US2750036A - Process for concentrating phosphate ores - Google Patents

Process for concentrating phosphate ores Download PDF

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US2750036A
US2750036A US416476A US41647654A US2750036A US 2750036 A US2750036 A US 2750036A US 416476 A US416476 A US 416476A US 41647654 A US41647654 A US 41647654A US 2750036 A US2750036 A US 2750036A
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flotation
phosphate
concentrate
froth
product
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Joseph L Hunter
Jr Harvie W Breathitt
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Minerals & Chemicals Corp Of A
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • B03D1/021Froth-flotation processes for treatment of phosphate ores

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  • Claim. (Cl. 209-166)
  • the present invention relates to a new and improved method of concentrating phosphate minerals from their ores.
  • the Crago process involves the steps of: (1) subjecting the ore to flotation with negative-ion reagents to separate a rougher phosphate concentrate from a silica tailing which is discarded, (2) deoiling the rougher concentrate with a mineral acid, and (3) subjecting the deoiled rougher concentrate ot flotation with positiveion reagents to produce a silicious froth-product which goes to waste, and a machine-discharge which is a high grade phosphate concentrate and the final product.
  • our novel process comprises four essential steps which are denoted 1, 2, 3 and 4 thereon.
  • the steps are: (1) subjecting the phosphate ore flotation feed, in an aqueous pulp, to retarded negative-ion froth flotation treatment, thereby producing a high grade frothproduct and also a machine-discharge of silicious gangue, too rich in phosphate to discard: (2) conditioning the machine-discharge with negative-ion reagents and then subjecting it, in an aqueous pulp, to scavenger flotation, thus obtaining a froth-product with a high insoluble content, and a tailing, composed largely of silicious gangue, which is, sent to waste; (3) treating the step 2 frothproduct with a mineral acid, followed by water rinsing, to kill the flotative efiect of the negative-ion reagents present; and (4) subjecting the acid-treated material from step 3, in
  • FIG. 2 Another embodiment of our invention is shown in Figure 2.
  • the process shown therein includes the same 4 essential steps above described, and the additional step 5 of cleaning the retarded froth-product from step 1, the middling machinedischarge being added to the scavenger flotation froth-product and the combined material treated in accordance with steps 3 and 4. It is to be understood that cleaning step 5 is not essential to our process and may or may not be used, as desired.
  • negative-ion flotation or flotation with negative-ion reagents
  • positive-ion flotation imply the use of cooperating agents, when necessary, along with the negative-ion or positive-ion collector.
  • Negative-ion and positive-ion collectors applicable for the present process are the same as those disclosed in the Crago patent, above mentioned.
  • retarded flotation By retarded flotation (step 1 of our process) is meant flotation treatment conducted in such a way that a relatively lightweight and rich froth-product is removed, and consequently, quite a bit of the phosphate accompanies the machine-discharge; in other words, the recovery, in the froth-product, of both weight and phosphate has been retarded.
  • phosphate flotation-to name a few (a) using lower than normal quantities of flotation reagents, (b) using acid water (preferably water acidified with sulfuric acid) as control water in the flotation ce1ls,.(c) adding a small quantity of acid to the pulp during conditioning (e. g., to the last conditioner) and (d) maintaining low pulp levels in the cells during flotation, thereby removing only the rich top portion of the froth.
  • Example I In this example of the use of our process, the step 1 retarding was accomplished by the use of lower than normal quantities of flotation reagents.
  • a 1,000 gm. charge of phosphate flotation feed (cell feed obtained from an actual recovery plant) was conditioned in an aqueous pulp of 70% solids content for two minutes with 0.35 of caustic soda, 2.0 of fuel oil and 0.25 of tall oil, all in pounds per ton of dry feed.
  • the conditioned material was pulped into a 1,000 gm. minerals separation airflow flotation machine and subjected to froth flotation therein, during which a retarded concentrate was removed.
  • the retarded concentrate was cleaned once, the products being a high grade phosphate concentrate and a middling.
  • the machine-discharge from the first (retarded) flotation operation was conditioned for two minutes in a 70% solids aqueous pulp with 0.1 caustic soda, 1.0 fuel oil and 0.15 tall oil, all in pounds per ton of original dry feed.
  • the conditioned machine-discharge was pulped into a 1,000 gm. minerals separation airflow flotation cell and subjected to froth flotation (scavenger flotation) therein, during which a scavenger concentrate was removed, leaving behind a tailing of silicious gangue which was sent to waste. 7
  • the scavenger concentrate was combined with the middling from the cleaner float and the whole, in a 50% solids aqueous pulp, agitated with sulfuric acid (1.0 lb. of sulfuric acid per ton of original dry feed) for three minutes.
  • the solids were then rinsed twice wtih neutral tap water to remove acid and spent reagents, pulped into a 500 gm. minerals separation airflow flotation machine and there subjected to flotation with positive-ion reagents.
  • a siliceous froth-product was removed (and discarded) leaving a high grade phosphate concentrate as the ma- Percent Percent Percent Percent Percent Pmduct Weight 13.
  • I. L. Insol. m il 1. Feed 100.0 28.4 100.0 2.
  • Example 11 This is an example of the use of the Crago process on feed from the same sample as that of Example 1.
  • a 1,000 gm. charge of the said feed was conditioned in an aqueous pulp of 70% solids for two minutes with 0.45 of caustic soda, 3.0 of fuel oil and 0.40 of tall oil, all in pounds per ton of dry feed.
  • the conditioned material was pulped into a 1,000 gm. minerals separation airflow flotation machine and subjected to froth flotation therein, during which a rougher concentrate (of phosphate values) froth-product was removed, leaving a siliceous tailing behind as the machine-discharge. This tailing was discarded.
  • the rougher concentrate was agitated in an aqueous pulp of 50% solids content for three minutes, with 2.0 pounds of H2504 per ton of dry original feed.
  • the solids were then rinsed twice with neutral water to remove acid and spent reagents after which they were pulped into a 500 gm. minerals separation airflow flotation machine.
  • Positive-ion reagents 0.05 of Armac-T and 0.14 of kerosene, both in pounds per ton of dry original feed
  • a froth flotation treatment during which a frothproduct composed mostly of siliceous gangue was removed, leaving a high grade phosphate concentrate behind as the machine-discharge.
  • the siliceous froth-product was discarded and the machine-discharge was the final product.
  • step 1 retardation by the use of lower than normal amounts of reagents, as in Example I.
  • the feed (a different one from that of Examples I and II) was conditioned with normal quantities of negative-ion reagents and then subjected to froth-flotation treatment in water containing sulfuric acid in such concentration that its pH was 2.6.
  • the resulting acid-retarded concentrate was of high enough grade to make a cleaner float unnecessary and thus the overall test procedure followed that of Figure 1.
  • This test showed good results: from ore of 31.3% B. P. L. content, a phosphate concentrate containing 74.3% B. P. L. and only 3.6% insoluble was effected; the recovery was 95.3%.
  • a method of concentrating phosphate minerals from their ores which comprise the following steps: (1) subjecting the ore, in an aqueous pulp, to retarded froth flotation treatment with negative-ion reagents thus producing a phosphate concentrate froth product and a machine-discharge composed mostly of siliceous gangue but containing a considerable quantity of phosphate; (2) subjecting the said machine-discharge in an aqueous pulp t0 scavenger flotation treatment to produce a low grade froth product and a siliceous tailing which can be discarded; (3) subjecting the scavenger froth product, in an aqueous pulp, to treatment with a mineral acid followed by rinsing with water, thereby effectively removing negative-ion reagents; (4) subjecting the acid-treated and rinsed material, in an aqueous pulp, to froth flotation treatment with positive-ion reagents, thereby producing a forth product composed mostly of siliceous

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  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

June 12, 1956 J. L. HUNTER ETAL 2,750,036
PROCESS FOR CONCENTRATING PHOSPHATE ORES Filed March 16, 1954 2 Sheets-Sheet l Phosphate Ore Feed Negative-lori Reagents such as Caustic Soda, Fatty Acid and Fuel Oil Conditioning Retarded Flotation (I gegative-lon l. ea ents such as Machine Discharge ccugfic soda, Froth-Product Fatty Acid and High Grade F Oil Phosphate Concentrate Conditioning Froth-Product Scavenger Concentrate Mineral Acid such as Sulfuric Acid Agitation (3) Water Rinsing PosLtive-lon Reagents Spent Reagentssuc as the Higher SIImes and Water Allphatlc Amines,etc. To waste l Flotation l4) Silicious Machine Discharge LFroth Product Phosphate Concentrate T0 was Flnal Hlgh Grode Phosphate Concentrate INVENTOR S. HARVlE W. BREATHITT,JR Hg BY JOSEPH L.HUNTER mew ATTORN EY June 12, 1956 J. L. HUNTER El'AL 2,750,036
PROCESS FOR CONCENTRATING PHOSPHATE ORES I Filed March 16, 1954 2 Sheets-Sheet 2 Phosphate Ore Feed Negative Ion Reagents such as Caustic Soda, Fatty Acid and Fuel Oil conditioning Retarded Flotation (I) L Negative Ion Reagents such as g ggggf' Caustic Soda, Froth Product 9 Fatty Acid and Phosphate Concentrate Fuel Oil 1 Cleaner Flotation (5) cndmmng Scavenger Flotation (2) Machine-Dischar e Froth'product Middnng g SillClOUS achine- Finished Concentrate Discharge to Waste Froth- Product Scavenger Concentrate Agitation (3) Water Rinsing Amines,etc. To Waste Flotation (4) Machine Discharge I Silicious Froth Product Phosphate Concentrate To waste Final High Grade Phosphate Concentrate INVENTORa HARVIE W. BREATHITT,JR. BY JOSEPH L. HUNTER ATTORNEY 44 no. 4 44444v4 vv 44.
United States Patent PROCESS FOR CONCENTRATING PHOSPHATE ORES Joseph L. Hunter, Bartow, and Harvie W. Breathitt, Jr.,
Lakeland, Fla., assignors to Minerals & Chemicals Corporation of America, a corporation of Maryland Application March 16, 1954, Serial No. 416,476
1 Claim. (Cl. 209-166) The present invention relates to a new and improved method of concentrating phosphate minerals from their ores.
The process described and claimed in U. S. Patent No. 2,293,640 to Crago for concentrating phosphate ores by flotation has attained wide acceptance in the phosphate industry; and, in fact, almost every phosphate mining operator in the Florida field uses the Crago process in his plant. Briefly, the Crago process involves the steps of: (1) subjecting the ore to flotation with negative-ion reagents to separate a rougher phosphate concentrate from a silica tailing which is discarded, (2) deoiling the rougher concentrate with a mineral acid, and (3) subjecting the deoiled rougher concentrate ot flotation with positiveion reagents to produce a silicious froth-product which goes to waste, and a machine-discharge which is a high grade phosphate concentrate and the final product.
While the Crago process is thus being extensively employed in the industry, we have invented a new and improved method of concentrating phosphate minerals from their ores which has the important advantage over the Crago process of requiring lesser amounts of reagents to effect better recovery from a given feed. The reduction in reagent consumption means a lower reagent cost per unit quantity of the feed for our process as compared with that of Crago.
From the following description of our process and the accompanying drawings, the advantages and utility of our invention will be clearly evident to one skilled in the art. It is to be understood, of course, that the drawings merely represent flow sheets of typical embodiments of our invention and that various modifications can be made without departing from the spirit and scope of the invention.
Referring at this time particularly to Figure 1 of the drawings, briefly, our novel process comprises four essential steps which are denoted 1, 2, 3 and 4 thereon. The steps are: (1) subjecting the phosphate ore flotation feed, in an aqueous pulp, to retarded negative-ion froth flotation treatment, thereby producing a high grade frothproduct and also a machine-discharge of silicious gangue, too rich in phosphate to discard: (2) conditioning the machine-discharge with negative-ion reagents and then subjecting it, in an aqueous pulp, to scavenger flotation, thus obtaining a froth-product with a high insoluble content, and a tailing, composed largely of silicious gangue, which is, sent to waste; (3) treating the step 2 frothproduct with a mineral acid, followed by water rinsing, to kill the flotative efiect of the negative-ion reagents present; and (4) subjecting the acid-treated material from step 3, in an aqeuous pulp, to positive-ion flotation, thereby removing most of the silicious gangue (which is sent to waste) and producing, as the machine-discharge, a high grade phosphate concentrate. The step 1 froth-product and the step 4 machine-discharge can be combined to form the final product.
Another embodiment of our invention is shown in Figure 2. Referring to Figure 2 it will be seen that the process shown therein includes the same 4 essential steps above described, and the additional step 5 of cleaning the retarded froth-product from step 1, the middling machinedischarge being added to the scavenger flotation froth-product and the combined material treated in accordance with steps 3 and 4. It is to be understood that cleaning step 5 is not essential to our process and may or may not be used, as desired.
The expressions negative-ion flotation (or flotation with negative-ion reagents) and positive-ion flotation, as employed herein, imply the use of cooperating agents, when necessary, along with the negative-ion or positive-ion collector. Negative-ion and positive-ion collectors applicable for the present process are the same as those disclosed in the Crago patent, above mentioned.
We prefer sulfuric acid for our step 3 deoiling but other mineral acids, or mixtures thereof, may also be used.
By retarded flotation (step 1 of our process) is meant flotation treatment conducted in such a way that a relatively lightweight and rich froth-product is removed, and consequently, quite a bit of the phosphate accompanies the machine-discharge; in other words, the recovery, in the froth-product, of both weight and phosphate has been retarded. There are a number of ways to retard phosphate flotation-to name a few: (a) using lower than normal quantities of flotation reagents, (b) using acid water (preferably water acidified with sulfuric acid) as control water in the flotation ce1ls,.(c) adding a small quantity of acid to the pulp during conditioning (e. g., to the last conditioner) and (d) maintaining low pulp levels in the cells during flotation, thereby removing only the rich top portion of the froth.
To facilitate the understanding of our invention and to demonstrate the superiority of our process over that of Crago, the following examples are given.
Example I In this example of the use of our process, the step 1 retarding was accomplished by the use of lower than normal quantities of flotation reagents.
A 1,000 gm. charge of phosphate flotation feed (cell feed obtained from an actual recovery plant) was conditioned in an aqueous pulp of 70% solids content for two minutes with 0.35 of caustic soda, 2.0 of fuel oil and 0.25 of tall oil, all in pounds per ton of dry feed. The conditioned material was pulped into a 1,000 gm. minerals separation airflow flotation machine and subjected to froth flotation therein, during which a retarded concentrate was removed. The retarded concentrate was cleaned once, the products being a high grade phosphate concentrate and a middling.
The machine-discharge from the first (retarded) flotation operation was conditioned for two minutes in a 70% solids aqueous pulp with 0.1 caustic soda, 1.0 fuel oil and 0.15 tall oil, all in pounds per ton of original dry feed. The conditioned machine-discharge was pulped into a 1,000 gm. minerals separation airflow flotation cell and subjected to froth flotation (scavenger flotation) therein, during which a scavenger concentrate was removed, leaving behind a tailing of silicious gangue which was sent to waste. 7
The scavenger concentrate was combined with the middling from the cleaner float and the whole, in a 50% solids aqueous pulp, agitated with sulfuric acid (1.0 lb. of sulfuric acid per ton of original dry feed) for three minutes. The solids were then rinsed twice wtih neutral tap water to remove acid and spent reagents, pulped into a 500 gm. minerals separation airflow flotation machine and there subjected to flotation with positive-ion reagents. A siliceous froth-product was removed (and discarded) leaving a high grade phosphate concentrate as the ma- Percent Percent Percent Percent Pmduct Weight 13. I. L. Insol. m il 1. Feed 100.0 28.4 100.0 2. Cleaned retarded concentrate 28.8 74. 5 3. 2 75. 6 3. Scavenger tailing 61. 2 2. 3 5. 4. Amino machine-discharge. 7.0 74. 5 2 7 18.4 5. Aminefroth-product an 9.3 1.0 6. Total concentrate (2and 4) 35.8 74.5 3.1 9 1.0
To summarize: from ore containing 28.4% B. P. L. there was obtained a phosphate concentrate of 74.5% B. P. L. (and only 3.1% insoluble) content, representing a recovery of 94.0% of the B. P. L. in said .ore. This beneficiation was achieved at a reagent cost (including the H2504), calculated from current prices, of 19 per ton of concentrate. The cost per ton of feed amounted to 6.79.
Example 11 This is an example of the use of the Crago process on feed from the same sample as that of Example 1.
A 1,000 gm. charge of the said feed was conditioned in an aqueous pulp of 70% solids for two minutes with 0.45 of caustic soda, 3.0 of fuel oil and 0.40 of tall oil, all in pounds per ton of dry feed. The conditioned material was pulped into a 1,000 gm. minerals separation airflow flotation machine and subjected to froth flotation therein, during which a rougher concentrate (of phosphate values) froth-product was removed, leaving a siliceous tailing behind as the machine-discharge. This tailing was discarded.
The rougher concentrate was agitated in an aqueous pulp of 50% solids content for three minutes, with 2.0 pounds of H2504 per ton of dry original feed. The solids were then rinsed twice with neutral water to remove acid and spent reagents after which they were pulped into a 500 gm. minerals separation airflow flotation machine. Positive-ion reagents (0.05 of Armac-T and 0.14 of kerosene, both in pounds per ton of dry original feed) were added to the pulp in the machine and it was then subjected to froth flotation treatment during which a frothproduct composed mostly of siliceous gangue was removed, leaving a high grade phosphate concentrate behind as the machine-discharge. The siliceous froth-product was discarded and the machine-discharge was the final product.
The results achieved by this test are tabulated below.
In this test, a phosphate concentrate of 74.7% B. P. L., representing a recovery of 91.8% was obtained from the feed ore. The reagent cost here (including H2804.) amounted to 24.7 per ton of concentrate or 8.6l per ton of feed.
A comparison of Examples I and II shows that the same quantities of negative-ion reagents (caustic soda, fuel oil and tall oil) were used for each but that considerably more H2SO4, Armac-T and kerosene were required for the latter. The two tests resulted in products of about equal grade but the Example I recovery was greater than that of Example II by 2.4% (94.0% vs. 91.8%). These two factors (differing reagent quantities for equal feed weights and differing recoveries) compounded to give our new method a reagent cost advantage of 5.7 per ton of concentrate over Cragos.
We prefer to accomplish step 1 retardation by the use of lower than normal amounts of reagents, as in Example I. However, there are additional ways of doing this (as hereinbefore pointed out), and to show that our process is not limited to the low reagent method we are including herein the results of a test of our procedure in which the retarding was brought about by the use of acid control water. In this example, the feed (a different one from that of Examples I and II) was conditioned with normal quantities of negative-ion reagents and then subjected to froth-flotation treatment in water containing sulfuric acid in such concentration that its pH was 2.6. The resulting acid-retarded concentrate was of high enough grade to make a cleaner float unnecessary and thus the overall test procedure followed that of Figure 1. This test showed good results: from ore of 31.3% B. P. L. content, a phosphate concentrate containing 74.3% B. P. L. and only 3.6% insoluble was effected; the recovery was 95.3%.
We claim:
A method of concentrating phosphate minerals from their ores which comprise the following steps: (1) subjecting the ore, in an aqueous pulp, to retarded froth flotation treatment with negative-ion reagents thus producing a phosphate concentrate froth product and a machine-discharge composed mostly of siliceous gangue but containing a considerable quantity of phosphate; (2) subjecting the said machine-discharge in an aqueous pulp t0 scavenger flotation treatment to produce a low grade froth product and a siliceous tailing which can be discarded; (3) subjecting the scavenger froth product, in an aqueous pulp, to treatment with a mineral acid followed by rinsing with water, thereby effectively removing negative-ion reagents; (4) subjecting the acid-treated and rinsed material, in an aqueous pulp, to froth flotation treatment with positive-ion reagents, thereby producing a forth product composed mostly of siliceous gangue which can be discarded and a residue which is a high grade phosphate concentrate; and (5) subjecting the phosphate concentrate froth product from step (1) to cleaner flotation to produce, as part of the final product, a froth product having a low insoluble content, and a middling residue which is combined with the step (2) scavenger froth product prior to the acid treatment step (3).
References Cited in the file of this patent UNITED STATES PATENTS 2,661,842 Duke et a1 Dec. 8, 1953
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2914173A (en) * 1957-07-19 1959-11-24 Int Minerals & Chem Corp Method of processing phosphate ore to recover metallic minerals
US2931502A (en) * 1956-07-02 1960-04-05 Saskatchewan Potash Method for flotation concentration in coarse size range
US3061097A (en) * 1958-12-24 1962-10-30 Philip A Mallinckrodt Flotation process for separating bituminous matter from associated gangue minerals
US3099620A (en) * 1960-08-31 1963-07-30 Int Minerals & Chem Corp Wet beneficiating of phosphate ores
US3349903A (en) * 1966-12-28 1967-10-31 Grace W R & Co Process for beneficiating unground pebble phosphate ore
US4289612A (en) * 1980-06-11 1981-09-15 Texasgulf Inc. Phosphate ore triple float
FR2509194A1 (en) * 1981-07-10 1983-01-14 Texas Gulf Inc Flotation of phosphate ore in three stages - with two cationic stages to recover extra phosphate values

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2661842A (en) * 1950-08-03 1953-12-08 Attapulgus Minerals & Chemical Concentration of phosphate ores

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2661842A (en) * 1950-08-03 1953-12-08 Attapulgus Minerals & Chemical Concentration of phosphate ores

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2931502A (en) * 1956-07-02 1960-04-05 Saskatchewan Potash Method for flotation concentration in coarse size range
US2914173A (en) * 1957-07-19 1959-11-24 Int Minerals & Chem Corp Method of processing phosphate ore to recover metallic minerals
US3061097A (en) * 1958-12-24 1962-10-30 Philip A Mallinckrodt Flotation process for separating bituminous matter from associated gangue minerals
US3099620A (en) * 1960-08-31 1963-07-30 Int Minerals & Chem Corp Wet beneficiating of phosphate ores
US3349903A (en) * 1966-12-28 1967-10-31 Grace W R & Co Process for beneficiating unground pebble phosphate ore
US4289612A (en) * 1980-06-11 1981-09-15 Texasgulf Inc. Phosphate ore triple float
FR2509194A1 (en) * 1981-07-10 1983-01-14 Texas Gulf Inc Flotation of phosphate ore in three stages - with two cationic stages to recover extra phosphate values

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