EP0059806A1 - Anode slime treatment process - Google Patents
Anode slime treatment process Download PDFInfo
- Publication number
- EP0059806A1 EP0059806A1 EP19810301045 EP81301045A EP0059806A1 EP 0059806 A1 EP0059806 A1 EP 0059806A1 EP 19810301045 EP19810301045 EP 19810301045 EP 81301045 A EP81301045 A EP 81301045A EP 0059806 A1 EP0059806 A1 EP 0059806A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- solution
- slime
- lead
- resulting
- leaching
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/06—Refining
- C22B13/10—Separating metals from lead by crystallising, e.g. by Pattison process
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
Definitions
- This invention relates to a process for recovering lead from anode slime in order to upgrade the slime.
- the leached slimes are then melted down in a small reverberatory (Dor6) furnace in which the impurities are oxidized, leaving so-called Dore metal containing the precious metals, silver and gold.
- Dore metal is then pasted to recover fine gold, fine silver, and any other precious metal present in the original slime.
- the present invention provides a process for upgrading anode slime containing lead and for recovering lead from the anode slime by leaching, in which leaching is carried out in a plurality of stages and the resulting solutions, together containing most of the lead content of the slime, are combined to form a solution from which lead acetate crystallizes.
- the process comprises the following steps:
- the solution resulting from step (b) preferably contains about 46% or more of the initial lead content of the slime.
- the amount of lead extracted in the two steps is approximately equal, but the first step extracts slightly more than the second.
- the slime is leached with a solution of ammonium acetate at a temperature not exceeding 80°C.
- a solution of ammonium acetate at a temperature not exceeding 80°C.
- lead dissolution is maximized and dissolution of the other metal is minimized.
- the leach solutions used in the two steps are preferably substantially identical but may be different, depending on the practical circumstances.
- the process can be utilized to upgrade any type of anode slime or mud produced in electrolytic refining of copper.
- the optimum processing parameters for any particule slime can be determined by making test runs based on the particular composition of such slime.
- the leaching of a slime to remove lead has need for a shorter period of time for those slimes containing low amounts of lead, and correspondingly a longer leach time for those slimes containing high amounts of lead.
- Leaching may be effected under agitation in any conventional leaching vessel with an aqueous ammonium acetate solution with concentration greater than 0.1 mole dm -3 , preferably from about 2 to 10 mole dm- 3 .
- concentration greater than 0.1 mole dm -3 , preferably from about 2 to 10 mole dm- 3 .
- the particular amounts of ammonium acetate used depend upon the concentration of lead in the slime be processed. For conventional slimes, amounts within the above range are adequate for an effective leach.
- the leaching solution is separated from the undissolved slime. This can be accomplished by any conventional technique, preferably by filtration.
- the leach slurry can be thickened prior to filtration or filtered directly from the leach.
- the final solid residue is dried and processed for shipment to plants for recovery of precious metals and other metal values. Because the lead has been removed, the dried processed anode slime is acceptable for treatment in recovery plants for selenium, tellurium, tin, silver, gold, and the like.
- the combined clarified or filtered solution is purified by the removal of the lead content by crystallization.
- the crystallized lead acetate from this purification step is recovered through filtration, decantation, or any solid-liquid separation techniques.
- the resultant clarified or filtered solution can be recycled back to the secondary leaching step for reuse, as shown in the drawing.
- a decopperized anode slime leaching experiment was carried out in a flask equipped with an agitator, a condenser, heating apparatus, and a temperature indicator and controller.
- the sample of anode slime used possessed the following assay:
- the lead, silver, copper, selenium, and tin containing solution was heated until the total volume was reduced to one-third of the initial volume and then cooled down to below 40°C. Meanwhile, lead acetate crystallized out from the mother liquor. After filtration and drying, lead acetate with a purity of greater than 99.9% was obtained.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Treatment Of Sludge (AREA)
Abstract
Description
- This invention relates to a process for recovering lead from anode slime in order to upgrade the slime.
- The presence of a large amount of lead in anode slime makes the recovery of precious metals and other valuable metals from the slime more difficult. A variety of techniques have been utilized to recover precious metals from the slime. None, however, has been commercially successful because of the large cost involved and the fact that it is difficult to recover precious metals from the slime. One type of technique involves direct smelting of slimes. This is disadvantageous as excessive formation of matte and slag causes heavy recirculation of precious metals. Such techniques involve roasting to convert copper to copper oxide followed by leaching of the roasted slimes with sulphuric acid. The leached slimes are then melted down in a small reverberatory (Dor6) furnace in which the impurities are oxidized, leaving so-called Dore metal containing the precious metals, silver and gold. The Dore metal is then pasted to recover fine gold, fine silver, and any other precious metal present in the original slime. This particular technique is, as noted, disadvantageous because of the excessive formation of matte and slag.
- A variety of other pyrometallurgical techniques combined with acid leachs and acid leach processes have also been attempted, but they are not suitable, mainly because it has not been possible to initially remove substantially all of the lead from the slime. It has not hitherto been found possible to remove the lead content of anode slime by acid leaching. The presence of lead in the slime has greatly inhibited the known processes from recovering precious metals from slime.
- The present invention provides a process for upgrading anode slime containing lead and for recovering lead from the anode slime by leaching, in which leaching is carried out in a plurality of stages and the resulting solutions, together containing most of the lead content of the slime, are combined to form a solution from which lead acetate crystallizes.
- In particular, the process comprises the following steps:
- (a) subjecting the slime to primary leaching by means of a first leach solution at a first temperature and for a first period of time such that the resulting solution contains about 48% or more of the initial lead content of the slime;
- (b) subjecting the residue from step (a) to secondary leaching by means of a second leach station at a second temperature and for a second period of time such that the resulting solution and that resulting from step (a) together contain about 94% or more of the initial lead content of the slime;
- (c) combining the solutions resulting from steps (a) and (b); and
- (d) concentrating the combined solution, the composition of the first and second leach solutions being such that lead acetate crystallizes out of the concentrated combined solution.
- The solution resulting from step (b) preferably contains about 46% or more of the initial lead content of the slime. In other words, for optimum efficiency, the amount of lead extracted in the two steps is approximately equal, but the first step extracts slightly more than the second.
- Preferably, the slime is leached with a solution of ammonium acetate at a temperature not exceeding 80°C. Thereby lead dissolution is maximized and dissolution of the other metal is minimized. The leach solutions used in the two steps are preferably substantially identical but may be different, depending on the practical circumstances.
- The invention will be described further, by way of example, with reference to the accompanying drawing, whose sole Figure is a flow sheet of a process according to the invention.
- The process can be utilized to upgrade any type of anode slime or mud produced in electrolytic refining of copper. The optimum processing parameters for any particule slime can be determined by making test runs based on the particular composition of such slime. Thus, for example, the leaching of a slime to remove lead, as discussed below, has need for a shorter period of time for those slimes containing low amounts of lead, and correspondingly a longer leach time for those slimes containing high amounts of lead.
- Leaching may be effected under agitation in any conventional leaching vessel with an aqueous ammonium acetate solution with concentration greater than 0.1 mole dm-3, preferably from about 2 to 10 mole dm-3. The particular amounts of ammonium acetate used depend upon the concentration of lead in the slime be processed. For conventional slimes, amounts within the above range are adequate for an effective leach.
- It is desirable to maintain a temperature of about 40°C throughout leaching and preferably not exceeding a temperature of about 600c and the leaching steps are carried out for a total time sufficient to leach substantially all of the lead from the slime, to leave a lead content of preferably no more than about 3% based on the weight of the slime being leached. In general, this will take a total leach time of between 1 to 3 hours, again the particular time being dependent upon the slime treated. In general each leach will last at least 20 minutes, preferably 1 to 2 hours.
- After leaching is completed, the leaching solution is separated from the undissolved slime. This can be accomplished by any conventional technique, preferably by filtration. The leach slurry can be thickened prior to filtration or filtered directly from the leach. The final solid residue is dried and processed for shipment to plants for recovery of precious metals and other metal values. Because the lead has been removed, the dried processed anode slime is acceptable for treatment in recovery plants for selenium, tellurium, tin, silver, gold, and the like. The combined clarified or filtered solution is purified by the removal of the lead content by crystallization. The crystallized lead acetate from this purification step is recovered through filtration, decantation, or any solid-liquid separation techniques. The resultant clarified or filtered solution can be recycled back to the secondary leaching step for reuse, as shown in the drawing.
- To more fully illustrate the determination of the optimum process parameters, the following examples are presented. It is to be understood, however, that these examples are given by way of illustration and not limitation.
- A decopperized anode slime leaching experiment was carried out in a flask equipped with an agitator, a condenser, heating apparatus, and a temperature indicator and controller.
-
- 845 gram (wet basis) samples of the slime together with the stoichiometric amount of ammonium acetate in various concentrations were placed in the said flask and heated for periods varying from 1 to 4 hours at a temperature of 40°C. The percentage of extraction of lead is set forth in Table I below.
- Samples of decopperized anode slime having an assay similar to that set forth in Example I were leached in a manner similar to that set forth in Example I but at various temperatures from 20 to 100°C. Ammonium acetate at a concentration of 6 mole dm-3 was used as the leaching reagent. The percentage of extraction of lead is set forth in Table II below.
- Samples of decopperized anode slime having an assay similar to that set forth in Example I were leached twice with ammonium acetate solutions of various concentrations at 40oC. Each time a period of 2 hours was used for leaching. The overall percentage of extraction of lead is set forth in Table III below.
- Samples of decopperized anode slime having an assay similar to that set forth in Example I were leached twice with 6 mole dm-3 ammonium acetate solution at various temperatures in the range from 20°C to 100°C. Each time a period of 2 hours was used for leach. The overall percentage of extraction of lead is set forth in Table IV below.
-
- The lead, silver, copper, selenium, and tin containing solution was heated until the total volume was reduced to one-third of the initial volume and then cooled down to below 40°C. Meanwhile, lead acetate crystallized out from the mother liquor. After filtration and drying, lead acetate with a purity of greater than 99.9% was obtained.
Claims (20)
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19810301045 EP0059806B1 (en) | 1981-03-12 | 1981-03-12 | Anode slime treatment process |
DE1981301045 DE59806T1 (en) | 1981-03-12 | 1981-03-12 | METHOD FOR PROCESSING ANODE SLUDGE. |
DE8181301045T DE3167023D1 (en) | 1981-03-12 | 1981-03-12 | Anode slime treatment process |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19810301045 EP0059806B1 (en) | 1981-03-12 | 1981-03-12 | Anode slime treatment process |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0059806A1 true EP0059806A1 (en) | 1982-09-15 |
EP0059806B1 EP0059806B1 (en) | 1984-11-07 |
Family
ID=8188237
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP19810301045 Expired EP0059806B1 (en) | 1981-03-12 | 1981-03-12 | Anode slime treatment process |
Country Status (2)
Country | Link |
---|---|
EP (1) | EP0059806B1 (en) |
DE (2) | DE59806T1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001021846A1 (en) * | 1999-09-17 | 2001-03-29 | Interpole Limited | Recovery of metallic lead and salt value from lead ores or from spent lead-acid storage batteries with acetic acid lixiviant |
CN112981111A (en) * | 2021-02-09 | 2021-06-18 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Method for selectively recovering copper from lead anode slime and method for recovering metal from lead anode slime |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1916303A (en) * | 1932-05-03 | 1933-07-04 | Leo P Curtin | Method of converting roasted lead ores and bag-house dust directly into lead salts |
US2328089A (en) * | 1940-09-14 | 1943-08-31 | Lillian R Birkenstein | Recovery of soluble lead salts from insoluble lead compounds |
DE750429C (en) * | 1940-12-13 | 1944-12-21 | Process for processing hut products containing lead antimon including by-products such as scrapes or smears | |
DE1948300B2 (en) * | 1969-09-24 | 1971-02-18 | Norddeutsche Affinerie | Copper electrolysis anode slime decomposi - tion |
FR2086064A1 (en) * | 1970-04-14 | 1971-12-31 | American Metal Climax Inc | |
US4002544A (en) * | 1975-04-03 | 1977-01-11 | Outokumpu Oy | Hydrometallurgical process for the recovery of valuable components from the anode slime produced in the electrolytical refining of copper |
US4047939A (en) * | 1975-06-13 | 1977-09-13 | Noranda Mines Limited | Slimes treatment process |
US4229270A (en) * | 1978-04-12 | 1980-10-21 | The International Nickel Co., Inc. | Process for the recovery of metal values from anode slimes |
EP0020826A1 (en) * | 1979-06-14 | 1981-01-07 | Institute Of Nuclear Energy Research | A hydrometallurgical process for recovering precious metals from anode slime |
DD146712A1 (en) * | 1979-10-19 | 1981-02-25 | Manfred Lux | METHOD FOR THE HYDROMETALLURGICAL REPRODUCTION OF ANODEN SLUDGE OF COPPER ELECTROLYSIS |
-
1981
- 1981-03-12 DE DE1981301045 patent/DE59806T1/en active Pending
- 1981-03-12 DE DE8181301045T patent/DE3167023D1/en not_active Expired
- 1981-03-12 EP EP19810301045 patent/EP0059806B1/en not_active Expired
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1916303A (en) * | 1932-05-03 | 1933-07-04 | Leo P Curtin | Method of converting roasted lead ores and bag-house dust directly into lead salts |
US2328089A (en) * | 1940-09-14 | 1943-08-31 | Lillian R Birkenstein | Recovery of soluble lead salts from insoluble lead compounds |
DE750429C (en) * | 1940-12-13 | 1944-12-21 | Process for processing hut products containing lead antimon including by-products such as scrapes or smears | |
DE1948300B2 (en) * | 1969-09-24 | 1971-02-18 | Norddeutsche Affinerie | Copper electrolysis anode slime decomposi - tion |
FR2086064A1 (en) * | 1970-04-14 | 1971-12-31 | American Metal Climax Inc | |
US4002544A (en) * | 1975-04-03 | 1977-01-11 | Outokumpu Oy | Hydrometallurgical process for the recovery of valuable components from the anode slime produced in the electrolytical refining of copper |
US4047939A (en) * | 1975-06-13 | 1977-09-13 | Noranda Mines Limited | Slimes treatment process |
US4229270A (en) * | 1978-04-12 | 1980-10-21 | The International Nickel Co., Inc. | Process for the recovery of metal values from anode slimes |
EP0020826A1 (en) * | 1979-06-14 | 1981-01-07 | Institute Of Nuclear Energy Research | A hydrometallurgical process for recovering precious metals from anode slime |
DD146712A1 (en) * | 1979-10-19 | 1981-02-25 | Manfred Lux | METHOD FOR THE HYDROMETALLURGICAL REPRODUCTION OF ANODEN SLUDGE OF COPPER ELECTROLYSIS |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001021846A1 (en) * | 1999-09-17 | 2001-03-29 | Interpole Limited | Recovery of metallic lead and salt value from lead ores or from spent lead-acid storage batteries with acetic acid lixiviant |
CN112981111A (en) * | 2021-02-09 | 2021-06-18 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Method for selectively recovering copper from lead anode slime and method for recovering metal from lead anode slime |
Also Published As
Publication number | Publication date |
---|---|
DE3167023D1 (en) | 1984-12-13 |
DE59806T1 (en) | 1983-04-14 |
EP0059806B1 (en) | 1984-11-07 |
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