reused by the addition of nitrogen oxides, for example, the addition of nitric acid or the addition of nitric oxide and oxygen.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Claims (22)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US45884683A | 1983-01-18 | 1983-01-18 | |
US458846 | 1983-01-18 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0119685A1 EP0119685A1 (fr) | 1984-09-26 |
EP0119685B1 true EP0119685B1 (fr) | 1988-08-03 |
Family
ID=23822319
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP84300292A Expired EP0119685B1 (fr) | 1983-01-18 | 1984-01-18 | Procédé hydrométallurgique pour traiter des arsénopyrites |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP0119685B1 (fr) |
AU (1) | AU566135B2 (fr) |
CA (1) | CA1219132A (fr) |
DE (1) | DE3473163D1 (fr) |
ZA (1) | ZA84153B (fr) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7915474B2 (en) | 2009-04-01 | 2011-03-29 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US7951988B2 (en) | 2009-04-01 | 2011-05-31 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8115047B2 (en) | 2009-04-01 | 2012-02-14 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8168847B2 (en) | 2009-04-01 | 2012-05-01 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8481800B2 (en) | 2009-04-01 | 2013-07-09 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
RU2657254C1 (ru) * | 2017-07-21 | 2018-06-09 | Федеральное государственное унитарное предприятие "Горно-химический комбинат" (ФГУП "ГХК") | Способ извлечения золота из упорных серебросодержащих сульфидных руд концентратов и вторичного сырья |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3534224A1 (de) * | 1985-09-23 | 1987-04-02 | Gock Eberhard Priv Doz Prof Dr | Verfahren zur nasschemischen gewinnung von edelmetallen aus kohlenstoffhaltigen arsenopyritkonzentraten |
AU582961B2 (en) * | 1986-05-29 | 1989-04-13 | Sasox Processing Pty Ltd | Improved hydrometallurgical arsenopyriteprocess |
EP0272060A3 (fr) * | 1986-12-18 | 1990-08-01 | Electrolytic Zinc Company Of Australasia Limited | Récupération hydrométallurgique de métaux et de soufre élémentaire à partir de sulfures métalliques |
ZA928157B (en) * | 1991-10-25 | 1993-06-09 | Sasox Processing Pty Ltd | Extraction or recovery of metal values. |
AU650802B2 (en) * | 1991-10-25 | 1994-06-30 | Sasox Processing Pty. Limited | Extraction or recovery of metal values |
AU670670B2 (en) * | 1993-01-27 | 1996-07-25 | R & O Mining Processing Ltd. | Hydrometallurgical recovery of metals from complex ores |
CN1045625C (zh) * | 1994-08-15 | 1999-10-13 | R&O矿业加工有限公司 | 含硫化锌的矿石和精矿中的硫化锌变成硫酸锌的湿法冶炼 |
RU2114196C1 (ru) * | 1995-09-19 | 1998-06-27 | Клиблей Генри Хадыевич | Способ гидрометаллургического извлечения редких металлов из технологически упорного сырья |
US9272936B2 (en) | 2009-04-01 | 2016-03-01 | Earth Renewal Group, Llc | Waste treatment process |
CN104263963B (zh) * | 2014-09-23 | 2016-08-24 | 铜仁市万山区盛和矿业有限责任公司 | 一种从硫砷铁矿中提取金的方法 |
CN104263961B (zh) * | 2014-09-23 | 2016-03-30 | 铜仁市万山区盛和矿业有限责任公司 | 一种从黄铁矿中提取金的方法 |
CN104263962B (zh) * | 2014-09-23 | 2016-08-17 | 铜仁市万山区盛和矿业有限责任公司 | 一种从磁黄铁矿中提取金的方法 |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE744120C (de) * | 1938-01-25 | 1944-01-10 | Dr Aurel Bognar | Verfahren zur Verarbeitung von Erzen oder sonstigen Bergwerks- und Huettenerzeugnissen |
FR1058809A (fr) * | 1951-01-19 | 1954-03-19 | Chemical Construction Corp | Perfectionnements à la récupération de la teneur en métaux precieux des mineraiscontenant de l'arsenic et de leurs concentrats |
US2805936A (en) * | 1954-08-16 | 1957-09-10 | Felix A Schaufelberger | Leaching of arsenide ores |
US2805940A (en) * | 1954-08-20 | 1957-09-10 | Bennedsen Hans Oluf | Process for extracting cobalt and nickel from their ores |
US2951741A (en) * | 1955-08-05 | 1960-09-06 | Metallurg Resources Inc | Process for treating complex ores |
US3793429A (en) * | 1972-02-18 | 1974-02-19 | Kennecott Copper Corp | Nitric acid process for recovering metal values from sulfide ore materials containing iron sulfides |
-
1983
- 1983-12-20 CA CA000443728A patent/CA1219132A/fr not_active Expired
-
1984
- 1984-01-09 ZA ZA84153A patent/ZA84153B/xx unknown
- 1984-01-16 AU AU23515/84A patent/AU566135B2/en not_active Ceased
- 1984-01-18 EP EP84300292A patent/EP0119685B1/fr not_active Expired
- 1984-01-18 DE DE8484300292T patent/DE3473163D1/de not_active Expired
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7915474B2 (en) | 2009-04-01 | 2011-03-29 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US7951988B2 (en) | 2009-04-01 | 2011-05-31 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8115047B2 (en) | 2009-04-01 | 2012-02-14 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8168847B2 (en) | 2009-04-01 | 2012-05-01 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
US8481800B2 (en) | 2009-04-01 | 2013-07-09 | Earth Renewal Group, Llc | Aqueous phase oxidation process |
RU2657254C1 (ru) * | 2017-07-21 | 2018-06-09 | Федеральное государственное унитарное предприятие "Горно-химический комбинат" (ФГУП "ГХК") | Способ извлечения золота из упорных серебросодержащих сульфидных руд концентратов и вторичного сырья |
Also Published As
Publication number | Publication date |
---|---|
EP0119685A1 (fr) | 1984-09-26 |
DE3473163D1 (en) | 1988-09-08 |
CA1219132A (fr) | 1987-03-17 |
AU2351584A (en) | 1984-07-19 |
ZA84153B (en) | 1985-04-24 |
AU566135B2 (en) | 1987-10-08 |
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