US3404777A - Froth flotation with secondary-alkyl primary amines - Google Patents

Froth flotation with secondary-alkyl primary amines Download PDF

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Publication number
US3404777A
US3404777A US454155A US45415565A US3404777A US 3404777 A US3404777 A US 3404777A US 454155 A US454155 A US 454155A US 45415565 A US45415565 A US 45415565A US 3404777 A US3404777 A US 3404777A
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Prior art keywords
ore
amine
flotation
sec
percent
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US454155A
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Charles L Ray
Robert E Baarson
Edward W Long
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Armour and Co
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Armour and Co
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    • 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
    • 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
    • B03D2203/06—Phosphate ores

Definitions

  • ABSTRACT OF THE DISCLOSURE Secondary-alkyl primary amines of a specific configuration and chain length, alone or in admixture with heterocyclic nitrogen compounds derived from gilsonite, are used as froth flotation collectors.
  • the ore Prior to flotation, the ore is ground, pulped in water, and sometimes, depending on the nature of the ore being treated, preconditioned with starch or dextrin, which is a depressant for the desired iron portion of the ore. It is generally preferred not to use a depressant. Then, a small amount of an amine collector which is preferably readily water-dispersible, and a frothing agent, is added, and the pulp subjected to flotation. The silica rich froth is floated away from the desired iron mineral residue, in one and generally several steps.
  • starch or dextrin which is a depressant for the desired iron portion of the ore. It is generally preferred not to use a depressant.
  • a small amount of an amine collector which is preferably readily water-dispersible, and a frothing agent, is added, and the pulp subjected to flotation.
  • the silica rich froth is floated away from the desired iron mineral residue, in one and generally several steps
  • phosphate flotation In phosphate flotation, one or more steps are used dependent upon the ore being treated.
  • the ore In the two step process, the ore is washed, deslimed, and then conditioned with caustic soda, and a hydrocarbon, such as fuel oil or kerosene.
  • a fatty acid collector such as tall oil, is then added and the mixture subjected to a first flotation.
  • Phosphate product is obtained as a rougher concentrate. This concentrate is then deoiled or freed of reagents by scrubbing with mineral acid. It is again deslimed in preparation for a second flotation step.
  • the second step involves flotation of the deoiled, deslimed rougher concentrate with a cationic amine collector.
  • the undesired silica is floated away from the phosphate mineral and is discarded.
  • the underflow, or unfloated portion of the ore remains as the desired phosphate product.
  • An object of this invention is to provide a novel amine collector for froth flotation.
  • Another object is to provide a novel collector mixture which, per unit amount, is even more efficient than said novel amine collector.
  • Still another object is to provide a more eflicient iron ore flotation process.
  • Another object is to provide a more etficient phosphate flotation process.
  • Typical secondary-alkyl primary amines falling within the above formula are sec-undecylamine, sec-dodecylamine, sec-tridecylamine, sec-tetradecylamine, sec-pentadecylamine, .sec-hexadecylamine, sec-heptadecylamine, sec-octadecylamine and all the isomeric versions thereof as well as mixtures of sec-alkyl primary amines and their isomeric forms such as would be derived from various unsaturated hydrocarbons including but not limited to the mixed C6 to C7, the C7 to C the C9 to C11, the Cu to C15, the C20 to C48, the C9 to cm, the Cu to C14, the C to C C to C sec-alkylamines.
  • l-methylalkylamines found useful are l-methyloctylamine, l-methyldecylamine, l-methyldodecylamine, l-rnethyltetradecylamine, l-methylhexadecylamine, and l-methyloctadecylamine.
  • the amine is usually partially or wholly neutralized by a mineral or organic acid such as hydrochloric acid or acetic acid. Such neutralization facilitates dispersibility in water.
  • the amine may be used as is or by dissolving it in a volume of a suitable organic solvent such as kerosene, pine oil, alcohol, and the like hefore use. It should be noted that these solvents sometimes have undesirable effects in flotation such as reducing flotation selectivity or producing uncontrollable frothing.
  • the concentration of amine used is about 0.01 pound to about 2.0 pounds per ton of ore, the preferred range in most instances being about 0.05 pound to about 1.0 pound per ton.
  • the gilsonite material referred to occurs as a byproduct in the manufacture of petroleum products from the aforementioned mineral gilsoniteby The American Gilsonite Company. It has been described as containing predominantly mixed alkylated pyridines, pyyroles, indoles, and quinolines, with some of the substituent carbon chains being olefinic. It also contains some unidentified nonnitrogeneous material. However, it is believed to be an inordinately complex mixture of chemical structures. Well over one-hundred different compounds are indicated as being present in the mixture, based on gas chromatographic procedures. The extreme complexity of such a mixture of materials renders a complete qualitative analysis almost prohibitive.
  • the composition of such mixed heterocyclic nitrogenous byproducts will vary with the composition of the original gilsonite, the point in the refining process from which they are extracted, the boiling range in which they are extracted and the like.
  • the invention herein described presupposes utilization of all such mixed heterocyclic nitrogenous compounds either in crude or in purified forms.
  • the preferred mixed heterocyclic nitrogen compounds in the practice of this invention are those which have a booiling range of about 200 F. to about 750 F. and particularly those which have an average boiling point within the range of about 450 to about 750 F.
  • Nitrogen distillate A crude mixture of nitrogen bases obtained by distillation and representative of 4(a) through 4(c) inclusive as above, plus some nonnitrogenous compounds.
  • Nitrogen bases concentrate oil An extracted mixture of cyclic tertiary amines plus some nonbasic nitrogen compounds.
  • the preferred amount of gilsonite material utilized should be approximately about 0.01 pound to about 2.0 pounds per ton of ore, the preferred range in most instances being about 0.05 pound to about 1.0 pound per ton, the exact amount varying from ore to ore. It is well known that the character of any ore governs the amounts of flotation reagents utilized in order to provide best results.
  • the gilsonite material may be applied to flotation pulp in several ways. First, since it usually occurs as a freefiowing liquid at low temperatures, it may be separately added to the pulp at the same time that the amine collector is added. In the preferred way, however, the gilsonite material is first blended with the amine collector and then a sufficient amount of acetic acid or hydrochloric acid is added to neutralize the primary amine collector to the desired degree, followed by dissolving or dispersing the blend to a suitable concentration in makeup water prior to addition to the pulp.
  • An even more preferred way is to disperse a blend of gilsonite material and amine collector in warm makeup water, followed by addition to the makeup water of enough acetic or hydrochlorice acid to solubilize or disperse the blend prior to addition to the pulp.
  • a blend of amine collector and gilsonite material is prepared, in such a ratio that the blend exists as a free-flowing liquid with a low freezing point, the gilsonite material acting as a liquifying agent for the primary amine collector which usually occurs as a paste or crystalline solid without considerable heating to melt the amine.
  • the gilsonite material and amine are added as a liquid blend, with very little or no heating, directly to the flotation pulp without the undesirable necessity for prior solubilizing or dispersing the amine collector in makeup water.
  • the invention accordingly comprises the several steps and the relation of one or more of such steps with respect to each of the others thereof, and a composition of matter possessing the characteristics, properties, and the relation of components which will be exemplified in the composition hereinafter described, and the scope of the invention will be indicated in the claims.
  • Example I In this flotation, the effectiveness of a mixture of secalkyl primary amines, as compared to a mixture of normal alkyl primary amines as collectors for coarse phosphate ore separation, was determined.
  • the alkyl group in each instance, varied from C to C in carbon length. Special attention was given to the amines ability to float the +28 mesh silica selectively.
  • the sec-alkyl primary amine collector s and alone or in admixture with a nitrogen distillate provides a e at 1600 r.p.m. as substantially better selectivity of bone phosphate lime (BPL) providing equal grade and improved recovery of Amine Collector Flotation (lbs/ton) Time Percent Name Amount in Solids Min.
  • BPL bone phosphate lime
  • FIG. I summarizes the above data in a very succinct manner.
  • the sec-alkyl primary amine collectors of this invention especially when admixed with nitrogen distillate as derived from gilsonite, elfect a better iron separation when compared to the coconut amine. Also, more of the desired iron fraction is recovered on an overall basis.
  • FIG. III illustrates this in a most dramatic way. It will be noted that the selectivity curves for the collectors of this invention are substantially better, than the amine collectors of the prior art.
  • alkyl group comprises mixture of 011 to C15 calrbtqns 100% neutralized with acetic acid and added as a 5% active so u 1011.
  • the sec-dodecyl primary amine used comprised a. mixture of the following isomers:
  • the above test results are portrayed graphically in The 11 1s yl primary amine (sC A) produces FIG. V.
  • the C sec-alkyl primary amine is the a higher percent Fe concentrate and higher recover of best of the group covered by thi in i iron.
  • the gilsonite material improves the recovery even Example VI further and lowers the amount of amine required to do so.
  • the above data and graphs venfy the In still another magnetite ore flotation test series superiority of the sec-alkyl primary amines wherein the (magnetic concentrate) to determine elfectiveness in cold alkyl group ranges from C to C and especially when pulp (about 40 F.) which is the usual environment in admixed with a nitrogen distillate derived from gilsonite, iron ore country, such as Minnesota, 2. C1145 sec-alkyl for froth flotation processes. They have better selectivity primary amine is compared to an amine blended with a of bone phosphate lime, even if the ore is coarse.
  • FIG. VI portrays the above results.
  • the above description shall be interpreted as illustrative sec-alkylamine of this invention performs considerably and not in a limiting sense. better in cold uplp with respect to percent Fe recover
  • the following cla1ms with minimum percent insolublesin the concentrate. are intended to cover all of the generic and specific
  • Table XIII numerically summarizes data features of the invention herein described, and all stateso that the improvement can be readily seen: ments of the scope of the invention which, as a matter of language, might be said to fall therebetween.
  • R is selected from the group consisting of hydrogen
  • x and y are positive integers having a sum from 9 to about 47, the total carbon atoms of the compound not exceeding 48.
  • a froth flotation process for separating iron ore concentrates from its crude ore comprising utilization of about .01 to 2. lbs. per ton of ore of an amine falling with the following formula:
  • R is selected from group consisting of hydrogen, an aliphatic radical, a carboxyaliphatic radical, an aminoaliphatic radical, and mixtures thereof, x and y are positive integers having a sum from 9 to about 47, the total carbon atoms of the compound not exceeding 48, as the collector,

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3459649A (en) * 1966-12-24 1969-08-05 Hoechst Ag Sylvite flotation from potassium-containing crude salts
US3710934A (en) * 1970-06-29 1973-01-16 Canadian Patents Dev Concentration of spodumene using flotation
US4319987A (en) * 1980-09-09 1982-03-16 Exxon Research & Engineering Co. Branched alkyl ether amines as iron ore flotation aids
US6814949B1 (en) * 1999-03-24 2004-11-09 Kemira Chemicals Oy Process for production of phosphoric acid by crystallization of phosphoric acid hemihydrate

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2389875A (en) * 1944-06-15 1945-11-27 Commercial Solvents Corp Surface active agents
US2578790A (en) * 1951-05-07 1951-12-18 Minerals Separation North Us Froth flotation of ferruginous impurities from finely divided granite rock
US2594612A (en) * 1949-11-01 1952-04-29 California Research Corp Recovery of zinc values by selective flotation of sulfide ores
US2914174A (en) * 1957-12-30 1959-11-24 Int Minerals & Chem Corp Phosphate mineral beneficiation process
US3265211A (en) * 1963-06-19 1966-08-09 Armour & Co Froth flotation with an amine composition

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2389875A (en) * 1944-06-15 1945-11-27 Commercial Solvents Corp Surface active agents
US2594612A (en) * 1949-11-01 1952-04-29 California Research Corp Recovery of zinc values by selective flotation of sulfide ores
US2578790A (en) * 1951-05-07 1951-12-18 Minerals Separation North Us Froth flotation of ferruginous impurities from finely divided granite rock
US2914174A (en) * 1957-12-30 1959-11-24 Int Minerals & Chem Corp Phosphate mineral beneficiation process
US3265211A (en) * 1963-06-19 1966-08-09 Armour & Co Froth flotation with an amine composition

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3459649A (en) * 1966-12-24 1969-08-05 Hoechst Ag Sylvite flotation from potassium-containing crude salts
US3710934A (en) * 1970-06-29 1973-01-16 Canadian Patents Dev Concentration of spodumene using flotation
US4319987A (en) * 1980-09-09 1982-03-16 Exxon Research & Engineering Co. Branched alkyl ether amines as iron ore flotation aids
US6814949B1 (en) * 1999-03-24 2004-11-09 Kemira Chemicals Oy Process for production of phosphoric acid by crystallization of phosphoric acid hemihydrate

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