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EP0609257B1 - Procede d'obtention de concentres de minerais de fer par flottation - Google Patents

Procede d'obtention de concentres de minerais de fer par flottation Download PDF

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Publication number
EP0609257B1
EP0609257B1 EP19920920650 EP92920650A EP0609257B1 EP 0609257 B1 EP0609257 B1 EP 0609257B1 EP 19920920650 EP19920920650 EP 19920920650 EP 92920650 A EP92920650 A EP 92920650A EP 0609257 B1 EP0609257 B1 EP 0609257B1
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EP
European Patent Office
Prior art keywords
alkyl
collector
flotation
phosphates
carbon atoms
Prior art date
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Expired - Lifetime
Application number
EP19920920650
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German (de)
English (en)
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EP0609257A1 (fr
Inventor
Berthold Schreck
Rita Köster
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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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
    • B03D1/0043—Organic compounds modified so as to contain a polyether group
    • 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
    • B03D1/01—Organic compounds containing nitrogen
    • 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
    • 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
    • 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
    • B03D2203/04—Non-sulfide ores

Definitions

  • the invention relates to a process for the production of iron ore concentrates by flotation of iron ores, in which mixtures of special ether amines with anionic collectors are used as collectors.
  • Iron ores are found in nature preferably in the form of oxides, among which magnetite, hematite, martite, limonite and goethite are the best known.
  • the main contaminants are silicates, especially quartz, as well as phosphorus and sulfur compounds.
  • the iron ore is usually first crushed and dry, but preferably ground wet and in water suspended.
  • a collector is then added, often in conjunction with other reagents, which include foaming agents, regulators, pushers (deactivators) and / or stimulants (activators), which supports the separation of the valuable minerals from the gangue minerals in the ore during the subsequent flotation.
  • these reagents are usually allowed to act on the finely ground ore for a certain time (conditioning).
  • the collector causes the surface of the impurities contained in the iron ore to become hydrophobic, so that these minerals adhere to the gas bubbles formed during the aeration.
  • the hydrophobicization of the mineral components takes place selectively in such a way that the gait is floated out and the concentrate remains as a residue (indirect flotation).
  • Aminic compounds are preferably used as collectors in the flotative processing of iron ores. These have the task of adsorbing as selectively as possible on the surface of the contaminants in order to ensure a high depletion of these undesirable constituents in the flotation concentrate. In addition, the collectors should develop a stable, but not too stable, flotation foam.
  • anionic surfactants as collectors or co-collectors in the flotation of non-sulfidic ores.
  • examples include alkyl phosphates and alkyl ether phosphates [ Erzmetall 30 , 505 (1977) ], ether carboxylic acids [ DE 22 37 359 A1 ], sulfosuccinamides and succinamates [ US-A-4,206,045; US-A-4,309,282 and US-A-4,139,481 ] as well as alkyl aspartic acids [ EP 0 270 018 A1 ].
  • US-A-4,472,270 describes iron ore flotation using ether amines and a non-polar hydrocarbon as a nonionic collector.
  • the object of the invention was therefore to develop an improved flotation process for the production of iron ore concentrates which is free from the disadvantages described.
  • the collector mixtures to be used according to the invention can selectively remove phosphorus impurities from iron ores and do not negatively influence the cationic flotation of the silicates.
  • the invention includes the knowledge that phosphorus and Silicate flotation can be carried out both separately and in one step.
  • the concentrates obtainable by the process according to the invention have phosphorus contents of less than 0.015% by weight, based on the concentrate.
  • Etheramines of the formula (I) are known compounds which are obtainable by the relevant preparative organic chemistry processes. Their preparation is usually based on fatty alcohol sulfates which are reacted with alkanolamines or aminoalkylalkanolamines in the presence of alkali metal hydroxides at temperatures of about 180 ° C., alkali metal sulfate being formed as a by-product [ DE 35 04 242 A1 ].
  • Suitable starting materials for the ether amines to be used according to the invention are fatty alcohol sulfates based on saturated or unsaturated fatty alcohols and primary amines or diamines. Typical examples are reaction products of octyl sulphate, decyl sulphate, lauryl sulphate, myristyl sulphate, cetyl sulphate, stearyl sulphate, oleyl sulphate, elaidyl sulphate, petroselinyl sulphate, linolyl sulphate, linolenyl sulphanol, arachyl sulphate, eraducylyl sulphate, badenoleyl sulphate amine, gadoleyl sulphanol amine, gadoleyl sulphanol amine , Aminopropylethanolamine and aminopropylpropanolamine.
  • sulfates based on technical fatty alcohol cuts can also be reacted with the amines mentioned.
  • anionic collectors are to be understood as anionic surfactants of the fatty acid type, alkyl sulfosuccinates, alkyl sulfosuccinamates, alkyl phosphates, alkyl ether phosphates, alkyl aspartic acids and ether carboxylic acids. All of these anionic surfactants are known compounds, the preparation of which - unless stated otherwise - for example in J. Falbe, U. Hasserodt (ed.), "Catalysts, Surfactants and Mineral Oil Additives, Thieme Verlag, Stuttgart, 1978 or J. Falbe (ed.) "Surfactants in Consumer Products", Springer Verlag, Berlin, 1986 .
  • Suitable fatty acids here are in particular the straight-chain fatty acids of the formula (II) obtained from vegetable or animal fats and oils, for example by splitting and optionally fractionating and / or separating by the crosslinking process.
  • R2 is an aliphatic hydrocarbon radical having 12 to 18 carbon atoms and 0, 1, 2 or 3 double bonds and Y is an alkali metal, alkaline earth metal or an ammonium radical.
  • the sodium and potassium salts of oleic and tall oil fatty acids are of particular importance.
  • Suitable alkylsulfosuccinates are sulfosuccinic acid monoesters of fatty alcohols of the formula (V) in which R6 represents a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms and Z has the meaning given above.
  • Suitable alkylsulfosuccinamates are sulfosuccinic acid monoamides of fatty amines of the formula (VI) , in which R7 represents a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms and Z has the meaning given above.
  • Suitable alkyl phosphates and alkyl ether phosphates are substances of the formulas (XI) and (XII) in which R12 and R13 independently of one another are an alkyl or alkenyl radical having 8 to 22 carbon atoms and p and q in the case of the alkyl phosphates are 0, in the case of the alkyl ether phosphates are numbers from 1 to 15 and Z has the meaning given above.
  • the phosphates can be present as mono- or diphosphates. In this case, preference is given to using mixtures of mono- and dialkylphosphates of the type obtained in the industrial production of such compounds.
  • Alkyl aspartic acids are to be understood as meaning compounds of the formula (XIII) in which R14 represents an alkyl or alkenyl radical having 8 to 22 carbon atoms and Z has the meaning given above.
  • Suitable ether carboxylic acids are compounds of the formula (XIV) in which R15 represents an alkyl or alkenyl radical having 8 to 22 carbon atoms and n represents 0 or numbers from 1 to 10 and Z has the meaning given above.
  • nonionic co-collectors selected from the group of fatty alcohol polyglycol ethers, are also used.
  • nonionic surfactants are known compounds, the preparation of which - unless stated otherwise - for example in J. Falbe, U. Hasserodt (ed.), "Catalysts, Surfactants and Mineral Oil Additives, Thieme Verlag, Stuttgart, 1978 or J. Falbe (ed.) "Surfactants in Consumer Products", Springer Verlag, Berlin, 1986 .
  • Suitable fatty alcohol polyglycol ethers are addition products of an average of n moles of ethylene and / or propylene oxide onto fatty alcohols, which follow the formula (XV) in which R16 represents a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms, R5 represents hydrogen or a methyl group and n represents numbers from 1 to 30, preferably 2 to 15.
  • the mixtures of the ether amines with the anionic and / if appropriate nonionic collectors can have a content of 5 to 95% by weight, preferably 10 to 60% by weight of the ether amines. Particularly advantageous results are achieved with mixtures which, in addition to ether amines, contain fatty acids, alkyl aspartic acids and / or ether carboxylic acids or alkyl sulfosuccinamates, alkyl phosphates and / or alkyl ether phosphates.
  • the collector mixture In order to achieve economically viable results in the flotation of iron ore, the collector mixture must be used in a certain minimum amount. However, a maximum amount must also not be exceeded, since otherwise the foam formation becomes too strong and the selectivity towards the contaminants to be flotated out decreases.
  • the amounts in which the collector mixtures to be used according to the invention can be used are usually 20 to 2000, preferably 50 to 1000 g per ton of raw ore.
  • the method according to the invention includes the use of reagents customary for flotation, such as foaming agents, regulators, activators, deactivators, etc.
  • the flotation is carried out under the conditions of the methods of the prior art.
  • the ground ore had the following grain size distribution: > 31 ⁇ m: 7.7% by weight 11 to 31 ⁇ m: 45.3% by weight ⁇ 11 ⁇ m: 47.0% by weight
  • the finely ground ore was then transferred to the desludging stage, diluted to about 8 l (solids content: 7% by weight), mixed with 3 ml of heat-treated corn starch (2.25% by weight) and the supernatant sludge was separated off after 2 minutes.
  • the desludged flotation task (volume: approx. 1 l) was transferred to a 2 l Denver agitator cell (type D1). Then 67 ml of sodium hydroxide and 12 ml of corn starch (2.25% by weight) were added, the cell was filled with flotation water and the slurry was conditioned with stirring for 2 minutes. The amine collector and the anionic and / or nonionic collector were then metered in. The Rougher flotation was then carried out at a stirring speed of 1200 rpm, at which a foam product and a concentrate were obtained in the cell. After metering the collector again, the flotation was carried out a second time and another foam product and the desired iron ore concentrate were obtained.
  • a magnetite ore of the chemical composition specified under II was used, which had a grain size of 89% by weight less than 43 ⁇ m.
  • Flotation was again carried out in a 2 l Denver cell (type D1) with a turbidity density of approx. 220 g / l in water with a calcium ion content of 4 mg / l.
  • the pH of the slurry was adjusted to 8.5 by adding sodium hydroxide; the stirring speed was 1200 rpm.
  • air was introduced and floated at a flow rate of 130 to 150 l / h.
  • the foam was removed over a period of 2 min in the general silicate flotation, with an additional phosphate flotation the flotation time was extended in accordance with the information in Table 7.
  • the amine collector was dosed as a 0.25% by weight aqueous solution, and the anionic collector mixtures were added as 5% by weight aqueous solutions.
  • a commercial foamer based on aldehydes, alcohols and esters with a dosage of 30 g / t was used in all flotation experiments and metered into the slurry undiluted.
  • Tab.7a Magnetite collector systems and dosing E.g.

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  • Manufacture And Refinement Of Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Des concentrés de minerais de fer sont obtenus par épuration par flottation de minerais de fer, en utilisant comme collecteurs des mélanges renfermant (a) au moins une étheramine de formule (I): R1O-[CnH2n]y-NH-[CmH2m-NH]xH, dans laquelle R1 désigne un reste d'hydrocarbure aliphatique linéaire ou ramifié de 6 à 22 atomes de carbone et à 0, 1, 2 ou 3 doubles liaisons, n et m désignent, indépendamment l'un de l'autre, un nombre égal à 1, 2 ou 3, x est égal à 0 ou au nombre 1, 2 ou 3, et y est égal à 2 ou 3, et (b) au moins un autre collecteur anionique et/ou non ionique.

Claims (5)

  1. Procédé pour préparer des concentrés de minerai de fer par flottation, dans lequel du minerai de fer broyé est mélangé à de l'eau pour former une suspension, de l'air étant ensuite injecté dans la suspension en présence d'un système de réactifs et la mousse produite étant séparée avec les matières solides flottées dans la suspension, ce procédé étant caractérisé en ce que les collecteurs utilisés sont des mélanges contenant
    a) au moins une étheramine de formule (I)

            R¹O-[CnH2n]y-NH-[CmH2m-NH]xH     (I)

    dans laquelle R¹ désigne un radical d'hydrocarbure aliphatique linéaire ou ramifié portant 6 à 22 atomes de carbone et 0, 1, 2 ou 3 liaisons doubles, n et m désignent, indépendamment l'un de l'autre, les chiffres 1, 2 ou 3, x désigne 0 ou les chiffres 1, 2 ou 3 et y les chiffres 2 ou 3, et
    b) au moins un autre collecteur anionique choisi dans le groupe des tensio-actifs anioniques, comprenant
    des acides gras,
    des alkylsulfosuccinates,
    des alkylsulfosuccinamates,
    des alkylphosphates et des alkylétherphosphates, de formules (XI) et (XII)
    Figure imgb0019
     dans lesquelles R¹² et R¹³, indépendamment l'un de l'autre, représentent un radical alkyle ou alcényle portant 8 à 22 atomes de carbone, p et q sont égaux à 0 dans le cas des alkylphosphates ou représentent des chiffres de 1 à 15 dans le cas des alkylétherphosphates et Z désigne un ion d'un métal alcalin ou un ion ammonium,
    des acides alkylaspartiques, et
    des acides éthercarboxyliques de formule (XIV)

            R¹⁵O-(CH₂CH₂O)n-CH₂-COOZ     (XIV)

    dans laquelle R¹⁵ désigne un radical alkyle ou alcényle portant 8 à 22 atomes de carbone, n est égal à 0 ou représente un chiffre de 1 à 10 et Z désigne un ion de métal alcalin ou un ion ammonium.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on met en oeuvre des étheramines de formule (I) dans laquelle R¹ désigne un radical alkyle portant 6 à 18 atomes de carbone.
  3. Procédé selon au moins l'une des revendications 1 à 2, caractérisé en ce qu'on met également en oeuvre des cocollecteurs non ioniques choisis dans le groupe des polyglycoléthers d'alcool gras.
  4. Procédé selon au moins l'une des revendications 1 à 3, caractérisé en ce que les mélanges mis en oeuvre comprennent une concentration de 5 à 95 % en poids d'étheramines de formule (I).
  5. Procédé selon au moins l'une des revendications 1 à 4, caractérisé en ce que les mélanges de collecteurs sont mis en oeuvre dans des quantités de 20 à 2000 g/t de minerai brut de fer.
EP19920920650 1991-10-04 1992-09-25 Procede d'obtention de concentres de minerais de fer par flottation Expired - Lifetime EP0609257B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4133063 1991-10-04
DE4133063A DE4133063A1 (de) 1991-10-04 1991-10-04 Verfahren zur herstellung von eisenerzkonzentraten durch flotation
PCT/EP1992/002224 WO1993006935A1 (fr) 1991-10-04 1992-09-25 Procede d'obtention de concentres de minerais de fer par flottation

Publications (2)

Publication Number Publication Date
EP0609257A1 EP0609257A1 (fr) 1994-08-10
EP0609257B1 true EP0609257B1 (fr) 1996-06-12

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US (1) US5540336A (fr)
EP (1) EP0609257B1 (fr)
AU (1) AU658226B2 (fr)
CA (1) CA2120742A1 (fr)
DE (2) DE4133063A1 (fr)
WO (1) WO1993006935A1 (fr)

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CN102259060A (zh) * 2010-12-07 2011-11-30 鞍钢集团矿业公司 低品位铁矿物浮选捕收剂

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US5724986A (en) * 1995-11-06 1998-03-10 Jones Medical Instrument Co. Casing and spirometer for metered dose inhaler
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US7480848B2 (en) * 2006-02-10 2009-01-20 The Directv Group, Inc. Methods and apparatus to select tornado error correction parameters
DE102006010939A1 (de) 2006-03-09 2007-09-13 Clariant International Limited Flotationsreagenz für Silikate
DE102006019561A1 (de) 2006-04-27 2007-10-31 Clariant International Limited Flotationsreagenz für silikathaltige Mineralien
WO2008077849A1 (fr) * 2006-12-22 2008-07-03 Akzo Nobel N.V. Formulations d'amine pour la flottation inverse par écumage de silicates provenant de minerai de fer
EP2017009B1 (fr) 2007-07-20 2013-07-03 Clariant (Brazil) S.A. Flottation inversée de minerai de fer par des collecteurs dans une nanoémulsion aqueuse
BRPI0705593B1 (pt) * 2007-11-22 2016-04-12 Univ Minas Gerais método de quantificação de aminas em resíduos de flotação de minério de ferro
CN101234367B (zh) * 2008-03-04 2011-04-06 昆明晶石矿冶有限公司 一种菱铁矿浮选捕收剂及其制备方法
DE102010004893A1 (de) 2010-01-19 2011-07-21 Clariant International Limited Flotationsreagenz für magnetit- und/oder hämatithaltige Eisenerze
MX2015017533A (es) 2013-07-05 2016-08-08 Akzo Nobel Chemicals Int Bv Sintesis de tensioactivos anionicos novedosos y su uso como recolectores en flotacion por espuma de minerales no sulfurosos.
CA2959949C (fr) * 2014-09-18 2023-02-14 Akzo Nobel Chemicals International B.V. Utilisation d'alcools ramifies et d'alcoxylates de ceux-ci en tant que collecteurs secondaires
WO2017127704A1 (fr) * 2016-01-21 2017-07-27 Mlinar Matthew Albert Flottation cationique de silice et d'apatite à partir de minerais de fer oxydés à un ph naturel
EP3481557A2 (fr) 2016-07-08 2019-05-15 Akzo Nobel Chemicals International B.V. Procédé de traitement de minerai de magnétite et composition collectrice
BR112019027874B1 (pt) 2017-07-04 2023-05-09 Nouryon Chemicals International B.V Processo para tratar minérios não sulfídicos carbonáticos com uma composição coletora, composição coletora para uso em processo e polpa
CA3068885C (fr) 2017-07-04 2024-03-19 Nouryon Chemicals International B.V. Procede de traitement de minerais siliceux non sulfures et composition de collecteur associee
AU2019289849B2 (en) 2018-06-19 2024-06-13 Clariant International Ltd Use of polyols for improving a process for reverse froth flotation of iron ore
PE20250721A1 (es) 2022-03-25 2025-03-06 Clariant Int Ltd Nuevos colectores cationicos para mejorar un proceso de flotacion por espuma de silicatos
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102259060A (zh) * 2010-12-07 2011-11-30 鞍钢集团矿业公司 低品位铁矿物浮选捕收剂
CN102259060B (zh) * 2010-12-07 2012-11-28 鞍钢集团矿业公司 低品位铁矿物浮选捕收剂

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Publication number Publication date
DE4133063A1 (de) 1993-04-08
EP0609257A1 (fr) 1994-08-10
DE59206582D1 (de) 1996-07-18
AU658226B2 (en) 1995-04-06
CA2120742A1 (fr) 1993-04-15
AU2651592A (en) 1993-05-03
US5540336A (en) 1996-07-30
WO1993006935A1 (fr) 1993-04-15

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