US20060182674A1 - Reduction of copper content in the molybdenite concentrate - Google Patents

Reduction of copper content in the molybdenite concentrate Download PDF

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Publication number
US20060182674A1
US20060182674A1 US11/331,406 US33140606A US2006182674A1 US 20060182674 A1 US20060182674 A1 US 20060182674A1 US 33140606 A US33140606 A US 33140606A US 2006182674 A1 US2006182674 A1 US 2006182674A1
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Prior art keywords
copper
leaching
molybdenite
leaching solution
solution
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US11/331,406
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English (en)
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Javier Jara
Sylvester Zuttah
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Application filed by Individual filed Critical Individual
Priority to US11/331,406 priority Critical patent/US20060182674A1/en
Priority to PCT/IB2006/000116 priority patent/WO2006082484A2/fr
Publication of US20060182674A1 publication Critical patent/US20060182674A1/en
Priority to US12/643,541 priority patent/US7794677B2/en
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    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/34—Obtaining molybdenum
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
    • 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
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • 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

  • Embodiments of the present invention generally relate to a method for mineral purification and more particularly to a method of removing metal sulfides from a molybdenite concentrate.
  • Copper ore deposits containing copper sulfide minerals may contain minor amounts of molybdenite (MoS 2 ). Recovery of the valuable molybdenite locked up in the ore is usually performed by a milling operation, followed by several flotation steps. The final molybdenite concentrate usually contains some sulfide minerals, and, to be commercial, the copper sulfide mineral content is typically reduced through a leaching step in which the copper sulfide minerals are dissolved by a leaching solution.
  • the leaching step is typically performed in a batch operation where the molybdenite concentrate is exposed to the leaching solution in a leaching vessel. After the leaching process, the leaching solution is separated from the molybdenite and is regenerated using chlorine gas. Due to the hazardous nature of the chlorine gas a batch operation with several safety procedures is required during the regenerating process, resulting in high labor, handling, and safety costs.
  • the batch operation using chlorine gas is suited to produce small amounts of material.
  • a continuous mode is normally more economical.
  • leaching can be performed uninterrupted because the leaching solution is replenished as it is being used.
  • more molybdenite concentrate can be leached in the same amount of time it takes for leaching in a batch mode operation.
  • the embodiments of the present invention generally provide a method for removing copper minerals from a molybdenite concentrate.
  • One embodiment of the invention provides a method for removing copper sulfides from a molybdenite concentrate by leaching the copper sulfides from the molybdenite concentrate with a leaching solution comprising ferric chloride, removing molybdenite from the leaching solution, introducing an acid into the leaching solution and introducing O 2 , O 3 , or a combination of both, into the leaching solution.
  • Another embodiment of the invention provides for obtaining commercial grade molybdenite from a copper ore.
  • the method includes separating a molybdenite concentrate from the copper ore, leaching copper from the molybdenite concentrate with a leaching solution comprising ferric chloride, removing molybdenite from the leaching solution, introducing an acid into the leaching solution and introducing O 2 , O 3 , or a combination of both, into the leaching solution.
  • An exemplary method includes pumping molybdenite concentrate into an autoclave vessel, introducing a solution of Fe(II) ions, Fe(III) ions, or a combination of both, into the autoclave vessel, introducing an acid into the autoclave vessel, introducing O 2 , O 3 or a combination of both, into the autoclave vessel, and filtering the molybdenite from a stream exiting the autoclave vessel.
  • the invention further provides a method for regenerating ferric chloride in a leaching solution.
  • An exemplary method includes adding a leaching solution comprising Fe(II) ions, Fe(III) ions, or a combination of both, to a mixture of mineral sulfides, and introducing an acid and O 2 , O 3 or a combination of both, into the leaching solution.
  • FIG. 1 is a block diagram for the process of reducing copper content in a molybdenite concentrate at atmospheric pressure.
  • FIG. 2 is a block diagram for the process of reducing copper content in a molybdenite concentrate under pressure.
  • FIG. 1 is a block diagram of a system 100 for carrying out a first process, according to one embodiment of the invention.
  • the system 100 includes introducing a molybdenite concentrate into a dissolution vessel 110 .
  • the molybdenite concentrate may be stored in a storage tank 120 , and typically includes 3-4% w/w copper sulfide minerals, such as, chalcopyrite, chalcocite, bornite, etc.
  • the dissolution vessel 110 is made from a material which will not 35 dissolve or etch in the conditions used during the dissolution process. In one embodiment, the material is glass.
  • a solution of hydrochloric acid is introduced into the dissolution vessel through inlet 140 .
  • the concentration of hydrochloric acid is kept between about 0.7 M and about 4.0 M, and more preferably at about 4.0 M, throughout the dissolution process.
  • a stream comprising ferrous chloride, ferric chloride, or a combination of the two is introduced to the dissolution vessel through inlet 190 .
  • Oxygen, ozone, or a combination of the two is introduced through inlet 130 into the slurry of the dissolution vessel so that gas bubbles are formed in the slurry and solution.
  • the dissolution vessel is kept at temperatures above about 90° C., and more preferably between about 100° C. and about 120° C.
  • the slurry is agitated by stirring methods, such as mechanical agitators which may include a motor, a shaft and an impeller.
  • the leach process is completed after about 10 minutes to about 120 minutes.
  • a stream of the slurry, which has been leached, is then filtered at filter 150 and the filter cake is rinsed with hot water.
  • the water used to rinse the slurry is heated to between about 60° C. and about 100° C., and preferably to about 60° C.
  • the water used for rinsing may also be acidic.
  • the solid separated from the filtrate is dried to a moisture content of less than about 5% w/w and contains molybdenite with a copper content of less than about 0.2% w/w.
  • the filtrate contains a higher concentration of iron ions than may be desirable, and thus the filtrate may then go through an optional iron removal process 170 to keep the iron ion concentration around 100 g/L.
  • One way to remove excess iron ions is by reducing the temperature of the filtrate which will decrease the solubility of the iron ions causing precipitation of excess iron chlorides.
  • the filtrate is then heated in preheater 180 , and reintroduced into the dissolution vessel 110 through inlet 190 .
  • FIG. 1 describes the continuous process at atmospheric pressure.
  • An alternative embodiment of FIG. 1 is a batch process.
  • oxygen, ozone, or a combination of the two, and hydrochloric acid are added to a predetermined volume of acid solution containing ferrous chloride, ferric chloride, or a combination of the two, in dissolution vessel 110 .
  • a desired level between about 20 g/L and 100 g/L
  • molybdenite concentrate is added to vessel 110 .
  • only hydrochloric acid is added to vessel 110 in order to maintain an acidity between 1 to 4 M, while ferric chloride concentration decreases with time due to production of ferrous chloride.
  • the O 2 /O 3 and hydrochloric acid are added to the stream of ferrous chloride, ferric chloride, or a combination of the two, prior to entering the dissolution vessel 110 .
  • FIG. 2 is a block diagram of a system 200 for carrying out a second process at pressures higher than atmospheric pressure, according to another embodiment of the invention.
  • System 200 includes many of the same steps as system 100 , and identical elements are numbered as they are in FIG. 1 .
  • Molybdenite concentrate in the form of an aqueous slurry is introduced from the storage tank 120 through a high pressure pump 205 into an autoclave 210 .
  • Oxygen, ozone, or a combination of the two, hydrochloric acid, and a solution of ferrous chloride, ferric chloride, or a combination of the two, are introduced into the autoclave 210 through inlets 130 , 140 , and 190 , respectively, as in system 100 .
  • autoclave 210 The conditions in autoclave 210 are similar to the conditions of dissolution vessel 110 of system 100 . However, in system 200 , oxygen, ozone, or a combination of the two, is introduced into autoclave 210 to elevate the pressure in the autoclave. The internal pressure of the autoclave is elevated to about 7 bar gauge compared to atmospheric pressure; however, other pressures are also contemplated, such as 20 to 30 bar. Additionally, autoclave 210 has an outlet 215 for the controlled removal of excess gas. A stream of the slurry which has been leached is then discharged into flash vessel 220 where the pressure of the slurry is reduced to atmospheric pressure, and part of the water evaporates as steam. The steam may be used to heat pre heater 280 .
  • the slurry and solution, at atmospheric pressure and about 50° C., are then filtered by filter 150 .
  • the solid separated from the solution is dried to a moisture content of less than about 5% w/w and contains molybdenite with a copper content of less than about 0.2% w/w.
  • the filtrate comprising ferrous chloride, ferric chloride, or a combination of both, acid, and cupric chloride then go through a copper removal process 160 where copper is precipitated out of solution.
  • the decopperized solution may then go through the optional iron removal process 170 before the solution is heated in pre heater 280 .
  • the filtration is then reintroduced into the autoclave vessel 210 through inlet 190 .
  • An alternative embodiment of the process of FIG. 2 is a batch process wherein oxygen, ozone, or a combination of the two, and hydrochloric acid are added to a predetermined volume of acid solution containing ferrous chloride, ferric chloride, or a combination of the two, in autoclave 210 .
  • a desired level between about 20 g/L and 100 g/L
  • molybdenite concentrate is added to autoclave 210 .
  • only hydrochloric acid is added to autoclave 210 in order to maintain an acidity between 1 to 4 M, while ferric chloride concentration decreases with time due to production of ferrous chloride.
  • the O 2 /O 3 and acid are added to the stream of ferrous chloride, ferric chloride, or a combination of the two, prior to entering the autoclave 210 .
  • the first and second processes carried out in the systems 100 and 200 take advantage of the fact that Fe(III) in a solution of ferric chloride (FeCl 3 ) will dissolve copper containing sulfide minerals, such as chalcopyrite and bornite.
  • ferrous chloride is oxidized to ferric chloride which can again be used to leach copper containing sulfides from the molybdenite concentrate.
  • Equations 4 and 5 above represent an example of the stoichiometry that might occur, and not every stoichiometric possibility of the high acid concentration reactions.
  • Agitation is provided by either a mechanical agitator which includes a motor, a shaft and an impeller providing agitation at 600 rmp, or a magnetic stirrer which creates a lower level of agitation than the mechanical agitator. It can be seen that upon increase in oxygen flow, the oxidation rate also increases, even if the level of agitation is significantly reduced as when agitation is performed by a magnetic stirrer.
  • the oxidation rates in the range of 28 to 69 g/L/h observed using oxygen and hydrochloric acid are significantly higher than the oxidation rates obtained using chlorine gas which are typically about 15 g/L/h.
  • the oxidation rate of Fe(II) to Fe(III) is increased when the oxygen pressure in the reaction vessel is increased.
  • the effect of oxygen pressure on the oxidation rate is presented in Table 2.
  • an oxygen pressure regulator is fixed to maintain an oxygen pressure of about 7 bar.
  • the reaction vessel has a small opening at the exit valve in order to release excess pressure. Attached to the exit valve is a wet meter which measures the exhaust gas flow as the gas exits the reaction vessel. The exhaust gas flow measured is not uniform, indicating that the oxygen is introduced to the reaction vessel in pulses.
  • Table 2 it can be seen that the oxidation rate increases three to four times when the operating pressure is 7 bar gauge compared to atmospheric pressure, while the gas consumption is three to four times lower.
  • the iron oxidation rate as a function of molar concentration of hydrochloric acid using ozone or oxygen is presented in Table 3.
  • the iron oxidation rates increase with increased HCl concentration, meaning that the gas is a more efficient oxidizer at higher HCl concentrations.
  • the presence of copper increases the oxidation rate by 33%, indicating that the presence of copper is a catalyst for iron oxidation.
  • the odidation potential of ozone gas is higher than the oxidation potential of oxygen gas, and as seen in Table 3, the oxidation rate of iron is higher when using ozone gas instead of oxygen gas under the same conditions.
  • the effectiveness of leaching copper from a molybdenite concentrate using ferric chloride is tested in several experiments using solutions of ferric chloride.
  • the leaching is performed on a disk filter cake sample containing 3.2% w/w Cu, 1.7% w/w Fe, and 49.2% w/w Mo which is fed to the copper leaching reactors.
  • a ferric chloride solution is added to the leaching reactor.
  • the ferric chloride solution is prepared by oxidizing ferrous chloride to ferric chloride in the presence of oxygen.
  • the molybdenite concentrate is agitated in the ferric chloride solution at atmospheric pressure and at 100° C. No oxygen is injected during these leaching tests.
  • Table 4 shows the experimental conditions and results for several leaching times followed by filtration at 60° C.
  • the residue left after leaching for 15 minutes has a copper content of 0.2% w/w after filtration, and the copper content continues to decrease to 0.05% w/w as the leaching time increases.
  • the mass ratio of consumed ferric chloride to initial concentrate is almost constant at about 0.08 for solid concentrations of 40% w/w.
  • the mass ratio is increased to about 0.09 to about 0.12 for solid concentrations of 20% w/w.
  • the occurrence of a constant mass ratio of consumed ferric chloride to initial concentrate indicates that when the copper sulfide reaction is almost complete (when the concentration of copper is below 0.2% w/w), the consumption of ferric chloride is negligible.
  • the amount of oxygen needed will be 2.5 kg of O 2 per 1 kg of Fe, or 250 kg of O 2 per metric ton of concentrate.
  • the oxygen flow rate is 0.5 L O 2 per minute for an hour in a 0.5 L solution.
  • such a flow rate yields 328 Kg O 2 per metric ton concentrate over a period of an hour, which would provide an excess amount of O 2 to react ferrous chloride to ferric chloride.
  • the amount of HCl required to assist in the iron oxidation is based on 0.33 kg HCl per 1 kg of Fe. With 100 kg Fe present per metric ton of concentrate, the amount of HCl needed is 33 kg per metric ton concentrate introduced into the dissolution vessel over a period of 1 hour.
  • the amount of O 2 consumed is less at higher pressures than at atmospheric pressures. Additionally, the oxidation rate of Fe is higher at the higher pressures. Therefore, less O 2 gas is needed for the process to operate. At about 7 bar gauge, the consumption of O 2 is 0.22 kg per kg of Fe (Table 2). This translates to 22 kg O 2 per metric ton of concentrate over a period of 1 hour.
  • both processes can be performed in a batch operation mode and a continuous operation mode.
  • a batch operation mode is very much like the experiments described above, where the concentrate is leached for a set amount of time, then filtered and the filtrate recycled into a new batch of concentrate.
  • a continuous operation mode a constant flow of gas and HCl is added to keep the concentration of ferric chloride at a level which is efficient for continuous leaching of the molybdenite concentrate.
  • Leached molybdenite concentrate can be removed as new unleached concentrate is introduced into the dissolution vessel.
  • a stream of iron chloride solution from the dissolution vessel can be removed to undergo dedecopperization and the optional iron removal before being recycled back into the dissolution vessel. This way, leaching can continue uninterrupted for an extended period of time.

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US11/331,406 2005-02-02 2006-01-12 Reduction of copper content in the molybdenite concentrate Abandoned US20060182674A1 (en)

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US11/331,406 US20060182674A1 (en) 2005-02-02 2006-01-12 Reduction of copper content in the molybdenite concentrate
PCT/IB2006/000116 WO2006082484A2 (fr) 2005-02-02 2006-01-25 Reduction de la teneur en cuivre d'un concentre de molybdenite
US12/643,541 US7794677B2 (en) 2005-02-02 2009-12-21 Reduction of copper content in the molybdenite concentrate

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US11/331,406 US20060182674A1 (en) 2005-02-02 2006-01-12 Reduction of copper content in the molybdenite concentrate

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011024164A1 (fr) * 2009-08-24 2011-03-03 Metal Tech Ltd. Procédé pour la séparation de multiples métaux issus de matières premières et système de mise en œuvre du procédé
JP2016191118A (ja) * 2015-03-31 2016-11-10 Ｊｘ金属株式会社 モリブデン精鉱からのレニウムの回収方法
JP2016191117A (ja) * 2015-03-31 2016-11-10 Ｊｘ金属株式会社 モリブデン精鉱からのモリブデンの回収方法
CN114908252A (zh) * 2022-05-12 2022-08-16 中南大学 一种硫化矿的浸出方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015199098A1 (fr) * 2014-06-25 2015-12-30 Jx日鉱日石金属株式会社 Procédé de traitement de minerai de molybdène contenant du cuivre
JP6196209B2 (ja) * 2014-12-10 2017-09-13 Ｊｘ金属株式会社 含銅モリブデン鉱の処理方法
CN105063351B (zh) * 2015-09-22 2017-10-27 北京矿冶研究总院 一种从复杂钼精矿中选择性分离铜铼的方法

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US3252787A (en) * 1963-06-11 1966-05-24 Oceanic Process Corp Process for producing titanium dioxide concentrate and other useful products from ilmenite and similar ores
US3560201A (en) * 1966-07-11 1971-02-02 Kennecott Copper Corp Method of precipitating metal values
US3674424A (en) * 1969-05-13 1972-07-04 Brenda Mines Ltd Process for purifying molybdenite concentrates
US3714325A (en) * 1970-11-17 1973-01-30 Us Interior Recovery of molybdenite
US3798026A (en) * 1972-03-27 1974-03-19 Cominco Ltd Copper hydrometallurgy
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US6159435A (en) * 1996-05-06 2000-12-12 Atomaer Pty Ltd Leaching of mineral ores
US6596053B2 (en) * 1999-07-08 2003-07-22 Cognis Corporation Processes for the recovery of copper from aqueous solutions containing nitrate ions

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011024164A1 (fr) * 2009-08-24 2011-03-03 Metal Tech Ltd. Procédé pour la séparation de multiples métaux issus de matières premières et système de mise en œuvre du procédé
US20120148461A1 (en) * 2009-08-24 2012-06-14 Metal Tech Ltd. Process for multi metal separation from raw materials and system for use
JP2016191118A (ja) * 2015-03-31 2016-11-10 Ｊｘ金属株式会社 モリブデン精鉱からのレニウムの回収方法
JP2016191117A (ja) * 2015-03-31 2016-11-10 Ｊｘ金属株式会社 モリブデン精鉱からのモリブデンの回収方法
CN114908252A (zh) * 2022-05-12 2022-08-16 中南大学 一种硫化矿的浸出方法

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US7794677B2 (en) 2010-09-14
US20100098605A1 (en) 2010-04-22
WO2006082484A2 (fr) 2006-08-10
WO2006082484A3 (fr) 2006-10-05

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