US2000350A - Froth flotation process for oxide ores - Google Patents

Froth flotation process for oxide ores Download PDF

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US2000350A
US2000350A US735424A US73542434A US2000350A US 2000350 A US2000350 A US 2000350A US 735424 A US735424 A US 735424A US 73542434 A US73542434 A US 73542434A US 2000350 A US2000350 A US 2000350A
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pulp
ketone
ore
froth
acid
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US735424A
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Patek John Mark
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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
    • B03D1/008—Organic compounds containing oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/002—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
    • 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

  • This invention relates to an improvement in the process of concentration by'fiotation of heavy mineral metal oxides and it consists in the treating of such ores while in the state of a pulp with sufiicient active acid, together with a saponiflable substance and a water-insoluble liquid ketone.
  • the heavy mineral metal oxides among which may be named magnetite, corundum, ilmenite, rutile, chromite, cuprite, zincite, franklinite, and pyrolusite, or some of them, have been treated by flotation heretofore for the purpose of concentrating the ores thereof.
  • the ratio of concentration has been low and unless the ore was initially sufiiciently high grade the concentrate has not been of commercial value, that is, sufficiently free of gangue substances as to permit economical smelting operations.
  • cassiterite there is no record of a commercial concentrate having been produced by flotation directly from any natural ore.
  • concentration of oxide ores by flotation has heretofore been of very little commercial moment because of the low ratio of concentration obtainable thereby.
  • the process of this invention is positive in its action.
  • the grade of concentrate is roughly independent of the percentage of the ore mineral in the pulp being treated.
  • a grade of concentrate of approximately sixty per cent tin can be obtained effectually from cassiterite pulps containing all the way from two to thirty percent of tin.
  • the reagents employed are effective over a substantial range of concentration and there are no critical balances which must be maintained in order to obtain the results desired.
  • the effects of the reagents are striking and easily recognizable and therefore the control of the. operation is simplifled, due to the fact that visual and other simple observations are all that is necessary in order to keep the process under control.
  • the process of this invention is carried on by reducing the ore to be treated to a proper pulp. This is done by grinding in any usual manner, or in case the particular material is in the form of 1 a slime or other very finely divided state it may i be possible to treat the same directly.
  • the pulp is fed into any one of the usual froth flotation machines in which the proper agitation and aeration are provided. There is added to the feed of pulp, or in any other manner desired, a small amount of a saponiflable substance.
  • This substance may be any one of a number of natural fatty acids, from fish, linseed, palm, cocoanut, tung, or red oil, or any high molecular weight, aliphatic or cyclic carboxylic acid, such as oleic acid, or oxidation products of normal or naphthenic petroleum, or naphthenic acids derived from any other source.
  • a 3 frother consisting of insoluble liquid ketone. For this purpose it has been found that the following will serve the purpose:
  • the result is generally over oiling, with no froth, or a poor, small bubble, or brittle froth that fails to produce a concentrate.
  • the sparingly soluble ketones not only produce a good froth when in combination with the fatty acid, but the ketone also serves to spread the fatty acid. It is advantageous at times, therefore, to dissolve a fatty acid in the ketone and to add the combination to the flotation cell. Although the ketone alone will produce a froth, such froth is brittle and ineffective, while the addition of the fatty acid brings about a strong and effective froth.
  • the process of this invention may be practiced as follows: 1000 grams of a cassiterite ore which has been ground in a ball mill are agitated and aerated in a flotation machine together with three grams of hydrochloric acid (concentrated) and one pound of sulfuric acid (con- To this 0.87 of a gram of oleic acid and 0.15 gram of Barrett oil No. 635, which is a fluid coal tar or tarry oil, and 0.20 of a gram of dipropyl ketone. A froth will be formed which will contain probably in excess of fifty per cent of tin, and in one specific case contained fifty-four per cent of tin. In this case the pulp undergoing treatment contained thirty per cent of tin.
  • the process of this invention at times may also be practiced as follows:
  • the pulp of cassiterite ore is prepared as described above, to which there is added approximately three pounds of concentrated sulfuric acid per ton of dry ore and ten pounds of sodium fluoride per ton of dry ore, which in the presence of sulfuric acid forms hydrofluoric acid.
  • the usual aeration and agitation treatment is carried on, producing a froth which may contain approximately sixty per cent of tin, for example, constituting as much as ninety-six per cent of the tin in the ore being treated.
  • the process may also at times be carried on by treating an ore containing, for example, 2.3 per cent tin, the ore being prepared in the form of a pulp and fed into the usual flotation machine together with three pounds of sulfuric acid per ton of dry ore, together with 2.4 pounds methyliso-butyl ketone and three pounds of oleic acid per ton of dry ore.
  • a froth will form which contains a concentrate containing approximately sixty per cent of tin.
  • the amount of reagents employed and particularly the amount of active acid may be varied to obtain the desired result. Even a separation of magnetite from andradite garnet may be made and in this case approximately thirty pounds of hydrochloric acid per ton of dry ore was found to give the best results when using a moderate amount of frothing and collecting agents.
  • the process of this invention makes it possible to recover heavy mineral oxide ores by flotation with results comparable to those obtained with sulfide ores which have heretofore been considered to be much more easily separated by flotation.
  • This invention depends to an extent upon the fact that the oxide minerals when in acid pulps exhibit surface phenomena which distinguish them from'the usual gangue materials and whichphenomena do not occur in neutral or alkaline solutions, but the invention is also dependent upon the discovery that an effective froth can be maintained in spite of the presence of active acid in substantial amounts.
  • the froth which is removed in the process of this invention may be retreated, if it is desired, to increase the percentage of heavy mineral metal oxide in the concentrate, or the tailings may be retreated, if it is desired, to increase the percentage of mineral recovered.
  • active acid is intended to mean one or more of the group consisting of hydrochloric, hydrofluoric, sulfuric, phosphoric, nitric, acetic, and tartaric acids.
  • Water-insoluble liquid ketone as used herein is intended to mean such ketones as are liquid at ordinary temperatures and which dissolve in water no more than economical operation of the process permits, in-
  • the process of separating the mineral constituents of an ore containing heavy mineral metal oxide wh'zh consists in mixing the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence of over one pound of active acid per ton of dry ore, a water-insoluble liquid lzetone, a saponiflable substance, supplying the pulp with air produce a froth containing a concentrate, and removing the froth.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

Patented May 7, 1935 UNITED STATES PATENT OFFICE John Mark Patek, Milwaukee, Wis.
No Drawing. Application July 16, 1934,
Serial No. 735,424
6 Claims.
This invention relates to an improvement in the process of concentration by'fiotation of heavy mineral metal oxides and it consists in the treating of such ores while in the state of a pulp with sufiicient active acid, together with a saponiflable substance and a water-insoluble liquid ketone.
The heavy mineral metal oxides, among which may be named magnetite, corundum, ilmenite, rutile, chromite, cuprite, zincite, franklinite, and pyrolusite, or some of them, have been treated by flotation heretofore for the purpose of concentrating the ores thereof. In such cases the ratio of concentration has been low and unless the ore was initially sufiiciently high grade the concentrate has not been of commercial value, that is, sufficiently free of gangue substances as to permit economical smelting operations. In the case of cassiterite there is no record of a commercial concentrate having been produced by flotation directly from any natural ore. Generally speaking, therefore, concentration of oxide ores by flotation has heretofore been of very little commercial moment because of the low ratio of concentration obtainable thereby.
Heretofore the flotation of heavy mineral oxide ores has been attempted by employing silicates for depressing the gangue materials and frothing and collecting agents for recovering the ore. In
' this method an extremely critical balance between frothing, collecting, and depressing reagents needed to be maintained if results of any advantage were to be obtained. Even when performing under optimum conditions, such methods have been relatively ineffectual, producing a'low ratio of concentration.
The process of this invention, however, is positive in its action. In the case of certain ores the grade of concentrate is roughly independent of the percentage of the ore mineral in the pulp being treated. For example, a grade of concentrate of approximately sixty per cent tin can be obtained effectually from cassiterite pulps containing all the way from two to thirty percent of tin. In the process of this invention the reagents employed are effective over a substantial range of concentration and there are no critical balances which must be maintained in order to obtain the results desired. The effects of the reagents are striking and easily recognizable and therefore the control of the. operation is simplifled, due to the fact that visual and other simple observations are all that is necessary in order to keep the process under control.
In this invention neither the amount of saponifiable substance nor ketone need be controlled so long as a suificient amount of each beused and their action is not based upon the use of starvation amounts thereof. The acid employed is an active acid and its presence in sufllcient quantities is very easily determined.
The process of this invention is carried on by reducing the ore to be treated to a proper pulp. This is done by grinding in any usual manner, or in case the particular material is in the form of 1 a slime or other very finely divided state it may i be possible to treat the same directly. The pulp is fed into any one of the usual froth flotation machines in which the proper agitation and aeration are provided. There is added to the feed of pulp, or in any other manner desired, a small amount of a saponiflable substance. This substance may be any one of a number of natural fatty acids, from fish, linseed, palm, cocoanut, tung, or red oil, or any high molecular weight, aliphatic or cyclic carboxylic acid, such as oleic acid, or oxidation products of normal or naphthenic petroleum, or naphthenic acids derived from any other source. There is also added a 3 frother consisting of insoluble liquid ketone. For this purpose it has been found that the following will serve the purpose:
Iso-amyl phenyl ketone Iso-butyl phenyl ketone Di-iso-amyl ketone Di-propyl ketone Di-iso-propyl ketone Ethyl benzyl ketone Ethyl butyl ketone Ethyl-iso-butyl ketone Ethyl octyl ketone Ethyl phenyl ketone Iso-butyl ketone Hexyl ketone Nonyl ketone Octyl ketone V n-propyl iso-butyl ketone n-propyl phenyl ketone Iso-propyl phenyl ketone centrated) acetic, or tartaric are suitable. At any rate, I have discovered that certain ores combine with substantial amounts of acid and that a slight .excess thereover is necessary to obtain the suc.- cessful results of the process of this invention, the quantity not being particularly important so long as an excess is present and the apparatus in which the process is being carried on is reasonably free from attack by the acid.
The process as outlined above is carried on in. highly acid condition as compared with flotation heretofore practiced. Under these conditions saponifiable substances, such as described above, are without frothing power and merely produce oiling, and are incapable of supporting any pulp. The discovery of this invention, however, depends to a certain extent upon the important fact that the sparingly soluble liquid ketone produces, with the saponiflable substance, 2. very strong froth regardless of the acidity of the pulp. Such frothers as have been commonly employed, as pine oil, or cresol, if employed in an acid pulp sufliciently acid to effect gangue mineral to the extent necessary, when used in combination with a fatty acid form drops in the flotation pulp and spread only with long and violent agitation of the pulp. The result is generally over oiling, with no froth, or a poor, small bubble, or brittle froth that fails to produce a concentrate. The sparingly soluble ketones, however, not only produce a good froth when in combination with the fatty acid, but the ketone also serves to spread the fatty acid. It is advantageous at times, therefore, to dissolve a fatty acid in the ketone and to add the combination to the flotation cell. Although the ketone alone will produce a froth, such froth is brittle and ineffective, while the addition of the fatty acid brings about a strong and effective froth.
At times the process of this invention may be practiced as follows: 1000 grams of a cassiterite ore which has been ground in a ball mill are agitated and aerated in a flotation machine together with three grams of hydrochloric acid (concentrated) and one pound of sulfuric acid (con- To this 0.87 of a gram of oleic acid and 0.15 gram of Barrett oil No. 635, which is a fluid coal tar or tarry oil, and 0.20 of a gram of dipropyl ketone. A froth will be formed which will contain probably in excess of fifty per cent of tin, and in one specific case contained fifty-four per cent of tin. In this case the pulp undergoing treatment contained thirty per cent of tin.
The process of this invention at times may also be practiced as follows: The pulp of cassiterite ore is prepared as described above, to which there is added approximately three pounds of concentrated sulfuric acid per ton of dry ore and ten pounds of sodium fluoride per ton of dry ore, which in the presence of sulfuric acid forms hydrofluoric acid. There is also added one-half pound of dipropyl ketone per ton of dry ore and 1.6 pounds of oleic acid per ton of dry i re. The usual aeration and agitation treatment is carried on, producing a froth which may contain approximately sixty per cent of tin, for example, constituting as much as ninety-six per cent of the tin in the ore being treated.
The process may also at times be carried on by treating an ore containing, for example, 2.3 per cent tin, the ore being prepared in the form of a pulp and fed into the usual flotation machine together with three pounds of sulfuric acid per ton of dry ore, together with 2.4 pounds methyliso-butyl ketone and three pounds of oleic acid per ton of dry ore. In such case a froth will form which contains a concentrate containing approximately sixty per cent of tin.
The amount of reagents employed and particularly the amount of active acid, may be varied to obtain the desired result. Even a separation of magnetite from andradite garnet may be made and in this case approximately thirty pounds of hydrochloric acid per ton of dry ore was found to give the best results when using a moderate amount of frothing and collecting agents.
The process of this invention makes it possible to recover heavy mineral oxide ores by flotation with results comparable to those obtained with sulfide ores which have heretofore been considered to be much more easily separated by flotation. This invention depends to an extent upon the fact that the oxide minerals when in acid pulps exhibit surface phenomena which distinguish them from'the usual gangue materials and whichphenomena do not occur in neutral or alkaline solutions, but the invention is also dependent upon the discovery that an effective froth can be maintained in spite of the presence of active acid in substantial amounts. The froth which is removed in the process of this invention may be retreated, if it is desired, to increase the percentage of heavy mineral metal oxide in the concentrate, or the tailings may be retreated, if it is desired, to increase the percentage of mineral recovered.
Herein in the specification and claims the term active acid" is intended to mean one or more of the group consisting of hydrochloric, hydrofluoric, sulfuric, phosphoric, nitric, acetic, and tartaric acids. The term Water-insoluble liquid ketone as used herein is intended to mean such ketones as are liquid at ordinary temperatures and which dissolve in water no more than economical operation of the process permits, in-
cluding those mentioned or referred to above.
The process of this invention has been described in detail above in connection with specific instances in which it may at times be usefully employed. It is not intended, however, that the protection of Letters Patent to be granted hereon be unnecessarily limited thereby, but it is intended that said protection should extend to the full field of the invention as represented by the scope of the claims appended hereto.
What I claim as my invention is:
1. The process of separating the mineral constituents of an ore containing a heavy mineral metal oxide which consists in mixing the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence of an active acid, a water-insoluble liquid ketone and a saponiflable substance, supplying the pulp with air to produce a froth containing a concentrate, and removing the froth.
2. The process of separating the mineral constituents of an ore containing heavy mineral metal oxide wh'zh consists in mixing the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence of over one pound of active acid per ton of dry ore, a water-insoluble liquid lzetone, a saponiflable substance, supplying the pulp with air produce a froth containing a concentrate, and removing the froth.
3. The process of separating the mineral :onstituents of an ore containing a heavy mineral metal oxide which consists in mix ng the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence of an active acid, a water-insoluble liquid ketone and a fatty acid substance, supplying the pulp with air to produce a froth containing a concentrate, and removing the froth. a
4. The process of separating the mineral constituents 01' an ore containing a heavy mineral metal oxide which consists in mixing the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence of an active acid, a dipropyl ketone and a saponinable substance, supplying the pulp with air to produce a irdth containing a concentrate, and removing the froth.
5. "Elle process of separating cassiterite from cessiterite ore which consists in mixing the ore in a flnely divided state with water so as to form a pulp, agitating the pulp in the presence of an active acid, dipropyl ketone and oleic acid, supplying the pulp with air to produce a froth with the cassiterite floating therein, and removing the froth.
6. The process of separating cassiterite from cassiterite ore which consists in mixing the ore in a finely divided state with water so as to form a pulp, agitating the pulp in the presence or over one pound of sulfuric acid per ton of dry ore, dipropyl ketone and oleic acid, supplying the pulp with air to produce a froth with the cassiterite fioatingtherein, and removing the froth.
' JOHN MARK PATEK.
US735424A 1934-07-16 1934-07-16 Froth flotation process for oxide ores Expired - Lifetime US2000350A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2557455A (en) * 1948-03-12 1951-06-19 American Cyanamid Co Flotation of ilmenite ores
US3167502A (en) * 1962-03-20 1965-01-26 Minerals & Chem Philipp Corp Process for recovering cassiterite from ores
US3286837A (en) * 1964-03-20 1966-11-22 Minerals & Chem Philipp Corp Beneficiation of tin ore
US4507198A (en) * 1982-12-20 1985-03-26 Thiotech, Inc. Flotation collectors and methods
US20120111772A1 (en) * 2007-06-18 2012-05-10 Tran Bo L Methyl isobutyl carbinol mixture and methods of using same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2557455A (en) * 1948-03-12 1951-06-19 American Cyanamid Co Flotation of ilmenite ores
US3167502A (en) * 1962-03-20 1965-01-26 Minerals & Chem Philipp Corp Process for recovering cassiterite from ores
US3286837A (en) * 1964-03-20 1966-11-22 Minerals & Chem Philipp Corp Beneficiation of tin ore
US4507198A (en) * 1982-12-20 1985-03-26 Thiotech, Inc. Flotation collectors and methods
US20120111772A1 (en) * 2007-06-18 2012-05-10 Tran Bo L Methyl isobutyl carbinol mixture and methods of using same
US8302778B2 (en) * 2007-06-18 2012-11-06 Nalco Company Methyl isobutyl carbinol mixture and methods of using same

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