WO2019007714A1 - PROCESS FOR TREATING NON-SULFURIZED SILICEOUS ORES AND ASSOCIATED COLLECTOR COMPOSITION - Google Patents

PROCESS FOR TREATING NON-SULFURIZED SILICEOUS ORES AND ASSOCIATED COLLECTOR COMPOSITION Download PDF

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Publication number
WO2019007714A1
WO2019007714A1 PCT/EP2018/066793 EP2018066793W WO2019007714A1 WO 2019007714 A1 WO2019007714 A1 WO 2019007714A1 EP 2018066793 W EP2018066793 W EP 2018066793W WO 2019007714 A1 WO2019007714 A1 WO 2019007714A1
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Prior art keywords
collector
carbon atoms
formula
ores
collector composition
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PCT/EP2018/066793
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English (en)
French (fr)
Inventor
Natalija Smolko-Schvarzmayr
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Akzo Nobel Chemicals International B.V.
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Priority to BR112019027877-0A priority Critical patent/BR112019027877B1/pt
Priority to EP18732097.3A priority patent/EP3648891B1/de
Priority to RU2020104700A priority patent/RU2741494C1/ru
Priority to CA3068885A priority patent/CA3068885C/en
Publication of WO2019007714A1 publication Critical patent/WO2019007714A1/en

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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.
  • DE ⁇ 63 etheramines with at least one anionic or non- ionic 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 1 1 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
  • 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, alkylamidocarboxylat.es, esters of alkylamidocarboxylat.es, alkylbenzensulphonat.es, 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.
  • the degree of branching is 0-2.2 and when R contains more than 12 carbon atoms the degree of branching is preferably between 1 .5 and 3.
  • 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.
  • degree of alkoxylation as used herein is meant the total number of alkylene oxide units A between the alkyl chain R and phosphorous containing unit, which corresponds with the value of p in formula I.
  • a degree of alkoxylation is an average number and does not have to be an integer.
  • 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%. In further embodiments 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 1 1 .
  • 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
  • водородн ⁇ е как ⁇ ное кактивное как кактрол ⁇ ество preferably of the formula RCOOY
  • sulphonated fatty acids that are preferably of the formula RCH(SO3Y)COOY
  • alkylsulfosuccinates that are preferably of the formula III
  • 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(SO3Y)COOY, alkylsulfosuccinates that are preferably of the formula III
  • alkylmaleates that are preferably of the formula IV
  • alk lamidocarboxylat.es that are preferably of the formula 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 , - CH(CH 3 ) 2 , -CH 2 CH(CH 3 ) 2 , -CH(CH3)CH 2 CH 3j Z is -H, -CH 3 or -CH 2 CH 3 , esters of the above alkylamidocarboxylat.es (following the formula V of the alkylamidocarboxylat.es compounds wherein Y is an alcohol derived hydrocarbon group, such as also described in US20160129456),
  • alkylbenzensulphonat.es that are preferably of the formula VI
  • alkylsulphonates that are preferably of the formula VII
  • alkoxylates alkoxylated fatty alcohols RO(A)H, alkoxylated fatty acids RC(O)O(A)H), alkyl glycosides R(C 6 O 6 Hn) k , alkylethanolamides of the formulae VIII or IX
  • each R, A and Z independently have the above-indicated meaning, f is 1 -25, preferably f is 1 -15, and most preferable 1 -10 k is 1 -5, preferably k is 1 -2, and each f is independently 1 to 25;
  • 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% In another preferred embodiment 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 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 (CDCI 3 ): ⁇ 4 to -1 ppm monophosphate; ⁇ -12 to -16 ppm pyro-phosphate; ⁇ -28 to -30 ppm polyphosphate.
  • the flotation was performed at RT (20 ⁇ 1 °C) and air supplied at 3.5 l/min speed. The rougher flotation, followed by two cleaning steps (1 .0L Denver cells), was performed. All fractions (tailings, middlings and concentrate) were collected and analyzed. Figure 1 illustrates the flotation steps performed and the different fractions collected.
  • collector composition 1 67 wt% oleic fatty acid, 23 wt% monophosphate of oleyl ethoxylate(4EO), 10 wt% pyrophosphate of oleyl alcohol ethoxylate(4EO) as prepared in Example 1A- invention
  • collector composition 2 67 wt% oleic fatty acid, 33 wt% monophosphate of oleyl ethoxylate(4EO) prepared by reacting the ethoxylated oleyl alcohol as employed in Example 1 A with polyphosphoric acid - comparison 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 is calculated according to the following equation:
  • Example 2 was repeated but the following two collector compositions were compared (see for dosage below Table 2)

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PCT/EP2018/066793 2017-07-04 2018-06-22 PROCESS FOR TREATING NON-SULFURIZED SILICEOUS ORES AND ASSOCIATED COLLECTOR COMPOSITION WO2019007714A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BR112019027877-0A BR112019027877B1 (pt) 2017-07-04 2018-06-22 Processo para tratar minérios não-sulfúricos siliciosos com uma composição de coletor, composição de coletor e polpa
EP18732097.3A EP3648891B1 (de) 2017-07-04 2018-06-22 Verfahren zur behandlung von kieseligen nichtschwefeligen erzen und sammelzusammensetzung dafür
RU2020104700A RU2741494C1 (ru) 2017-07-04 2018-06-22 Способ обработки кремнистых несульфидных руд и соответствующая композиция собирателей
CA3068885A CA3068885C (en) 2017-07-04 2018-06-22 Process to treat siliceous non-sulfidic ores and collector composition therefor

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EP17179626.1 2017-07-04
EP17179626 2017-07-04

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020157106A1 (en) 2019-02-01 2020-08-06 Basf Se Mixture of fatty acids and alkylether phosphates as a collector for phosphate ore flotation
EP4364852A1 (de) 2022-11-04 2024-05-08 Nouryon Chemicals International B.V. Sammlerzusammensetzung und flotationsverfahren

Citations (8)

* 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
EP0544185A1 (de) 1991-11-27 1993-06-02 Henkel KGaA Verfahren zur Gewinnung von Mineralien aus nichtsulfidischen Erzen durch Flotation
US20160129456A1 (en) 2013-07-05 2016-05-12 Akzo Nobel Chemicals International B.V. The Synthesis of New Anionic Surfactants and Their Use as Collectors in Froth Flotation of Non-Sulphidic Ores

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (8)

* 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
EP0544185A1 (de) 1991-11-27 1993-06-02 Henkel KGaA Verfahren zur Gewinnung von Mineralien aus nichtsulfidischen Erzen durch Flotation
US20160129456A1 (en) 2013-07-05 2016-05-12 Akzo Nobel Chemicals International B.V. The Synthesis of New Anionic Surfactants and Their Use as Collectors in Froth Flotation of Non-Sulphidic Ores

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020157106A1 (en) 2019-02-01 2020-08-06 Basf Se Mixture of fatty acids and alkylether phosphates as a collector for phosphate ore flotation
EP4364852A1 (de) 2022-11-04 2024-05-08 Nouryon Chemicals International B.V. Sammlerzusammensetzung und flotationsverfahren
WO2024094486A1 (en) 2022-11-04 2024-05-10 Nouryon Chemicals International B.V. Beneficiation process for non-sulfidic minerals or ores

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BR112019027877B1 (pt) 2023-03-21
BR112019027877A2 (pt) 2020-07-07
CA3068885C (en) 2024-03-19
RU2741494C1 (ru) 2021-01-26
CA3068885A1 (en) 2019-01-10
EP3648891B1 (de) 2021-09-01

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