US2826301A - Oxidizing agents including sodium peroxide in phosphate flotation - Google Patents
Oxidizing agents including sodium peroxide in phosphate flotation Download PDFInfo
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- US2826301A US2826301A US525776A US52577655A US2826301A US 2826301 A US2826301 A US 2826301A US 525776 A US525776 A US 525776A US 52577655 A US52577655 A US 52577655A US 2826301 A US2826301 A US 2826301A
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- United States
- Prior art keywords
- flotation
- ore
- sodium peroxide
- phosphate
- feed
- Prior art date
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- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 title claims description 38
- 239000007800 oxidant agent Substances 0.000 title claims description 29
- 229910019142 PO4 Inorganic materials 0.000 title claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims description 21
- 239000010452 phosphate Substances 0.000 title claims description 21
- 238000005188 flotation Methods 0.000 title description 54
- 238000000034 method Methods 0.000 claims description 29
- 230000003750 conditioning effect Effects 0.000 claims description 18
- 239000007900 aqueous suspension Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 description 31
- 239000000203 mixture Substances 0.000 description 29
- 239000000047 product Substances 0.000 description 23
- 239000007787 solid Substances 0.000 description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 21
- 239000003153 chemical reaction reagent Substances 0.000 description 21
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 19
- 238000011084 recovery Methods 0.000 description 19
- 239000002002 slurry Substances 0.000 description 19
- 235000019731 tricalcium phosphate Nutrition 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 239000011707 mineral Substances 0.000 description 9
- 235000010755 mineral Nutrition 0.000 description 9
- 230000001143 conditioned effect Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 239000011435 rock Substances 0.000 description 6
- 239000003784 tall oil Substances 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 239000003518 caustics Substances 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 5
- 238000009291 froth flotation Methods 0.000 description 5
- 239000000295 fuel oil Substances 0.000 description 5
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 229910052586 apatite Inorganic materials 0.000 description 4
- 239000000306 component Substances 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002367 phosphate rock Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 238000005273 aeration Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000037361 pathway Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002426 superphosphate Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- -1 sylvinite Chemical compound 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical compound [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 229910052587 fluorapatite Inorganic materials 0.000 description 1
- 229940077441 fluorapatite Drugs 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 101150115538 nero gene Proteins 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052585 phosphate mineral Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
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
- B03D1/002—Inorganic compounds
-
- 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
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S209/00—Classifying, separating, and assorting solids
- Y10S209/902—Froth flotation; phosphate
Definitions
- This invention relates to a process of beneficiating or concentrating the values of non-metallic minerals. More particularly, the process of the present invention relates to the beneficiating or concentrating of phosphate minerals from phosphatic ores. In general, the process of the present invention is applicable to beneficiation of any non-metallic ore such as, for example, apatite, fluorapatite, sylvinite, langbeinite, fluorspar, feldspar, and the like.
- Apatite which has a chemical composition equivalent to 3Ca (PO -CaF is the usual mineral form of phosphate found in nature. Extensive deposits of this mineral are found in Florida, Tennessee, and certain parts of the Western United States. This mineral is usually mixed in varying proportions with heavy metals, iron and aluminum compounds, and gangue materials, such as quartz, silicates, and calcium carbonate. Since all of the compounds in the mixture except for apatite can boot little, if any, nutritive value to plants and animals, a great deal of eifort has been made to develop processes for the concentration of apatite from the mined ore.
- aqueous suspension or pulped phosphatic rock When an aqueous suspension or pulped phosphatic rock is reagentized with a composition containing this combination and the same agitated and aerated in an aqueous suspension, the phosphatic values and components of the rock are found to rise and become segregated in the upper portion of such suspension while the siliceous values are found to settle or deposit in the lower portion of such a suspension.
- the beneficiated or enriched phosphatic material is withdrawn and further beneficiated and concentrated by reflotation, by the use of spirals or tables, or by other means well known to the art.
- the enriched phosphatic material from these beneficiation and concentrating treatments which 'contains from 60% to 75%, and even as high as 80% of'tricalcium phosphate computed as bone phosphate of lime, is suitable as a raw material in the production of superphosphate, phosphoric acid, triple superphosphate and other phosphatic compounds.
- the air is usually introduced from an outside source and diffused by an agitator impeller or some other means, so that there is an adequate number of bubbles to carry the selectively reagentized solids to the surface of the slurry.
- the degree of agitation should be sufficient to adequately diffuse the air to bring about contact between the bubbles and the solids to be floated, and to aid the raising of the flotation concentrate. Excessive agitation should be avoided because, even though it may improve dispersion of the air, it may also hinder the raising of the flotation concentrate. It has been shown that suflicient aeration can be generated chemically by treating a carbonate with an acid to produce CO or by electrolysis of the pulp water. By controlling the slimes, pH and air, it is possible to improve the recovery and concentration of the beneficiation product.
- a further object of this invention is to improve the beneficiation of phosphatic ores through minimizing the effects of slimes While at the same time improving the aeration of the pulp particles subjected to flotation, thus aiding in raising the flotation product to the surface.
- the reagentizing of phosphatic ores or phosphorousbearing materials for the purpose of beneficiating or con centrating these phosphatic values has been practiced for many years.
- the present invention is directed to the discovery of and use of an improved reagentizing composition for this purpose.
- the phosphatic material such as Florida pebble phosphate rock or any other phosphatic rock, such as Montana or Tennessee rock, has been sized to approximately 14 mesh +200 mesh and has been dewatered to approximately solids, it is subjected to the novel treatment as herein outlined. It has --b een discovered that when this iphosphatic slurry, which,
- Slime coatings which are reducing in nature, frequently adhere to the surface of non-metallic minerals, for example phosphate ores. These slimes, if not treated prior to flotation, will greatly increase the quantity of flotation reagents required to obtain a satisfactory flotation prod uct. Conditioning of the feed with an oxidizing agent prior to reagentizing and flotation will convert the slimes to an oxidized state and thereby reduce the quantity of flotation reagents required to effect an eificient flotation operation.
- t is preferred to treat an aqueous pulp of the flotation feed, which has a solids concentration of approximately 70%, with the required amount of oxidizing agent prior to adding the usual flotation reagents. It is possible to treat the flotation feed slurry with the oxidizing agent at the same time that the conventional flotation reagents are added, but a slightly greater quantity of flotation reagents will be required to obtain equivalent recovery and grade if this method is followed.
- the oxidizing agent may be added to the slurry in a solid form if desired. Generally, however, a solution of, or the liquid form of, oxidizing agent is employed.
- Certain oxidizing agents such as sodium peroxide, can be used to maintain the pH at the proper level without the need for addition of any caustic or acid, or if these pH adjusting reagents are added, usually not as much is required as heretofore used.
- oxidizing agents may be used to condition the ores prior to treatment with a negative ion flotation reagent, such as a fatty acid mixture and a frothing agent, such as fuel oil. Satisfactory results are obtained using as oxidizing agents or as mixtures of an oxidizing agent and another compound sodium peroxide, sodium peroxide and lithium fluoride, and sodium peroxide and hydrogen peroxide.
- Suflicient quantity of conditioning agent must be added to the aqueous pulp of the ore to adjust the pH to the optimum level.
- This pH level depends upon the properties of the ore and upon the conditioning agent used. For example, in the flotation of phosphatic rock the pH of the reagentized pulp should be between about 7 and 9,
- the conditioning agent When sodium peroxide is used as the conditioning agent a satisfactory recovery and grade of the flotation product can be obtained when the reagent is added at the rate of between about 0.2 and about 2.0 pounds per ton of solids in the feed.
- the preferred rate of addition of sodium peroxide is between about 0.45 and about 0.85 pound per ton of solids in the feed.
- the conditioning agent is a mixture of sodium peroxide and lithium fluoride
- a satisfactory recovery and grade of the product can be obtained when the weight ratio of sodium peroxide to lithium fluoride is about 3:2 and when the mixture is added at the rate of between about 0.2 and about 2.0 pounds per ton of solids in the feed.
- the preferred rate of addition of the sodium peroxide-lithium fluoride mixture is between about 0.45 and about 0.85 pound per ton of solids in the feed.
- the conditioning agent is a mixture of sodium peroxide and hydrogen peroxide a satisfactory recovery and grade of the product can be obtained when the weight ratio of sodium peroxide to hydrogen peroxide is about 1:6, and when the mixture is added at the rate of between about 0.5 and about 3.0 pounds per ton of solids in the feed.
- the preferred rate of addition of the sodium peroxide-hydrogen peroxide mixture is between about 1.75 and about 2.25 pounds per ton of solids in the feed.
- the collecting agent used in conjunction with the above named conditioning and oxidizing agents is a negative ion or anionic active type reagent.
- crude tall oil which is a mixture of the higher fatty acids
- the preferred rate of addition of crude tall oil is between about 0.5 and about 0.75 pound per ton of solids in the feed.
- the frothing agent is usually a liquid hydrocarbon, such as kerosene, diesel oil, fuel oil, the heavier solvent naphthas, crude oil, and the like.
- the frothing agent may be added at the rate of between about 0.1 and about 6.0 pounds per ton of solids in the feed. Under certain conditions, it is not necessary to add a frothing agent to the flotation feed.
- Phosphatic ores and other non-metallic ores previously described may be conditioned with an oxidizing agent prior to subjecting the ores to beneficiation operations other than flotation.
- the ore may be treated with-an oxidizing. agent and other suitable reagents and then subjected to a tabling operation. If phosphatic ore is being beneficiated, a tabling operation of conventional construction will allow a collection and segregation of phosphatic material on the one hand, and siliceous and heavy mineral, bodies on the other hand.
- Phosphatic ore when treated with an oxidizing agent and other suitable agents may be beneficiated in a spiral operation, where the reagentized feed is conducted in a downwardly spiralling path so as to permit the phosphatic material to be selectively centrifugally moved to the outer side of the spiral pathway, while the siliceous bodies and other impurities are collected from the inner portion of the spiral pathway.
- the BPL recovery obtained in Example V using a conventional reagent may be somewhat lower than what normally would be expected under these conditions. It is believed that improper decanting of the feed after conditioning with NaOH may have caused a decrease in the BPL recovery. Nevertheless, the BPL recovery obtained when the feed has been conditioned with NaOH and properly decanted will be lower than the BPL recovery obtained by using Na O to condition the ore.
- EXAMPLES VII TO IX The same standard conditions were used for Examples VII to IX except for the variations indicated in Table 3. About 1000 grams of Florida phosphate rock, having a size of about 28 +200 mesh, was placed in a mixing chamber, diluted to about 70% solids and then agitated. Conditioning agents were then added, and after about two minutes agitation, a crude tall oil collector was added. The reagentized slurry was agitated for about one minute and then subjected to flotation in a laboratory flotation cell. The flotation product was collected for 45 seconds.
- Example VII VIII IX Reagents, lbs/ton: Oonditioners- Example IX is presented for purposes of comparing the recovery and grade of products obtained when an oxidizing agent is used with the products obtained when no oxidizing agent is used.
- EXAMPLE X Sodium peroxide has been used as a conditioning agent in the flotation section of a commercial scale phosphate recovery plant. Deslimed phosphate ore was conditioned with sodium peroxide, fatty acid mix and kerosene, and then beneficiated in the flotation section. Sodium peroxide was added at the rate of about 0.39 pound per ton of solids in the feed, and the fatty acid was added at the rate of about 0.92 pound per ton of solids in the feed. The pH was maintained at about 8.7. The concentrate obtained by this method analyzed 76.28% BPL (bone phosphate of lime) and 3.82% insoluble material. The product contained about 87% of the BPL from the flotatation feed. A lower BPL recovery and a product containing less BPL were obtained when sodium hydroxide Was used as a conditioning agent with the same quantity of flotation reagents.
- BPL bone phosphate of lime
- the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent containing sodium peroxide.
- the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent prior to subjecting the phosphate ore to beneficiation operations, said oxidizing agent being selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride.
- the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent and flotation reagents, said oxidizing agent being selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride.
- the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride prior to treating the phosphate ore with a negative ion collecting agent and a frothing agent.
- an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride prior to treating the phosphate ore with a negative ion collecting agent and a frothing agent.
- sufiicient oxidizing agent is added to adjust the pH of the slurry to between about 8 and about 9.
- the steps comprising the separation of the mined ore into a fraction of approximately 14 +200 mesh, treating an aqueous suspension of the ore with suflicient sodium peroxide to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent and a frothing agent,
- the steps comprising the separation of the mined ore into a fraction of approximately 14 +200 mesh, treating an aqueous suspension of the ore with a mixture of sodium peroxide and lithium fluoride, said mixture having a weight ratio of Na O to LiF of about 3:2, said mixture being of suflicient quantity to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent, and subjecting the treated ore to a froth flotation operation to recover a flotation product richer in phosphate than the feed material.
- the steps comprising the separation of the mined ore into a fraction of approximately -14 +200 mesh, treating an aqueous suspension of the ore with a mixture of sodium peroxide and hydrogen peroxide, said mixture having a weight ratio of Na O to H of about 1:6, said mixture being of suflicient quantity to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent and a frothing agent, subjecting the treated ore to a froth flotation operation to recover a flotation product richer in phosphate than the feed material.
- the step comprising the conditioning of an aqueous suspension of the. ore with an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride and at the same time adding a collecting agent and a frothing agent.
- an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride
- suflicient oxidizing agent is added to adjust the pH of the slurry to between about 8 and about 9.
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Description
OXIDIZING AGENTS INCLUDING SODIUM PER- OXIDE IN PHGSPHATE FLOTATION Ira M. Le Baron, Evanston, Ill., assignor to International Minerals & Chemical Corporation, a corporation of New York No Drawing. Application August 1, 1955 Serial No. 525,776
12 Claims. (Cl. 209-166) This invention relates to a process of beneficiating or concentrating the values of non-metallic minerals. More particularly, the process of the present invention relates to the beneficiating or concentrating of phosphate minerals from phosphatic ores. In general, the process of the present invention is applicable to beneficiation of any non-metallic ore such as, for example, apatite, fluorapatite, sylvinite, langbeinite, fluorspar, feldspar, and the like.
Apatite, which has a chemical composition equivalent to 3Ca (PO -CaF is the usual mineral form of phosphate found in nature. Extensive deposits of this mineral are found in Florida, Tennessee, and certain parts of the Western United States. This mineral is usually mixed in varying proportions with heavy metals, iron and aluminum compounds, and gangue materials, such as quartz, silicates, and calcium carbonate. Since all of the compounds in the mixture except for apatite can boot little, if any, nutritive value to plants and animals, a great deal of eifort has been made to develop processes for the concentration of apatite from the mined ore. Several methods involve the desliming, dewatering and separation of either pulped or unpulped material in order to effect a beneficiation and concentration of the ,phosphatic component. One commonly used method involves the reagentizing of such dewateredore with a collecting agent used in conjunction with a relatively high boiling hydrocarbon oil or liquid, together with the use of a basic com ponent such as caustic. When an aqueous suspension or pulped phosphatic rock is reagentized with a composition containing this combination and the same agitated and aerated in an aqueous suspension, the phosphatic values and components of the rock are found to rise and become segregated in the upper portion of such suspension while the siliceous values are found to settle or deposit in the lower portion of such a suspension. The beneficiated or enriched phosphatic material is withdrawn and further beneficiated and concentrated by reflotation, by the use of spirals or tables, or by other means well known to the art. The enriched phosphatic material from these beneficiation and concentrating treatments, which 'contains from 60% to 75%, and even as high as 80% of'tricalcium phosphate computed as bone phosphate of lime, is suitable as a raw material in the production of superphosphate, phosphoric acid, triple superphosphate and other phosphatic compounds.
Various methods of operating beneficiating processes of this type to improve the recovery and the grade of the phosphate in the beneficiation product have been attempted in the past. Some of the factors which control the recovery and grade of phosphate in the benefieiation product are the properties of the ore, the pH of the slurry,
nited States P t 2,826,301 Patented Mar. 11, 1958 the type and quantity of reagents and the type and quantity of aeration."
Although many non-metallic minerals are found in nature in an oxidized state, the surface of these minerals may be coated with slimes which are in a reduced state. It has been observed that when these slimes are present in the ore, considerable quantities of flotation reagents are required to beneficiate the ore unless the slimes are treated or removed in some manner. It has also been observed that in flotation and other beneficiating and concentrating operations, the pH is critical and a close control is necessary in order to obtain optimum recovery and concentration of values in the product. It is Well known that a flotation operation can also be controlled with the feed rate of the air and the degree of dispersion of the bubbles. The air is usually introduced from an outside source and diffused by an agitator impeller or some other means, so that there is an adequate number of bubbles to carry the selectively reagentized solids to the surface of the slurry. The degree of agitation should be sufficient to adequately diffuse the air to bring about contact between the bubbles and the solids to be floated, and to aid the raising of the flotation concentrate. Excessive agitation should be avoided because, even though it may improve dispersion of the air, it may also hinder the raising of the flotation concentrate. It has been shown that suflicient aeration can be generated chemically by treating a carbonate with an acid to produce CO or by electrolysis of the pulp water. By controlling the slimes, pH and air, it is possible to improve the recovery and concentration of the beneficiation product.
it is an object of the present invention to provide an improved process of beneficiating or concentrating ores.
It isa further object of this invention to provide an improved process of beneficiating or concentrating phosphatic ores.
It is a further object of this invention to provide an improved process of beneficiating or concentrating phosphatic ores by the froth flotation method.
It is a further object of this invention to treat phosphatic ore so as to improve the efiiciency of selectively reagentizing and floating the phosphatic components to the exclusion of the gangue.
A further object of this invention is to improve the beneficiation of phosphatic ores through minimizing the effects of slimes While at the same time improving the aeration of the pulp particles subjected to flotation, thus aiding in raising the flotation product to the surface.
It is still a further object of this invention to subject phosphatic ores to froth flotation while collecting a concentrate having improved sales appeal both as to grade and appearance.
Still further objects of the invention will be apparent upon a more complete understanding of the invention as hereinafter more fully described.
The reagentizing of phosphatic ores or phosphorousbearing materials for the purpose of beneficiating or con centrating these phosphatic values has been practiced for many years. The present invention is directed to the discovery of and use of an improved reagentizing composition for this purpose. After the phosphatic material, such as Florida pebble phosphate rock or any other phosphatic rock, such as Montana or Tennessee rock, has been sized to approximately 14 mesh +200 mesh and has been dewatered to approximately solids, it is subjected to the novel treatment as herein outlined. It has --b een discovered that when this iphosphatic slurry, which,
is the usual feed for negative ion flotation, is conditioned with an oxidizing agent, prior to the negative ion treatment and flotation operation, the recovery and grade of the phosphatic beneficiation product ultimately obtained can be and is improved.
Slime coatings, which are reducing in nature, frequently adhere to the surface of non-metallic minerals, for example phosphate ores. These slimes, if not treated prior to flotation, will greatly increase the quantity of flotation reagents required to obtain a satisfactory flotation prod uct. Conditioning of the feed with an oxidizing agent prior to reagentizing and flotation will convert the slimes to an oxidized state and thereby reduce the quantity of flotation reagents required to effect an eificient flotation operation.
t is preferred to treat an aqueous pulp of the flotation feed, which has a solids concentration of approximately 70%, with the required amount of oxidizing agent prior to adding the usual flotation reagents. It is possible to treat the flotation feed slurry with the oxidizing agent at the same time that the conventional flotation reagents are added, but a slightly greater quantity of flotation reagents will be required to obtain equivalent recovery and grade if this method is followed. The oxidizing agent may be added to the slurry in a solid form if desired. Generally, however, a solution of, or the liquid form of, oxidizing agent is employed.
It is well known in the art that pH control is an important factor in obtaining optimum flotation conditions. Caustic soda is usually used to adjust the pH in the negative ion flotation of phosphatic materials. If an oxidizing agent used in the practice of the instant process lowers the pH of the feed slurry below the optimum pH, the addition of caustic will raise the pH to the desired level. Similarly, if the oxidizing agent raises the pH above the optimum level, the addition of caustic solution is omitted and an acid solution, such as sulfuric acid is added to lower the I pH to the desired level. Certain oxidizing agents, such as sodium peroxide, can be used to maintain the pH at the proper level without the need for addition of any caustic or acid, or if these pH adjusting reagents are added, usually not as much is required as heretofore used.
Various oxidizing agents may be used to condition the ores prior to treatment with a negative ion flotation reagent, such as a fatty acid mixture and a frothing agent, such as fuel oil. Satisfactory results are obtained using as oxidizing agents or as mixtures of an oxidizing agent and another compound sodium peroxide, sodium peroxide and lithium fluoride, and sodium peroxide and hydrogen peroxide.
The most satisfactory results are obtained when sodium peroxide is used to condition the ore prior to treatment with flotation reagents. Sodium peroxide, not only oxidizes the slime coating and aids in attaining the desired pH of the slurry without need for additional caustic or acid, but it also serves as a source of finally dispersed gas bubbles which aid the flotation operation considerably. One of the decomposition products of sodium peroxide is oxygen. The oxygen forms as finely dispersed bubbles which attach to solid particles and carry them to the surface of the flotation slurry. Although air is supplied to the flotation machines from an outside source, it is difficult to obtain a dispersion of gas by this method that is as fine and as effective as that obtained by the decomposition of sodium peroxide in situ. Similar results are obtained when hydrogen peroxide is used to condition the ore prior to treatment with flotation reagents.
Suflicient quantity of conditioning agent must be added to the aqueous pulp of the ore to adjust the pH to the optimum level. This pH level depends upon the properties of the ore and upon the conditioning agent used. For example, in the flotation of phosphatic rock the pH of the reagentized pulp should be between about 7 and 9,
but the-preferred pH is between about 8 and about 9.
When sodium peroxide is used as the conditioning agent a satisfactory recovery and grade of the flotation product can be obtained when the reagent is added at the rate of between about 0.2 and about 2.0 pounds per ton of solids in the feed. However, the preferred rate of addition of sodium peroxide is between about 0.45 and about 0.85 pound per ton of solids in the feed.
When the conditioning agent is a mixture of sodium peroxide and lithium fluoride, a satisfactory recovery and grade of the product can be obtained when the weight ratio of sodium peroxide to lithium fluoride is about 3:2 and when the mixture is added at the rate of between about 0.2 and about 2.0 pounds per ton of solids in the feed. However, the preferred rate of addition of the sodium peroxide-lithium fluoride mixture is between about 0.45 and about 0.85 pound per ton of solids in the feed.
When the conditioning agent is a mixture of sodium peroxide and hydrogen peroxide a satisfactory recovery and grade of the product can be obtained when the weight ratio of sodium peroxide to hydrogen peroxide is about 1:6, and when the mixture is added at the rate of between about 0.5 and about 3.0 pounds per ton of solids in the feed. However, the preferred rate of addition of the sodium peroxide-hydrogen peroxide mixture is between about 1.75 and about 2.25 pounds per ton of solids in the feed.
The collecting agent used in conjunction with the above named conditioning and oxidizing agents is a negative ion or anionic active type reagent. When crude tall oil, which is a mixture of the higher fatty acids, is used as a collector, a satisfactory recovery and grade of the flotation product can be obtained when the collector is added at the rate of between about 0.3 and about 3.0 pounds per ton of solids in the feed. The preferred rate of addition of crude tall oil is between about 0.5 and about 0.75 pound per ton of solids in the feed.
The frothing agent is usually a liquid hydrocarbon, such as kerosene, diesel oil, fuel oil, the heavier solvent naphthas, crude oil, and the like. The frothing agent may be added at the rate of between about 0.1 and about 6.0 pounds per ton of solids in the feed. Under certain conditions, it is not necessary to add a frothing agent to the flotation feed. I
Phosphatic ores and other non-metallic ores previously described may be conditioned with an oxidizing agent prior to subjecting the ores to beneficiation operations other than flotation. For example, the ore may be treated with-an oxidizing. agent and other suitable reagents and then subjected to a tabling operation. If phosphatic ore is being beneficiated, a tabling operation of conventional construction will allow a collection and segregation of phosphatic material on the one hand, and siliceous and heavy mineral, bodies on the other hand. Phosphatic ore when treated with an oxidizing agent and other suitable agents may be beneficiated in a spiral operation, where the reagentized feed is conducted in a downwardly spiralling path so as to permit the phosphatic material to be selectively centrifugally moved to the outer side of the spiral pathway, while the siliceous bodies and other impurities are collected from the inner portion of the spiral pathway.
As illustrative of the character of the instant invention, but in 'nowise intending to be limited thereby, the following examples are described.
EXAMPLES I TO V The same standard conditions were used for Examples I to V except for the variations indicated in Table 1. Florida phosphate rock was beneficiated and deslimed to obtain a fraction of about -28 +200 mesh. Approximately 1000 grams (dry basis) of this fraction was diluted with water to about 70% solids, placed in a mixing chamber with the conditioning agent, and agitated for about one minute. After excess liquid was decanted, a crude tall oil collector and a fuel oil frother were added 5 to the mixing chamber. The reagentized slurry was diluted with water to about 70% solids and agitated for about one minute. The slurry was placed in a laboratory flotation cell and flotation product was collected for 45 seconds.
Table 1 Example I II III IV V Gonditloning Agent... NaqOr NarOr Nero; NerOr NaOl-I 0.2 0,5 0.8 2.0 0.5 0. 68 0. 68 0. 68 0. 68 0. 68 Frother 3.0 3.0 3.0 3.0 3.0 BPL in Feed, w ght percent.. 31. 2 32. 3 31. 2 32. 8 32. 1 Product:
Recovered, weight percent 41. 6 51. 2 51. 51. 1 20. 0 BPL, weight percent 63. 4 66. l 50. 5 50. 6 63. 5 BPL Recovery,
weight percent.-. 83. 5 88. 1 81. 5 78. 2 33. 4 Tails, BPL, weight percent 8. 86 8. 04 11. 99 15. 02 26. 80
The BPL recovery obtained in Example V using a conventional reagent may be somewhat lower than what normally would be expected under these conditions. It is believed that improper decanting of the feed after conditioning with NaOH may have caused a decrease in the BPL recovery. Nevertheless, the BPL recovery obtained when the feed has been conditioned with NaOH and properly decanted will be lower than the BPL recovery obtained by using Na O to condition the ore.
EXAMPLE VI Tennessee phosphate rock was beneficiated and deslimed to obtain a flotation feed of about +28 +200 mesh. Six hundred grams of the beneficiated rock was placed in a mixing chamber and diluted to about 70% solids. The slurry was agitated while heat was applied and while the reagents were added. The slurry was heated to about 120 F. and sodium peroxide was added. The temperature was increased to 180 F., crude tall oil was added, and about one minute later fuel oil was added. After about one minute of further agitation, kerosene and naphthenic acid were added. After about one minute the reagentized slurry was subjected to flotation in a laboratory cell and the concentrate and tails were collected. The quantity of reagents, on the basis of pounds per ton of solids, is as follows:
Table 2 Reagent:
Na 0 "lbs/ton of Solids" 0.5 Crude tall oil do 0.75 Fuel oil do 1.8 Kerosene .do 0.15 Naphthenic acid do 0.8 BPL in feed, weight percent 68.9 Product:
Recovered, weight percent 77.7 BPL, weight percent 72.5 BPL recovery, weight percent 81.9 Tails, BPL, weight percent 53.75
EXAMPLES VII TO IX The same standard conditions were used for Examples VII to IX except for the variations indicated in Table 3. About 1000 grams of Florida phosphate rock, having a size of about 28 +200 mesh, was placed in a mixing chamber, diluted to about 70% solids and then agitated. Conditioning agents were then added, and after about two minutes agitation, a crude tall oil collector was added. The reagentized slurry was agitated for about one minute and then subjected to flotation in a laboratory flotation cell. The flotation product was collected for 45 seconds.
6 Table 3 Example VII VIII IX Reagents, lbs/ton: Oonditioners- Example IX is presented for purposes of comparing the recovery and grade of products obtained when an oxidizing agent is used with the products obtained when no oxidizing agent is used.
EXAMPLE X Sodium peroxide has been used as a conditioning agent in the flotation section of a commercial scale phosphate recovery plant. Deslimed phosphate ore was conditioned with sodium peroxide, fatty acid mix and kerosene, and then beneficiated in the flotation section. Sodium peroxide was added at the rate of about 0.39 pound per ton of solids in the feed, and the fatty acid was added at the rate of about 0.92 pound per ton of solids in the feed. The pH was maintained at about 8.7. The concentrate obtained by this method analyzed 76.28% BPL (bone phosphate of lime) and 3.82% insoluble material. The product contained about 87% of the BPL from the flotatation feed. A lower BPL recovery and a product containing less BPL were obtained when sodium hydroxide Was used as a conditioning agent with the same quantity of flotation reagents.
Having now thus fully described and illustrated the invention, what is desired to be secured by Letters Patent is:
1. In the process of beneficiating an aqueous pulp of phosphate ore, the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent containing sodium peroxide.
2. In the process of beneficiating an aqueous pulp of phosphate ore, the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent prior to subjecting the phosphate ore to beneficiation operations, said oxidizing agent being selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride.
3. In the process of beneficiating an aqueous pulp of phosphate ore, the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent and flotation reagents, said oxidizing agent being selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride.
4. In the process of concentrating phosphate ore by flotation operations, the step comprising the conditioning of an aqueous suspension of the ore with an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride prior to treating the phosphate ore with a negative ion collecting agent and a frothing agent.
5 A process as described in claim '4 wherein sufiicient oxidizing agent is added to adjust the pH of the slurry to between about 8 and about 9.
6. In the process of concentrating phosphate ore by flotation operations, the steps comprising the separation of the mined ore into a fraction of approximately 14 +200 mesh, treating an aqueous suspension of the ore with suflicient sodium peroxide to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent and a frothing agent,
and subjecting the treated ore to a froth flotation operation to recover a flotation product richer in phosphate than the feed material. e
7; In the process of concentrating phosphate ore by flotation operations, the steps comprising the separation of the mined ore into a fraction of approximately 14 +200 mesh, treating an aqueous suspension of the ore with a mixture of sodium peroxide and lithium fluoride, said mixture having a weight ratio of Na O to LiF of about 3:2, said mixture being of suflicient quantity to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent, and subjecting the treated ore to a froth flotation operation to recover a flotation product richer in phosphate than the feed material.
8. In the process of concentrating phosphate ore by flotation operations, the steps comprising the separation of the mined ore into a fraction of approximately -14 +200 mesh, treating an aqueous suspension of the ore with a mixture of sodium peroxide and hydrogen peroxide, said mixture having a weight ratio of Na O to H of about 1:6, said mixture being of suflicient quantity to adjust the pH of the slurry to between about 8 and about 9, treating the conditioned ore with a collecting agent and a frothing agent, subjecting the treated ore to a froth flotation operation to recover a flotation product richer in phosphate than the feed material.
9. In the process of concentrating phosphate ore by flotation operations, the step comprising the conditioning of an aqueous suspension of the. ore with an oxidizing agent selected from the group consisting of sodium peroxide, a mixture of sodium peroxide and hydrogen peroxide, and a mixture of sodium peroxide and lithium fluoride and at the same time adding a collecting agent and a frothing agent.
10. A process as described in claim 9 wherein suflicient oxidizing agent is added to adjust the pH of the slurry to between about 8 and about 9.
11. A process as described in claim 6 wherein the sodium peroxide, the collecting agent and the frothing agent are added simultaneously to an aqueous suspension of the ore.
12. A process as described in claim 8 wherein the mixture of sodium peroxide and hydrogen peroxide, the collecting agent and the frothing agent are added simultaneously to an aqueous suspension of the ore.
References Cited in the file of this patent UNITED STATES PATENTS 2,571,866 Greene Oct. 16, 1951 2,666,587 Runke Jan. 19, 1954 2,682,337 Hodges et al. June 29, 1954
Claims (1)
1. IN THE PROCESS OF BENEFICIATING AN AQUEOUS PULP OF PHOSPHATE ORE, THE STEP COMPRISING THE CONDITIONING OF AN AQUEOUS SUSPENSION OF THE ORE WITH AN OXIDIZING AGENT CONTAINING SODIUM PEROXIDE.
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US525776A US2826301A (en) | 1955-08-01 | 1955-08-01 | Oxidizing agents including sodium peroxide in phosphate flotation |
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US525776A US2826301A (en) | 1955-08-01 | 1955-08-01 | Oxidizing agents including sodium peroxide in phosphate flotation |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3067875A (en) * | 1959-02-25 | 1962-12-11 | Int Minerals & Chem Corp | Ore beneficiation process |
US3314537A (en) * | 1964-11-23 | 1967-04-18 | Minerals & Chem Philipp Corp | Treatment of phosphate rock slimes |
US3361257A (en) * | 1964-10-14 | 1968-01-02 | Armour Agricult Chem | Phosphate flotation |
US3923647A (en) * | 1972-05-08 | 1975-12-02 | Vojislav Petrovich | Froth flotation method for recovery of minerals |
US4828686A (en) * | 1987-06-05 | 1989-05-09 | University Of Utah | Chemical conditioning of fine coal for improved flotation and pyrite rejection |
US5008006A (en) * | 1987-06-05 | 1991-04-16 | Miller Jan D | Chemical conditioning of fine coal for improved flotation and pyrite rejection |
US5147528A (en) * | 1990-04-12 | 1992-09-15 | Falconbridge Limited | Phosphate beneficiation process |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2571866A (en) * | 1947-08-20 | 1951-10-16 | Minerals Separation North Us | Concentration of land pebble phosphate |
US2666587A (en) * | 1952-06-23 | 1954-01-19 | Sidney M Runke | Beneficiation of beryllium ores by froth flotation |
US2682337A (en) * | 1950-12-29 | 1954-06-29 | Swift & Co | Froth flotation of phosphate values involving ph control |
-
1955
- 1955-08-01 US US525776A patent/US2826301A/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2571866A (en) * | 1947-08-20 | 1951-10-16 | Minerals Separation North Us | Concentration of land pebble phosphate |
US2682337A (en) * | 1950-12-29 | 1954-06-29 | Swift & Co | Froth flotation of phosphate values involving ph control |
US2666587A (en) * | 1952-06-23 | 1954-01-19 | Sidney M Runke | Beneficiation of beryllium ores by froth flotation |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3067875A (en) * | 1959-02-25 | 1962-12-11 | Int Minerals & Chem Corp | Ore beneficiation process |
US3361257A (en) * | 1964-10-14 | 1968-01-02 | Armour Agricult Chem | Phosphate flotation |
US3314537A (en) * | 1964-11-23 | 1967-04-18 | Minerals & Chem Philipp Corp | Treatment of phosphate rock slimes |
US3923647A (en) * | 1972-05-08 | 1975-12-02 | Vojislav Petrovich | Froth flotation method for recovery of minerals |
US4828686A (en) * | 1987-06-05 | 1989-05-09 | University Of Utah | Chemical conditioning of fine coal for improved flotation and pyrite rejection |
US5008006A (en) * | 1987-06-05 | 1991-04-16 | Miller Jan D | Chemical conditioning of fine coal for improved flotation and pyrite rejection |
US5147528A (en) * | 1990-04-12 | 1992-09-15 | Falconbridge Limited | Phosphate beneficiation process |
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