Patent US3888748A successfully refreshed from Google Patents.
US3888748A
Expired / Lapsed
US
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Recovery of metal values from ore concentrates
Assignee: EIDP Inc
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Filing: 1973-06-04
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Granted: 1975-06-10
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Expires: 1993-06-04
Abstract
Abstract A hydrometallurgical process to recover metal value e.g., copper, from sulfide ore concentrates, e.g., chalcopyrite, bornite and chalcocite characterized by: (1) nitric acid-sulfuric acid leach whereby the acidity is just sufficient to retain iron in solution while extracting substantially all of the copper and reducing nitrate to a low level, (2) reduction of nitrate to <1 g./liter, (3) iron precipitation as jarosite, and (4) electrowinning to recover high purity copper.
Inventors
- 👤 Henry M Brennecke
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 18:05
CPC Classifications
C; C25; C25C; C25C1/00; C25C1/12
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
266 words
A HYDROMETALLURGICAL PROCESS FOR RECOVERY OF METALS FROMS ORE CONCENTRATES HAVING COPPER, IRON AND SULFUR THEREIN WHICH COMPRISES A. CONTACTING SAID CONCENTRATE IN AN AQUEOUS MEDIUM WITH A COMBINATION OF NITRIC AND SULFURIC ACIDS AT A TEMPERATURE OF AT LEAST 50*C, UNTIL THE NITRATE IS REDUCED TO LESS THAN ABOUT 30 GRAMS PER LITER IN THE PRESENCE OF CONCENTRATE; B. SEPARATING THE LIQUID AND SOLID FROM STEP (A); C. CONTACTING THE SOLIDS FROM STEP (B) WITH AN AQUEOUS SOLUTION CONTAINING NITRIC ACID IN EXCESS OF THAT REQUIRED TO DISSOLVE THE COPPER IN SAID SOLIDS AT A TEMPERATURE OF AT LEAST 50:C. UNTIL SUBSTANTIALLY ALL OF THE COPPER IN SAID SOLIDS IS DISSOLVED WHEREIN THE TOTAL AMOUNT OF AQUEOUS SOLUTION IN STEPS (A) AND (C) CONTAINS SUFFICIENT ACID TO MAINTAIN COPPER AND IRON IN SOLUTION AND SUFFICIENT WATER TO PRODUCE ABOUT 2-10 PARTS OF COPPER PER 100 PARTS OF LIQUID FROM STEP (B); D. SEPARATING THE SOLIDS FROM STEP (C) AND DIRECTING THE LIQUID FROM STEP (C) TO STEP (A); E. HEATING THE LIQUID FROM STEP (B) TO A TEMPERATURE IN THE RANGE OF 140*-200*C. TO REDUCE THE NITRATE CONCENTRATION THEREIN TO LESS THAN ABOUT ONE PART PER 1,000 PARTS OF SOLUTION; F. PRECIPITATING IRON FROM THE LIQUID FROM STEP (E) AS JAROSITE; G. ELECTROWINNING COPPER FROM THE LIQUID OF STEP (F); AND H. RECYCLING AT LEAST A PORTION OF THE LIQUID FROM STEP (G) TO FURTHER CONTACT CONCENTRATE; SAID PROCESS BEING FURTHER CHARACTERIZED IN THAT OXIDIZING CONDITIONS ARE MAINTAINED IN STEPS (E) AND (F) UNTIL SUBSTANTIALLY ALL OF THE IRON IS PRESENT AS THE FERRIC ION.
Claim 2
Dependent Claim
266 words
A HYDROMETALLURGICAL PROCESS FOR RECOVERY OF METALS FROMS ORE CONCENTRATES HAVING COPPER, IRON AND SULFUR THEREIN WHICH COMPRISES A. CONTACTING SAID CONCENTRATE IN AN AQUEOUS MEDIUM WITH A COMBINATION OF NITRIC AND SULFURIC ACIDS AT A TEMPERATURE OF AT LEAST 50*C, UNTIL THE NITRATE IS REDUCED TO LESS THAN ABOUT 30 GRAMS PER LITER IN THE PRESENCE OF CONCENTRATE; B. SEPARATING THE LIQUID AND SOLID FROM STEP (A); C. CONTACTING THE SOLIDS FROM STEP (B) WITH AN AQUEOUS SOLUTION CONTAINING NITRIC ACID IN EXCESS OF THAT REQUIRED TO DISSOLVE THE COPPER IN SAID SOLIDS AT A TEMPERATURE OF AT LEAST 50:C. UNTIL SUBSTANTIALLY ALL OF THE COPPER IN SAID SOLIDS IS DISSOLVED WHEREIN THE TOTAL AMOUNT OF AQUEOUS SOLUTION IN STEPS (A) AND (C) CONTAINS SUFFICIENT ACID TO MAINTAIN COPPER AND IRON IN SOLUTION AND SUFFICIENT WATER TO PRODUCE ABOUT 2-10 PARTS OF COPPER PER 100 PARTS OF LIQUID FROM STEP (B); D. SEPARATING THE SOLIDS FROM STEP (C) AND DIRECTING THE LIQUID FROM STEP (C) TO STEP (A); E. HEATING THE LIQUID FROM STEP (B) TO A TEMPERATURE IN THE RANGE OF 140*-200*C. TO REDUCE THE NITRATE CONCENTRATION THEREIN TO LESS THAN ABOUT ONE PART PER 1,000 PARTS OF SOLUTION; F. PRECIPITATING IRON FROM THE LIQUID FROM STEP (E) AS JAROSITE; G. ELECTROWINNING COPPER FROM THE LIQUID OF STEP (F); AND H. RECYCLING AT LEAST A PORTION OF THE LIQUID FROM STEP (G) TO FURTHER CONTACT CONCENTRATE; SAID PROCESS BEING FURTHER CHARACTERIZED IN THAT OXIDIZING CONDITIONS ARE MAINTAINED IN STEPS (E) AND (F) UNTIL SUBSTANTIALLY ALL OF THE IRON IS PRESENT AS THE FERRIC ION.
Claim 3
Dependent Claim
42 words
The process of claim 1 wherein Steps (a) and (c) are conducted at a temperature of at least 85*C., Step (e) is conducted at a temperature in the range 160*-180*C. and Step (f) is conducted at a temperature in the range 140*-200*C.
Claim 4
Dependent Claim
28 words
The process of claim 2 wherein the major copper containing mineral in said concentrate is selected from the class consisting of chalcopyrite, chalcocite, bornite, diginite and mixtures thereof.
Claim 5
Dependent Claim
33 words
The process of claim 1 wherein Steps (a) and (c) are conducted at a temperature in the range 100*-115*C. and Steps (e) and (f) are conducted at a temperature in the range 160*-180*C.
Claim 6
Dependent Claim
21 words
The process of claim 2 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate iron as ammonojarosite.
Claim 7
Dependent Claim
21 words
The process of claim 4 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate iron as ammonojarosite.
Claim 8
Dependent Claim
24 words
The process of claim 1 wherein Step (a) is conducted in at least two stages with countercurrent flow of liquid and solids between stages.
Claim 9
Dependent Claim
33 words
The process of claim 7 wherein Steps (a) and (c) are conducted at a temperature in the range 100*-115*C. and Steps (e) and (f) are conducted at a temperature in the range 160*-180*C.
Claim 10
Dependent Claim
12 words
The process of claim 8 wherein said concentrate consists essentially of chalcopyrite.
Claim 11
Dependent Claim
27 words
The process of claim 5 wherein no more than about 60 parts of free sulfuric acid are present in 1,000 parts of the liquid from Step (f).
Claim 12
Dependent Claim
34 words
The process of claim 2 wherein the ratio of ferrous ion to nitrate ion is controlled to permit substantially complete removal of said nitrate ion and oxidation of said ferrous ion in Step (e).
Claim 13
Dependent Claim
22 words
The process of claim 7 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate the iron as ammonojarosite.
Claim 14
Dependent Claim
27 words
The process of claim 7 wherein no more than about 60 parts of free sulfuric acid are present in 1,000 parts of the liquid from Step (f).
Claim 15
Dependent Claim
22 words
The process of claim 8 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate the iron as ammonojarosite.
Claim 16
Dependent Claim
22 words
The process of claim 13 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate the iron as ammonojarosite.
Claim 17
Dependent Claim
256 words
The process for the recovery of copper from copper sulfide concentrates containing predominantly chalcopyrite which comprises a. contacting said concentrate with an aqueous solution of nitric and sulfuric acids in a plurality of stages using substantially countercurrent flow of solution and solids between stages; said solution initially containing, based upon the iron and copper in said concentrate, about 1.4-1.7 parts of sulfuric acid per part of copper, about 2.0-3.0 parts of sulfuric acid per part of iron, and about 2.0-4.0 parts of nitric acid per part of copper and water to produce a solution containing about 4-9 parts of copper per 100 parts of solution and wherein nitrate is reduced to less than about 10 grams per liter in the presence of fresh concentrate; b. separating the liquid and solids from the initial stage of Step (a) and separating the solids from the final stage of Step (a); c. heating the liquid from Step (b) to a temperature in the range 160*-180*C. to reduce the nitrate concentration to less than about 1 gram per liter; d. precipitating iron from the liquid from Step (c) as ammonojarosite by contacting the liquid with ammonia or ammonium ion at a temperature in the range 160*-180*C; e. electrowinning the copper from the liquid of Step (d); and f. recycling at least a portion of the liquid from Step (e) to Step (a); said process being further characterized in that oxidizing conditions are maintained in Steps (c) and (d) until substantially all of the iron is present as the ferric ion.
Claim 18
Dependent Claim
256 words
The process for the recovery of copper from copper sulfide concentrates containing predominantly chalcopyrite which comprises a. contacting said concentrate with an aqueous solution of nitric and sulfuric acids in a plurality of stages using substantially countercurrent flow of solution and solids between stages; said solution initially containing, based upon the iron and copper in said concentrate, about 1.4-1.7 parts of sulfuric acid per part of copper, about 2.0-3.0 parts of sulfuric acid per part of iron, and about 2.0-4.0 parts of nitric acid per part of copper and water to produce a solution containing about 4-9 parts of copper per 100 parts of solution and wherein nitrate is reduced to less than about 10 grams per liter in the presence of fresh concentrate; b. separating the liquid and solids from the initial stage of Step (a) and separating the solids from the final stage of Step (a); c. heating the liquid from Step (b) to a temperature in the range 160*-180*C. to reduce the nitrate concentration to less than about 1 gram per liter; d. precipitating iron from the liquid from Step (c) as ammonojarosite by contacting the liquid with ammonia or ammonium ion at a temperature in the range 160*-180*C; e. electrowinning the copper from the liquid of Step (d); and f. recycling at least a portion of the liquid from Step (e) to Step (a); said process being further characterized in that oxidizing conditions are maintained in Steps (c) and (d) until substantially all of the iron is present as the ferric ion.
Claim 19
Dependent Claim
46 words
The process of claim 16 wherein said aqueous solution of nitric and sulfuric acids in Step (a) contains 1.5-1.6 parts of sulfuric acid per part of copper, 2.5-2.7 parts of sulfuric acid per part of iron, and 3.0-3.5 parts of nitric acid per part of copper.
Claim 20
Dependent Claim
19 words
The process of claim 17 wherein the purge is taken as a portion of the liquid from Step (e).
Claim 21
Dependent Claim
30 words
The process of claim 18 wherein the concentration of ferrous ion in the liquid introduced in Step (c) is at least 2.3 parts per part by weight of nitrate ion.
Claim 22
Dependent Claim
30 words
The process of claim 16 wherein the concentration of ferrous ion in the liquid introduced in Step (c) is at least 2.3 parts per part by weight of nitrate ion.
Claim 23
Dependent Claim
273 words
A hydrometallurgical process for recovery of metals from ores having copper, iron and sulfur therein which comprises a. contacting said ore in an aqueous medium with a combination of nitric and sulfuric acids at a temperature of at least 50*C. until the nitrate is reduced to less than about 30 grams per liter and at least 2.0 parts by weight of ferrous ion per part by weight of nitrate is generated in the presence of ore; b. separating the liquid and solid from Step (a); c. contacting the solids from Step (b) with an aqueous solution containing nitric acid in excess of that required to dissolve the copper in said solids at a temperature of at least 50*C. until substantially all of the copper in said solids is dissolved wherein the total amount of aqueous solution in Steps (a) and (c) contains sufficient acid to maintain copper and iron in solution and sufficient water to produce about 2-10 parts of copper per 100 parts of liquid from Step (b); d. separating the solids from Step (c) and directing the liquid from Step (c) to Step (a); e. heating the liquid from Step (b) to reduce the nitrate concentration therein to less than about 1 part per 1,000 parts of solution; f. precipitating iron from the liquid from Step (e); g. electrowinning copper from the liquid of Step (f); and h. recycling at least a portion of the liquid from Step (g) to further contact ore; said process being further characterized in that oxidizing conditions are maintained in Steps (e) and (f) until substantially all of the iron is present as the ferric ion.
Claim 24
Dependent Claim
273 words
A hydrometallurgical process for recovery of metals from ores having copper, iron and sulfur therein which comprises a. contacting said ore in an aqueous medium with a combination of nitric and sulfuric acids at a temperature of at least 50*C. until the nitrate is reduced to less than about 30 grams per liter and at least 2.0 parts by weight of ferrous ion per part by weight of nitrate is generated in the presence of ore; b. separating the liquid and solid from Step (a); c. contacting the solids from Step (b) with an aqueous solution containing nitric acid in excess of that required to dissolve the copper in said solids at a temperature of at least 50*C. until substantially all of the copper in said solids is dissolved wherein the total amount of aqueous solution in Steps (a) and (c) contains sufficient acid to maintain copper and iron in solution and sufficient water to produce about 2-10 parts of copper per 100 parts of liquid from Step (b); d. separating the solids from Step (c) and directing the liquid from Step (c) to Step (a); e. heating the liquid from Step (b) to reduce the nitrate concentration therein to less than about 1 part per 1,000 parts of solution; f. precipitating iron from the liquid from Step (e); g. electrowinning copper from the liquid of Step (f); and h. recycling at least a portion of the liquid from Step (g) to further contact ore; said process being further characterized in that oxidizing conditions are maintained in Steps (e) and (f) until substantially all of the iron is present as the ferric ion.
Claim 25
Dependent Claim
20 words
The process of claim 21 wherein the nitrate is reduced before a substantial amount of the ferrous ion is generated.
Claim 26
Dependent Claim
26 words
The process of claim 21 wherein at least 2.3 parts by weight of ferrous in per part by weight of nitrate are generated in Step (a).
Claim 27
Dependent Claim
17 words
The process of claim 23 wherein Step (e) is conducted at a temperature in the range 140*-200*C.
Claim 28
Dependent Claim
26 words
The process of claim 24 wherein no more than about 60 parts of free sulfuric acid are present in 1,000 parts of liquid from Step (f).
Claim 29
Dependent Claim
34 words
The process of claim 22 wherein the ratio of ferrous ion to nitrate ion is controlled to permit substantially complete removal of said nitrate ion and oxidation of said ferrous ion in Step (e).
Claim 30
Dependent Claim
24 words
The process of claim 22 wherein Step (a) is conducted in at least two stages with countercurrent flow of liquid and solids between stages.
Claim 31
Dependent Claim
21 words
The process of claim 24 wherein ammonia or the ammonium ion is introduced in Step (f) to precipitate iron as ammonojarosite.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-06-09 | 1978-12-09 | 1979-06-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-06-09 | 1982-12-09 | 1983-06-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-06-09 | 1986-12-09 | 1987-06-10 | $7700.00 | Window Closed / Lapsed |