CN113186402A - Method for recovering metallic copper in selenium steaming slag - Google Patents
Method for recovering metallic copper in selenium steaming slag Download PDFInfo
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- CN113186402A CN113186402A CN202110472027.0A CN202110472027A CN113186402A CN 113186402 A CN113186402 A CN 113186402A CN 202110472027 A CN202110472027 A CN 202110472027A CN 113186402 A CN113186402 A CN 113186402A
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- 239000010949 copper Substances 0.000 title claims abstract description 113
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 112
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000011669 selenium Substances 0.000 title claims abstract description 81
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 81
- 239000002893 slag Substances 0.000 title claims abstract description 80
- 238000010025 steaming Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 57
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000605 extraction Methods 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 239000012074 organic phase Substances 0.000 claims abstract description 25
- 238000004070 electrodeposition Methods 0.000 claims abstract description 24
- 239000003350 kerosene Substances 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 9
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 11
- 238000005352 clarification Methods 0.000 claims description 9
- 238000002386 leaching Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 aldoxime ketone compound Chemical class 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 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
- C22B7/007—Wet processes by acid leaching
-
- 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
- C22B15/0084—Treating solutions
- C22B15/0086—Treating solutions by physical methods
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering metal copper in steamed selenium slag, which comprises the following steps: (1) soaking the selenium steaming slag in sulfuric acid to obtain copper separating liquid of the selenium steaming slag; (2) extracting the copper separating liquid of the selenium steaming residue by using an extractant LIX984 diluted by sulfonated kerosene to obtain a copper-containing organic phase; (3) carrying out back extraction on the copper-containing organic phase by using kerosene to remove an extracting agent, wherein the main component of a back-extracted solution is copper sulfate, carrying out electrodeposition to recover metal copper, returning the extracting agent to be circularly used for extracting copper liquor of the selenium steaming slag, and using sulfuric acid generated in the electrodeposition process to circularly soak the selenium steaming slag; the method is simple, the copper recovery rate is high, no waste liquid is generated in the whole process, and the method can be popularized to the recovery of copper in copper-containing materials.
Description
Technical Field
The invention relates to the technical field of valuable metal recovery in selenium steaming slag, in particular to a method for recovering metal copper in the selenium steaming slag.
Background
In the copper electrolysis process, anode sludge containing valuable metals is produced in large quantities. The common smelter needs to recover the valuable metals in the anode mud. In the anode mud treatment, selenium steaming is firstly carried out, selenium steaming slag contains a large amount of valuable metals, and then sulfuric acid is used for leaching. The copper ions in the leaching solution are generally 5-10 g/L, the sulfuric acid concentration is 20-60 g/L, the chloride ions are 10-15 g/L, and other impurity ions are also contained, and the leaching solution is also called as copper separating solution of selenium steaming slag.
At present, copper separating liquid of selenium steaming slag is generally concentrated to produce copper sulfate, and then soda ash is added to produce basic copper carbonate. The process has the advantages of low recovery efficiency, high production cost and no production of high-benefit metal copper. Therefore, a new method is developed to recover the copper in the selenium steaming slag, the economic benefit of the recovery process is improved, and the problem to be solved in the industry is urgently solved.
Disclosure of Invention
The invention aims to provide a method for recovering copper metal from steamed selenium slag, aiming at the problems of low recovery efficiency, high production cost and low economic benefit of the copper metal recovered from the steamed selenium slag at present.
The invention discloses a method for recovering metal copper in steamed selenium slag, which comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 15-20 g/L to 40-60 ℃, adding selenium steaming slag with the mass of 30-100% of that of the sulfuric acid solution, stirring at the stirring speed of 1-3R/S for reaction for 70-100 h, and filtering a leaching solution to obtain a copper separating solution of the selenium steaming slag, wherein the mass concentration of copper in the copper separating solution of the selenium steaming slag is 5-10 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, performing 2-stage extraction at normal temperature under the condition that the ratio of O/A to O/A is 1: 1-1: 3 to recover copper in the copper separating liquid of the selenium steaming slag, separating a water phase and an organic phase to obtain a copper extraction liquid and a copper-containing organic phase, and returning the copper extraction liquid to soak the selenium steaming slag; the extracting agent is LIX984 diluted to 20-25% by volume by sulfonated kerosene;
(3) copper-containing organic phasePerforming 2-stage back extraction on kerosene at normal temperature under the condition that the ratio of O/A is 1: 1-1: 6 to obtain a back extraction solution and an extractant, wherein the back extraction solution mainly comprises copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 150-200A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
And when the copper separating liquid of the selenium steaming slag is extracted, the mixing time is 10-30 min, and the clarification time is 10-30 min.
When the copper-containing organic phase is subjected to back extraction by adopting kerosene, the mixing time is 10-30 min, and the clarification time is 10-30 min.
The extractant adopted in the invention is LIX984 diluted by sulfonated kerosene to 20-25% in volume fraction, and the LIX984 is an imported aldoxime ketone compound extractant, so that the extraction efficiency is high, the selectivity is strong, the Cu/Fe separation coefficient is high, the extractant is suitable for a high-acid environment, the phase separation speed is high, and the saturation capacity is large.
According to the invention, the selenium steaming slag is soaked and separated by sulfuric acid, valuable metal copper in the selenium steaming slag is recovered by utilizing copper separating liquid of the selenium steaming slag, and the extraction and electrodeposition methods are adopted, so that the prepared copper product has high purity and low copper loss rate, and an extractant used in the production process and produced extracted liquid can be recycled, so that the production cost is low, and the economic benefit is high.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
Example 1
A method for recovering metallic copper in steamed selenium slag comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 18g/L to 50 ℃, adding 50% of the selenium steaming slag of the sulfuric acid solution, stirring and reacting for 80 hours at the stirring speed of 2R/S, and filtering the leachate to obtain copper separating liquid of the selenium steaming slag, wherein the mass concentration of copper in the copper separating liquid of the selenium steaming slag is 8.2 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, and performing 2-stage extraction to recover copper in the copper separating liquid of the selenium steaming slag at normal temperature under the condition that the ratio of O/A is 1: 2, wherein the mixing time of each stage of extraction is 20min, and the clarification time is 20 min; after extraction, separating the water phase from the organic phase to obtain copper-extracted liquid and a copper-containing organic phase, and returning the copper-extracted liquid to soak the selenium-steaming residue; the extracting agent is LIX984 diluted to 23% by volume by sulfonated kerosene;
(3) carrying out 2-stage back extraction on the copper-containing organic phase by adopting kerosene under the conditions of normal temperature and 1: 5 of phase ratio O/A, wherein the mixing time of each stage of back extraction is 20min, the settling time is 20min, and a back extraction liquid and an extracting agent are obtained, wherein the main component of the back extraction liquid is copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 180A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
Example 2
A method for recovering metallic copper in steamed selenium slag comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 20g/L to 60 ℃, adding the selenium steaming slag with the mass concentration of 100% of the sulfuric acid solution, stirring and reacting for 100 hours at the stirring speed of 1R/S, and filtering the leachate to obtain copper separating liquid of the selenium steaming slag, wherein the mass concentration of copper in the copper separating liquid of the selenium steaming slag is 5 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, and performing 2-stage extraction to recover copper in the copper separating liquid of the selenium steaming slag at normal temperature under the condition that the ratio of O/A to O/A is 1: 3, wherein the mixing time of each stage of extraction is 10min, and the clarification time is 10 min; after extraction, separating the water phase from the organic phase to obtain copper-extracted liquid and a copper-containing organic phase, and returning the copper-extracted liquid to soak the selenium-steaming residue; the extracting agent is LIX984 diluted by sulfonated kerosene to 25% by volume;
(3) the copper-containing organic phase adopts kerosene to perform 2-stage back extraction at normal temperature under the condition that the ratio of O/A to O/A is 1: 4, the mixing time of each stage of back extraction is 10min, and the copper-containing organic phase is clarifiedThe time is 10min to obtain back extraction solution and extractant, the back extraction solution contains copper sulfate as main component, and the metal copper is recovered by electrodeposition with electrodeposition current density of 150A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
Example 3
A method for recovering metallic copper in steamed selenium slag comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 15g/L to 40 ℃, adding selenium steaming slag with the mass concentration of 40% of that of the sulfuric acid solution, stirring at the stirring speed of 3R/S for reaction for 70 hours, and filtering a leaching solution to obtain copper separating liquid of the selenium steaming slag, wherein the mass concentration of copper in the copper separating liquid of the selenium steaming slag is 10 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, and performing 2-stage extraction to recover copper in the copper separating liquid of the selenium steaming slag at normal temperature under the condition that the ratio of O/A to O/A is 1: 1, wherein the mixing time of each stage of extraction is 30min, and the clarification time is 30 min; after extraction, separating the water phase from the organic phase to obtain copper-extracted liquid and a copper-containing organic phase, and returning the copper-extracted liquid to soak the selenium-steaming residue; the extracting agent is LIX984 diluted by sulfonated kerosene to 25% by volume;
(3) carrying out 2-stage back extraction on the copper-containing organic phase by adopting kerosene under the conditions of normal temperature and 1: 1 of phase ratio O/A, wherein the mixing time of each stage of back extraction is 30min, the settling time is 30min, and a back extraction liquid and an extracting agent are obtained, wherein the main component of the back extraction liquid is copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 200A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
Example 4
A method for recovering metallic copper in steamed selenium slag comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 16g/L to 55 ℃, adding 80% of steamed selenium slag by mass of the sulfuric acid solution, stirring and reacting for 75 hours at the stirring speed of 1R/S, and filtering a leaching solution to obtain a copper separating solution of the steamed selenium slag, wherein the mass concentration of copper in the copper separating solution of the steamed selenium slag is 9 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, and performing 2-stage extraction to recover copper in the copper separating liquid of the selenium steaming slag at normal temperature under the condition that the ratio of O/A is 1: 2.5, wherein the mixing time of each stage of extraction is 25min, and the clarification time is 25 min; after extraction, separating the water phase from the organic phase to obtain copper-extracted liquid and a copper-containing organic phase, and returning the copper-extracted liquid to soak the selenium-steaming residue; the extracting agent is LIX984 diluted by sulfonated kerosene to 22% in volume fraction;
(3) carrying out 2-stage back extraction on the copper-containing organic phase by adopting kerosene under the conditions of normal temperature and 1: 3 of phase ratio O/A, wherein the mixing time of each stage of back extraction is 18min, the settling time is 18min, and obtaining a back extraction liquid and an extractant, wherein the main component of the back extraction liquid is copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 160A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
Example 5
A method for recovering metallic copper in steamed selenium slag comprises the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 17g/L to 45 ℃, adding 60% of steamed selenium slag by mass of the sulfuric acid solution, stirring at the stirring speed of 2R/S for reaction for 85 hours, and filtering a leaching solution to obtain a copper separating solution of the steamed selenium slag, wherein the mass concentration of copper in the copper separating solution of the steamed selenium slag is 7 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, and performing 2-stage extraction to recover copper in the copper separating liquid of the selenium steaming slag at normal temperature under the condition that the ratio of O/A is 1: 2.5, wherein the mixing time of each stage of extraction is 20min, and the clarification time is 20 min; after extraction, separating the water phase from the organic phase to obtain copper-extracted liquid and a copper-containing organic phase, and returning the copper-extracted liquid to soak the selenium-steaming residue; the extracting agent is LIX984 diluted to 24% by volume by sulfonated kerosene;
(3) carrying out 2-stage back extraction on the copper-containing organic phase by adopting kerosene under the conditions of normal temperature and 1: 6 of phase ratio O/A, wherein the mixing time of each stage of back extraction is 20min, the settling time is 20min, and a back extraction liquid and an extracting agent are obtained, wherein the main component of the back extraction liquid is copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 190A/m2The extractant returns to the step (2) to be circularly used for extracting the copper separating liquid of the selenium steaming slag,the sulfuric acid generated in the electrodeposition process is returned and recycled for soaking the selenium-steaming slag.
Claims (3)
1. A method for recovering metallic copper in steamed selenium slag is characterized by comprising the following steps:
(1) heating a sulfuric acid solution with the mass concentration of 15-20 g/L to 40-60 ℃, adding selenium steaming slag with the mass of 30-100% of that of the sulfuric acid solution, stirring at the stirring speed of 1-3R/S for reaction for 70-100 h, and filtering a leaching solution to obtain a copper separating solution of the selenium steaming slag, wherein the mass concentration of copper in the copper separating solution of the selenium steaming slag is 5-10 g/L;
(2) adding an extracting agent into the copper separating liquid of the selenium steaming slag, performing 2-stage extraction at normal temperature under the condition that the ratio of O/A to O/A is 1: 1-1: 3 to recover copper in the copper separating liquid of the selenium steaming slag, separating a water phase and an organic phase to obtain a copper extraction liquid and a copper-containing organic phase, and returning the copper extraction liquid to soak the selenium steaming slag; the extracting agent is LIX984 diluted to 20-25% by volume by sulfonated kerosene;
(3) carrying out 2-stage back extraction on the copper-containing organic phase by adopting kerosene at normal temperature under the condition that the ratio of O/A is 1: 1-1: 6 to obtain a back extraction solution and an extractant, wherein the back extraction solution mainly comprises copper sulfate, metal copper is recovered by electrodeposition, and the electrodeposition current density is 150-200A/m2And (3) returning the extracting agent to the step (2) for circularly extracting the copper separating liquid of the selenium steaming slag, and returning the sulfuric acid generated in the electrodeposition process for circularly soaking the selenium steaming slag.
2. The method for recovering the metallic copper in the steamed selenium slag according to claim 1, which is characterized in that: and when the copper separating liquid of the selenium steaming slag is extracted, the mixing time is 10-30 min, and the clarification time is 10-30 min.
3. The method for recovering the metallic copper in the steamed selenium slag according to claim 1, which is characterized in that: when the copper-containing organic phase is subjected to back extraction by adopting kerosene, the mixing time is 10-30 min, and the clarification time is 10-30 min.
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2021
- 2021-04-29 CN CN202110472027.0A patent/CN113186402A/en active Pending
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