EP1504820A1 - In einem Erzflotationsverfahren verwendbare Zusammensetzung von Mercaptanen. - Google Patents

In einem Erzflotationsverfahren verwendbare Zusammensetzung von Mercaptanen. Download PDF

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Publication number
EP1504820A1
EP1504820A1 EP04291383A EP04291383A EP1504820A1 EP 1504820 A1 EP1504820 A1 EP 1504820A1 EP 04291383 A EP04291383 A EP 04291383A EP 04291383 A EP04291383 A EP 04291383A EP 1504820 A1 EP1504820 A1 EP 1504820A1
Authority
EP
European Patent Office
Prior art keywords
flotation
composition according
product
ndm
ore
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.)
Granted
Application number
EP04291383A
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English (en)
French (fr)
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EP1504820B1 (de
Inventor
Didier Anglerot
Annie Commarieu
Thierry Aubert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arkema France SA
Original Assignee
Arkema SA
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
Priority claimed from FR0307180A external-priority patent/FR2855987B1/fr
Application filed by Arkema SA filed Critical Arkema SA
Publication of EP1504820A1 publication Critical patent/EP1504820A1/de
Application granted granted Critical
Publication of EP1504820B1 publication Critical patent/EP1504820B1/de
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Classifications

    • 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
    • B03D1/004—Organic compounds
    • B03D1/014—Organic compounds containing phosphorus
    • 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
    • B03D1/004—Organic compounds
    • B03D1/008—Organic compounds containing oxygen
    • 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
    • B03D1/004—Organic compounds
    • B03D1/012—Organic compounds containing sulfur
    • 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
    • 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
    • B03D2201/02—Collectors
    • 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
    • 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
    • B03D2203/025—Precious metal ores
    • 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
    • B03D2203/04—Non-sulfide ores
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • 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

Definitions

  • the present invention relates to the field of metal mining, and more especially the flotation of ores, in particular ores based on oxides and sulphides. It relates more particularly to a new composition based on mercaptans which can be used, in particular, in combination with a flotation agent, and at a process for the recovery, by flotation, of valuable metal compounds.
  • Flotation is a well-known process aimed at extracting a metal from from low-grade ores through a concentration step. This step is located before further processing including heat treatment (also referred to as smelting) or leaching and refining. This is particularly the case of oxide ores and / or sulphides of lead, zinc, copper, silver, gold, molybdenum and metals belonging to the platinum group: platinum, palladium, rhodium, ruthenium, iridium and osmium.
  • Ores contain compounds (such as oxides or sulfides) of metals to extract (or valuable metal compounds), in the form of crystals that are dispersed in a gangue composed of various impurities, in particular siliceous.
  • the Minerals are, after extraction from the mine, crushed and then ground in a wet environment to give particles of sufficient fineness to release the crystals of the compounds desired.
  • the highly heterogeneous mixture of crystals of sought compounds and on the other hand gangue particles is therefore introduced into water containing appropriate additives, in particular still flotation agents called flotation collectors.
  • Air is injected into the aqueous suspension as well obtained, placed in a suitable device (usually a flotation cell), to create bubbles that adhere to the crystals of the compounds (such as oxides and / or sulphides) containing the desired metal.
  • a suitable device usually a flotation cell
  • the adhesion of bubbles to said crystals is favored by the action of the agent or flotation agents used.
  • the crystals of metal compounds then rise to the surface and are recovered in the form of a foam, also called flotation concentrate.
  • the gangue particles are recovered in the lower part of the flotation cell.
  • the flotation concentrate has a desired metal content which is therefore considerably higher than that of the original ore. This content depends on the initial ore content and selectivity of the flotation process. The quantity of recovered metal in the form of flotation concentrate is in turn dependent on process efficiency.
  • Flotation agents commonly used in the mining industry metals include, for example, alkaline xanthates of alkyl radicals having less of 6 carbon atoms, in particular potassium ethyl, amyl or isobutyl xanthate, mercaptobenzothiazoles, thiocarbamates, dithiocarbamates and dithiophosphates.
  • the flotation concentrates by example in the case of copper, are then introduced, for the treatment step thermal (or smelting), in an oven at temperatures that may exceed 1500 ° C.
  • the desired metal is separated in the molten state from the other substances, including impurities from the ore gangue, which must be removed in the form of a slag.
  • French patent application FR 2 371 967 thus discloses the use for obtaining flotation concentrates of a solution of n-dodecyl mercaptan in a polyglycol.
  • this document teaches such use for obtaining flotation concentrates in increased copper content.
  • South African patent ZA 8405787 describes the implementation as a collector flotation of a tert-dodecyl mercaptan solution in cresylic acid. This document also describes the application of such collectors for the treatment of ores of copper.
  • the object of the invention is to propose such a means, the description of which is given in the following text.
  • the percentages that are indicated are, in the absence of indications to the contrary, percentages corresponding to levels weight.
  • N-dodecyl mercaptan is the thiol derivative of the straight chain alkyl radical having 12 carbon atoms, of formula nC 12 H 25 -SH. It is a commercially available product.
  • tert-dodecyl mercaptan is meant a mixture of compounds of formula: R-SH wherein R is an alkyl radical having 9 to 15 carbon atoms and having at least one tertiary carbon, which is attached to the SH group.
  • the average number of carbon atoms of the alkyl radical is 12.
  • the content in the mixture of the compound of formula (I) in which R is a dodecyl radical is greater than 50%, preferably greater than or equal to 60% by weight. .
  • Such a mixture is also commercially available, and may be prepared by the process described in patent application EP 0101356.
  • the product (B) is chosen from the group comprising phenols optionally substituted with one or more C 1 -C 4 alkyl radicals, cresols, naphthols, xylenols and indanols, as well as mixtures of these compounds.
  • cresols optionally substituted with one or more C 1 -C 4 alkyl radicals, cresols, naphthols, xylenols and indanols, as well as mixtures of these compounds.
  • cresols cresols, naphthols, xylenols and indanols
  • cresylic acid Such mixtures, in which the compounds are generally present in the form of their different isomers, are referred to herein as "cresylic acid”.
  • composition according to the invention advantageously comprises from 75 to 85% of the combination (A) of NDM and CT, and from 15 to 25% of the product (B).
  • the product (B) used is cresylic acid.
  • the product (B) used is MIBC or a propylene oxide oligomer of molecular weight between 50 and 2000, preferably between 100 and 800.
  • composition according to the invention is a solution.
  • a composition according to the invention in which the NDM / TDM ratio is neighbor of 1 is particularly advantageous.
  • the subject of the present invention is also a method of recovery by flotation, valuable metal compounds contained in ores, including introducing into a suitable cell at least one flotation collector, characterized in that it further comprises introducing into said cell a quantity effective of the composition as defined above.
  • a collector (or agent) flotation a selected compound among the alkaline xanthates of alkyl radicals having less than 6 carbon atoms, the mercaptobenzothiazoles, as well as thiocarbamates, dithiocarbamates and alkaline dithiophosphates.
  • a particularly advantageous flotation collector is an alkaline xanthate an alkyl radical having less than 6 carbon atoms or an alkaline dithiophosphate.
  • flotation agent ethyl, amyl or isobutyl xanthate. potassium or sodium.
  • the amount of composition based on NDM and TDM, as defined above, to be introduced into the process can be determined easily by the person skilled in the art from preliminary tests, according to various parameters such as the desired metal content of the ore.
  • This quantity corresponds generally at a weight ratio expressed on the basis of the weight of ore processed between 2 g / ton and 150 g / ton, preferably between 5 and 50 g / ton.
  • the report of weight of the composition according to the invention on the total weight of flotation agent can vary within very wide limits, for example between 0.5 and 200%, preferably between and 125%.
  • the process according to the invention may be suitable for the recovery of compounds metals, such as oxides and / or sulphides, comprising one or more metals selected from the group containing: lead, zinc, copper, molybdenum, nickel, cobalt, palladium, osmium, ruthenium, rhodium, iridium, and platinum. said The process may also be suitable for recovering said metals in the native state.
  • compounds metals such as oxides and / or sulphides, comprising one or more metals selected from the group containing: lead, zinc, copper, molybdenum, nickel, cobalt, palladium, osmium, ruthenium, rhodium, iridium, and platinum.
  • the process may also be suitable for recovering said metals in the native state.
  • the introduction of the composition according to the invention and the collector (s) of Flotation can be simultaneous or sequential.
  • an introduction sequence of the flotation collector (s), followed by that of the composition based on of NDM and TDM, according to the invention are preferable.
  • composition according to the invention can be introduced as well at the primary flotation than secondary flotation (carried out on the sterile fraction corresponding to the particles decanted in the lower part of the cell, during the primary flotation).
  • Example 1 (reference) Flotation of platinum ore with xanthate and dithiophosphate as flotation agents:
  • This flotation test is performed on UG2 type platinum sulphide ore from a South African mine in the Rustenburg area, with a platinum 2.5 ppm.
  • Step 1 Preparation of an aqueous suspension of the ore by grinding and sieving
  • 1150 g of this mineral are mixed with 572 g of water and introduced into a mill ball.
  • the ore is ground for 30 minutes.
  • the suspension is sieved on a mesh screen 0.1 mm, and thus recovering an aqueous suspension A containing 933 g of dry ore, the particles of which have a mean diameter (measured by particle size laser) of 40 ⁇ m.
  • Step 2 Introduction of flotation additives into the aqueous suspension of the ore
  • Step 3 Primary Flotation
  • step 2 After about 1 minute of rest, the mixture obtained in step 2 is subjected to flotation for 5 minutes at a pH of about 8 in a 2.5-liter laboratory cell of the Wemco type.
  • This concentrate has a platinum content of 18 ppm (corresponding to the selectivity) and contains 51.2% of the Pt contained in the ore processed (the latter percentage) corresponding to the performance).
  • Step 4 Secondary Flotation
  • the sterile fraction corresponding to the decanted particles is recovered in the lower part of the flotation cell, to which is added 13 mg of isobutyl xanthate of sodium and 9.7 mg of sodium dithiophosphate.
  • cresylic acid After mixing for 4 minutes, 5.6 mg of cresylic acid is added, and adjusts the volume of water to 2.5 1.
  • the product obtained is subjected to flotation for 3 minutes in the same conditions as in step 3.
  • the total recovery rate of platinum (or total yield) is 58%.
  • NDM and TDM used are the products marketed by the Company Atofina.
  • cresylic acid used also comes from the company Studtgers-Oils Tar and Derivatives.
  • Reference Example 1 is repeated by introducing in step 2, in addition to the flotation agents, 28 mg of the solution prepared according to Example 2.
  • step 4 of Reference Example 1 is also repeated by adding 28 mg of the solution of Example 2. 5 g of concentrate are recovered. flotation having a platinum content of 10 ppm, corresponding to 1.9% yield.
  • the total yield is therefore 68.3%.
  • Example 4 (Reference) Flotation of platinum ore with xanthate and dithiophosphate as flotation agents:
  • This flotation test is performed on UG2 type platinum sulphide ore from a South African mine in the Rustenburg area, with a platinum 2 ppm.
  • Step 1 Preparation of an aqueous suspension of the ore by grinding and sieving
  • Step 2 Introduction of flotation additives into the aqueous suspension of the ore
  • cresylic acid comprising about 25% of a mixture of meta and para cresol, 27% of a mixture of 2,4-xylenol and 2,5-xylenol, and about 30% of a mixture of methyl ethyl phenol and propyl ethyl phenol.
  • a cresylic acid is marketed by the Merisol Company.
  • Step 3 Primary Flotation
  • step 2 After about 1 minute of contacting the ingredients, the resulting mixture in step 2 is floated for 5 minutes at a pH of about 8 in a cell 2.5 liter laboratory type Wemco. The volume of the solution is kept at 2.5 liters per addition of water for the duration of the flotation.
  • the mass of concentrate collected by skimming on the surface of the cell Flotation is 124 g.
  • the platinum content of said concentrate (corresponding to selectivity) is 12.2 ppm and the amount of platinum recovered (expressed as a percentage of that contained in the treated ore, corresponding to the yield) is 80%.
  • Example 2 is repeated using as a cresylic acid that used in step 2 of example 4.
  • Reference Example 4 is repeated, introducing in step 2, in addition to the flotation agents, 30 grams (per ton of ore) of the prepared solution according to Example 5.
  • the concentrate mass collected is 88.7 g, for a selectivity of 14 ppm and a yield of 65.9%.
  • Example 2 is repeated, replacing the cresylic acid with an oligomer propylene oxide of average molecular weight 425, marketed by the company BAYER under the name ARCOL® PPG-425.
  • the mass of concentrate collected is 115.6 g, for a selectivity of 12.6 ppm and a yield of 76.4%.
  • Example 2 is repeated, replacing the cresylic acid with MIBC.
  • the mass of concentrate collected is 104.8 g, for a selectivity of 12.8 ppm and a yield of 70.5%.
EP04291383A 2003-06-16 2004-06-03 In einem Erzflotationsverfahren verwendbare Zusammensetzung von Mercaptanen. Active EP1504820B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
FR0307180A FR2855987B1 (fr) 2003-06-16 2003-06-16 Composition de mercaptans utilisable dans un procede de flottation de minerais
FR0307180 2003-06-16
FR0403696 2004-04-08
FR0403696A FR2857278B1 (fr) 2003-06-16 2004-04-08 Compositions de mercaptans utilisables dans un procede de flottation de minerais

Publications (2)

Publication Number Publication Date
EP1504820A1 true EP1504820A1 (de) 2005-02-09
EP1504820B1 EP1504820B1 (de) 2006-09-20

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EP04291383A Active EP1504820B1 (de) 2003-06-16 2004-06-03 In einem Erzflotationsverfahren verwendbare Zusammensetzung von Mercaptanen.

Country Status (13)

Country Link
US (1) US7014048B2 (de)
EP (1) EP1504820B1 (de)
CN (1) CN100556553C (de)
AT (1) ATE340032T1 (de)
AU (1) AU2004202612B8 (de)
CA (1) CA2470343C (de)
CL (1) CL2004001496A1 (de)
DE (1) DE602004002439D1 (de)
FR (1) FR2857278B1 (de)
MX (1) MXPA04005870A (de)
PE (1) PE20050459A1 (de)
RU (1) RU2346751C2 (de)
ZA (1) ZA200404728B (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7014048B2 (en) * 2003-06-16 2006-03-21 Arkema Composition formed of mercaptans which can be used in a process for the flotation of ores
CN100551544C (zh) * 2007-02-13 2009-10-21 金堆城钼业股份有限公司 辉钼矿选矿起泡剂
CN102806148A (zh) * 2012-09-07 2012-12-05 西北矿冶研究院 一种高硫铜矿捕收剂
CN106423581A (zh) * 2016-11-15 2017-02-22 中南大学 一种铅锑锌硫化矿混合浮选捕收剂、其制备及应用

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CN101264467B (zh) * 2007-03-13 2011-04-13 金堆城钼业股份有限公司 辉钼矿浮选起泡剂
CN101543805B (zh) * 2008-03-28 2012-07-18 鞍钢集团矿业公司 一种铁矿物浮选鳌合捕收剂
CA2952568C (en) 2014-01-31 2018-07-10 Goldcorp Inc. Process for separation of at least one metal sulfide from a mixed sulfide ore or concentrate
US9447481B1 (en) * 2015-10-07 2016-09-20 Chevron Phillips Chemical Company Lp Dipentene dimercaptan compositions and use thereof as a mining chemical collector
US9512248B1 (en) 2015-12-28 2016-12-06 Chevron Phillips Chemical Company Lp Mixed decyl mercaptans compositions and use thereof as chain transfer agents
US10294200B2 (en) 2015-12-28 2019-05-21 Chevron Phillips Chemical Company, Lp Mixed branched eicosyl polysulfide compositions and methods of making same
US10040758B2 (en) 2015-12-28 2018-08-07 Chevron Phillips Chemical Company Lp Mixed decyl mercaptans compositions and methods of making same
US9505011B1 (en) * 2015-12-28 2016-11-29 Chevron Phillips Chemical Company Lp Mixed decyl mercaptans compositions and use thereof as mining chemical collectors
US10011564B2 (en) 2015-12-28 2018-07-03 Chevron Phillips Chemical Company Lp Mixed decyl mercaptans compositions and methods of making same
US9512071B1 (en) 2015-12-28 2016-12-06 Chevron Phillips Chemical Company Lp Mixed decyl mercaptans compositions and methods of making same
CN108212538B (zh) * 2018-01-31 2019-04-26 中南大学 一种烃基硫醚基醇类化合物及其制备方法与应用
CN111266195B (zh) * 2020-03-05 2021-09-07 中南大学 一种氧化锌矿浮选组合捕收剂及其应用
CN112774869B (zh) * 2020-12-25 2022-09-16 厦门紫金矿冶技术有限公司 黄铁矿抑制剂及其制备和在铜铅锌多金属硫化矿中的应用
CN113275130A (zh) * 2021-06-08 2021-08-20 青岛鑫润矿业科技有限公司 一种更廉价的锡石浮选辅助捕收剂

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7014048B2 (en) * 2003-06-16 2006-03-21 Arkema Composition formed of mercaptans which can be used in a process for the flotation of ores
CN100551544C (zh) * 2007-02-13 2009-10-21 金堆城钼业股份有限公司 辉钼矿选矿起泡剂
CN102806148A (zh) * 2012-09-07 2012-12-05 西北矿冶研究院 一种高硫铜矿捕收剂
CN106423581A (zh) * 2016-11-15 2017-02-22 中南大学 一种铅锑锌硫化矿混合浮选捕收剂、其制备及应用
CN106423581B (zh) * 2016-11-15 2019-01-11 中南大学 一种铅锑锌硫化矿混合浮选捕收剂、其制备及应用

Also Published As

Publication number Publication date
EP1504820B1 (de) 2006-09-20
US7014048B2 (en) 2006-03-21
RU2004118077A (ru) 2006-02-27
US20050167339A1 (en) 2005-08-04
ATE340032T1 (de) 2006-10-15
AU2004202612B8 (en) 2009-12-17
CN100556553C (zh) 2009-11-04
PE20050459A1 (es) 2005-08-25
CN1575854A (zh) 2005-02-09
MXPA04005870A (es) 2005-06-08
AU2004202612A1 (en) 2005-01-06
ZA200404728B (en) 2005-04-26
DE602004002439D1 (de) 2006-11-02
AU2004202612B2 (en) 2009-08-20
CA2470343A1 (fr) 2004-12-16
FR2857278A1 (fr) 2005-01-14
CA2470343C (fr) 2011-01-25
FR2857278B1 (fr) 2005-08-26
CL2004001496A1 (es) 2005-02-25
RU2346751C2 (ru) 2009-02-20

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