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
  • 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 extraction of minerals from non-sulfidic ores by flotation, in which esters of dicarboxylic acids with fatty acid monoalkanolamides, optionally in a mixture with other anionic or nonionic surfactants, are used as collectors.
• Flotation is a generally used sorting process for separating valuable minerals from the gangue, which is used to prepare mineral ores.
• the ore is first ground and dry, but preferably wet, and suspended in water.
• a collector is added, often in conjunction with other reagents, which include foaming agents, regulators, pushers (deactivators) and / or Beieber (activators), to separate the valuable minerals from the gangue minerals in the ore during the subsequent flotation supports.
• these reagents are usually allowed to act on the finely ground ore for a certain time (conditioning).
• the collector causes the surface of the minerals to become hydrophobic, so that these minerals adhere to the gas bubbles formed during the aeration.
• the mineral components are made hydrophobic selectively in such a way that the undesirable ones Components of the ore do not adhere to the gas bubbles and remain behind, while the mineral-containing foam is stripped off and further processed.
• the aim of flotation is to extract the mineral of value from the ores in the highest possible yield and at the same time to obtain the best possible enrichment of the mineral.
• collectors In the flotative processing of non-sulfidic ores, mainly anionic or cationic surfactants are used as collectors. These have the task of adsorbing as selectively as possible on the surface of the valuable minerals in order to ensure a high concentration in the flotation concentrate. In addition, the collectors should develop a stable, but not too stable, flotation foam.
• collectors frequently used in the flotation of non-sulfidic ores, such as. B. fatty acids or alkyl sulfosuccinates [ Aufberei ⁇ tionstechnik, 26, 632 (1985)], but in many cases do not lead to a satisfactory yield of valuable minerals with economically justifiable collector quantities.
• the object of the invention was therefore to provide collectors with improved properties in the sense of a more economical design of the flotation process.
• the invention relates to a process for the extraction of minerals from non-sulfidic ores by flotation, in which ground ore is mixed with water to form a suspension, air is introduced into the suspension in the presence of a collector system and the resulting foam together with the foam contained therein separates flotated solids, and furthermore as a collector ester of Dicarboxylic acids with fatty acid monoalkanolamides are used which follow one of the formulas (I) to (VI),
• R ⁇ -CO for an acyl radical having 6 to 22 carbon atoms and 0, 1, 2 or 3 double bonds
• R for hydrogen or a methyl group
• m for numbers from 1 to 10
• X for hydrogen, an alkali metal or an ammonium radical stands.
• salt-type minerals e.g. B. fluorite, Scheelite, barite, apatite, iron oxides and other metal oxides, e.g. B. to understand the oxides of titanium and zirconium, as well as certain silicates and aluminosilicates.
• esters of dicarboxylic acids with fatty acid monoalkanolamides are known substances which are prepared using the relevant methods organic synthesis can be produced.
• a suitable method for their preparation is e.g. B. in reacting dicarboxylic acids, dicarboxylic acid monoesters or anhydrides with fatty acid monoalkanolamides.
• the preparation of such esters is further described in patent applications GB 615.665, CH 248.209, CH 256.764 and DE-A-3506838.
• esters which are distinguished by particularly advantageous properties in the process according to the invention are obtained on the basis of maleic acid, succinic acid, glutaric acid, adipic acid, citralonic acid or itaconic acid and mixtures of these acids with one another.
• Suitable amide components are fatty acid monoalkanolamides which follow the formula (VII)
• R ⁇ -CO and R 2 have the meanings given above.
• the acyl radical R * CO can be obtained, for example, from caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, elaidic acid, petroselinic acid, linoleic acid, linolenic acid, gadoleic acid, arachidonic acid, behenic acid or erucic acid deduce.
• the fatty acids on which the fatty acid alkanolamides are based can also be in the form of technical mixtures such as, for example, B.
• the alkanol residue is derived from monoethanol-1,2-amine or monopropanol-1,2-amine. Ester, which are distinguished properties in the inventive process by particularly advantageous Eigen ⁇ amides are obtained on the basis of Fettklaremonoalkanol ⁇ , in which R ⁇ -CO lenstoffatomen acyl radicals having 12 to 18 coal and 0 or 1 double bond and R 2 is hydrogen .
• the process according to the invention permits the use of the esters of dicarboxylic acids with fatty acid monoalkanolamides as collectors for the extraction of minerals from non-sulfidic ores by flotation alone or in the presence of further anionic or nonionic surfactants.
• anionic surfactants are to be understood as meaning fatty acids, alkyl sulfates, alkyl ether sulfates, alkyl sulfosuccinates, alkyl sulfosuccinamates, alkyl benzene sulfonates, alkyl sulfonates, petroleum sulfonates, acyl lactylates, sarcosides, alkyl phosphates and alkyl ether phosphates. All of these anionic surfactants are known compounds, the preparation of which - unless otherwise stated - e.g. in J. Falbe, U.
• Hasserodt ed.
• Catalysts ed.
• surfactants ed.
• mineral oil additives ed.
• J. Falbe ed.
• Suitable fatty acids here are in particular the straight-chain fatty acids of the formula (VIII) obtained from vegetable or animal fats and oils, for example by splitting and optionally fractionating and / or separating according to the crosslinking process.
• VIII straight-chain fatty acids of the formula (VIII) obtained from vegetable or animal fats and oils, for example by splitting and optionally fractionating and / or separating according to the crosslinking process.
• R3 represents an aliphatic hydrocarbon radical having 12 to 18 carbon atoms and 0, 1, 2 or 3 double bonds and Y represents an alkali metal, alkaline earth metal or an ammonium radical.
• Y represents an alkali metal, alkaline earth metal or an ammonium radical.
• Suitable alkyl sulfates are the water-soluble salts of sulfuric acid semiesters of fatty alcohols of the formula (IX),
• R ⁇ represents a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms and Z represents an alkali metal or an ammonium radical.
• the water-soluble salts of sulfuric acid semiesters of fatty alcohol polyglycol ethers of the formula are suitable as alkyl ether sulfates
• R5 is a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms
• R *> is hydrogen or a methyl group
• n is 1 to 30, preferably 2 to 15 and Z has the meaning given above.
• Suitable alkvisulfosuccinates are sulfosuccinic acid monoesters of fatty alcohols of the formula (XI) R -00C-CH 2 -CH-C00Z (XI)
• 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 alkylsulfosuccinamates are sulfosuccinic acid monoamides from fatty acids of the formula (XII)
• R ⁇ is a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms and Z has the meaning given above.
• Suitable alkylbenzenesulfonates are substances of the formula (XIII)
• R represents a straight-chain or branched alkyl radical having 4 to 16, preferably 8 to 12 carbon atoms and Z has the meaning given above.
• Suitable alkyl sulfonates are substances of the formula (XIV)
• R 10 -S0 3 Z (XIV) in the RIO stands for a straight-chain or branched alkyl radical having 12 to 18 carbon atoms and Z has the meaning given above.
• Suitable petroleum sulfonates are substances which are obtained by reacting lubricating oil fractions with sulfur trioxide or oleu and then neutralizing with sodium hydroxide solution. Products in which the hydrocarbon residues predominantly have chain lengths of 8 to 22 carbon atoms are particularly suitable here.
• Suitable acyl lactylates are substances of the formula (XV)
• R 11 represents an aliphatic, cycloaliphatic or alicyclic, optionally substituted by hydroxyl groups, hydrocarbon radical having 7 to 23 carbon atoms and 0, 1, 2 or 3 double bonds and Z has the meaning given above.
• acyl lactylates in flotation is described in DE-A-3238060.
• Suitable sarcosides are substances of the formula (XVI)
• R * represents an aliphatic hydrocarbon radical having 12 to 22 carbon atoms and 0, 1, 2 or 3 double bonds.
• Suitable alkyl phosphates and alkyl ether phosphates are substances of the formulas (XVII) and (XVIII)
• R 3 and d R 1 ⁇ 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 zero, in the case of the alkyl ether phosphates are numbers from 1 to 15 and Z has the meaning given above be ⁇ sits.
• 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 preparation of such compounds.
• nonionic surfactants are to be understood as meaning fatty alcohol polyglycol ethers, alkylphenol polyglycol ethers, fatty acid polyglycol esters, fatty acid amide polyglycol ethers, fatty amine polyglycol ethers, mixed ethers, hydroxy mixed ethers and alkyl glycosides. All of these nonionic surfactants are Known compounds whose preparation - unless otherwise stated - for example in J.Falbe, U.
• Hasserodt ed.
• Catalysts ed.
• surfactants ed.
• mineral oil additives ed.
• J.Falbe ed.
• Suitable fatty alcohol polyol ethers are addition products of an average of n moles of ethylene and / or propylene oxide onto fatty alcohols, which follow the formula (XIX)
• R ⁇ -5 is a linear or branched alkyl radical having 8 to 22, preferably 12 to 18 carbon atoms
• R *> is hydrogen or a methyl group
• n is a number from 1 to 30, preferably 2 to 15.
• Suitable alkylphenol polyglycol ethers are addition products of an average of n moles of ethylene and / or propylene glycol onto alkylphenols which follow the formula (XX)
• R 1 ⁇ represents an alkyl radical having 4 to 15, preferably 8 to 10 carbon atoms and R6 and n have the meanings given above.
• Suitable fatty acid polycoesters are addition products of an average of n moles of ethylene and / or propylene oxide with fatty acids which follow the formula (XXI)
• R 1-7 represents an aliphatic hydrocarbon radical having 5 to 21 carbon atoms and 0, 1, 2 or 3 double ligatures and R 6 and n have the meanings given above.
• Suitable fatty acid amide polyglycol ethers are addition products of an average of n moles of ethylene oxide and / or propylene oxide onto fatty acid amides, which follow the formula (XXII)
• Suitable fatty amine polyol ethers are addition products of an average of n moles of ethylene and / or propylene oxide onto fatty amines, which follow the formula (XXIII)
• R 19 represents an alkyl radical having 6 to 22 carbon atoms and R & n have the meanings given above.
• Reaction products of fatty alcohol polyglycol ethers with alkyl chlorides of the formula (XXIV) are suitable as mixed ethers,
• R 20 represents an aliphatic carbon radical having 6 to 22 carbon atoms and 0, 1, 2 or 3 double bonds
• R 20 represents an alkyl radical having 1 to 4 carbon atoms and R ⁇ and n have the meanings given above.
• R21 represents an alkyl radical having 6 to 16 carbon atoms
• R 2 represents an alkyl radical having 1 to 4 carbon atoms
• R ⁇ and n have the meanings given above.
• Suitable alkyl olvcosides are substances of the formula (XXVI)
• G represents a symbol for a glycose unit derived from a sugar with 5 or 6 carbon atoms, x for a number between 1 and 10 and R23 for an aliphatic hydrocarbon radical with 6 to 22 carbon atoms and 0, 1, 2 or 3 double bonds.
• G is preferably a Glucose unit and x for numbers from 1.1 to 1.6.
• esters of dicarboxylic acids with fatty acid monoalkanolamides are used not alone but in a mixture with other anionic or nonionic surfactants, these mixtures advantageously have a content of 5 to 95% by weight, preferably 10 to 60% by weight, of the ester.
• the surfactant mixture must be used in a certain minimum amount. However, a maximum amount of surfactant mixture must not be exceeded, since otherwise the foam formation becomes too strong and the selectivity towards the valuable minerals decreases.
• esters or their mixtures with other anionic or nonionic surfactants are used in the sense of the invention depend on the type of ores to be floated and on their content of valuable minerals. As a result, the amounts required in each case can vary within wide limits.
• the esters to be used according to the invention or their mixtures with anionic or nonionic surfactants are used in amounts of 50 to 2000, preferably 100 to 1500 g, per ton of crude 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 State of the art.
• a preferred field of application of the method is the flotation of salt-type minerals, in particular apatite ores.
• collector AI maleic acid oleic acid monoethanola idester
• the flotation task had the following grain size distribution:
• the collectors according to the invention were used alone and in combination with an alkyl sulfosuccinate Na / NH4 salt (B1) or a technical oleic acid (B2) as co-collectors, the mixing ratio collector: co-collectors 50:50 to 70:30 Parts by weight was.
• a Denver laboratory flotation machine type D1 was floated in the 2-1 cell, the cleaning stages (2 to 4 Post-cleanings) were carried out in a corresponding 1-1 cell.
• Water of 3 ° d was used as the flotation water; the cloud density during pre-flotation was approx. 500 g / 1.
• a phenol-formaldehyde condensate (Cl) was used in a dosage of 200 g / t.
• the pH of the slurry was adjusted to 10 with sodium hydroxide.
• the conditioning of the reagents was carried out with stirring at a stirrer speed of 1000 rpm, the conditioning time for pushers and collectors was 5 minutes in each case.
• the flotation was carried out at a speed of 1100 rpm (2-1 cell) or 1000 rpm (1-1 cell), the flotation time was approximately 4 minutes, during which the flotation foam was removed manually.
• Example 1 In the cleaning flotations, the flotation concentrate of the pre-flotation (rougher concentrate) was added to the 1-1 cell without the addition of reagents and flotated at 1000 rpm for about 4 minutes.
• Example 1 and Comparative Example 1 were each carried out with 4 cleaning stages, and Examples 2 to 5 with two cleaning stages. The results obtained are summarized in Tab. 1.
• Examples 1 to 5 show that when the esters are used as collectors in the sense of the invention, a higher P 2 ⁇ 5 output can be achieved with the same dosage than using the standard collector oleic acid.
• the esters are combined with standard collectors, an increase in the selectivity towards the valuable minerals is observed, so that fewer cleaning stages are required to achieve salable mineral concentrates.
• Tab. 1 Flotation of minor apatite ore in the Denver cell; Percentages by weight
• the ore was already ground up in the slurry. After wet sieving, a particle size fraction of 50-100 ⁇ m was used as the task. A modified Hallimond tube with a volume of 165 ml and a stirring speed of 400 rpm was used as the flotation cell. In each case, 2 g of ore (dry content) were conditioned and floated at pH 10 (adjusted with sodium hydroxide) in water at 20 ° d (calcium ions only). The conditioning time for the hardening water was 5 minutes, for the collector 10 minutes; the flotation was carried out over a period of 2 minutes.
• the collectors according to the invention were used alone or in a mixture with co-collectors.
• the alkyl sulfosuccinate (B1, comparative test V2) was used as the reference substance.
• the results of the flotation tests are summarized in Table 2.
• Examples 6 to 8 show that the use of the esters of dicarboxylic acids with fatty acid monoalkanol amides - alone or in mixtures with standard collectors - as collectors in the sense of the invention improve both the phosphate content in the concentrate and the mass and thus also the phosphate yield.
• Tab. 2 Flotation of Swedish apatite ore in the modified Hallimond tube

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• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

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• 1990
  • 1990-05-25 DE DE4016792A patent/DE4016792A1/de not_active Withdrawn
• 1991
  • 1991-05-17 CA CA002083818A patent/CA2083818A1/en not_active Abandoned
  • 1991-05-17 AU AU78612/91A patent/AU636763B2/en not_active Expired - Fee Related
  • 1991-05-17 WO PCT/EP1991/000922 patent/WO1991018674A1/de not_active Application Discontinuation
  • 1991-05-17 BR BR919106501A patent/BR9106501A/pt unknown
  • 1991-05-17 EP EP91909196A patent/EP0530233A1/de not_active Ceased
  • 1991-05-24 ZA ZA913964A patent/ZA913964B/xx unknown
• 1992
  • 1992-11-24 FI FI925328A patent/FI925328A0/fi not_active Application Discontinuation

Non-Patent Citations (1)

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