GB2207619A - Ore purification - Google Patents

Ore purification Download PDF

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Publication number
GB2207619A
GB2207619A GB08718420A GB8718420A GB2207619A GB 2207619 A GB2207619 A GB 2207619A GB 08718420 A GB08718420 A GB 08718420A GB 8718420 A GB8718420 A GB 8718420A GB 2207619 A GB2207619 A GB 2207619A
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United Kingdom
Prior art keywords
flotation
apatite
solution
process according
carbon atoms
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.)
Withdrawn
Application number
GB08718420A
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GB8718420D0 (en
Inventor
Alan Reginald Minihan
Stephen Raymond Hayes
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Unilever PLC
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Unilever PLC
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Publication date
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Priority to GB08718420A priority Critical patent/GB2207619A/en
Publication of GB8718420D0 publication Critical patent/GB8718420D0/en
Publication of GB2207619A publication Critical patent/GB2207619A/en
Withdrawn legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • B03D1/021Froth-flotation processes for treatment of phosphate ores
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/008Organic compounds containing oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/01Organic compounds containing nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; Specified applications
    • B03D2203/02Ores
    • B03D2203/04Non-sulfide ores
    • B03D2203/06Phosphate ores

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  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Physical Water Treatments (AREA)

Abstract

Calcium phosphate containing materials, e.g. apatite can be separated from contaminant materials, e.g. calcite and silicates, by a selective froth flotation process. This process uses a mixture of a class of amine oxides and a branched chain C16 to C20 fatty acid and provides a high usable concentration of the apatite with good separation from the gangue.

Description

ORE PURIFICATION Field of the Invention: This invention relates to a froth flotation process for ore purification. More particularly, the invention relates to a process for the separation of the phosphate mineral known as apatite from contaminants which are mined with it.
Background to the Invention: Froth flotation has for many years been used to select from ground mineral ores desirable components and many chemicals have been employed for various purposes in the flotation processes hitherto used.
As is well known the principles of the process involve the preferential flotation of one component from the ground ore in the froth which rises to the top of the aqueous dispersion containing the selected chemicals, whilst other components of the ground ore pass through the system. Depending on the conditions, the desirable component can be floated out with the froth or, alternatively, passed out with the residual slurry for further separation at a later stage in the process.
The factors affecting these processes are highly complex and relate, obviously, to the type of ore under treatment, the chemicals used, the quality of the water used in the flotation process and many other factors such as the interaction of the flotation chemicals on each other and on the components of the ground ore to be treated.
Apatite is a group of calcium phosphate minerals which have the general formula Ca5 X(PO4)3 were X is a monovalent ion which may be F, C1, OH or d CO It occurs as hexagonal crystals, granular masses and other forms and is a major constituent of phosphate rock. This latter source comprises an apatite in association with calcium carbonate and other minerals, for example those which are silicate based.
This invention is particularly concerned with the extraction of apatite from ores containing significant amounts of calcite and silicate minerals. A typical ore to which the present invention can most readily be applied will contain between 5% and 35% apatite of the order of 10% to 40% calcite and the remainder various silicate compositions. In view of the large amounts of minerals which are treated by flotation processes, the cost effectiveness of the flotation chemicals is of great significance and even relatively minor improvements in yield can be of great commercial importance. Hitherto, the tendency has been to use relatively cheap materials such as tall oil, kerosene fractions and vegetable oils.
General description of the invention: The invention provides a process for the selective froth flotation of calcium phosphate containing materials in an aqueous flotation bath in the presence of calcium carbonate which comprises performing the flotation in the presence of a mixture of i) an amine oxide of formula R1R2R3N-0 in which R1 is an alkyl radical containing 1 to 3 carbon atoms, R2 is an alkyl radical containing 1 to 3 carbon atoms, and R3 is an alkyl radical containing 6 to 22 carbon atoms and ii) a branched chain C16 to C20 fatty acid. This process provides a high usable concentration of the desired apatite with good separation from the gangue.
Usually the flotation will be performed at a pH in the range from about 8 to about 12, preferably about 9 to about 10. The amine oxide and branched fatty acid will usually be present in the mixture in a weight ratio of from about 1:10 to about 1:1, preferably from about 1:3 to about 1:1. The process of the invention is of particular value wherein the electrolyte content of the feedstock water is above about 500 ppm.
The invention extends to the calcium phosphate containing materials obtained as a product of the process of the invention.
Literature: The applicants are aware of US 4337149 (Sherex Chemical Co) which describes a froth flotation process using amine oxides as promoters in the separation of phosphate ore but this disclosure does not describe the use of amine oxides with branched fatty acids to obtain the benefit identified by the applicants. The Tennessee Valley Authority disclosed the use of mixtures of branched C16-C18 fatty acids to recover Florida phosphate ore in US Defensive Publication T980002.
Test Method Microflotation Experiments: These used a microflotation cell based on Partridge and Smith and further modified by Harris (Mintek). Flotation experiments were carried out in electrolyte solutions with compositions designed to mimic those in use at the Foskor plant (Phalaborwa area) Eastern Transvaal. The hardness of these waters are well in excess of levels reached under normal conditions in equilibration with the minerals in distilled water.
Sample Preparation: 2g crushed, sieved (45-106 Am) pure mineral (Canadian fluorapatite, Iceland spar calcite or Phalaborwa diopside) was stirred vigorously in distilled water for five minutes. At the end of this period, the dispersion was allowed to settle. The supernatant liquid and any suspended fines ('slimes') was decanted off and the mineral washed into a 600 ml beaker with 250 mls distilled water and held under constant stirring. 4.8 mls of solution A and 4.8 mls of solution B were introduced, in order to duplicate the electrolyte composition of fresh river water in which mineral is conditioned with flotation chemicals at the Foskor plant.
(i) Solution A Solution B 1 litre of distilled 1 litre of distilled water containing water containing 10.29g CaCl2.2H2O 22.74g MgSO4.7H2O 2.05 NaCl 4.20g NaHCO3 0.75g KC1 0.21g NaF Mineral Conditioning: The silicate slurry was adjusted to 9.5 (dil. NaOH) and x mls of 0.5% (w/w) sodium silicate solution was added to the slurry with continued stirring. The pH was then restored to 9.5 and the suspension left stirring for 15 minutes. After this, 2.0 mg of surfactant (as a 0.1 mg ml 1 solution) was added under continuous stirring and the pH restored to 9.5 if necessary. A further 15 minutes of stirring was then allowed for conditioning of the mineral. 1.2 mls of solution C and 1.2 mls of solution D were added to 200 mi distilled water which was then added to the slurry, still under continuous stirring. A final pH adjustment to 9,5 was then carried out if necessary. This solution addition allows duplication of the electrolyte composition of a mixture of river water and recycled plant water ('reclaimed water') in which apatite flotation takes place at Foskor. The slurry was conditioned for a final 15 minutes.
(ii) Solution C Solution D 1 litre distilled 1 litre distilled water containing water containing 44.10g CaC12.2H2O 236.54g of MgSO4.7H2O 11.07g NaCl 0.87g of NaHCO3 0.84g of NaF 22.62g of K2SO4 90.88g of Na2SO4 The liquid/mineral slurry was then transferred to the microflotation cell, washing with distilled water to ensure quantitative transfer of the mineral and to make up a total volume of 600 ml (the volume of the micro-flotation apparatus).
Flotation of Mineral: Nitrogen gas was passed through the suspended mineral in the cell at the rate of .1 13 ml min for 5 minutes. At the end of this time, the gas flow was stopped and the mineral floated was collected, oven dried and weighed.
These test procedures were followed using tetradecyldimethylamine oxide obtainable from Akzo under the trade name Aromox DMl4D-W as the amine oxide component and isostearic acid obtainable from Unichema under the trade name Prisorene 3508 as the branched fatty acid. The tall oil was of commercial standard the nonionic surfactant was Nonylphenyltetraethyoxylate obtained from Union Carbide under the trade name Tergitol NP-4. The sodium silicate solution used had a weight ratio of Si2:Na2O of 2:1 and was obtained from Crosfield Chemicals under the tradename Crystal 120A. Comparative experiments were performed using a mixture of the amine oxide: branched fatty acid in a weight ratio of 3:7 at a level of 2 mg in the test method. This combination was compared with mixtures of each component with standard flotation components as currently employed at Foskor .The results are given in Tables I, II and III. NM indicates no measurements was made.
The term 'selectivity' is a measure of the separation of the desired apatite and the calcite. It is the difference between the percentages of these components which are floated.
Table I (tall oil and amine oxide) Volume (mls) % component floated Silicate Apatite Calcite Diopside Selectivity Solution Solution 0 35.3 30.2 1.9 5.1 1 12.8 28.3 NM (15.5) 2 7.5 21.1 NM (13.6) 3 4.4 17.6 NM (13.2) 5 4.2 7.9 1.4 (3.7) Table II (iso-stearic acid and nonionic surfactant) Volume (mls) % component floated Silicate Apatite Calcite Diopside Selectivity Solution Solution 0 62.8 57.0 6.4 5.8 1 57.0 43.9 NM 13.1 2 27.5 38.8 NM (1.3) 3 17.8 36.4 NM (18.6) 5 16.5 24.9 1.6 (8.4) Table III (iso-stearic acid and amine oxide) Volume (mls) % component floated Silicate Apatite Calcite Diopside Selectivity Solution Solution 0 50.5 29.8 0.8 20.7 1 46.1 19.5 NM 26.6 2 49.5 12.2 NM 37.3 3 32.6 13.8 NM 18.8 4 16.8 NM NM NM 5 8.2 14.0 0.5 (5.8) 8 NM 7.8 NM NM These results demonstrate the use of amine oxides and branched fatty acids together provide a high usable flotation of the desired apatite together with good separation from the gangue components.

Claims (6)

Claims
1. A process for the selective froth flotation of calcium phosphate containing materials in an aqueous flotation bath in the presence of calcium carbonate which comprises performing the flotation in the presence of a mixture of i) an amine oxide of formula R1R2R3N-0 in which R1 is an alkyl radical containing 1 to 3 carbon atoms, R2 is an alkyl radical containing 1 to 3 carbon atoms, and R3 is an alkyl radical containing 6 to 22 carbon atoms and ii) a branched chain C16 to C20 fatty acid.
2. A process according to claim 1 wherein the flotation is performed at a pH in the range from about 8 to about 12, preferably about 9 to about 10.
3. A process according to claim 1 or 2 when the amine oxide and branched fatty acid are present in the mixture in a weight ratio of from 1:10 to 1:1, preferably from 1:3 to 1:1.
4. A process according to any preceding claim wherein the electrolyte content of the feedstock water is at least about 500 ppm.
5. A process according to claim 1 substantially as herein described.
6. Calcium phosphate containing materials concentrated by the process of any preceding claim.
GB08718420A 1987-08-04 1987-08-04 Ore purification Withdrawn GB2207619A (en)

Priority Applications (1)

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GB08718420A GB2207619A (en) 1987-08-04 1987-08-04 Ore purification

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5147528A (en) * 1990-04-12 1992-09-15 Falconbridge Limited Phosphate beneficiation process
WO2003089144A1 (en) * 2002-04-20 2003-10-30 Clariant Gmbh Use of fatty amine salts in conjunction with fatty acids as auxiliary agents for the flotation of potassium salts (sylvinite)
CN103041928A (en) * 2012-12-21 2013-04-17 张飞 Carbonate type phosphorite foam flotation reagent and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4337149A (en) * 1981-05-11 1982-06-29 Sherex Chemical Company, Inc. Promoters for use in the anionic circuit of froth flotation of mineral ores

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4337149A (en) * 1981-05-11 1982-06-29 Sherex Chemical Company, Inc. Promoters for use in the anionic circuit of froth flotation of mineral ores

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
US DEFENSIVE PUBLICATION T980002 *
WO 81/00527 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5147528A (en) * 1990-04-12 1992-09-15 Falconbridge Limited Phosphate beneficiation process
WO2003089144A1 (en) * 2002-04-20 2003-10-30 Clariant Gmbh Use of fatty amine salts in conjunction with fatty acids as auxiliary agents for the flotation of potassium salts (sylvinite)
CN103041928A (en) * 2012-12-21 2013-04-17 张飞 Carbonate type phosphorite foam flotation reagent and preparation method thereof

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Publication number Publication date
GB8718420D0 (en) 1987-09-09

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