WO2024256057A1 - Séparation de cu et de ni à partir de minerai à l'aide de h2o2 - Google Patents

Séparation de cu et de ni à partir de minerai à l'aide de h2o2 Download PDF

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Publication number
WO2024256057A1
WO2024256057A1 PCT/EP2024/059466 EP2024059466W WO2024256057A1 WO 2024256057 A1 WO2024256057 A1 WO 2024256057A1 EP 2024059466 W EP2024059466 W EP 2024059466W WO 2024256057 A1 WO2024256057 A1 WO 2024256057A1
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Prior art keywords
ore
concentrate
froth flotation
process according
flotation
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English (en)
Inventor
Mitchell LANCASTER
Alun Pryce James
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Solvay SA
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Solvay SA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/02—Froth-flotation processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/018—Mixtures of inorganic and organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/06—Depressants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; Specified applications
    • B03D2203/02—Ores

Definitions

  • the present relates to a process for extracting Ni and Cu from an ore comprising Ni and Cu and separating Ni from Cu.
  • Ni and Cu are of economic importance. Such Ni-and Cu- containing ores can be subjected to froth flotation to recover the desired mineral and discard any gangue minerals.
  • this process comprises aeration of a dispersion of the ground ore to form a froth on the surface.
  • the froth contains hydrophobic particles whereas the underflow contains hydrophilic particles.
  • the froth is then separated from the underflow to produce a purified concentrate.
  • a process for extracting Ni and Cu from an ore comprising Ni and Cu and separating Ni from Cu comprising the steps of: a) subjecting the ore to a first froth flotation to provide a first concentrate comprising Ni and Cu and a first underflow, b) subjecting the first concentrate to a second froth flotation to provide a second concentrate and a second underflow, and c) recovering Cu in the second concentrate and Ni in the second underflow, wherein the second froth flotation is conducted in the presence of H2O2.
  • the present invention further relates to the use of H2O2 for extracting Ni and Cu from an ore comprising Ni and Cu and separating Ni from Cu by froth flotation.
  • a depressant means one depressant or more than one depressant.
  • ore refers to a naturally occurring mineral from which a metal and other elements can be extracted. Metals are commonly present as oxides, aresenides, sulfides, sulfates or silicates.
  • conditioning refers to treating a ground ore with reagents, such as collectors, frothers, froth phase modifiers, dispersants, depressants, suppressants, pH regulators, and activators for a certain time period before subjecting the conditioned ore to froth flotation. Conditioning is applied to increase yield and/or ease of separation during froth flotation.
  • reagents such as collectors, frothers, froth phase modifiers, dispersants, depressants, suppressants, pH regulators, and activators for a certain time period before subjecting the conditioned ore to froth flotation. Conditioning is applied to increase yield and/or ease of separation during froth flotation.
  • froth flotation refers to a method for separating minerals from a dispersion of ground ore by applying a gas, usually air, through the dispersion to form a froth or float on the surface.
  • the float contains hydrophobic particles whereas the underflow contains hydrophilic particles.
  • the float can also synonymously be called “froth” or “concentrate” and the underflow can also synonymously be called “tails” or “tailings”.
  • the concentrate refers to material obtained after removal of gangue minerals, leaving minerals of value in the concentrate. Froth flotation can be carried out using equipment and procedures known in the art, such as a Denver, Galigher, Wemco, Outokumpo, Sala, or a Jameson cell.
  • Ni-Cu-ore refers to an ore comprising minerals containing Ni and Cu ions, e.g., in the form of nickel sulfides and cupper sulfides.
  • Such an ore may comprise as nickel containing mineral violarite, millerite, lattice substituted/doped pyrrhotite and/or pentlandite.
  • Such an ore may comprise as copper containing mineral chalcopyrite, chalcocite, and/or bornite.
  • collector refers to a compound that increases the amount of desired mineral that is formed in the froth, i.e., a compound that renders the minerals water-repellents and increase attachment of the desired mineral to the air bubbles during froth flotation.
  • Alkyl xanthate salts and dialkyl xanthogen formate are widely used collectors, in particular for Cu.
  • frother refers to a compound that increases the amount and/or stability of the froth that is formed during froth flotation.
  • frothers are surface-active compounds that commonly contain a polar group and a hydrocarbon chain.
  • Non-limiting examples of frothers include phenols, alkylaryl sulfonates, aliphatic alcohols, alkoxy paraffins, polyglycol ethers, and polyglycol ethers.
  • Different flotation reagents are disclosed in the “ Handbook of Flotation Reagents: Chemistry, Theory and Practice” , vol 2, 2007, Elsevier B.V. by S. M. Bulatovic.
  • froth phase modifier refers to a compound that controls the interaction of collectors between specific minerals. These compounds show an activating or depressing action in flotation.
  • froth phase modifier is a generic term that may encompass depressants, pH regulators and activators.
  • dispenser refers to compounds, usually polymers, that either increase the stability of the ore in the slurry or that prevent the formation of slimes during flotation.
  • depressant refers to a compound that reduces the amount of specific minerals that attach to air bubbles during froth flotation.
  • depressants selectively inhibit the interaction of a specific mineral with the collector.
  • the depressant is selective for certain minerals and not others, it is preferred that the depressant is a depressant for gangue minerals and/or a Ni depressant.
  • pH regulator refers to a compound that regulates the pH value.
  • inorganic acids such as aqueous HC1
  • inorganic bases such as lime.
  • lime can be a pH regulator and a froth phase modifier.
  • grade refers to the mass of a desired material based on the amount of ore: In case the grade is based on a concentrate, the grade refers to the mass of a desired material based on the amount of dried concentrate.
  • the present invention relates to a process for extracting Ni and Cu from an ore comprising Ni and Cu and separating Ni from Cu, the process comprising the steps of: a) subjecting the ore to a first froth flotation to provide a first concentrate comprising Ni and Cu and a first underflow, b) subjecting the first concentrate to a second froth flotation to provide a second concentrate and a second underflow, and c) recovering Cu in the second concentrate and Ni in the second underflow, wherein the second froth flotation is conducted in the presence of H2O2.
  • the term “for extracting Ni and Cu” encompasses partial extraction of Ni and Cu.
  • the term “for separating Ni from Cu” encompasses partial separation of Ni from Cu.
  • Ni and Cu do not need to be separated completely from each other and the Ni to Cu wt. -ratio in the concentrate is different than in the ore.
  • the Ni to Cu wt.-ratio in the concentrate is lower than the Ni to Cu wt.-ratio in the ore.
  • the concentrate can be enriched with Cu.
  • the Ni to Cu wt.-ratio is larger in the underflow than the Ni to Cu wt.-ratio in the ore.
  • the second froth flotation is conducted at a pH value of above 10.0, preferably at a pH value of above 12.0. It is preferred that the first froth flotation is conducted at a lower pH value than the second froth flotation. In an embodiment, the first froth flotation is conducted at a pH value of 8.0 to 13.0, preferably at a pH value of 8.5 to 10.0. It is preferred that the pH value is conducted at a uniform pH value. It is further preferred that the pH value is adjusted before the ore is conditioned.
  • the H2O2 will alter the surface structure of the Ni- containing minerals while not altering the surface structure of Cu-containing minerals, thus making the Ni-containing minerals more hydrophilic and increasing the amount of Ni-containing minerals in the underflow.
  • the ore is conditioned before the first froth flotation to provide a conditioned ore.
  • the conditioning is conducted at a pH value of 8.0 to 13.0, preferably at a pH value of 8.5 to 10.0. It is preferred that the pH value is conducted at a uniform pH value. It is further preferred that the pH value is adjusted before the ore is conditioned.
  • the pH is measured by a glass pH electrode placed into the slurry present during the process step concerned (second froth flotation and/or conditioning), most often following the grind of the ore.
  • the probe is calibrated with commercially available, certified buffer solutions.
  • a flotation reagent selected from collectors, frothers, froth phase modifiers, dispersants, depressants, suppressants, pH regulators, activators, and two or more thereof is added during the process.
  • a flotation reagent may be added before the first froth flotation and/or before the second froth flotation.
  • a froth flotation stage is conducted, comprising a conditioning step and subsequently a froth flotation step.
  • the first froth flotation may also be referred to as rougher stage and the second froth flotation may also be referred to as cleaning stage.
  • a collector selected from metal alkyl xanthates, preferably potassium amyl xanthate, phosphonic acids, phosphoric acid esters, carboxylic acids and salts thereof, metal alkyl sulfates, metal alkyl sulfonates, dialkyl or diaryl dithiophosphoric acids and salts thereof, mercaptobenzothiazole, xanthogen formates, alkyl ethoxycarbonyl thioureas, tertiary dodecyl mercaptans, and mixtures of two or more thereof is added to the ore before the first froth flotation. It is preferred that the collector is a Cu- and Ni-sulfide collector.
  • the collector comprises a metal alkyl xanthate.
  • metal preferably refers to alkali metals in this context, such as sodium and potassium.
  • metal alkyl xanthates are sodium isopropyl xanthate, potassium isopropyl xanthate, sodium ethyl xanthate, potassium ethyl xanthate, sodium isobutyl xanthate, potassium isobutyl xanthate, sodium amyl xanthate and potassium amyl xanthate. It is particularly preferred that sodium isopropyl xanthate is added as a collector during the process.
  • the second concentrate contains at least 70 %, at least 75 % Cu or at least 80 % Cu based on the amount of Cu in the ore and has a total Ni content of below 2.0 wt.-% based on the dried total weight of the float. In an embodiment, the second concentrate contains at least 80 % Cu based on the amount of Cu in the first concentrate. In a preferred embodiment, the second concentrate contains at least 85 % Cu or at least 90 % Cu based on the amount of Cu in the first concentrate. Put differently, the second concentrate has a Cu recovery of at least 85 % or at least 90 % based on the first concentrate.
  • the concentrate contains at least 8.5 g Cu.
  • the amount of Cu and Ni can preferably be determined by wavelength-dispersive XRF (x-ray fluorescence) measurements, for example measured by an Epsilon 1 benchtop XRF analyzer from Malvern Panalytical.
  • the amount of Cu and Ni can be determined by ICP- OES (inductively coupled plasma optical emission spectrometry) or SIMS (secondary ion mass spectrometry) analysis.
  • the second concentrate has a total Ni content of below 4.0 wt.-%, below 3.5 wt.-%, below 3.0 wt.-%, below 2.5 wt.-% or preferably of below 2.0 wt.-%.
  • the total Ni content also known as Ni grade, is based on the dried weight of the second concentrate.
  • the second concentrate has a total Cu content of at least 5 wt.-%, at least 10 wt.-%, or preferably of at least 12 wt.-%.
  • the total Cu content, also known as Cu grade is based on the dried weight of the second concentrate.
  • the ore comprises 0.01 to 10.0 wt.-%, 0.05 to 8.0 wt.- % or 0.1 to 5.0 wt.-% Cu. In an embodiment, the ore comprises 0.01 to 10.0 wt.- %, 0.05 to 8.0 wt.-% or 0.1 to 5.0 wt.-% Ni.
  • the second concentrate has a Cu to Ni selectivity of at least 30 % at least 35 % or at least 40 %.
  • the selectivity “S” of the second concentrate is defined as follows:
  • the type of ore is not particularly limited as long as it contains Ni and Cu. However, it is preferred that the ore comprises 0.5 wt.-% to 5.0 wt.-% Cu and 0.5 wt.-% to 3.0 wt.-% Ni, as the process is optimized for ore containing Ni and Cu in said ranges.
  • the ore comprises nickel sulfides, iron sulfides and/or copper sulfides, preferably pyrrhotite, chalcopyrite and/or pentlandite, more preferably the ore comprises pentlandite as Ni-containing mineral and chalcopyrite as Cu-containing mineral.
  • the present invention relates to a process for extracting nickel sulfide and copper sulfide from an ore comprising nickel sulfide and copper sulfide and separating the nickel sulfide from the copper sulfide, the process comprising the steps of: a) subjecting the ore to a first froth flotation to provide a first concentrate comprising sickle sulfide and copper sulfide, and a first underflow, b) subjecting the first concentrate to a second froth flotation to provide a second concentrate and a second underflow, and c) recovering copper sulfide in the second concentrate and nickel sulfide in the second underflow, wherein the second froth flotation is conducted in the presence of H2O2.
  • the H2O2 is added as a 10 wt.-% to 80 wt.-% H2O2 aqueous solution. It is preferred to use the H2O2 in concentrated aqueous solution, e.g. as 50 wt.-% aqueous solution. Such concentrated aqueous solutions may comprise stabilizers.
  • the H2O2 is used in an amount of 200 g to 2500 g H2O2 per It of the ore, preferably in an amount of 400 g to 2000 g H2O2 per It of the ore, more preferably in an amount of 800 g to 1700 g H2O2 per It of the ore. In a particularly preferred embodiment, H2O2 is used in an amount of 900 g to 1600 g H2O2 per It of the ore.
  • the ore is provided with a particle size Pso of 10 pm to 400 pm, preferably by grinding the ore before the first froth flotation.
  • a ground dispersion of the ore is also referred to as pulp.
  • the ore is provided with a particle size Pso of 100 pm to 300 pm.
  • the particle size may be determined by sieving, using a set of screens or meshes, e.g., a vibratory sieve shaker, to separate the various particles by their respective size.
  • the Pso particle size refers to a weight-based particle size distribution.
  • the particle size is determined by sieve analysis, e.g., according to ASTM C136/C136M-19.
  • Grinding can be performed by any method known in the art, such as ball or rod milling.
  • Providing the ore with the above-mentioned particle size increases the surfaces area of the ore, thus facilitating the conditioning process.
  • this particle size range facilitates the froth flotation process.
  • the conditioned ore is subjected to a first froth flotation for at least 5 minutes, at least 10 minutes, or at least 25 minutes and to a second froth flotation for at least 5 minutes, at least 10 minutes, or at least 25 minutes.
  • the concentrate may be separated continuously or in a batch-wise fashion from the underflow.
  • the ore is conditioned before the first froth flotation and/or the first concentrate is conditioned before the second froth flotation.
  • the conditioning preferably takes place in the presence of a froth flotation reagent as described above.
  • the first concentrate contains less sulfur and more Ni and Cu compared to the respective content in the ore.
  • the first flotation increases the Cu and Ni content in the concentrate while gangue minerals are discarded in the underflow.
  • the second concentrate may contain less sulfur and less Ni and more Cu compared to the respective content in the first concentrate.
  • the second froth flotation increases the Cu content while in particular the Ni content is decreased.
  • pH measurements were taken on a Sensorex S200C pH probe interfaced to a ThermoFisher Orion DualStar pH meter.
  • the pH meter was calibrated daily using pH 4, 7, and 10 buffers purchased from ThermoFisher. Calibration was completed daily prior to any flotation testing.
  • Ni and Cu containing ore comprising the minerals chalcopyrite, pentlandite and pyrrhotite.
  • the ore contained 2.33 wt.-% Cu, 1.57 wt.-% Ni, and 11.2 wt.-% S.
  • a rougher flotation stage was employed to increase the Cu and Ni content while rejecting gangue minerals, such as pyrrhotite.
  • the slurry was agitated at 1000-1100 rpm, collector (sodium isobutyl xanthate) was added and conditioned for 1-2 min., and frother (polyglycol ether-based; DowfrothTM 250A) was added and conditioned for 1 min. Air was used as the flotation gas and turned on following the conditioning stage. A single concentrate was collected over 7 min. by scraping the froth every 15 sec. More collector was added at 3 min. and 5 min. and conditioned for 1 min. with the air turned off before resuming flotation.
  • the collected concentrate was transferred to another Denver cell, while the tailings were filtered and dried.
  • the Cu grade of the dried first concentrate was 8.1 wt.-%.
  • the Ni grade of the dried first concentrate was 5.1 wt.-%.
  • the Cu and Ni grade was measured using an ICP-OES analyzer.
  • the metals were dissolved by acid digestion and reference samples with a predetermined concentration of metal ions were used for calibration. Subsequently the Cu/Ni separation took place using a second froth flotation step.
  • the float from the rougher stage (15-25 wt.-% solids) was agitated at 900- 1000 rpm while the pH was raised to >12 with a lime slurry.
  • H2O2 was then added (Comparative Example: 0 g / It ore; Example 1 : 1500 g / 1 1 ore; Example 2: 800 g / It ore) as a 50 wt.-% aqueous solution and allowed to condition for 10-30 min. prior to flotation.
  • the H2O2 addition amount was controlled through injecting a known volume of solution into the slurry through a syringe. The air was turned on, and concentrates are collected at 1, 3, and 6 min. (cumulatively). The froth was scraped for 5 sec., 10 sec., and 15 sec., respectively for each concentrate. All concentrates and tailings were filtered dried at 70 °C for 24 hrs and assayed.
  • the results are summarized in the Table below.
  • the Cu and Ni recovery are based on the amount of Cu and Ni, respectively, in the first concentrate.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne un procédé d'extraction de Ni et de Cu à partir d'un minerai comprenant du Ni et du Cu et de séparation de Ni de Cu, le procédé comprenant les étapes consistant à: a) soumettre le minerai à une première flottation par mousse pour fournir un premier concentré comprenant Ni et Cu et un premier sous-écoulement, b) soumettre le premier concentré à une seconde flottation par mousse pour fournir un second concentré et un second sous-écoulement, et c) récupérer du Cu dans le second concentré et du Ni dans le second sous-écoulement, la seconde flottation par mousse étant conduite en présence de H2O2.
PCT/EP2024/059466 2023-06-13 2024-04-08 Séparation de cu et de ni à partir de minerai à l'aide de h2o2 Pending WO2024256057A1 (fr)

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US202363507919P 2023-06-13 2023-06-13
US63/507,919 2023-06-13

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1096514A (fr) * 1978-01-09 1981-02-24 Ernest M. Dottori Traduction non-disponible
CA1104274A (fr) * 1978-12-04 1981-06-30 Gordon E. Agar Separation des sulfures par oxydation selective
US4362552A (en) * 1979-01-29 1982-12-07 Vojislav Petrovich Froth flotation of ores
WO2000074856A1 (fr) * 1999-06-07 2000-12-14 Valtion Teknillinen Tutkimuskeskus Procede de preparation de concentre de nickel
CN115365013A (zh) * 2022-09-30 2022-11-22 中南大学 一种硫化铜镍矿浮选的组合抑制剂及其应用

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1096514A (fr) * 1978-01-09 1981-02-24 Ernest M. Dottori Traduction non-disponible
CA1104274A (fr) * 1978-12-04 1981-06-30 Gordon E. Agar Separation des sulfures par oxydation selective
US4362552A (en) * 1979-01-29 1982-12-07 Vojislav Petrovich Froth flotation of ores
WO2000074856A1 (fr) * 1999-06-07 2000-12-14 Valtion Teknillinen Tutkimuskeskus Procede de preparation de concentre de nickel
CN115365013A (zh) * 2022-09-30 2022-11-22 中南大学 一种硫化铜镍矿浮选的组合抑制剂及其应用

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
S. M. BULATOVIC: "Handbook of Flotation Reagents: Chemistry, Theory and Practice", vol. 2, 2007, ELSEVIER B.V., article "Flotation of Nickel and Nickel-Copper Ores"

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