US3355017A - Method for effecting ore flotation - Google Patents

Method for effecting ore flotation Download PDF

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Publication number
US3355017A
US3355017A US598597A US59859766A US3355017A US 3355017 A US3355017 A US 3355017A US 598597 A US598597 A US 598597A US 59859766 A US59859766 A US 59859766A US 3355017 A US3355017 A US 3355017A
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United States
Prior art keywords
ore
copper
ton
flotation
promoter
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Expired - Lifetime
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US598597A
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Inventor
Wystrach Vernon Paul
Rauhut Michael Mckay
Freyberger Wilfred Lawson
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Wyeth Holdings LLC
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American Cyanamid Co
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02—Phosphorus compounds
    • C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
    • C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
    • C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
    • C07F9/657163—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms the ring phosphorus atom being bound to at least one carbon atom
    • 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
    • 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
    • Y10S209/901—Froth flotation; copper

Definitions

  • ABSTRACT oF THE DISCLOSURE A promoter which in aqueous solution ionizes to give a dithiophosphinate ion and which has been found to be particularly effective for the flotation of middling particles of base metal sulfide ores.
  • the present invention relates to the beneficiation of sulfide ores containing middling particles for the recovery of mineral values therein. More particularly, it relates to a process of flotation in which a sulfide ore containing a substantial amount of middling particles is floated in the presence of a promoter or collector compound which in aqueous solution ionizes to give a dithiophosphinate ion of the formula:
  • each R represents an alkyl group from 2 to 12 carbon atoms, floating ofl a concentrate enriched in metal values and containing metal-bearing middling particles, and rejecting precipitated tailings poor in mineral values.
  • the compounds hereinabove defined may be utilized as the free acid, or a salt thereof, such as the ammonium, sodium, potassium or calcium salt as a promoter or collector in the ore flotation treatment of sulfideo-res in which middling particles comprise a major proportion of the ore to be treated.
  • middling particles which result from either coarse grinding or from intimate association of the component minerals which make up an ore and frequently exist even after fine grinding are composed of two or more mineral species.
  • such polyphase particles are generally more difficult to concentrate by no: tation than free mineral grains.
  • InLsome free-milling ores the values are readily separated from the gangue by crushing and grinding and floating to permit the application of flotation techniques.
  • a middling treatment problem is presented. The extractive metallurice gist is thus compelled to compromise 'between obtaining a desired high recovery of mineral values and the grade of the concentrate produced.
  • the dithiophosphinate promoters hereinabove defined surprisingly provide a means of solving this vexing middling treatment problem. Moreover, these promoters aremore eflective than known collectors usually employed in floating coarse mineral particles, particularly particles in the plus 150 Tyler mesh range. This property affords the possibility of treating larger tonnages of ore in a concentrating plant through the decrease of the fineness of grind Without sacrificing metal recovery from the ore.
  • the middlings in this rougher concentrate, may be then reground and, thus,- only a comparatively small portion. of the total quantity of ore must be reground to separate the mineral values from the gangue.
  • a secondary, cleaner float may then be made in which the ore particles are separated from any gangue as the particles are then all fairly small, the particles of ore have less gang'ue attached, and a high grade of concentrate is obtained.
  • the dithiophosphinate promoters exhibit enhanced selectivity between sulfides of the base metals, such as copper, and the sulfides of iron, such as iron pyrites.
  • This selectivity is a vital factor in the differential flotation of copper and iron sulfides as well as in the separation of other mixed sulfide ores into their valu- 3 able components by flotation, permitting the production of flotation concentrates of higher metal content and lowering of refining costs.
  • the dithiophosphinates of the present invention may be used as the sole promoters for a particular ore. Alternatively, they may be employed in combination with commonly used promoters, such as alkali metal, xanthates, clithiophosphates, mercaptobenzothiazole derivatives, substituted thioureas, xanthoyl formates, xanthate esters and alkyl thionocarbamates.
  • promoters such as alkali metal, xanthates, clithiophosphates, mercaptobenzothiazole derivatives, substituted thioureas, xanthoyl formates, xanthate esters and alkyl thionocarbamates.
  • the promoters of the present invention can be prepared in a straightforward manner as set forth in United States Letters Patent No. 3,238,248 wherein secondary phosphine, sulfur, water and a base, such as ammonium hydroxide, are reacted to produce the salt of a secondary dithiophosphinic acid. These salts can be readily converted to the corresponding acids, esters or other salts, if desired.
  • the dithiophosphinate promoters or collectors contemplated herein are:
  • X is represented by the substituent wherein Y represents hydrogen, ammonium, substituted ammonium, alkali metal, such as lithium, potassium or sodium, an alkaline earth metal, such as calcium; and R through R may be the same or different aliphatic hydrocarbon from 2 to 12 carbon atoms.
  • the following examples demonstrate the utility of the dithiophosphinates as flotation promoters.
  • the dithiophosphinates are compared to promoters currently in regular plant use on specified ores. Such regular usage was established after comparative testing of known promoters to permit selection of a promoter which up to the present time give optimum recovery of values in the flotation of the specified ores.
  • Example 1 A Mexican copper ore was ground to minus 48 mesh in particle size. Two flotation tests were conducted on representative portions of this ground ore. In Test 1, the ore was floated with 5.0 lb./ton lime, 0.2 lb./ton pine oil as frother and 0.023 lb./ton of sodium diisobutyldithiophosphate as promoter. This procedure represented standard plant practice on this copper ore. In Test 2, the ground ore was treated by an identical flotation procedure as in Test 1 except that 0.023 lb./ton of ammonium diisobutyldithiophosphinate was employed as flotation promoter. Copper concentrates were removed over a period of 9 minutes, were screened, infrasized and analyzed for copper to permit the calculation of the total percentage of copper floated from each size fraction as given in Table 1, below.
  • the dithiophosphinate promoter gave generally higher copper recoveries in the coarser sizes than were obtained with the dithiophosphate promoter. Also the total copper recovery was higher with the dithiophosphinate promoter. Microscopical examination of the various concentrates indicated that the increase in copper recovery was due to the flotation of a higher percentage of middling particles when the dithiophosphinate was employed as the flotation promoter.
  • Example 2 A copper ore from the Western United States was ground to minus 65 mesh and floated in the presence of 2.0 -lb./ton lime, 0.05 lb./ton cresylic acid as frother and 0.12 lb./ton of promoter.
  • sodium diethyldithiophosphate (Test 1) and ammonium diisobutyldithiophosphinate (Test 2) were used as the respective promoters.
  • the flotation operation was conducted for a period of 5 minutes and copper concentrates were produced which were screened, infrasized and assayed for copper. This technique permitted the determination of copper recoveries in various size ranges as shown in Table II, below.
  • Example 3 Two flotation tests were conducted on a South American copper ore which was ground to minus 48 mesh in particle size in the presence of 2.75 lb./ton lime. In Test 1, the ground ore was floated with 0.02 lb./ton of the methyl ether of polypropylene glycol as frother and a.
  • Example 4 A South American copper ore (1 6% copper) was ground at 55% solids in Water to minus65 Tyler mesh in the presence of 5.0 lb./ton of calcium oxide.
  • Test 1 employed as promoter 0.06 lb./ton of sodium isopropyl xanthate and 0.02 isopropyl ethylthionocarbamate.
  • Test 2 used 0.08 lb./ton of ammonium isobutyldithiophosphinate as promoter in lieu of the promoter utilized in Test 1.
  • dialkyl C to C dithiophosphinates as ammonium salts defined generically hereinabove were used as promoters on the same ore and by the same meth ed as described in Test 2 of Example 4 with the following copper recoveries and concentrate grades:
  • the ground ore is diluted to 18% solids in a' laboratory Fagergren cell.
  • 0.022 lb./ton of the ammonium salt of diisobutyldithiophosphinic acid is added with stirring. Then 0.013 lbl/ ton of frother, pine oil, is added and conditioning continued 1 minute.
  • the ore is then floated for 2 minutes, at which point 0.013 lb./ ton of pine oil is added and conditioned 30 seconds. Flotation is then continued for 3 minutes and the total concentrates combined. This total concentrate contains 91.2% of the copper in the flotation feed at a concentrate grade of 17.8% Cu.
  • Example 9 An African ore containing both sulfide and oxide copper (4.2% sulfide C-u, 3.4% oxide Cu) is ground at 65% solids in water to minus 65 Tyler mesh. The ground ore is then diluted to 22% solids in a laboratory Fagergren flotation machine. The pH of the pulp is 8.9. To this pulp 0.19 lb./t on of the ammonium salt of diisobutyldithiophosphinic acid is added and conditioned for four minutes. Then, 0.07 lb./ ton of methyl amyl alcohol as frother is added and conditioned for one minute longer. The ore is floated for five minutes to make a sulfide copper concentrate.
  • Example 10 A Missouri copper-lead ore (2.3% Pb, 0.36% Cu) is ground to minus 48 Tyler mesh in the presence of 0.04 lb./t-n sodium isopropyl xanthate and 0.05 lb./ton sodium sulfide. Then 0.015 lb./ton of the ammonium salt of diisobutyldithiophosphinic acid is added to the ore pulp in the flotation cell along with 0.09 lb./ton of frother (a mixture of two parts of secondary heptyl alcohol with one part creosote). Flotation is commenced immediately and continued for minutes to make a combined copperlead coarser concentrate. The pH of the flotation pulp is 8.3. The concentrate assays 47.9% Pb and 7.2% Cu, and contains 96.3% of the lead and 92.0% of the copper originally present in the ore.
  • frother a mixture of two parts of secondary heptyl alcohol with one part creoso
  • Example 11 A Missouri lead-zinc sulfide ore (0.94% Pb, 5.3% Zn) is ground at 60% solids in Water to minus 65 Tyler mesh in the presence of 0.050 lb./ton sodium cyanide. The ground ore is then diluted to 22% solids in a laboratory Fagergren flotation machine and the collector and 0.082 lb./ ton of pine oil frother added. The resulting mixture is conditioned for two minutes, after which flotation is carried out for five minutes to produce a lead concentrate. To the pulp remaining in the Fagergren machine, 1.0 lb./ ton of Ca(OH) is added and conditioned for two minutes.
  • Example 12 A Missouri lead ore (1.9% Pb) is ground at 60% solids with Water to minus 65 Tyler mesh in the presence of 0.02 lb. NaCN/ ton. The ground ore is then diluted to 22% solids in a laboratory Fagergren flotation machine. The pH of the pulp is 8.7. To this pulp 0.05 lb./ton of ammonium diisobutyldithiophosphinate is added and conditioned for two minutes, after which 0.082 lb./ton of pine oil is added and conditioning continued for one minute. The ore is then floated for two minutes to make a lead concentrate which assayed 32.5% Pb and represented a recovery of 94.0% of the lead.
  • Example 13 Flotation tests were conducted on the same lead ore and by the same procedure as described in Example 12.
  • the use of 0.05 lb./ton of the tertiary butylamine salt of dioctyl dithiophosphinic acid as promoter produced a lead concentrate assaying 35.1% Pb and representing a lead recovery of 94.6%.
  • Example 14 A Tennessee zinc ore (6.0% Zn) is ground at 60% solids in water to minus 48 Tyler mesh. The ground ore is diluted to 22% solids in a laboratory Fagergren flotation machine. The pH of this pulp is 9.3. To this pulp is added 1.0 lb. copper sulfate pentahydrate/ton and the pulp is conditioned five minutes. Then 0.10 lb./ ton of ammonium diisobutyldithiophosphinate is added and conditioned three minutes, followed by addition of 0.074 lb./ton of a polypropylene glycol frother with a conditioning period of one minute.
  • the ore is then floated three minutes, at which point 0.074 lb./ton of frother is added and conditioned one-half minute, followed by two minutes of flotation.
  • the resulting zinc concentrate assayed 38.5% Zn and the zinc recovery was 98.6%.
  • Example 15 Marked selectivity obtainable with dithiophosphinate promoter is diflerential flotation is illustrated in this example.
  • Y represents a member selected from the group consisting of H, ammonium, alkali metal, and alkaline earth metal; and each R represents an alkyl group having 10 2 to 12 carbon atoms or a lower cycloalkyl; and floating 013? an enriched concentrate containing middling particles of desired metal values.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US598597A 1963-12-06 1966-12-02 Method for effecting ore flotation Expired - Lifetime US3355017A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4511541A (en) * 1982-12-02 1985-04-16 J. R. Simplot Company Process for the recovery of cadmium and other metals from solution
US4587013A (en) * 1984-11-28 1986-05-06 American Cyanamid Company Monothiophosphinates as acid, neutral, or mildly alkaline circuit sulfide collectors and process for using same
US4855507A (en) * 1988-03-28 1989-08-08 American Cyanamid Company 1,4-Disubstituted-2,3,5,6-tetrahydroxy-1,4-diphosphorinanes and their oxides or sulfides
US4968416A (en) * 1988-03-28 1990-11-06 American Cyanamid Company 1,4-disubstituted-2,3,5,6-tetrahydroxy-1,4-diphosphorinanes and their oxides or sulfides and their use in froth flotation
GB2267851A (en) * 1992-06-09 1993-12-22 American Cyanamid Co Metals recovery by flotation
US20130092605A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Froth Flotation Processes
US20130092603A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Collector Compositions and Methods of Using the Same
US20130092604A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Froth Flotation Processes
US12030062B2 (en) 2017-10-12 2024-07-09 Cytec Industries Inc. Methods for flotation recovery of value material from coarse-sized particles

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106188135B (zh) * 2016-07-07 2018-05-01 广东省石油化工研究院 一种二异丁基二硫代次膦酸钠的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2206284A (en) * 1939-10-21 1940-07-02 American Cyanamid Co Concentrated aqueous solutions of the ammonium salts of disubstituted dithiophosphoric acids
US2727067A (en) * 1954-01-26 1955-12-13 Lubrizol Corp Preparation of phosphinodithioic acid anhydrides by heating the corresponding acids
US2797238A (en) * 1954-01-26 1957-06-25 Lubrizol Corp Method for preparing organic phosphinodithioic compounds
US2881200A (en) * 1954-01-26 1959-04-07 Lubrizol Corp Method for preparing esters of di(organo) phosphinodithioic acids
US2919025A (en) * 1956-04-04 1959-12-29 American Cyanamid Co Flotation reagent composition
CA620135A (en) * 1961-05-16 R. Norman George Esters of organic dithiophosphinic acids and methods for preparing same
US3238248A (en) * 1962-11-06 1966-03-01 American Cyanamid Co Preparation of organophosphorus compounds

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2984551A (en) * 1958-10-13 1961-05-16 American Cyanamid Co Phosphine-aldehyde derivatives as gasoline additives

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA620135A (en) * 1961-05-16 R. Norman George Esters of organic dithiophosphinic acids and methods for preparing same
US2206284A (en) * 1939-10-21 1940-07-02 American Cyanamid Co Concentrated aqueous solutions of the ammonium salts of disubstituted dithiophosphoric acids
US2727067A (en) * 1954-01-26 1955-12-13 Lubrizol Corp Preparation of phosphinodithioic acid anhydrides by heating the corresponding acids
US2797238A (en) * 1954-01-26 1957-06-25 Lubrizol Corp Method for preparing organic phosphinodithioic compounds
US2881200A (en) * 1954-01-26 1959-04-07 Lubrizol Corp Method for preparing esters of di(organo) phosphinodithioic acids
US2919025A (en) * 1956-04-04 1959-12-29 American Cyanamid Co Flotation reagent composition
US3238248A (en) * 1962-11-06 1966-03-01 American Cyanamid Co Preparation of organophosphorus compounds

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4511541A (en) * 1982-12-02 1985-04-16 J. R. Simplot Company Process for the recovery of cadmium and other metals from solution
US4587013A (en) * 1984-11-28 1986-05-06 American Cyanamid Company Monothiophosphinates as acid, neutral, or mildly alkaline circuit sulfide collectors and process for using same
US4855507A (en) * 1988-03-28 1989-08-08 American Cyanamid Company 1,4-Disubstituted-2,3,5,6-tetrahydroxy-1,4-diphosphorinanes and their oxides or sulfides
US4968416A (en) * 1988-03-28 1990-11-06 American Cyanamid Company 1,4-disubstituted-2,3,5,6-tetrahydroxy-1,4-diphosphorinanes and their oxides or sulfides and their use in froth flotation
GB2267851A (en) * 1992-06-09 1993-12-22 American Cyanamid Co Metals recovery by flotation
GB2267851B (en) * 1992-06-09 1995-12-13 American Cyanamid Co Improved metal recovery by flotation
US20130092605A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Froth Flotation Processes
US20130092603A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Collector Compositions and Methods of Using the Same
US20130092604A1 (en) * 2011-10-18 2013-04-18 Cytec Technology Corp. Froth Flotation Processes
US9302272B2 (en) * 2011-10-18 2016-04-05 Cytec Technology Corp. Froth flotation processes
US9302273B2 (en) * 2011-10-18 2016-04-05 Cytec Technology Corp. Froth flotation processes
US9302274B2 (en) * 2011-10-18 2016-04-05 Cytec Technology Corp. Collector compositions and methods of using the same
US12030062B2 (en) 2017-10-12 2024-07-09 Cytec Industries Inc. Methods for flotation recovery of value material from coarse-sized particles

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