CN111549233A - Method for recovering lead and bismuth from copper anode mud smelting slag - Google Patents
Method for recovering lead and bismuth from copper anode mud smelting slag Download PDFInfo
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- CN111549233A CN111549233A CN202010257271.0A CN202010257271A CN111549233A CN 111549233 A CN111549233 A CN 111549233A CN 202010257271 A CN202010257271 A CN 202010257271A CN 111549233 A CN111549233 A CN 111549233A
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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- 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
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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- 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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0028—Smelting or converting
- C22B15/003—Bath smelting or converting
- C22B15/0034—Bath smelting or converting in rotary furnaces, e.g. kaldo-type furnaces
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- 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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0056—Scrap treating
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- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to the field of non-ferrous metal smelting, and particularly relates to a method for recovering lead and bismuth from copper anode slime smelting slag, which comprises the following steps: (1) adding copper anode slime smelting slag, a reducing agent and a slagging agent into a hearth of a Kaldo furnace, and heating to 1100-1150 ℃ for reduction smelting; (2) separating first slag after the reduction smelting is finished; (3) cooling the Kaldo furnace, and separating a second batch of slag before discharging the melt; (4) pouring the melt in the furnace into a metal ladle, and continuously cooling until the upper layer of the melt in the metal ladle forms a slag shell; (5) and casting the melt in the metal ladle into ingots, and stripping off slag shells to obtain metal ingots, namely the lead-bismuth alloy. According to the scheme of the invention, the high-efficiency separation of lead and bismuth in the copper anode slime smelting slag can be realized only by using the Kaldo furnace and related matched equipment, the content of lead and bismuth in the finally obtained alloy can be up to more than 90%, the process is simple, and the equipment investment is low.
Description
Technical Field
The invention belongs to the field of non-ferrous metal smelting, and particularly relates to a method for recovering lead and bismuth from copper anode slime smelting slag.
Background
Anode mud generated by copper electrolysis is generally smelted by a Kaldo furnace fire method to obtain copper anode mud smelting slag, and the smelting slag is processed by the following two methods: one is directly returned to a copper smelting system for treatment, but the quality of electrolytic copper is greatly influenced due to the high bismuth content in the slag; the other method is direct sale, the price is calculated according to the content of gold and silver in each batch of smelting slag, the problems of smelting slag accumulation and excessive bismuth in copper electrolyte are solved, the loss of valuable metals such as gold and silver is large, and the problem of environmental protection in solid waste transportation is also large.
In order to solve the above problems, some methods for recovering valuable metals by wet-processing copper anode slime smelting slag have appeared in the same industry, such as "a method for recovering valuable metals from carrodo furnace smelting slag by wet separation" (patent publication No. CN106086440B) and "a method for separating antimony and bismuth from carrodo furnace slag hydrochloric acid leachate" (application publication No. CN109136578A) in chinese patent, however, this method has low recovery rate, complex process, complicated equipment, large sewage treatment capacity, and difficult treatment.
A chinese patent "a method for extracting a lead-bismuth alloy from copper anode slime smelting waste residue" (application publication No. CN109536730A), published as 2019, 03 and 29, discloses a method for treating smelting waste residue by a "dry method": reducing, smelting and slagging in a Kaldo furnace, and removing copper, nickel and silver in an intermediate frequency furnace to obtain the lead-bismuth alloy with high purity. Although the method realizes the recovery of lead and bismuth and the purity of the lead and bismuth alloy is higher, in the practical operation, the crude lead and bismuth alloy obtained by the Kaldo furnace is transferred into the intermediate frequency furnace, and the melt with high temperature cannot be transferred for a long distance, so the melt needs to be cast into ingots, and then the alloy ingots are transferred into the intermediate frequency furnace to be melted again and are subjected to impurity removal for multiple times. This method has at least the following drawbacks: firstly, auxiliary materials are required to be added for many times to remove impurities for many times, and the process is complex; secondly, adding auxiliary materials to remove impurities, wherein most of the processing components are removed, but part of the added auxiliary materials also remain in the melt, so that the obtained alloy components are more complex; thirdly, the ingot is transferred and melted again after being cast, so that a large amount of heat is lost in the process, and the energy utilization rate is low; fourthly, the intermediate frequency furnace belongs to an open furnace body, and the environmental pollution is serious in the operation process.
Disclosure of Invention
The invention aims to provide a method for recovering lead and bismuth from copper anode slime smelting slag, which can realize the efficient recovery of lead and bismuth in the copper anode slime smelting slag, and has the advantages of simple process, less used equipment and less impurities of the obtained lead-bismuth alloy.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for recovering lead and bismuth from copper anode slime smelting slag comprises the following steps:
(1) adding copper anode slime smelting slag, a reducing agent and a slagging agent into a hearth of a Kaldo furnace, and heating to 1100-1150 ℃ for reduction smelting;
(2) separating first slag after the reduction smelting is finished;
(3) cooling the Kaldo furnace, and separating a second batch of slag before discharging the melt;
(4) pouring the melt in the furnace into a metal ladle, and continuously cooling until the upper layer of the melt in the metal ladle forms a slag shell;
(5) and casting the melt in the metal ladle into ingots, and stripping off slag shells to obtain metal ingots, namely the lead-bismuth alloy.
By adopting the scheme, the copper anode mud smelting slag is reduced and smelted in a Kaldo furnace, lead, bismuth, copper and the like are reduced into metal simple substances, and the slag formed by barium, silicon dioxide and the like is separated; because the solidification temperatures of different substances are different, after the melt is cooled, the copper simple substance in the melt is also solidified into a solid state and enters the slag to be separated; and (3) introducing the melt in the furnace into a metal ladle, continuously cooling, continuously solidifying new impurities and forming a slag shell on the upper surface of the melt in the metal ladle, and directly leaving the slag shell in the metal ladle to realize the separation from the lead-bismuth alloy melt during casting. According to the scheme of the invention, the high-efficiency separation of lead and bismuth in the copper anode slime smelting slag can be realized only by using the Kaldo furnace and related matched equipment, the content of lead and bismuth in the finally obtained alloy can be up to more than 90%, the process is simple, and the equipment investment is low.
Specifically, in the step (1), the copper anode slime smelting slag is firstly crushed into blocks with the particle size of 1-2 cm, and then the blocks are added into a Kaldo furnace. The heating process before reduction smelting has the function of drying the materials. The size of material particles has great influence on the melting degree of the material and the smelting time of the material, the material with overlarge particles is difficult to melt, and the melted material and the unmelted material are easy to be wrapped, so that the material spraying phenomenon is generated; too powder then the gas permeability of material is relatively poor, and the material is difficult to dry, and the easy system negative pressure of adding the in-process of material is taken out to the system and is leaded to equipment pipeline to block up, through a large amount of experiments, particle size 1 ~ 2cm is best.
In the step (1), the adding amount of the reducing agent coke is 3-4% calculated by the total mass of the added copper anode slime smelting slag; the addition amount of the slag former sodium carbonate is 2-3%. Copper anode mud smelting slag, a reducing agent and a slagging agent are added into a hearth of the Kaldo furnace in 2-3 batches.
After the materials are added into a hearth of the Kaldo furnace, natural gas and oxygen are introduced for combustion and heating, wherein the flow of the natural gas is 2.0-3.0 Nm3And/min, wherein the flow ratio of oxygen to natural gas is 1.8-2.0, and the Kaldo furnace starts to rotate to heat and dry the material.
In the process of smelting reduction reaction, coke is used as a reducing agent, sodium carbonate is used as a slag former, natural gas and oxygen provide heat to realize the smelting reduction process of the Kaldo furnace, and through practice, the heating process simultaneously plays a drying role on materials, the flow ratio of oxygen to natural gas can be slightly larger, such as 2.0, and the flow ratio of oxygen to natural gas can be properly reduced after the materials are melted, such as 1.8, so that the reduction smelting is more facilitated. The coke addition amount is controlled to be about 3-4% of the addition material, the reduction effect is optimal, the generated ash content is reduced, the sodium carbonate addition amount is controlled to be 2-3% of slag, the alloy separation is good, and the slag fluidity is good.
Preferably, in the temperature rise process of the Kaldo furnace, the rotating speed of the Kaldo furnace is gradually increased to 8r/min under the conditions that the keeping current is less than 20mA and the torque is less than 10 Nm. The Kaldo furnace starts to increase the rotating speed after the materials are dried and mixed uniformly, and current and torque need to be paid attention to in the period, for example, the rotating speed can be increased at a speed of 2 revolutions per 20min until the rotating speed reaches about 8 revolutions per minute.
Preferably, in the step (2), after the reduction smelting is finished, sampling and detecting that the lead content of the slag in the Kaldo furnace is less than 2%, and then separating the first batch of slag. The smelting reduction end point is judged by the grade of lead in the slag, and the grade of other components can be adopted for judgment. The smaller the content of lead in the slag is, the better the lead content in the slag is, but when the content of lead in the slag is lower than 2%, the reduction smelting is continued, and the fluctuation of the content of other valuable metals in the slag is small, so that the point is taken as the end point of the reduction smelting, and the energy consumption is the most reasonable.
Preferably, in the step (3), after the Kaldo furnace inner body is cooled to 820-850 ℃, separating the second batch of slag. Slag is still continuously separated out in the cooling process of the melt in the furnace, and the copper grade in the separated slag is very high, because the solidification point of the copper simple substance is different from other metals in the furnace, particularly different from the solidification points of the lead and bismuth simple substances, a large amount of copper is continuously solidified and enters the slag after being cooled, the slag is second batch of slag, the copper grade can reach more than 50 percent, and the slag can be directly used as copper concentrate to return to a copper smelting system for treatment. The setting of the temperature is to take the service life of the furnace bricks of the Kaldo furnace into consideration, the service temperature of the furnace bricks cannot be lower than 820 ℃, so that the slag is removed and the melt is poured out at the temperature of more than 820 ℃, and the operation does not affect the next furnace smelting operation of the Kaldo furnace.
And (4) cooling the melt in the metal ladle to 450-500 ℃, then casting the melt, and separating the slag shell remained in the metal ladle after casting. Pouring the melt into a metal ladle inevitably causes the temperature of the melt to be slightly reduced, some slag is separated out, and if the melt is directly cast, the alloy is provided with scum, so that the appearance and the uniformity of the alloy are influenced. And (3) continuously cooling to ensure that the melt in the metal ladle is fully separated out of slag, wherein the slag forms a slag shell on the upper layer of the melt in the metal ladle due to low temperature, the slag shell is left in the metal ladle after casting and is directly separated and collected, and the copper grade of the slag shell is up to more than 50% after inspection and analysis, and the slag shell and second slag can be returned to a copper smelting system for treatment.
By adopting the scheme, the recovery of lead and bismuth in the copper anode slime smelting slag can be realized only by one set of Kaldo furnace equipment, the content of the obtained alloy lead and bismuth is up to more than 90%, most impurities in the smelting slag can be removed only by cooling and separating slag particles in the process, particularly, the copper grade of most separated slag is up to more than 50%, and the slag can be directly treated as copper concentrate. The scheme of the invention has the advantages of simple process, environment-friendly process and low equipment requirement, products in the separation process can be effectively recycled, and the trouble caused by adding auxiliary materials for many times and separating impurities for many times is also avoided.
Detailed Description
The technical solution of the present invention is further described below with reference to examples.
Crushing 12t of copper anode slime smelting slag into small blocks with the particle size of 1-2 cm, adding 0.36t of coke and 0.24t of sodium carbonate into a hearth of a Kaldo furnace in 3 batches, slowly rotating the furnace body, introducing natural gas and oxygen, wherein the flux of the natural gas is 2.5Nm3Min, the flux ratio of oxygen to natural gas is 2.0, burning and heating are carried out, materials in the furnace are dried simultaneously, after the drying is finished, the rotating speed of the furnace body is gradually increased, and the rotating speed is increased by 2 revolutions every 20min until the rotating speed is 8 r/min; the materials in the furnace are gradually in a molten state, the natural gas flux is increased to 3.0Nm after the temperature is greatly 1100 DEG C3And/min, the flux ratio of oxygen to natural gas is 1.8, and reduction smelting is started. Gradually separating out and increasing slag in the furnace, taking slag samples to detect the lead content in the slag every 20min when the reduction end point is reached according to experience, respectively sampling upper slag and lower slag due to too much slag, finishing the reduction smelting after the lead content in the upper slag and the lower slag is less than 2 percent, and discharging the slag (due to slag contentThe amount is large, in order to avoid the lower-layer slag from bringing out the melt, a 10-15 cm slag layer on the surface layer of the melt is reserved in the furnace firstly), and the first batch of slag is obtained.
And cooling the Kaldo furnace, continuously separating out slag particles in the furnace, and slagging off (wherein a slag layer on the surface of the melt is completely removed to the greatest extent) after the melt temperature is 850 ℃ to obtain a second batch of slag.
And after slagging off is finished, guiding the melt in the furnace into a metal ladle and continuously cooling, gradually forming a slag shell on the upper surface of the melt, casting to prepare a lead-bismuth alloy ingot after the temperature of the melt reaches 480 ℃, and separating the slag shell from the metal ladle after casting is finished.
The analytical data of the copper anode slime smelting slag, the slag of each stage and the melt are shown in table 1.
TABLE 1 analysis data of slag and melt at each stage
The data in the table show that the lead and bismuth content in the melt after the first batch of slag is separated can only reach more than seventy percent, and the melt still contains a large amount of impurities, but by adopting the scheme of the invention, the high content of more than ninety percent of the lead and bismuth alloy can be realized only by separating slag layers for multiple times in the process of gradually cooling the melt, and although the amount of slag separated in the cooling process is less, the copper grade of two batches of slag is very high, and the slag can be directly used as copper concentrate for processing, wherein the copper concentrate is more than fifty percent. And no smoke is generated in the melt casting process, so that the environmental pollution is reduced to the minimum.
Claims (9)
1. A method for recovering lead and bismuth from copper anode slime smelting slag comprises the following steps:
(1) adding copper anode slime smelting slag, a reducing agent and a slagging agent into a hearth of a Kaldo furnace, and heating to 1100-1150 ℃ for reduction smelting;
(2) separating first slag after the reduction smelting is finished;
(3) cooling the Kaldo furnace, and separating a second batch of slag before discharging the melt;
(4) pouring the melt in the furnace into a metal ladle, and continuously cooling until the upper layer of the melt in the metal ladle forms a slag shell;
(5) and casting the melt in the metal ladle into ingots, and stripping off slag shells to obtain metal ingots, namely the lead-bismuth alloy.
2. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (1), the copper anode slime smelting slag is firstly crushed into blocks with the grain size of 1-2 cm, and then the blocks are added into a Kaldo furnace.
3. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (1), the adding amount of the reducing agent coke is 3-4% calculated by the total mass of the added copper anode slime smelting slag; the addition amount of the slag former sodium carbonate is 2-3%.
4. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (1), after the materials are added into a hearth of the Kaldo furnace, natural gas and oxygen are introduced for combustion heating, wherein the flow rate of the natural gas is 2.0-3.0 Nm3And/min, wherein the flow ratio of oxygen to natural gas is 1.8-2.0, and the Kaldo furnace starts to rotate to heat and dry the material.
5. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (1), in the temperature rising process of the Kaldo furnace, the rotating speed of the Kaldo furnace is gradually increased to 8r/min under the conditions that the current is kept less than 20mA and the torque is kept less than 10 Nm.
6. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (2), after the reduction smelting is finished, sampling and detecting that the lead content of the slag in the Kaldo furnace is less than 2%, and then separating the first batch of slag.
7. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: in the step (3), after the Kaldo furnace inner body is cooled to 820-850 ℃, separating a second batch of slag.
8. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: and (4) cooling the melt in the metal ladle to 450-500 ℃, then casting the melt, and separating the slag shell remained in the metal ladle after casting.
9. The method for recovering lead and bismuth from copper anode slime smelting slag according to claim 1, characterized by comprising the following steps: and (4) collecting the second batch of slag obtained in the step (3) and the slag shell obtained in the step (5) and then returning the second batch of slag and the slag shell to a copper smelting system as copper concentrate for treatment.
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| CN113088713A (en) * | 2021-04-07 | 2021-07-09 | 紫金铜业有限公司 | Copper anode mud smelting slag treatment method for prolonging service life of Kaldo furnace |
| CN114672661A (en) * | 2022-03-04 | 2022-06-28 | 金川集团股份有限公司 | Method for judging precious metal smelting converting end point of Kaldo furnace |
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| CN113088713A (en) * | 2021-04-07 | 2021-07-09 | 紫金铜业有限公司 | Copper anode mud smelting slag treatment method for prolonging service life of Kaldo furnace |
| CN114672661A (en) * | 2022-03-04 | 2022-06-28 | 金川集团股份有限公司 | Method for judging precious metal smelting converting end point of Kaldo furnace |
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