CN114990338A - Method for efficiently extracting tin from silver separating residues of copper anode slime - Google Patents
Method for efficiently extracting tin from silver separating residues of copper anode slime Download PDFInfo
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- CN114990338A CN114990338A CN202210493664.0A CN202210493664A CN114990338A CN 114990338 A CN114990338 A CN 114990338A CN 202210493664 A CN202210493664 A CN 202210493664A CN 114990338 A CN114990338 A CN 114990338A
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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
- C22B7/006—Wet processes
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
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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
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- C22B30/02—Obtaining antimony
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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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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 technical field of non-ferrous metal smelting, and particularly relates to a method for efficiently extracting tin from silver separating slag of copper anode slime, which comprises the following steps: uniformly mixing the silver-containing slag, the carbon-containing material and the auxiliary agent of the copper anode slime, pressing the mixed material into blocks, roasting by adopting microwave at the temperature of 350-950 ℃ for 1.5-4.5 h; crushing and grinding the obtained roasting slag, adding the crushed roasting slag into a sulfuric acid-containing solution, stirring and slurrying, adding an alkali-containing solution, heating to leach tin, recovering other valuable elements from the obtained tin leaching slag, adding a calcium-containing reagent into the tin leaching solution to precipitate tin, recovering antimony from the obtained tin-precipitated solution, and washing the tin-precipitated slag to obtain tin concentrate. The beneficial effects of the invention are as follows: the method has low treatment cost and stable tin recovery effect, is more suitable for actual industrial production, and the recovery rate of tin from the silver separating slag of the copper anode slime to tin concentrate in the method is not lower than 90.0 percent.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a method for efficiently extracting tin from silver separating slag of copper anode slime.
Background
The copper anode slime is insoluble substances which fall off at the anode in the copper smelting electrolytic refining process, contains precious metals such as gold, silver, platinum, palladium and the like and rare dispersed metals such as tellurium, selenium and the like, and is one of important sources of a plurality of metal resources. The copper anode slime treatment process usually comprises the steps of pretreatment, copper and arsenic removal, gold leaching, silver separation, refining and the like, wherein residues left after silver separation are called silver separation residues, contain trace amounts of gold and silver, and also contain valuable metals such as tin, lead, antimony and the like, and still have considerable resource utilization value, and the tin contained in the residues has the highest extraction value due to large value and high grade.
In order to extract tin in the silver-separating slag of the copper anode slime, in the prior art, the silver-separating slag and a vulcanizing agent and other various auxiliary agents are mixed, the mixture is placed into a 1200-1500 ℃ reaction furnace after ball milling for 0.5-2 hours, and smelting is carried out for 1-2 hours under the condition of blowing air, so as to obtain lead-tin-rich smoke dust, the idea of the scheme is to extract tin through volatilization at high temperature, antimony and lead are volatilized while the tin is volatilized, the obtained volatile matter is a mixture of lead, tin and antimony, and the like, not only is the grade of the tin low, but also the subsequent treatment is difficult due to the difficulty in separating tin and antimony, and the problem of gold and silver dispersion also exists;
the silver separating residue is deleaded and silver-removed in an acid chloride system, barium is removed by heating concentrated sulfuric acid, sodium stannate solution is obtained by alkali fusion, water immersion and the like, and sodium stannate product is obtained by evaporation crystallization after the sodium stannate solution is purified, so that the scheme has the advantages of long flow, more waste water, difficult operation of chloride crystallization and hot concentrated sulfuric acid, hardening of alkali fusion material and the like, and does not have industrial application prospect; or leaching the silver separating residue by adopting a mixed solution of hydrochloric acid and chlorine salt, separating gold, silver and lead, and separating barium by adopting a carbonate conversion-hydrochloric acid leaching mode to obtain a tin concentrate. The method has feasibility, but practices show that when raw material components or roasting conditions fluctuate, the effect of the method on tin extraction is unstable, the consumption of an oxidant is large during oxidizing acid leaching, and the treatment cost is high.
The invention content is as follows:
in view of the above problems, the present invention provides a method for separating and recovering tin from silver separating residue of copper anode slime, so as to solve any one of the above and other potential problems in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for efficiently extracting tin from silver separating slag of copper anode slime specifically comprises the following steps of:
s1) uniformly mixing the silver-separating residue of the copper anode slime, the carbon-containing material and the auxiliary agent, and pressing the mixed material into blocks.
S2) roasting the lump material for 1.5-4.5 h under microwave, wherein the roasting temperature is 350-950 ℃, and the roasting slag is obtained.
S3) crushing and grinding the roasted slag, adding the crushed roasted slag into a sulfuric acid-containing solution, stirring and slurrying, adding an alkali-containing solution, heating to leach tin to obtain a tin-leaching solution and tin-leaching slag, and recycling other valuable elements from the tin-leaching slag;
s4) adding a calcium-containing reagent into the tin immersion liquid to obtain a liquid after tin precipitation and tin precipitation slag, sending the liquid after tin precipitation to antimony recovery, and washing the tin precipitation slag to obtain tin concentrate.
Further, the carbon-containing material in the S1) is one or more of coal powder, charcoal powder, coke powder and graphite powder, the auxiliary agent is one or more of sodium sulfide, potassium sulfide, calcium sulfide and magnesium sulfide, and the silver-separating residue, the carbon-containing material and the auxiliary agent are mixed according to the mass ratio of 1: 0.3-1.8: 0.05-0.3.
Further, the sulfuric acid-containing solution in the step S3) can be a waste acid solution, the addition amount is controlled by the pH of a slurrying end point, the pH of the slurrying end point is controlled to be 1-10, the alkali-containing solution is a solution or waste liquid of sodium hydroxide and potassium hydroxide, the concentration of hydroxyl is 0.5-3.5 mol/L, the sulfuric acid-containing solution is added according to the volume mass ratio of the alkali-containing solution to the roasting slag of 0.5-10, the tin leaching temperature is 40-90 ℃, and the tin leaching time is 0.5-4 h.
Further, the calcium reagent in S4) is one or a combination of more of calcium oxide, calcium hydroxide, calcium chloride and calcium sulfate, the calcium reagent is added according to the molar ratio of calcium to tin of 1.0-3.0, the tin precipitation temperature is 20-90 ℃, and the tin precipitation time is 0.5-4 h.
Compared with the prior art, the process has the beneficial effects and outstanding advantages that:
1) by adding the auxiliary agent as the roasting auxiliary agent and pressing the materials into blocks, the microwave roasting effect becomes stable, and when the silver slag components or the microwave roasting temperature fluctuate, the concentration of tin in the leaching solution is basically unchanged.
2) The method comprises the steps of slurrying with sulfuric acid solution, and leaching with alkali-containing solution, so that the leaching of tin is realized in one step, the flow is shortened, and the treatment cost is reduced.
3) The sulfuric acid-containing solution and the alkali-containing solution can be waste liquid in production, so that the treatment cost can be reduced, and the waste liquid discharge can be reduced.
Drawings
FIG. 1 is a flow chart of the method for efficiently extracting tin from silver separating slag of copper anode slime.
Detailed Description
The present invention will be described in further detail below with reference to examples, but the scope of the present invention is not limited to these examples.
As shown in figure 1, the method for efficiently extracting tin from the silver separating slag of the copper anode slime specifically comprises the following steps of:
s1) uniformly mixing the silver-separating slag of the copper anode slime, the carbon-containing material and the auxiliary agent according to a set proportion, and pressing the mixed material into blocks to obtain blocks;
s2) placing the lump material obtained in S1) under microwave for roasting to obtain roasting slag;
s3) crushing and grinding the roasting slag obtained in the step S2), adding the crushed roasting slag into a sulfuric acid-containing solution, stirring and slurrying, adding an alkali-containing solution, and then heating to leach tin to obtain a tin leaching solution and tin leaching slag;
s4) adding a calcium-containing reagent into the tin immersion liquid obtained in S3) to carry out tin precipitation to obtain a tin precipitation liquid and tin precipitation slag, sending the tin precipitation liquid to antimony recovery, and washing the tin precipitation slag to obtain tin concentrate.
The mass ratio of the silver-containing slag, the carbon-containing material and the auxiliary agent in the copper anode slime in S1) is 1: 0.3-1.8: 0.05-0.3.
The carbon-containing material is one or more of coal powder, charcoal powder, coke powder and graphite powder;
the auxiliary agent is one or more of sodium sulfide, potassium sulfide, calcium sulfide and magnesium sulfide.
And in the S2), the roasting temperature is 350-950 ℃, and the roasting time is 1.5-4.5 h.
The specific process in S3) comprises the following steps:
s3.1) crushing the roasting slag, and grinding to obtain roasting slag powder;
s3.2) adding the roasting slag powder into a sulfuric acid solution for slurrying, wherein the pH of the slurrying end point is controlled to be 1-10;
s3.3) adding the alkali-containing solution and the roasting slag powder according to the volume-to-mass ratio of 0.5-10, wherein the tin leaching temperature is 40-90 ℃, and the tin leaching time is 0.5-4 h, so as to obtain a tin leaching solution and tin leaching slag.
The sulfuric acid-containing solution is a waste acid solution;
the alkali-containing solution is a solution of sodium hydroxide and potassium hydroxide or a waste alkali solution, and the concentration of hydroxyl in the alkali-containing solution is 0.5-3.5 mol/L.
The technological parameters of tin deposition in the step S4) are as follows:
the calcium reagent is added according to the molar ratio of calcium to tin of 1.0-3.0, the tin precipitation temperature is 20-90 ℃, and the tin precipitation time is 0.5-4 h.
The calcium reagent is one or the combination of more of calcium oxide, calcium hydroxide, calcium chloride and calcium sulfate,
in the method, the yield of tin in the tin concentrate obtained after the silver separating residue of the copper anode slime is treated is not lower than 90.0%.
Example 1
And (3) mixing 100g of silver-containing slag, 105g of charcoal powder and 20g of sodium sulfide uniformly, pressing into blocks, and then roasting for 1.5 hours at 530 ℃ by using microwave to obtain the roasting slag. Crushing and grinding the roasting slag, adding the vulcanized liquid, mixing, pulping, monitoring the pH value of the slurry, stopping adding the vulcanized liquid when the pH value is 3, adding 300mL of antimony precipitation waste liquid, uniformly stirring, heating to 75 ℃, stirring for 2.5 hours, filtering to obtain tin immersion slag and tin immersion liquid, recovering other valuable elements from the tin immersion slag, adding calcium oxide into the tin immersion liquid according to the molar ratio of calcium to tin of 1.4, heating to 90 ℃, stirring for 1 hour, filtering, recovering antimony from filtrate, washing filter residues to obtain tin concentrate, and obtaining the yield of tin from silver separation slag to tin concentrate, wherein the yield of tin is 90.6%.
Example 2
And (3) uniformly mixing 500g of silver-divided slag, 260g of charcoal powder and 110g of calcium sulfide, pressing into blocks, and then roasting for 2.5 hours at 600 ℃ by using microwave to obtain the roasting slag. Crushing and grinding the roasting slag, adding a waste acid stock solution, mixing, pulping, monitoring the pH of slurry, stopping adding the waste acid stock solution when the pH is 5, adding 2.0L of alkali liquor with 1.2mol/L of sodium hydroxide, uniformly stirring, heating to 80 ℃, stirring for 3.5 hours, filtering to obtain tin immersion slag and tin immersion liquid, recycling other valuable elements from the tin immersion slag, adding calcium chloride into the tin immersion liquid according to the molar ratio of calcium to tin of 1.4, heating to 75 ℃, stirring for 1.5 hours, filtering, recycling antimony from filtrate, washing filter residues to obtain tin concentrate, and obtaining the yield of tin from silver separation slag to tin concentrate of 91.0%.
Example 3
And (3) uniformly mixing 300g of silver-divided slag, 130g of charcoal powder and 63g of potassium sulfide, pressing into blocks, and then roasting for 3.0 hours at 700 ℃ by using microwave to obtain the roasting slag. Crushing and grinding the roasting slag, adding copper electrolysis waste liquid, mixing, pulping, monitoring the pH value of slurry, stopping adding the copper electrolysis waste liquid when the pH value is 7, adding 1.2L of alkali liquid with the potassium hydroxide concentration of 1.5mol/L, uniformly stirring, heating to 80 ℃, stirring for 3.0 hours, filtering to obtain tin immersion slag and tin immersion liquid, recovering other valuable elements from the tin immersion slag, adding calcium hydroxide into the tin immersion liquid according to the calcium-tin molar ratio of 2.0, heating to 65 ℃, stirring for 4 hours, filtering, recovering antimony from filtrate, washing filter residues to obtain tin concentrate, and obtaining the yield of tin from silver separation slag to tin concentrate of 91.9%.
Aiming at the problems, the invention provides the method for efficiently extracting tin from the silver separating slag of the copper anode slime.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (9)
1. A method for efficiently extracting tin from silver separating slag of copper anode slime is characterized by comprising the following steps of:
s1) uniformly mixing the silver-separating slag of the copper anode slime, the carbon-containing material and the auxiliary agent according to a set proportion, and pressing the mixed material into blocks to obtain blocks;
s2) placing the lump material obtained in S1) under microwave for roasting to obtain roasting slag;
s3) crushing and grinding the roasting slag obtained in the step S2), adding the crushed roasting slag into a sulfuric acid-containing solution, stirring and slurrying, adding an alkali-containing solution, and then heating to leach tin to obtain a tin leaching solution and tin leaching slag;
s4) adding a calcium-containing reagent into the tin immersion liquid obtained in S3) to carry out tin precipitation to obtain a tin precipitation liquid and tin precipitation slag, sending the tin precipitation liquid to antimony recovery, and washing the tin precipitation slag to obtain tin concentrate.
2. The method as claimed in claim 1, wherein the mass ratio of the silver-containing slag, the carbon-containing material and the auxiliary agent in the copper anode slime in S1) is 1: 0.3-1.8: 0.05-0.3.
3. The method of claim 2, wherein the carbon-containing material is one or more of pulverized coal, charcoal powder, coke powder and graphite powder;
the auxiliary agent is one or more of sodium sulfide, potassium sulfide, calcium sulfide and magnesium sulfide.
4. The method as claimed in claim 2, wherein the roasting temperature in S2) is 350-950 ℃, and the roasting time is 1.5-4.5 h.
5. The method as claimed in claim 1, wherein the specific process in S3) is:
s3.1) crushing the roasting slag, and grinding to obtain roasting slag powder;
s3.2) adding the roasting slag powder into a sulfuric acid solution for slurrying, wherein the pH of the slurrying end point is controlled to be 1-10;
s3.3) adding the alkali-containing solution and the roasting slag powder according to the volume-to-mass ratio of 0.5-10, wherein the tin leaching temperature is 40-90 ℃, and the tin leaching time is 0.5-4 h, so as to obtain a tin leaching solution and tin leaching slag.
6. The method of claim 5, wherein the sulfuric acid containing solution is a spent acid solution;
the alkali-containing solution is a solution of sodium hydroxide and potassium hydroxide or a waste alkali solution, and the concentration of hydroxyl in the alkali-containing solution is 0.5-3.5 mol/L.
7. The method according to claim 1, wherein the process parameters of tin deposition in S4) are as follows:
the calcium reagent is added according to the molar ratio of calcium to tin of 1.0-3.0, the tin precipitation temperature is 20-90 ℃, and the tin precipitation time is 0.5-4 h.
8. The method according to claim 7, wherein the calcium reagent is one or more of calcium oxide, calcium hydroxide, calcium chloride and calcium sulfate.
9. The method according to claim 1, wherein the yield of tin in the tin concentrate obtained after the treatment of the copper anode slime silver separating slag in the method is not lower than 90.0%.
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