US3883345A
Expired / Lapsed
US
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Process for the recovery of antimony
Assignee: NL Industries Inc
•
Filing: 1971-08-10
•
Granted: 1975-05-13
•
Expires: 1991-08-10
Abstract
Abstract A process for the recovery of antimony values from a material containing the same is described wherein the material is subjected to a controlled roasting step, the resulting calcine leached with an alkaline solution to extract antimony values and the antimony-pregnant solution acidified to precipitate antimony values. The roasting step is carried out in a reducing environment thus assuring that the calcine contains only trivalent antimony and broadening the operable feed to the process. The acidification step is preferably one which regenerates the leaching solution for recycle to the process.
Inventors
- 👤 Frank R Caldon
- 👤 Joseph E Pimentel
- 👤 Clifford J Lewis
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 07:52
CPC Classifications
C; C22; C22B; C22B30/00; C22B30/02
Claims Analysis
Total Claims: 43
Claim 1
Independent Claim
115 words
A process for the recovery of antimony values from ore containing the same which comprises the steps of: roasting the antimony-containing material in the presence of a reducing agent under controlled conditions of time and temperature to produce a calcine; leaching said calcine in an alkaline solution to produce a mixture of an antimony-pregnant aqueous solution and a solid residue; filtering said mixture; discarding said solid residue from the process; adjusting the hydrogen ion concentration of said filtered antimony-pregnant solution with an acid-former to cause the antimony values in said pregnant solution to precipitate as an antimony concentrate; separating said precipitated antimony concentrate and; drying said antimony concentrate to yield a high purity antimony salt.
Claim 2
Dependent Claim
115 words
A process for the recovery of antimony values from ore containing the same which comprises the steps of: roasting the antimony-containing material in the presence of a reducing agent under controlled conditions of time and temperature to produce a calcine; leaching said calcine in an alkaline solution to produce a mixture of an antimony-pregnant aqueous solution and a solid residue; filtering said mixture; discarding said solid residue from the process; adjusting the hydrogen ion concentration of said filtered antimony-pregnant solution with an acid-former to cause the antimony values in said pregnant solution to precipitate as an antimony concentrate; separating said precipitated antimony concentrate and; drying said antimony concentrate to yield a high purity antimony salt.
Claim 3
Dependent Claim
27 words
A process according to claim 1 in which the antimony containing material is an antimony ore in which the antimony occurs substantially as an antimony oxide mineral.
Claim 4
Dependent Claim
27 words
A process according to claim 1 in which the antimony containing material is an antimony ore in which the antimony occurs substantially as an antimony sulfide mineral.
Claim 5
Dependent Claim
23 words
A process according to claim 1 in which the antimony containing material is a mixture of antimony oxide minerals and antimony sulfide minerals.
Claim 6
Dependent Claim
22 words
A process according to claim 1 in which the antimony containing material is an antimony concentrate produced from an ore containing antimony.
Claim 7
Dependent Claim
14 words
A process according to claim 1 in which the alkaline solution is potassium carbonate.
Claim 8
Dependent Claim
15 words
A process according to claim 1 in which the aqueous alkaline solution is sodium carbonate.
Claim 9
Dependent Claim
21 words
A process according to claim 1 in which the aqueous alkaline solution is a mixture of sodium carbonate and potassium carbonate.
Claim 10
Dependent Claim
35 words
A process according to claim 1 in which the aqueous alkaline solution used is selected from the class consisting of solutions of sodium hydroxide, calcium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or mixtures thereof.
Claim 11
Dependent Claim
17 words
The process of claim 1 in which the reducing agent is coal or coke produced from coal.
Claim 12
Dependent Claim
15 words
The process of claim 1 in which the reducing agent is coke derived from petroleum.
Claim 13
Dependent Claim
12 words
The process of claim 1 in which the reducing agent is charcoal.
Claim 14
Dependent Claim
26 words
ThE process of claim 1 in which the reducing agent is a gaseous hydrocarbon selected from the class consisting of methane, carbon monoxide, and natural gas.
Claim 15
Dependent Claim
13 words
The process of claim 1 in which the acid-former is carbon dioxide gas.
Claim 16
Dependent Claim
14 words
The process of claim 1 in which the acid-former used is sulfur dioxide gas.
Claim 17
Dependent Claim
13 words
The process of claim 1 in which the acid-former used is sulfuric acid.
Claim 18
Dependent Claim
13 words
The process of claim 1 in which the acid-former used is nitric acid.
Claim 19
Dependent Claim
13 words
The process of claim 1 in which the acid-former used is hydrochloric acid.
Claim 20
Dependent Claim
13 words
The process of claim 1 in which the acid-former used is sulfur trioxide.
Claim 21
Dependent Claim
16 words
The process of claim 1 in which the acid-former used is a mixture of acid-forming gases.
Claim 22
Dependent Claim
16 words
The process of claim 1 in which the acid-former used is a mixture of mineral acids.
Claim 23
Dependent Claim
26 words
The process of claim 1 in which the antimony-containing material is ground to a particle size such that it passes through 28 Mesh Standard Tyler Screen.
Claim 24
Dependent Claim
20 words
The process of claim 1 in which the reducing agent is sized to pass a 28 Mesh Standard Tyler Screen.
Claim 25
Dependent Claim
33 words
The process of claim 1 in which the ratio of reducing agent to antimony in the mixture roasted is between 0.2 lbs. and 10.0 lbs. of reducing agent for each pound of antimony.
Claim 26
Dependent Claim
19 words
The process of claim 1 in which the roasting temperature is controlled to one between about 300* and 1,000*C.
Claim 27
Dependent Claim
20 words
The process of claim 1 in which the calcine leaching time is between about 10 minutes and about 120 minutes.
Claim 28
Dependent Claim
27 words
The process of claim 1 in which the hydrogen ion concentration of the antimony-pregnant leach solution is adjusted to a pH value of between 4.0 and 12.0.
Claim 29
Dependent Claim
147 words
A process for the production of a high purity antimony compound which comprises the steps of: grinding an antimony containing material and a carbon containing material; mixing said ground materials in a ratio of carbon to antimony between 0.2 and 10.0; heating said mix to a temperature of between 300* and 1,000*C for a period of 10 minutes to 120 minutes; agitating the calcine so formed in an aqueous carbonate solution for a time period of 10 minutes to 120 minutes to result in an antimony-pregnant solution and an insoluble residue; separating said antimony-pregnant solution from said insoluble residue; treating said antimony-pregnant solution with carbon dioxide gas to precipitate an antimony compound and to regenerate aqueous carbonate; separating the regenerated carbonate solution from the precipitated antimony compound; recycling said solution to the leaching step; and drying the antimony precipitate to result in a high purity antimony compound.
Claim 30
Dependent Claim
147 words
A process for the production of a high purity antimony compound which comprises the steps of: grinding an antimony containing material and a carbon containing material; mixing said ground materials in a ratio of carbon to antimony between 0.2 and 10.0; heating said mix to a temperature of between 300* and 1,000*C for a period of 10 minutes to 120 minutes; agitating the calcine so formed in an aqueous carbonate solution for a time period of 10 minutes to 120 minutes to result in an antimony-pregnant solution and an insoluble residue; separating said antimony-pregnant solution from said insoluble residue; treating said antimony-pregnant solution with carbon dioxide gas to precipitate an antimony compound and to regenerate aqueous carbonate; separating the regenerated carbonate solution from the precipitated antimony compound; recycling said solution to the leaching step; and drying the antimony precipitate to result in a high purity antimony compound.
Claim 31
Dependent Claim
18 words
The process of claim 28 in which the heat treatment is carried out in a direct fired roaster.
Claim 32
Dependent Claim
31 words
The process of claim 28 in which the heat treatment step is carried out in an indirectly heated roaster in which the products of combustion do not contact the roaster charge.
Claim 33
Dependent Claim
33 words
The process of claim 28 in which the heat treatment step is carried out in a batch-type furnace in such a manner that the furnace charge can be rabbled during the roasting operation.
Claim 34
Dependent Claim
30 words
The process of claim 28 in which the carbonate content of the leaching solution is maintained between 30 g. and 500 g. of potassium carbonate per liter of leach solution.
Claim 35
Dependent Claim
34 words
The process of claim 28 in which the hydrogen ion content of the antimony-pregnant solution is adjusted by introduction of carbon dioxide gas to a pH range of between pH 4.0 and pH 9.0.
Claim 36
Dependent Claim
19 words
The process of claim 33 in which the pH is adjusted to approximately pH 7.0 with a mineral acid.
Claim 37
Dependent Claim
25 words
The process of claim 28 in which the calcine is comminuted to substantially a 20 Mesh Standard Tyler Screen size prior to the leaching step.
Claim 38
Dependent Claim
82 words
A PROCESS FOR THE PRODUCTION OF AN ALKALI CARBONATE SOLUTION CONTAINING DISSOLVED ANTIMONY THEREIN, WHICH COMPRISES THE STEPS OF: HEAT TREATING A MIXTURE OF AN ANTIMONY-CONTAINING MATERIAL AND A CARBON-CONTAINING MATERIAL, SAID HEAT TREATMENT BEING IN THE RANGE OF 800* TO 1,000*C; AGITATING SAID HEAT TREATED MIXTURE IN AN AQUEOUS SOLUTION OF AN ALKALI CARBONATE TO RESULT IN AN ANTIMONY-PREGNANT ALKALI CARBONATE SOLUTION AND AN INSOLUBLE RESIDUE; SEPARATING SAID RESIDUE FROM SAID SOLUTION; AND FURTHER PROCESSING SAID SOLUTION FOR ITS ANTIMONY VALUES.
Claim 39
Dependent Claim
82 words
A PROCESS FOR THE PRODUCTION OF AN ALKALI CARBONATE SOLUTION CONTAINING DISSOLVED ANTIMONY THEREIN, WHICH COMPRISES THE STEPS OF: HEAT TREATING A MIXTURE OF AN ANTIMONY-CONTAINING MATERIAL AND A CARBON-CONTAINING MATERIAL, SAID HEAT TREATMENT BEING IN THE RANGE OF 800* TO 1,000*C; AGITATING SAID HEAT TREATED MIXTURE IN AN AQUEOUS SOLUTION OF AN ALKALI CARBONATE TO RESULT IN AN ANTIMONY-PREGNANT ALKALI CARBONATE SOLUTION AND AN INSOLUBLE RESIDUE; SEPARATING SAID RESIDUE FROM SAID SOLUTION; AND FURTHER PROCESSING SAID SOLUTION FOR ITS ANTIMONY VALUES.
Claim 40
Dependent Claim
18 words
The process of claim 36 in which the alkali carbonate solution is an aqueous solution of potassium carbonate.
Claim 41
Dependent Claim
19 words
The process of claim 36 in which the antimony dissolving step is carried out at ambient temperatures and pressures.
Claim 42
Dependent Claim
19 words
The process of claim 36 in which the antimony dissolving step is carried out at elevated temperatures and pressures.
Claim 43
Dependent Claim
17 words
The process of claim 36 in which the alkali carbonate solution is a solution of sodium carbonate.
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US2331395A
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US2325176A
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-05-12 | 1978-11-11 | 1979-05-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-05-12 | 1982-11-11 | 1983-05-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-05-12 | 1986-11-11 | 1987-05-13 | $7700.00 | Window Closed / Lapsed |