CN115449637A - Method for efficiently separating and extracting selenium, copper and tellurium from copper anode slime in gradient manner - Google Patents
Method for efficiently separating and extracting selenium, copper and tellurium from copper anode slime in gradient manner Download PDFInfo
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- CN115449637A CN115449637A CN202211262366.7A CN202211262366A CN115449637A CN 115449637 A CN115449637 A CN 115449637A CN 202211262366 A CN202211262366 A CN 202211262366A CN 115449637 A CN115449637 A CN 115449637A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000010949 copper Substances 0.000 title claims abstract description 121
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 120
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 48
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 41
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 35
- 239000011669 selenium Substances 0.000 title claims abstract description 35
- 238000002386 leaching Methods 0.000 claims abstract description 58
- 238000000926 separation method Methods 0.000 claims abstract description 32
- 239000002893 slag Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052737 gold Inorganic materials 0.000 claims abstract description 6
- 239000010931 gold Substances 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000004576 sand Substances 0.000 claims abstract description 3
- 229910052709 silver Inorganic materials 0.000 claims abstract description 3
- 239000004332 silver Substances 0.000 claims abstract description 3
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 17
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- 239000010431 corundum Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 5
- 239000008151 electrolyte solution Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001180 sulfating effect Effects 0.000 description 1
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
-
- 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
- C22B1/06—Sulfating roasting
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
-
- 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
- C22B15/0002—Preliminary treatment
- C22B15/001—Preliminary treatment with modification of the copper constituent
- C22B15/0013—Preliminary treatment with modification of the copper constituent by roasting
- C22B15/0017—Sulfating or sulfiding roasting
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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
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0082—Leaching or slurrying with water
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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
- C22B7/007—Wet processes by acid leaching
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- 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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Abstract
The invention provides a method for efficiently separating and extracting selenium, copper and tellurium from copper anode slime in a gradient way, which comprises the following steps: step one, O 2 ‑SO 2 Roasting to separate selenium to obtain roasted sand and selenium concentrate; step two, carrying out water leaching or acid leaching on the calcine to separate copper to obtain copper separation slag and a copper sulfate-rich solution, and placing the copper separation slag in an oven for drying; and thirdly, carrying out alkaline leaching on the copper-separating residue to separate tellurium to obtain tellurium-separating residue and a sodium tellurite-containing solution, and drying the tellurium-separating residue in a drying oven for subsequent recovery of gold and silver. The embodiment of the invention provides an efficient step separation and extraction method for copper anode slimeThe method for preparing selenium, copper and tellurium has the following beneficial effects: the invention realizes the high-efficiency gradient extraction of selenium, copper and tellurium in the copper anode slime by gradually separating the selenium, copper and tellurium in the copper anode slime.
Description
Technical Field
One or more embodiments of the present disclosure relate to the technical field of metal smelting, and in particular, to a method for efficiently and stepwise separating and extracting selenium, copper, and tellurium from copper anode slime.
Background
Tellurium has good physical properties, is an indispensable key material for manufacturing elements such as photoelectricity, semiconductors, refrigeration and the like, and is widely applied to the high-tech fields such as aerospace, military, electrical and the like. Tellurium often accompanies in minerals such as copper, lead, nickel and the like, and according to statistics, tellurium mainly comes from copper anode slime and lead anode slime, and about 90% of tellurium is produced in copper anode slime globally, and the significance of efficiently extracting tellurium from copper anode slime is great. Copper anode slime is composed of various substances of anode copper which are insoluble in electrolyte during electrolytic refining, and usually contains elements such As Au, ag, cu, pb, se, te, sn, as and the like. At present, a series of researches on extracting tellurium from copper anode slime have been carried out at home and abroad, and the researches mainly comprise a sulfating roasting-alkaline leaching method, an oxidizing roasting-sulfuric acid leaching method, a soda roasting-sulfuric acid leaching method, a chlorination tellurium extraction method, an acid oxidation leaching method, a pressurized alkaline leaching method and the like. Currently, the sulfatizing roasting process is a common process for treating copper anode slime, and about half of the world's copper anode slime is treated by this process. The leaching rate of tellurium in the process of separating tellurium from copper anode slime of the current copper smelting enterprises is reported to be low, and the comprehensive recovery rate is less than 60%. Researchers have developed a lot of work aiming at the problem that the leaching rate of alkaline leaching tellurium is low, and mainly provide methods such as mixed acid leaching, pressurized high-alkaline leaching, acid oxidation leaching, external field strengthening and the like. Chinese patent CN111606308A discloses a method for efficiently separating and recovering tellurium from copper anode slime separated from copper slag, which realizes an efficient tellurium leaching process by using a hydrochloric acid oxidation system for the copper anode slime separated from copper slag, and the tellurium leaching rate is more than 90%. Chinese patent CN110550611A discloses a method for efficiently leaching tellurium from copper anode slime separated copper slag under the action of an external field, which uses sodium hydroxide as a leaching agent and sodium chlorate as an oxidant to leach the separated copper slag under the action of the external field reinforcement of ultrasonic-microwave synergy, so that the efficient leaching of tellurium under normal pressure is realized, and the tellurium leaching rate is improved by 26-35%. Although the methods can improve the tellurium leaching rate to a certain extent, the methods have the problems of long process flow, high equipment requirement and high generation cost, and are difficult to industrially popularize and apply.
In summary, the present application provides a method for efficiently separating and extracting selenium, copper, and tellurium from copper anode slime in a gradient manner to solve the above problems.
Disclosure of Invention
The invention aims to solve the problems in the background art, and one or more embodiments of the specification aim to provide a method for efficiently separating and extracting selenium, copper and tellurium from copper anode slime in a gradient manner, and the method is low in production cost and good in economic benefit.
In view of the above, one or more embodiments of the present disclosure provide a method for efficiently and stepwise extracting selenium, copper, and tellurium from copper anode slime, including the following steps:
step one, O 2 -SO 2 Roasting and selenium separation: drying, crushing and grinding the copper anode slime, sieving the copper anode slime with a sieve of 100 to 200 meshes for later use, adding a proper amount of the copper anode slime into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Heating the atmosphere furnace, roasting and preserving heat to obtain roasted sand subjected to selenium steaming and selenium enrichment;
step two, calcine water leaching or acid leaching copper separation: carrying out water leaching or acid leaching on the calcine obtained in the step one to separate copper to obtain a copper sulfate-rich solution and copper separation slag: crushing and grinding the calcine, sieving the calcine by a sieve with 100-200 meshes for later use, adding a proper amount of calcine into a conical flask, adding a certain amount of deionized water or sulfuric acid, leaching for a period of time in a water bath at a certain temperature, filtering, separating solid from liquid to obtain copper-separated slag and a copper sulfate-rich solution, and drying the copper-separated slag in an oven;
step three, carrying out alkaline leaching on the copper separation slag to separate tellurium: grinding the copper separation slag obtained in the second step to a certain particle size for later use, adding a proper amount of copper separation slag into a conical flask, then adding NaOH solution, leaching for a period of time in a water bath at a certain temperature, filtering, carrying out solid-liquid separation to obtain tellurium separation slag and a solution containing sodium tellurite, and drying the tellurium separation slag in an oven for subsequent recovery of gold and silver.
Preferably, O is introduced in the first step 2 :SO 2 The flow ratio of (1) is 2.
Preferably, the copper anode slime in the first step is derived from the composition of various substances of anode copper insoluble in the electrolyte during the electrolytic refining process, and contains one or more element combinations of Au, ag, cu, pb, se, te, S and As, and can also be copper anode slime or a material containing copper telluride after arsenic, antimony and bismuth are removed, wherein the mass percentages of the elements in the copper anode slime are Cu (5-40%), te (0.5-10%), se (0.5-10%), pb (1-10%) and Ag (2-15%).
Preferably, O in the first step 2 、SO 2 The gas is a pure gas or a mixed gas filled with an inert gas.
Preferably, the leaching conditions in the second step are that the leaching temperature is 25-95 ℃, the stirring speed is 300-500 r/min, the liquid-solid ratio is 1-8, the leaching reaction time is 0.5-5 h, and the acid leaching and copper separating conditions in the second step are that the sulfuric acid concentration is 0-400 g/L.
Preferably, the alkaline leaching in the third step is carried out under the conditions that the concentration of a NaOH solution is 50-400 g/L, the leaching temperature is 25-95 ℃, the liquid-solid ratio is 1-8.
According to the above, the method for efficiently and stepwisely separating and extracting selenium, copper and tellurium from copper anode slime provided in the embodiment of the invention has the following beneficial effects: the selenium, copper and tellurium in the copper anode slime are separated step by step, so that the selenium, copper and tellurium in the copper anode slime are extracted in a high-efficiency step mode; simultaneous calcination of O used 2 SO can be obtained by compressing air 2 Is a byproduct obtained after the copper smelting flue gas is purified, so the method has lower production cost and achieves the effects of high-efficiency and gradient recycling and economy of the comprehensive treatment of the copper anode slime.
Drawings
In order to more clearly illustrate one or more embodiments or prior art solutions of the present specification, the drawings that are needed in the description of the embodiments or prior art will be briefly described below, and it is obvious that the drawings in the following description are only one or more embodiments of the present specification, and that other drawings may be obtained by those skilled in the art without inventive effort from these drawings.
FIG. 1 is a process flow diagram of the present invention
FIG. 2 is a schematic view of the present invention 2 -SO 2 A relation graph with selenium volatilization rate and tellurium leaching rate;
FIG. 3 shows the copper anode slime O of the present invention 2 -SO 2 XRD pattern of the product after roasting.
Detailed Description
To make the objects, technical solutions and advantages of the present disclosure more apparent, the present disclosure is further described in detail below with reference to specific embodiments.
The copper anode mud used in the embodiment of the invention comprises the following chemical components: cu (20.22%), pb (8.36%), se (6.64%), S (6.69%), ag (4.89%), te (2.87%), sn (4.26%), ba (4.01%), as (4.34%).
Example 1
The method comprises the following steps: grinding 20.0g of dried copper anode slime raw material to 200 meshes of sieve, adding the copper anode slime into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, control of O 2 :SO 2 The flow ratio of the copper anode slime to the selenium anode slime is 5, then the temperature of the atmosphere furnace is increased to 600 ℃ at the heating rate of 10 DEG/min, and the copper anode slime calcine and the selenium enrichment are obtained after roasting and heat preservation are carried out for 2 hours.
Step two: grinding 15.0g of the calcine obtained in the first step to 200-mesh sieve, adding the ground calcine into a conical flask, adding a certain amount of deionized water to control the liquid-solid ratio to be 1, leaching for 3 hours in a water bath kettle with the stirring speed of 400r/min and the temperature of 85 ℃, filtering, and separating solid from liquid to obtain copper separation slag and a copper sulfate-rich solution.
Step three: and (3) grinding 5.0g of the dried copper separation slag obtained in the second step to a state of being sieved by a 200-mesh sieve, adding the ground copper separation slag into a NaOH solution with the concentration of 100g/L, controlling the liquid-solid ratio to be 4. The volatilization rate of selenium is 98.22%, the leaching rate of copper is 92.16% and the leaching rate of tellurium is 73.11%.
Example 2
The method comprises the following steps: grinding 20.0g of dried copper anode mud raw material to 200 meshes of sieve, adding the copper anode mud into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, control of O 2 :SO 2 The flow ratio of (1) is 6.
Step two: taking 15.0g of the calcine obtained in the first step, grinding the calcine to pass through a 200-mesh sieve, adding the ground calcine into a conical flask, adding a certain amount of deionized water to control the liquid-solid ratio to be 1.
Step three: and (3) grinding 5.0g of the dried copper separation slag obtained in the step two to 200-mesh sieve, adding the ground copper separation slag into a NaOH solution with the concentration of 100g/L, controlling the liquid-solid ratio to be 4. The volatilization rate of selenium is 98.16%, the leaching rate of copper is 91.35%, and the leaching rate of tellurium is 75.18%.
Example 3
The method comprises the following steps: grinding 20.0g of dried copper anode mud raw material to 200 meshes of sieve, adding the copper anode mud into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, control of O 2 :SO 2 The flow ratio of the copper anode slime to the selenium anode slime is 7.
Step two: taking 15.0g of the calcine obtained in the first step, grinding the calcine to pass through a 200-mesh sieve, adding the ground calcine into a conical flask, adding a certain amount of deionized water to control the liquid-solid ratio to be 1.
Step three: and (3) grinding 5.0g of the dried copper separation slag obtained in the step two to 200-mesh sieve, adding the ground copper separation slag into a NaOH solution with the concentration of 100g/L, controlling the liquid-solid ratio to be 4. The volatilization rate of selenium is 98.46%, the leaching rate of copper is 90.59%, and the leaching rate of tellurium is 83.27%.
Example 4
The method comprises the following steps: grinding 20.0g of dried copper anode mud raw material to 200 meshes of sieve, adding the copper anode mud into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, control of O 2 :SO 2 The flow ratio of (1) is 8.
Step two: grinding 15.0g of the calcine obtained in the step one until the calcine is sieved by a 200-mesh sieve, adding the ground calcine into a conical flask, adding a certain amount of deionized water to control the liquid-solid ratio to be 1.
Step three: and (3) grinding 5.0g of the dried copper separation slag obtained in the step one to pass through a 200-mesh sieve, adding the ground copper separation slag into a NaOH solution with the concentration of 100g/L, controlling the liquid-solid ratio to be 4. The volatilization rate of selenium is 93.54%, the leaching rate of copper is 88.92% and the leaching rate of tellurium is 75.07%.
Example 5:
the method comprises the following steps: grinding 20.0g of dried copper anode slime raw material to 200 meshes of sieve, adding the copper anode slime into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, control of O 2 :SO 2 The flow ratio of the copper anode slime to the selenium anode slime is 7.
Step two: grinding 15.0g of the calcine obtained in the step one until the calcine is sieved by a 200-mesh sieve, adding the ground calcine into a conical flask, adding a certain amount of deionized water to control the liquid-solid ratio to be 1.
Step three: and (3) grinding 5.0g of the dried copper separation slag obtained in the second step to a 200-mesh sieve, adding the ground copper separation slag into a NaOH solution with the concentration of 100g/L, controlling the liquid-solid ratio to be 4. The volatilization rate of selenium is 98.23%, the leaching rate of copper is 86.74% and the leaching rate of tellurium is 82.09%.
It is intended that the one or more embodiments of the present specification embrace all such alternatives, modifications and variations as fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit or scope of the disclosure are intended to be included within the scope of the disclosure.
Claims (6)
1. A method for efficiently separating and extracting selenium, copper and tellurium from copper anode slime in a gradient way is characterized by comprising the following steps:
step one, O 2 -SO 2 Roasting and selenium separation: drying, crushing and grinding the copper anode slime, sieving the copper anode slime with a sieve of 100 to 200 meshes for later use, adding a proper amount of the copper anode slime into a corundum crucible, placing the corundum crucible in an atmosphere furnace, and simultaneously introducing O into the atmosphere furnace 2 、SO 2 Gas, heating the atmosphere furnace, roasting and preserving heat to obtain roasted sand subjected to selenium steaming and seleniumEnrichment;
step two, calcine water leaching or acid leaching copper separation: carrying out water leaching or acid leaching on the calcine obtained in the step one to separate copper to obtain a copper sulfate-rich solution and copper separation slag: crushing and grinding the calcine, sieving the calcine by a sieve of 100-200 meshes for later use, adding a proper amount of calcine into a conical flask, adding a certain amount of deionized water or sulfuric acid, leaching for a period of time in a water bath at a certain temperature, filtering, separating solid from liquid to obtain copper separating slag and a copper sulfate-rich solution, and drying the copper separating slag in a drying oven;
step three, carrying out alkaline leaching on the copper separation residue to separate tellurium: grinding the copper separation slag obtained in the second step to a certain particle size for later use, adding a proper amount of copper separation slag into a conical flask, then adding NaOH solution, leaching for a period of time in a water bath at a certain temperature, filtering, carrying out solid-liquid separation to obtain tellurium separation slag and a solution containing sodium tellurite, and drying the tellurium separation slag in an oven for subsequent recovery of gold and silver.
2. The method for efficiently and stepwisely separating and extracting selenium, copper and tellurium from copper anode slime according to claim 1, wherein O is introduced into the first step 2 :SO 2 The flow ratio of (A) is 2.
3. The method As claimed in claim 1, wherein the copper anode slime in the first step is derived from the composition of various substances insoluble in the electrolyte solution during the electrolytic refining process of the copper anode slime, and contains one or more elements selected from Au, ag, cu, pb, se, te, S and As, or copper anode slime or material containing copper telluride from which arsenic, antimony and bismuth are removed, and the copper anode slime contains, by mass, cu (5-40%), te (0.5-10%), se (0.5-10%), pb (1-10%) and Ag (2-15%).
4. The method for efficiently and stepwise separating and extracting selenium, copper and tellurium from copper anode slime as claimed in claim 1, wherein O in the first step 2 、SO 2 The gas is a pure gas or a mixed gas filled with an inert gas.
5. The method for efficiently and stepwisely separating and extracting selenium, copper and tellurium from copper anode slime according to claim 1, wherein the leaching conditions in the second step are that the leaching temperature is 25-95 ℃, the stirring speed is 300-500 r/min, the liquid-solid ratio is 1-8.
6. The method for efficiently and stepwise separating and extracting selenium, copper and tellurium from copper anode slime according to claim 1, wherein the alkaline leaching in the third step is carried out under the conditions that the concentration of NaOH solution is 50-400 g/L, the leaching temperature is 25-95 ℃, the liquid-solid ratio is 1-8, and the leaching time is 0.5-5 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102745657A (en) * | 2012-07-30 | 2012-10-24 | 阳谷祥光铜业有限公司 | Method for extracting tellurium from tellurium copper slags |
| CN107574300A (en) * | 2017-08-29 | 2018-01-12 | 山东恒邦冶炼股份有限公司 | A kind of mixed processing technique of copper, lead anode slurry |
| CN112695200A (en) * | 2020-12-22 | 2021-04-23 | 万载志成实业有限公司 | Method for recovering selenium, gold and silver from copper anode slime |
| US11408051B2 (en) * | 2017-03-30 | 2022-08-09 | Dundee Sustainable Technologies Inc. | Method and system for metal recovery from arsenical bearing sulfides ores |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102745657A (en) * | 2012-07-30 | 2012-10-24 | 阳谷祥光铜业有限公司 | Method for extracting tellurium from tellurium copper slags |
| US11408051B2 (en) * | 2017-03-30 | 2022-08-09 | Dundee Sustainable Technologies Inc. | Method and system for metal recovery from arsenical bearing sulfides ores |
| CN107574300A (en) * | 2017-08-29 | 2018-01-12 | 山东恒邦冶炼股份有限公司 | A kind of mixed processing technique of copper, lead anode slurry |
| CN112695200A (en) * | 2020-12-22 | 2021-04-23 | 万载志成实业有限公司 | Method for recovering selenium, gold and silver from copper anode slime |
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