EP0270018B1 - Utilisation d'Acides N-alkyle et N-alkényle aspartiques comme co-collecteurs pour la flottation de minerais non sulfurés - Google Patents

Utilisation d'Acides N-alkyle et N-alkényle aspartiques comme co-collecteurs pour la flottation de minerais non sulfurés

Info

Publication number
EP0270018B1
EP0270018B1 EP87117541A EP87117541A EP0270018B1 EP 0270018 B1 EP0270018 B1 EP 0270018B1 EP 87117541 A EP87117541 A EP 87117541A EP 87117541 A EP87117541 A EP 87117541A EP 0270018 B1 EP0270018 B1 EP 0270018B1
Authority
EP
European Patent Office
Prior art keywords
alkyl
flotation
collectors
alkenyl
aspartic acids
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.)
Expired - Lifetime
Application number
EP87117541A
Other languages
German (de)
English (en)
Other versions
EP0270018A3 (en
EP0270018A2 (fr
Inventor
Beatrix Dr. Kottwitz
Wolfgang Von Rybinski
Rita Köster
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to AT87117541T priority Critical patent/ATE77262T1/de
Publication of EP0270018A2 publication Critical patent/EP0270018A2/fr
Publication of EP0270018A3 publication Critical patent/EP0270018A3/de
Application granted granted Critical
Publication of EP0270018B1 publication Critical patent/EP0270018B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • B03D1/01—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
    • B03D1/008—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
    • 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 the use of N-alkyl and / or N-alkenylaspartic acids as co-collectors in the flotation of non-sulfidic ores and a process for separating non-sulfidic ores by flotation.
  • Flotation is a generally used sorting process for the processing of mineral raw materials to separate valuable minerals from the gangue.
  • Non-sulfidic minerals such as apatite, fluorite, scheelite and other salt-like minerals, cassiterite and other metal oxides, such as titanium or zirconium oxides, as well as certain silicates and aluminosilicates can be prepared by flotation processes.
  • the ore is pre-crushed and dry, but preferably ground wet and suspended in water.
  • suspensions are usually added to collectors, often in conjunction with auxiliary reagents such as foaming agents, regulators, pushers (deactivators) and / or stimulants (activators), in order to support the separation of the valuable minerals from the gangue components of the ore during the subsequent flotation.
  • auxiliary reagents such as foaming agents, regulators, pushers (deactivators) and / or stimulants (activators)
  • these reagents are usually allowed to act on the finely ground ore for a certain time (conditioning). As a result, a foam is generated on the surface of the suspension, the collector ensuring that the surface of the minerals is rendered hydrophobic.
  • the mineral-containing foam is stripped off and worked up using known methods.
  • the aim of the flotation is to extract the mineral of value from the ores in the highest possible yield, while at the same time maintaining the best possible enrichment.
  • Anionic and cationic surfactants are mainly used as collectors in the flotative processing of non-sulfidic ores. These should adsorb as selectively as possible on the valuable mineral surface in order to achieve a high concentration in the flotation concentrate. In addition, the collectors should develop a stable, but not too stable, flotation foam. For ores containing gangue minerals from anionic collectors, e.g. Unsaturated and saturated fatty acids, especially tall oil fatty acids and oleic acids, alkyl sulfates or sulfonates, are not hydrophobicized, these are sufficient as collectors. For more difficult to float ores, such as tin ore, more selective collectors, such as Phosphonic acids (DD-C-76 974) or alkylsulfosuccinamides (US-A-3 830 366) are used.
  • Phosphonic acids DD-C-76 974
  • alkylsulfosuccinamides US-A
  • Suitable organic phosphonates are water-soluble salts of organic phosphonic acids, for example salts of styrene phosphonic acid, for the flotation of non-sulfidic ores, in particular tin ores. as for example in X. International Mineral Proc. Congress - IMM, E. Tmür, pages 626 to 627, London 1973 (0.S. Bogandow).
  • Collectors frequently used in the flotation of non-sulfidic ores are, for example, alkyl monocarboxylic acids, such as unsaturated long-chain fatty acids, such as the tall oil fatty acid mentioned above.
  • alkyl monocarboxylic acids such as unsaturated long-chain fatty acids, such as the tall oil fatty acid mentioned above.
  • di- and tricarboxylic acids are also used as flotation collectors (H. Schubert, H. Baldauf, A. Serrano, XII International Mineral Proc. Congress, Sao Paulo 1977).
  • the anionic and nonionic collectors used for the flotation of non-sulfidic ores do not lead to a satisfactory output of the valuable minerals with economically justifiable collector quantities.
  • the present invention was therefore based on the object of providing improved collectors in the sense of a more economical design of the flotation processes, with which larger yields of valuable minerals can be achieved either with constant collector quantities and constant selectivity, or constant mineral mineral yields with reduced collector quantities.
  • N-alkyl and / or N-alkenylaspartic acids can advantageously be used as co-collectors in the flotation of non-sulfidic ores.
  • the present invention relates to the use of N-alkyl and / or N-alkenylaspartic acids, the alkyl and / or alkenyl radicals of which are straight-chain or branched, have 8 to 18 carbon atoms and optionally a hydroxyl group and / or an ether bridge instead of a CH2 group own, or their salts as co-collectors in the flotation of non-sulfidic ores.
  • N-alkyl and N-alkenylaspartic acids their alkali or ammonium salts can also be used advantageously.
  • the corresponding potassium salts and preferably the corresponding sodium salts of N-alkyl and / or N-alkenylaspartic acids are advantageously used.
  • N-alkyl and / or N-alkenyl amino acids and their alkali or ammonium salts are generally known from the literature. It takes place on the one hand by means of the various alkylation reactions on the nitrogen of the amino acid, as described for example in Houben-Weyl Volume 11/2, and on the other hand by the addition of primary or secondary amines to unsaturated carboxylic acids (J. March "Advanced Organic Chemistry: Reactions, Mechanism and Structure ", McGraw-Hill, 1977).
  • the latter process starting from maleic acid esters, is used to prepare the N-alkyl and / or N-alkenylaspartic acids and salts referred to here.
  • the maleic acid esters with the corresponding amine component can either be in a solvent (US Pat. No. 2,438,092) or solvent-free, optionally with the addition of a catalyst such as, for example, acetic acid, alkali metal thiocyanates or O, N-dialkylphosphocarbamates (SU-A-77 10 87) be implemented.
  • anionic and / or nonionic collectors can also be used.
  • N-alkyl and / or N-alkenyl aspartic acids used as anionic collector tallow alkyl sulfosuccinamides and / or oleic acid.
  • a reaction product of propylene glycol glucoside with ⁇ -dodecane epoxide can advantageously be used as the nonionic collector.
  • the amounts in which the co-collectors to be used according to the invention are used depend in each case on the type of non-sulfidic ores to be floated and on their content of valuable mineral. As a result, the amounts required can vary within wide limits.
  • the co-collectors according to the invention are used in collector mixtures in amounts of 50 to 2000 g / t crude ore.
  • the N-alkyl and / or N-alkenylaspartic acids to be used according to the invention are used in combination with anionic, cationic and / or nonionic collectors in the known flotation processes for non-sulfidic ores instead of the known collectors.
  • the customary reagents such as foaming agents, regulators, activators, deactivators, etc. are also added to the aqueous slurries of the ground ores.
  • the flotation is carried out under the conditions of the methods of the prior art.
  • N-alkyl and / or N-alkenylaspartic acids to be used according to the invention can be used, for example, as co-collectors in the flotative processing of Scheelite ore, Cassiterite ore and Fluorite ore.
  • Another object of the invention is a process for the separation of non-sulfidic ores by flotation, in which ground ore is mixed with water to form an ore suspension, air is introduced into the suspension in the presence of the collector mixture and the resulting foam is separated off together with the mineral contained therein.
  • This process is characterized in that N-alkyl and / or N-alkenylaspartic acids are used as co-collectors.
  • the ore sample has the following grain size distribution: 28% - 25 ⁇ m 43% 25-100 ⁇ m 29% 100-200 ⁇ m
  • Combinations of a sulfosuccinamide derived from a tallow amine with sodium salts of N-alkylaspartic acids in a weight ratio of 2: 1 were used as collector mixtures according to the invention.
  • the chain length of the N-alkylaspartic acids was C 16/18 (example 1) and C 12/14 (example 2).
  • the above-mentioned tallow alkyl sulfosuccinamide (Comparative Example 1) was used as a comparative collector.
  • the flotation experiments were carried out using a Humbold-Wedag laboratory flotation machine from KHD Industrieanlagen AG, Humbold-Wedag, Cologne (see Seifen-Fette-Wwachs 105) (1979), p. 248) in a 1 l flotation cell.
  • Deionized water was used to make the slurry.
  • the cloud density was 400 g / l.
  • Water glass with a dosage of 2,000 g / t was used as the pusher.
  • the conditioning time of the pusher was 10 min at a stirring speed of 2,000 l / min.
  • the type of collector dosage is shown in Table 1.
  • the conditioning time of the collector was 3 minutes.
  • a valuable South African cassiterite ore was floated, which essentially contains granite, tourmaline and magnetite as a gait.
  • the flotation task had the following grain size distribution: 49.5% - 25 ⁇ m 43.8% 25-63 ⁇ m 6.7% + 63 ⁇ m
  • the flotation experiments were carried out in a 1 1 laboratory flotation cell at room temperature. Water glass with a dosage of 2,000 g / t was used as the pusher, the pH of the slurry was adjusted to pH 5 with sulfuric acid before the addition of the collector. Flotation was carried out with a turbidity of 500 g ore per liter of tap water with a hardness of 16 ° dH. The flotation time of the pre-flotation was 4 min at a stirring speed of 1200 l / min.
  • the Na salt of N-tallow alkyl aspartic acid with a chain length of 16 to 18 carbon atoms was used as the co-collector according to the invention.
  • the mixing ratio of collector to co-collector was 1: 2 (example 3).
  • Technical styrenephosphonic acid was used for comparative example 2.
  • a Mexican fluorite ore was floated with predominantly silicates as gait.
  • the flotation task had the following grain size distribution: 35% - 25 ⁇ m 50% 25 - 80 ⁇ m 15% + 80 ⁇ m
  • the pre-flotation concentrate was further ground before the subsequent cleaning stages.
  • the grain size was then: 98% - 44 ⁇ m
  • the flotation experiments were carried out in a 1 1 Denver cell using extremely hard water (350 ° dH).
  • the trigger was alkaline-digested starch with a dosage of 1,000 g / t.
  • the Na salt of N-tallow alkyl aspartic acid with a chain length of 16 to 18 carbon atoms in combination with oleic acid in a ratio of 1: 9 was used as the co-collector according to the invention (example 4).
  • the standard collector was oleic acid (Comparative Example 3).

Landscapes

  • Manufacture And Refinement Of Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Water Treatments (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
  • Detergent Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (6)

  1. Utilisation des acides N-alcoyl- et/ou N-alcényl aspartiques dont les radicaux alcoyl et/ou alcényle sont linéaires ou ramifiés, possèdent de 8 à 18 atomes de carbone et le cas échéant un groupe hydroxyle et/ou à la place d'un radical CH₂ possède un pont éther ou utilisation de leurs sels comme cocollecteurs lors de la flottation des minerais non sulfurés.
  2. Utilisation selon la revendication 1, caractérisée en ce que l'on met en oeuvre les sels de potassium, les sels d'ammonium et de préférence les sels de sodium des acides N-alcoyl- et/ou N-alcényl aspartiques.
  3. utilisation selon les revendications 1 et 2, caractérisée en ce qu'à côté des acides N-alcoyl- et N-alcényl aspartiques, on met en oeuvre additionnellement des collecteurs anioniques et/ou non ioniques dans un rapport allant de 20 : 1 à 1 : 20.
  4. Utilisation selon la revendication 3, caractérisée en ce qu'à côté des acides N-alcoyl- et/ou N-alcényl aspartiques, on met en jeu comme collecteurs anioniques une alcoylsuccinamide de suif et/ou de l'acide oléique.
  5. Utilisation selon la revendication 3, caractérisée en ce qu'à côté des acides N-alcoyl- et/ou N-alcényl aspartiques, on met en jeu un produit de transformation obtenu à partir de propylène glycol de glucoside avec de l'α-époxyde de dodécane en tant que collecteur non ionique.
  6. Utilisation selon les revendications 1 à 5, caractérisée en ce que les acides alcoyl et/ou alcényl aspartiques dans les mélanges de collecteurs, sont utilisés en quantités allant de 50 à 2000 g/t de minerai d'origine.
EP87117541A 1986-12-05 1987-11-27 Utilisation d'Acides N-alkyle et N-alkényle aspartiques comme co-collecteurs pour la flottation de minerais non sulfurés Expired - Lifetime EP0270018B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87117541T ATE77262T1 (de) 1986-12-05 1987-11-27 Verwendung von n-alkyl- und nalkenylasparagins|uren als co-sammler fuer die flotation nichtsulfidischer erze.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3641579 1986-12-05
DE19863641579 DE3641579A1 (de) 1986-12-05 1986-12-05 N-alkyl- und n-alkenylasparaginsaeuren als co-sammler fuer die flotation nichtsulfidischer erze

Publications (3)

Publication Number Publication Date
EP0270018A2 EP0270018A2 (fr) 1988-06-08
EP0270018A3 EP0270018A3 (en) 1990-04-18
EP0270018B1 true EP0270018B1 (fr) 1992-06-17

Family

ID=6315539

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87117541A Expired - Lifetime EP0270018B1 (fr) 1986-12-05 1987-11-27 Utilisation d'Acides N-alkyle et N-alkényle aspartiques comme co-collecteurs pour la flottation de minerais non sulfurés

Country Status (13)

Country Link
US (1) US4790932A (fr)
EP (1) EP0270018B1 (fr)
CN (1) CN1011296B (fr)
AT (1) ATE77262T1 (fr)
AU (1) AU601244B2 (fr)
BR (1) BR8706570A (fr)
CA (1) CA1320769C (fr)
DE (2) DE3641579A1 (fr)
ES (1) ES2031869T3 (fr)
FI (1) FI84321C (fr)
MX (1) MX169159B (fr)
PT (1) PT86278B (fr)
ZA (1) ZA879141B (fr)

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* Cited by examiner, † Cited by third party
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SE467239B (sv) * 1989-04-05 1992-06-22 Berol Nobel Ab Foerfarande foer flotation av jordartsmetallinnehaallande mineral samt medel daerfoer
DE4133063A1 (de) * 1991-10-04 1993-04-08 Henkel Kgaa Verfahren zur herstellung von eisenerzkonzentraten durch flotation
RU2192314C1 (ru) * 2001-07-16 2002-11-10 Иркутский государственный технический университет Способ флотации кальцито-флюоритовых руд
SE0302986D0 (sv) * 2003-11-13 2003-11-13 Akzo Nobel Nv Use of a derivative of aspartic acid as a collector in froth flotation processes
RU2259888C1 (ru) * 2004-02-13 2005-09-10 Читинский государственный университет (ЧитГУ) Способ обогащения карбонатно-флюоритовых руд и поточная линия для его осуществления
RU2268089C1 (ru) * 2004-08-17 2006-01-20 Федеральное государственное унитарное предприятие "Государственный научно-исследовательский, проектный и конструкторский институт горного дела и металлургии цветных металлов" ФГУП "Гипроцветмет" Способ флотационного обогащения флюоритовых руд
RU2360742C1 (ru) * 2007-12-10 2009-07-10 Государственное образовательное учреждение высшего профессионального образования Читинский государственный университет (ЧитГУ) Способ флотации руд и поточная линия для его осуществления
CN102120592B (zh) * 2011-04-25 2012-03-21 化工部长沙设计研究院 一种利用NaCl与碳酸锂混盐浮选提取碳酸锂的方法
RU2564550C1 (ru) * 2014-03-12 2015-10-10 Общество с ограниченной ответственностью "ЗабТехноКом" Способ флотации флюоритовых руд
US11472723B2 (en) 2016-10-20 2022-10-18 Newsouth Innovations Pty Limited Method for removing heavy metals from an aqueous solution
AU2017381628B2 (en) * 2016-12-23 2020-01-02 Akzo Nobel Chemicals International B.V. Process to treat phosphate ores
CN107520058B (zh) * 2017-08-23 2019-05-17 中南大学 一种金红石用选矿组合试剂及其选矿方法
CN112237996B (zh) * 2020-09-27 2021-08-17 中南大学 一种细粒辉锑矿和黄铁矿分离的浮选抑制剂及其应用
CN116903490B (zh) * 2021-08-09 2025-07-11 山东富斯特油脂科技有限公司 糖基丙胺类化合物、制备方法及其作为浮选剂的应用
US12138638B2 (en) 2021-09-09 2024-11-12 Clariant International Ltd Composition and method for use of 1-alkyl-5-oxopyrrolidine-3-carboxylic acids as collectors for phosphate and lithium flotation
FI4399029T3 (fi) * 2021-09-09 2025-05-07 Clariant Int Ltd Koostumus ja menetelmä 1-alkyyli-5-oksopyrrolidiini-3-karboksylihappojen käyttämiseksi fosfaatin ja litiumin vaahdotuksen kokoojana

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Also Published As

Publication number Publication date
ATE77262T1 (de) 1992-07-15
FI875336L (fi) 1988-06-06
PT86278B (pt) 1990-11-07
ZA879141B (en) 1988-06-06
AU8210987A (en) 1988-06-09
CA1320769C (fr) 1993-07-27
CN87107280A (zh) 1988-06-15
ES2031869T3 (es) 1993-01-01
FI84321B (fi) 1991-08-15
FI84321C (fi) 1991-11-25
FI875336A0 (fi) 1987-12-03
DE3641579A1 (de) 1988-06-16
MX169159B (es) 1993-06-23
BR8706570A (pt) 1988-07-12
DE3779878D1 (de) 1992-07-23
PT86278A (en) 1988-01-01
CN1011296B (zh) 1991-01-23
AU601244B2 (en) 1990-09-06
EP0270018A3 (en) 1990-04-18
US4790932A (en) 1988-12-13
EP0270018A2 (fr) 1988-06-08

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