EP3648891B1 - Procédé de traitement de minerais silicieux non sulfuriques et composition collectrice associée - Google Patents

Procédé de traitement de minerais silicieux non sulfuriques et composition collectrice associée Download PDF

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EP3648891B1
EP3648891B1 EP18732097.3A EP18732097A EP3648891B1 EP 3648891 B1 EP3648891 B1 EP 3648891B1 EP 18732097 A EP18732097 A EP 18732097A EP 3648891 B1 EP3648891 B1 EP 3648891B1
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collector
carbon atoms
ores
formula
phosphate
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EP3648891A1 (fr
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Natalija Smolko-Schvarzmayr
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Nouryon Chemicals International BV
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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
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/014—Organic compounds containing phosphorus
    • 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
    • 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
    • B03D2203/06—Phosphate ores

Definitions

  • the present invention relates to a process to treat siliceous non-sulfidic ores, such as siliceous phosphate ores, and to collector compositions that are suitably used in such processes.
  • Froth flotation is a physico-chemical process used to separate mineral particles considered economically valuable from those considered waste. It is based on the ability of air bubbles to attach onto those particles previously rendered hydrophobic. The particle-bubble combinations then rise to the froth phase from where it discharges the flotation cell whilst the hydrophilic particles remain in the flotation cell. Particle hydrophobicity is, in turn, induced by special chemicals called collectors. In direct flotation systems, it is the economically valuable minerals which are rendered hydrophobic by the action of the collector. Similarly, in reverse flotation systems, the collector renders hydrophobicity to those mineral particles considered waste. The efficiency of the separation process is quantified in terms of recovery and grade.
  • Recovery refers to the percentage of valuable product contained in the ore that is removed into the concentrate stream after flotation.
  • Grade refers to the percentage of the economically valuable product in the concentrate after flotation. A higher value of recovery or grade indicates a more advantageous flotation system.
  • the secondary collector is primarily responsible for improvement of the recovery, efficiency, frothing characteristics, etc and the primary collector for the selectivity.
  • DE 4016792 discloses, like DE 4010279 and DE 4133063 , a process to treat siliceous non-sulfidic ores by a flotation process.
  • DE 792 as collector composition mixtures of esters of dicarboxylic acid with fatty acid monoalkylamides are used, optionally in combination with further anionic or non-ionic surfactants.
  • DE 279 as collector composition dicarboxylic acid N alkylmonoamides are used, optionally in combination with further anionic or non-ionic surfactants.
  • etheramines with at least one anionic or nonionic co-collector component are used as collector composition.
  • EP 544185 discloses a process to treat non-sulfidic siliceous ores by using a collector composition that contains as a primary collector a sulfosuccinate and optionally a further surfactant that may be chosen from a big group of possibilities and that also includes an alkyl phosphate or alkyletherphosphate.
  • the use of phosphate compounds as a primary collector is not disclosed or suggested in EP 544185 .
  • EP 544185 furthermore does not disclose alkyldiphosphate, alkyltriphosphate or alkyltetraphosphate compounds. In none of the Examples of EP 544185 the use of a phosphate in a collector composition is demonstrated, nor is the difference between different phosphate compounds suggested.
  • GB 1093504 discloses a process to treat a siliceous ore by using a phosphorous atom-containing compound of the formula RaHbPcOd wherein c can be 1 or 2.
  • the phosphate compounds can be alkylated and preferably are hypophosphates. Pyrophosphates are also suggested but not actually tested.
  • the process to treat the ores is aimed at separating off several minerals of value from the ores.
  • the flotation process of GB 504 wherein phosphate is the mineral of value, Example 11, is a flotation process at preferably a low pH, wherein the phosphate is collected in the froth.
  • the phosphate compound in this Example is a lauryl alcohol based hypophosphate and the results of the flotation process are - with P2O5 assay of 28% - subject to improvement
  • the invention now provides a process to treat siliceous non-sulfidic ores with a collector composition that comprises a phosphate compound of the formula I wherein R is linear or branched, saturated or unsaturated hydrocarbon group containing 1 to 24 carbon atoms, A is an alkylene oxide unit; Y is H, Na, K or an ammonium or alkylated ammonium, n is 1 - 3, p is 0 - 25, X is chosen from the same groups as R-Ap or Y.
  • the invention furthermore relates to a collector composition for the process to treat siliceous non-sulfidic ores
  • the collector composition comprises the above phosphate compound of the formula I as a primary collector, and a secondary collector that comprises a monophosphate compound and one or more other secondary collector compounds that can be an anionic collector compound selected from the group of fatty acids, alkylsulfosuccinates, alkylmaleates, alkylamidocarboxylates, esters of alkylamidocarboxylates, alkylbenzensulphonates, alkylsulfonates, sulphonated fatty acids or a nonionic collector compound of the group of ethoxylates, glycosides, ethanolamides or a mixture of two or more of these anionic and nonionic collectors.
  • the present invention provides an improved process to treat siliceous ores and collector compositions for use therein which provide the required grade of separation of the desired product from the ore and an improved recovery and selectivity.
  • the present invention additionally provides an improvement in that a reduced total amount of the collector composition can be employed in the flotation process.
  • US 4,287,053 discloses a phosphate depressant for treating siliceous phosphate ores. Depressants however are known to have a distinctly different function than collectors. Also US 2,424,552 discloses phosphates as a depressant, which are in this document all inorganic phosphates. In the examples hexametaphosphate is used. The document does not disclose organic phosphates, such as phosphates containing a hydrocarbon group.
  • the DB is preferably between 0 and 2.2 and p is higher than 0.
  • R contains 1 to 12 carbon atoms preferably at least one unit A is present which is a propylene oxide unit. Even more preferably when R contains 1 to 10 carbon atoms, p is between 1 and 25, yet more preferable between 4 and 10 and most preferable between 5 and 8.
  • R contains 1 to 10 carbon atoms even more preferably one or more of the A units are propylene oxide or butylene oxide, or when R contains 1 to 10 carbon atoms in another more preferable embodiment a block of propylene oxide units A is first bound to R and next a block of ethylene oxide units A.
  • R is a group containing 12 to 16 carbon atoms
  • p is preferably higher than 0, and in a further preferred embodiment the groups A are propylene oxide, ethylene oxide or a combination of both propylene oxide and ethylene oxide.
  • R contains 12 - 16 carbon atoms it is preferably branched. Even more preferably, the degree of branching is between 0.2 and 3.
  • R contains more than 16 carbon atoms it is preferably linear and unsaturated. More preferably when p is higher than 0, and R contains more than 16 carbon atoms, one or more of the groups A are ethylene oxide. Yet even more preferably when R contains more than 16 carbon atoms the degree of unsaturation is between 0.2 - 2, most preferably 0.5 - 1.1.
  • R is a group containing 8 to 16 carbon atoms, even more preferably R is a group containing 9 to 15 carbon atoms.
  • R is a saturated hydrocarbon group.
  • R has up to and including 12 carbon atoms it is preferably linear or branched to a limited degree.
  • each A is independently a propylene oxide group or ethylene oxide group. Even more preferred A is an ethylene oxide group.
  • the value of p is preferably 0-15, more preferably 1-10, most preferably 2-8. If R contains more than 12 carbon atoms, the value of p is preferably chosen higher than when R contains up to and including 12 carbon atoms.
  • DA degree of alkoxylation
  • the alkylene oxide units A are suitably ethylene oxide, propylene oxide or butylene oxide.
  • the degree of unsaturation (DU) as used herein is meant the total number of double bonds in the alkyl chain. It should be noted that degree of unsaturation is an average value for the R groups as present in the phosphate compound of formula I or formula II and hence does not have to be an integer.
  • the degree of branching (DB) as used herein is meant the total number of (terminal) methyl groups present on the R alkyl chain minus one (side chains that are alkyls other than methyls being counted by their terminal methyls). It should be noted that degree of branching is an average value for the R groups as present in the phosphate compound of formula I and hence does not have to be an integer.
  • n 1.
  • the process of the invention relates to the separation of apatite from non-sulfidic siliceous ores.
  • Siliceous ores are ores that contain silicas (SiO2). In preferred embodiments the siliceous ores contain between 5 and 80 wt% of silica. Even more preferred siliceous ores contain between 20 and 75% by weight of silica.
  • the amount of phosphate minerals such as apatite in the siliceous ore in embodiments is between 8 and 40% by weight, preferably 10-30 wt%.
  • the ores may contain other main minerals such as iron oxide minerals, further defined below.
  • the process is a process for selective flotation of apatite.
  • the process is a direct flotation, even more preferred it is a direct flotation process to isolate the phosphate minerals from the siliceous ores.
  • the pH during the process of the present invention is preferably between 8 and 11.
  • the collector composition of the present invention for use in a process to treat non-sulfidic siliceous ores contains a primary collector that comprises a phosphate of the above formula (I) wherein R, X, Y, A, p and n have the same meaning as above, a monophosphate secondary collector compound that is preferably of the formula II and one or more other secondary collectors that may be an anionic collector selected from the group of fatty acids that are preferably of the formula RCOOY, sulphonated fatty acids that are preferably of the formula RCH(SO 3 Y)COOY, alkylsulfosuccinates that are preferably of the formula III alkylmaleates that are preferably of the formula IV alkylamidocarboxylates that are preferably of the formula V wherein in all above structures and formulae II-V, each R, A, p, Y independently has the meaning as defined above for formula I, m is 0-7 , B is -H, -CH 3 ,
  • the monophosphate secondary collector compound can be separately and purposively added to the collector composition and can be chosen from the group of compounds as defined above with formula II but monophosphate compounds can be inherently formed in the process to prepare the primary collector phosphate compound of above formula I. If in the composition obtained when manufacturing the phosphate compound of formula I such other phosphates are not removed, a composition is obtained that inherently contains both a primary collector of the present invention and a monophosphate secondary collector.
  • the primary collector is present in an amount of 5-60 wt %, more preferably 10-60 wt%, the monophosphate secondary collector in an amount of 5-75 wt%, more preferably 10-75 wt%, and any other secondary collector in an amount of 1- 50 wt%, wherein the wt% is the wt% on total solids content of the collector composition.
  • the amount of monophosphate secondary collector is between 25 and 75 wt%, more preferably 30 and 65 wt%, on total solids content of the collector composition because monophosphates as explained above are often formed in processes to prepare di- and tri and tetraphosphates and for the purpose of using the higher phosphates in a collector composition it is not needed to separate off the monophosphates, as they can play a role as a secondary collector.
  • Other secondary collectors are preferably present in an amount of 5- 50 wt%.
  • the amount of the phosphate compound of formula I in the collector compositions and process of the present invention is preferably between 5 and 50wt%
  • the amount of the phosphate compound of formula I in the collector compositions and process of the present invention is between 5 and 45 wt% , even more preferred between 10 and 40 wt%, most preferred between 15 and 35 wt% on total phosphate.
  • the collector composition can be added to the flotation in concentrated form (i.e. 5 -100 wt% solids, preferably 50 - 100wt% solids) or as 1-5 weight % aqueous solution.
  • the process and collector composition of the invention may involve other additives and auxiliary materials which are typically present in a froth flotation process that can be added at the same time or, preferably, separately during the process.
  • Further additives that may be present in the flotation process are depressants (such as starch, dextrin, quebracho), dispersants (such as water glass), frothers/froth regulators/froth modifiers/defoamers (such as MIBC, Texanol, alkoxylated low molecular weight alcohols), and pH-regulators (such as NaOH).
  • the present invention relates to a pulp comprising crushed and ground ore, a primary collector or a collector composition as defined herein, and optionally further flotation aids.
  • This pulp can be prepared by first grounding the ore and then adding collector composition or by adding at least part of the collector composition to the ore and milling the ore to pulp in the presence of at least part of the collector composition.
  • the siliceous ores that can be used in the process of the invention may include further minerals than silicas and phosphates.
  • the mineral composition of most of the siliceous ore deposits throughout the world is generally similar, differing only in percentage of each mineral present according to their origin.
  • Further minerals present in the siliceous ores may be gneisses, granites and pegmatites and there may be mentioned in particular-ilmenite, rutile, monazite, zircon, silljmanite, kyanite, andalusite, garnet, spinel, corundum, staurolite, tourmaline and epidote.
  • the amount of the collector used in the process of reversed flotation of the present invention will depend on the amount of impurities present in the ore and on the desired separation effect, but in some embodiments will be in the range of from 10-1000 g/ton dry ore, preferably in the range of from 20-500 g/ton dry ore, more preferably 25-200 g/ton dry ore.
  • Oleyl alcohol (60.0 g) ethoxylated with 4 equivalents of EO was added to a glass reactor with a flange equipped with an overhead stirrer. The reactor was flushed with nitrogen for 10 minutes. The mixture was heated with an oil bath to 55°C and methylsulfonic acid (3.69 g) was added. Phosphorus pentoxide (9.71 g) was added portion wise, keeping temperature at 55°C. Stirring at 55°C under nitrogen atmosphere was continued overnight. The final product was analyzed by 31 P-NMR spectroscopy.
  • Isotridecanol (40 g, 200 mmol) was added to a glass reactor with a flange equipped with an overhead stirrer. The reactor was flushed with nitrogen for 15 minutes. The mixture was heated with an oil bath to 55°C and methylsulfonic acid (5.39 g, 5.39 mmol) was added. Phosphorus pentoxide (14.2 g, 100.0 mmol) was added portion wise, keeping temperature at 55°C. Stirring at 55°C under nitrogen atmosphere was continued overnight. The final product was analyzed by 31 P-NMR spectroscopy. 31 P -NMR (CDCl 3 ): ⁇ 4 to -1 ppm monophosphate; ⁇ -12 to -16 ppm pyro-phosphate; ⁇ -28 to -30 ppm polyphosphate.
  • Number of cleaning steps is depending on how much solid material there are in the froth products. Flotation goes on till there are no more particles in the froth. Time above indicate how long that takes.
  • the collectors displayed in Table 1 were used in the flotation procedure above, and the flotation results with these collectors are displayed in Table 1.
  • the selectivity factor should be as high as possible.
  • Table 1 Flotation results presented as P2O5 recovery and grade Phosphate collector component Dosage, g/t Fraction Amount of phosphate as P 2 O 5 Selectivity factor Grade % recovery % Invention Collector 1 (oleyl alcohol+4EO mono- and pyrophosphate mix) 130 Rougher concentrate 29.49 96.6 1.8 1 st cleaner concentrate 36.56 94.6 0.7 2 nd cleaner concentrate 39.00 91.8 0.3 Comparison Collector 2 Oleyl alcohol+4EO only monophosphate) 150 Rougher concentrate 28.78 96.4 2.0 1 st cleaner concentrate 36.67 93.5 0.6 2 nd cleaner concentrate 39.50 87.8 0.2
  • Example 2 was repeated but the following two collector compositions were compared (see for dosage below Table 2)

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Claims (10)

  1. Procédé de traitement de minerais siliceux non sulfurés avec une composition de collecteurs qui comprend un composé de phosphate de formule I
    Figure imgb0016
     dans lequel R représente un groupe hydrocarboné saturé ou insaturé, linéaire ou ramifié, contenant de 8 à 24 atomes de carbone, A représente un motif oxyde d'alkylène ; Y représente H, Na, K ou un ammonium ou un ammonium alkylé, n vaut de 1 à 3, p vaut de 0 à 25, X est choisi parmi les mêmes groupes que R-Ap ou Y, ou dans lequel R représente un groupe hydrocarboné saturé ou insaturé, linéaire ou ramifié qui contient de 1 à 12 atomes de carbone et au moins un motif A est présent qui est un motif oxyde de propylène.
  2. Procédé selon la revendication 1 dans lequel R représente un groupe contenant de 9 à 20 atomes de carbone.
  3. Procédé selon la revendication 1 ou 2 dans lequel n vaut 1.
  4. Procédé selon l'une quelconque des revendications 1 à 3 dans lequel p vaut de 1 à 8.
  5. Procédé selon l'une quelconque des revendications 1 à 4 dans lequel le procédé est un procédé pour isoler les phosphates des minerais.
  6. Procédé selon la revendication 5 dans lequel le procédé est un procédé de flottation directe pour isoler l'apatite des minerais.
  7. Procédé selon l'une quelconque des revendications 1 à 6 dans lequel le pH pendant le procédé est compris entre 8 et 11.
  8. Composition de collecteurs à utiliser dans le procédé selon l'une quelconque des revendications 1 à 7 contenant un collecteur primaire qui comprend un composé de phosphate de formule I
    Figure imgb0017
     dans lequel R représente un groupe hydrocarboné saturé ou insaturé, linéaire ou ramifié, contenant de 8 à 24 atomes de carbone, A représente un motif oxyde d'alkylène ; Y représente H, Na, K ou un ammonium ou un ammonium alkylé, n vaut de 1 à 3, p vaut de 0 à 25, X est choisi parmi les mêmes groupes que R-Ap ou Y, ou dans lequel R représente un groupe hydrocarboné saturé ou insaturé, linéaire ou ramifié qui contient de 1 à 12 atomes de carbone et au moins un motif A est présent qui est un motif oxyde de propylène ;
    un composé collecteur secondaire de monophosphate, et
    un ou plusieurs autres collecteurs secondaires qui sont un collecteur anionique choisi dans le groupe des acides gras, des sulfosuccinates d'alkyle, des maléates d'alkyle, des amidocarboxylates d'alkyle, des esters d'amidocarboxylates d'alkyle, des benzensulfonates d'alkyle, des sulfonates d'alkyle, des acides gras sulfonés, ou un collecteur non ionique du groupe des alcoxylates, des alkylglucosides, des alkyléthanolamides, ou un mélange de deux ou plus de ces collecteurs anioniques et non ioniques.
  9. Composition de collecteurs selon la revendication 8 dans laquelle la quantité du composé de phosphate de formule I est comprise entre 5 et 45 % en poids sur le phosphate total.
  10. Pâte comprenant du minerai siliceux concassé et broyé et une composition de collecteurs selon la revendication 8 ou 9.
EP18732097.3A 2017-07-04 2018-06-22 Procédé de traitement de minerais silicieux non sulfuriques et composition collectrice associée Active EP3648891B1 (fr)

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EP17179626 2017-07-04
PCT/EP2018/066793 WO2019007714A1 (fr) 2017-07-04 2018-06-22 Procédé de traitement de minerais siliceux non sulfurés et composition de collecteur associée

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CA3127400A1 (fr) 2019-02-01 2020-08-06 Basf Se Melange d'acides gras et de phosphates d'alkylether utilise en tant que collecteur pour la flottation de minerai de phosphate
EP4364852A1 (fr) 2022-11-04 2024-05-08 Nouryon Chemicals International B.V. Composition de collecteur et procédé de flottation

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2424552A (en) 1945-05-01 1947-07-29 Clemmer Julius Bruce Froth flotation of nonmetallic minerals
GB1093504A (en) 1965-03-28 1967-12-06 Chem & Phosphates Ltd Flotation of siliceous ores
US4287053A (en) 1980-05-05 1981-09-01 Tennessee Valley Authority Beneficiation of high carbonate phosphate ores
DE4010279A1 (de) 1990-03-30 1991-10-02 Henkel Kgaa Verfahren zur gewinnung von mineralien aus nichtsulfidischen erzen durch flotation
DE4016792A1 (de) 1990-05-25 1991-11-28 Henkel Kgaa Verfahren zur gewinnung von mineralien aus nichtsulfidischen erzen durch flotation
DE4133063A1 (de) 1991-10-04 1993-04-08 Henkel Kgaa Verfahren zur herstellung von eisenerzkonzentraten durch flotation
DE4138911A1 (de) 1991-11-27 1993-06-03 Henkel Kgaa Verfahren zur gewinnung von mineralien aus nichtsulfidischen erzen durch flotation
RU2078619C1 (ru) * 1994-12-16 1997-05-10 Акционерное общество "Химпром" Реагент-собиратель для флотации несульфидных руд
RU2259237C1 (ru) * 2004-03-15 2005-08-27 ФГУП "Всероссийский научно-исследовательский институт химической технологии" Способ получения фосфорсодержащих собирателей для флотации руд
RU2283187C1 (ru) * 2005-03-03 2006-09-10 Сергей Анатольевич Щелкунов Композиция для флотации фосфорсодержащих руд
WO2015000931A2 (fr) 2013-07-05 2015-01-08 Akzo Nobel Chemicals International B.V. Synthèse de nouveaux tensio-actifs anioniques et leur utilisation comme collecteurs dans une flottation par moussage de minerais non sulfurés

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CA3068885A1 (fr) 2019-01-10
RU2741494C1 (ru) 2021-01-26
WO2019007714A1 (fr) 2019-01-10
CA3068885C (fr) 2024-03-19
BR112019027877A2 (pt) 2020-07-07
EP3648891A1 (fr) 2020-05-13

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