CN114231746A - Method for recovering copper from copper smelting waste acid and gypsum slag - Google Patents
Method for recovering copper from copper smelting waste acid and gypsum slag Download PDFInfo
- Publication number
- CN114231746A CN114231746A CN202111442400.4A CN202111442400A CN114231746A CN 114231746 A CN114231746 A CN 114231746A CN 202111442400 A CN202111442400 A CN 202111442400A CN 114231746 A CN114231746 A CN 114231746A
- Authority
- CN
- China
- Prior art keywords
- copper
- filtrate
- gypsum slag
- waste acid
- acidolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000010949 copper Substances 0.000 title claims abstract description 67
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 65
- 239000002893 slag Substances 0.000 title claims abstract description 37
- 238000003723 Smelting Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002253 acid Substances 0.000 title claims abstract description 31
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 28
- 239000010440 gypsum Substances 0.000 title claims abstract description 28
- 239000002699 waste material Substances 0.000 title claims abstract description 28
- 239000000706 filtrate Substances 0.000 claims abstract description 33
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 16
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 12
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 6
- 239000010865 sewage Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006386 neutralization reaction Methods 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003350 kerosene Substances 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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
- C22B15/0065—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
-
- 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
- C22B30/04—Obtaining arsenic
-
- 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
Abstract
The invention relates to a method for recovering copper in copper smelting waste acid and gypsum slag, which comprises the following steps: the method includes the steps that water is added into copper smelting and gypsum slag, and stirring and slurrying are carried out to obtain slurry; adding acid into the slurry or washing waste acid by a system to carry out stirring acidolysis, and enabling the pH = 1.5-3.0 of acidolysis solution; performing filtration on the acidolysis solution to obtain a filtrate A, returning the filtrate A to the second step, performing 2-6 times of circular acidolysis, and filtering to obtain a filtrate B; extracting the filtrate B to obtain a copper sulfate solution and an extract liquid respectively; the copper sulfate solution returns to the copper electrolysis system; fifthly, adding sodium sulfide to precipitate arsenic after the pH of the raffinate is adjusted to be = 3.5-5.0, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant. The method has the advantages of simple and feasible process, small environmental pollution and low cost, can realize resource recovery and harmless treatment of the copper in the neutralized gypsum slag, and effectively solves the problem of pollution of the neutralized slag to the surrounding environment in landfill, stockpiling and solidification.
Description
Technical Field
The invention relates to the technical field of hazardous waste recycling and harmless treatment, in particular to a method for recovering copper in waste acid and gypsum residues in copper smelting.
Background
Copper lead zinc smelting enterprises can generate a large amount of heavy metal wastewater every year in the smelting process, the heavy metal wastewater is generally treated in a lime neutralization mode, and a large amount of neutralization slag can be generated in the treatment process. The waste acid generated in the process of washing the flue gas by the copper smelting system is treated by a lime neutralization method, and the waste residue in the waste acid neutralization treatment process is the neutralized residue.
The waste acid neutralization residues contain valuable metals such as copper, zinc, arsenic, lead and the like, and have the characteristics of high toxicity and serious pollution, and if the treatment and the management are improper, the environment can be seriously damaged. And the waste residues occupy a large amount of land, and toxic and harmful components are easy to permeate underground and diffuse to the periphery, so that the soil and underground water are polluted, and harmful gas and dust can be generated by fine particles such as dust. Therefore, the comprehensive recovery and treatment of the neutralization slag are always important subjects in the field of environmental protection.
The copper content in the copper smelting waste acid neutralization slag is 1% -2%, the neutralization slag contains heavy metals such as lead, zinc and arsenic, and the arsenic content is 2% -8%. The neutralization slag is unstable slag, is not treated and stacked, has potential environmental safety hidden trouble and is also waste of resources. Therefore, it is important to recycle valuable metals such as copper, lead, and zinc in the neutralized slag and to stabilize the neutralized slag.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for recovering copper in copper smelting waste acid and gypsum slag by harmless treatment.
In order to solve the problems, the method for recovering copper in copper smelting waste acid and gypsum slag comprises the following steps:
the method includes the steps that water is added into copper smelting and gypsum slag, and stirring and slurrying are carried out to obtain slurry;
adding acid into the slurry or washing waste acid by a system to carry out stirring acidolysis, and enabling the pH = 1.5-3.0 of acidolysis solution;
performing filtration on the acidolysis solution to obtain a filtrate A, returning the filtrate A to the second step, performing 2-6 times of circular acidolysis, and filtering to obtain a filtrate B;
extracting the filtrate B to obtain a copper sulfate solution and an extract liquid respectively; the copper sulfate solution returns to the copper electrolysis system;
fifthly, adding sodium sulfide to precipitate arsenic after the pH of the raffinate is adjusted to be = 3.5-5.0, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant.
The method comprises the step of enabling the using amount of the water to be 3-6 times of the mass of the copper smelting neutralization gypsum slag.
The acid in the step II is sulfuric acid with the volume concentration of 10-20%.
The extraction condition in the fourth step is room temperature, and the organic phase is composed of a LIX-based extractant and kerosene; the ratio of the filtrate B to the extractant is 1: 1-1: 3.
and adding a sodium hydroxide solution with the mass concentration of 30% into the raffinate in the step fifthly to adjust the pH value.
And fifthly, the addition amount of the sodium sulfide is 2-3 times of the arsenic content in the solution.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, metal elements such as copper, arsenic and the like in the neutralized gypsum slag in copper smelting are separated by acid, and meanwhile, the high-efficiency recovery of metals is realized by adopting heavy metal processes such as copper extraction recovery and arsenic vulcanization recovery, so that the heavy metals such as arsenic are further enriched and have good stability, thereby realizing the resource recovery and harmless treatment of copper in the neutralized gypsum slag, and effectively solving the problem of pollution of the neutralized slag to the surrounding environment in landfill, stockpiling and solidification.
2. The invention has simple and feasible process, little environmental pollution and low cost.
Detailed Description
A method for recovering copper in copper smelting waste acid and gypsum slag comprises the following steps:
the method comprises the steps of adding water with the mass being 3-6 times that of gypsum slag in copper smelting, stirring and slurrying to obtain slurry.
Adding 10-20% of sulfuric acid or system washing waste acid into the slurry, stirring and carrying out acidolysis, and enabling the pH = 1.5-3.0 of acidolysis solution.
And obtaining filtrate A after filtering the acidolysis solution, returning the filtrate A to the second step, performing 2-6 times of circular acidolysis, and filtering by a filter press to obtain filtrate B.
Fourth, an organic phase composed of a LIX-based extractant and kerosene is added to filtrate B for extraction at room temperature, and the ratio of the filtrate B to the extractant is 1: 1-1: 3, respectively obtaining a copper sulfate solution and an extract liquid; the copper sulfate solution is returned to the copper electrolysis system.
And fifthly, adding a sodium hydroxide solution with the mass concentration of 30% into the raffinate to adjust the pH = 3.5-5.0, adding sodium sulfide 2-3 times of the arsenic content in the solution to precipitate arsenic, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant.
Embodiment 1 a method for recovering copper in copper smelting waste acid and gypsum slag, comprising the following steps:
the method comprises the steps of adding 4kg of water into 1kg of copper smelting and gypsum slag, stirring and slurrying to obtain slurry.
Wherein: the main components of the copper smelting neutralization gypsum slag are as follows: 30.0% of water, 1.2% of Cu and CaSO4 58.0%、As 3.3%。
And adding 0.3kg of washing waste acid into the slurry, stirring and carrying out acidolysis, wherein the pH of the acidolysis solution is = 1.5.
And thirdly, filtering the acidolysis solution to obtain filtrate A, returning the filtrate A to the second step, performing 3 times of circular acidolysis, and filtering to obtain filtrate B.
And fourthly, under the room temperature condition, extracting the filtrate B by using an organic phase consisting of a 10% volume concentration LIX extraction agent and kerosene, performing back extraction by using 100g/L sulfuric acid to obtain a back extraction copper sulfate solution and an extract, performing back extraction on the copper sulfate solution containing 30-50 g/L of copper, and returning to the copper electrolysis system.
And fifthly, adding sodium hydroxide with the mass concentration of 30% into the raffinate to adjust the pH value, adding 30g of sodium sulfide to precipitate arsenic after the pH value is adjusted to =4.0, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant.
Embodiment 2 a method for recovering copper in copper smelting waste acid and gypsum slag, comprising the following steps:
the method comprises the steps of adding 5kg of water into 1kg of copper smelting and gypsum slag, stirring and slurrying to obtain the slurry.
Wherein: the main components of the copper smelting neutralization gypsum slag are as follows: 31.0% of water, 0.8% of Cu, CaSO462.0% and As2.1%.
And adding 0.2kg of washing waste acid into the slurry, stirring and carrying out acidolysis, wherein the pH of the acidolysis solution is = 2.0.
And thirdly, filtering the acidolysis solution to obtain filtrate A, and returning the filtrate A to the second step for 5 times of circular acidolysis and filtering to obtain filtrate B.
And fourthly, under the room temperature condition, extracting the filtrate B by using an organic phase consisting of a 10% volume concentration LIX extraction agent and kerosene, performing back extraction by using 100g/L sulfuric acid to obtain a back extraction copper sulfate solution and an extract, performing back extraction on the copper sulfate solution containing 30-50 g/L of copper, and returning to the copper electrolysis system.
And fifthly, adding sodium hydroxide with the mass concentration of 30% into the raffinate to adjust the pH value, adding 20g of sodium sulfide to precipitate arsenic after the pH value is adjusted to =4.0, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant.
Claims (6)
1. A method for recovering copper in copper smelting waste acid and gypsum slag comprises the following steps:
the method includes the steps that water is added into copper smelting and gypsum slag, and stirring and slurrying are carried out to obtain slurry;
adding acid into the slurry or washing waste acid by a system to carry out stirring acidolysis, and enabling the pH = 1.5-3.0 of acidolysis solution;
performing filtration on the acidolysis solution to obtain a filtrate A, returning the filtrate A to the second step, performing 2-6 times of circular acidolysis, and filtering to obtain a filtrate B;
extracting the filtrate B to obtain a copper sulfate solution and an extract liquid respectively; the copper sulfate solution returns to the copper electrolysis system;
fifthly, adding sodium sulfide to precipitate arsenic after the pH of the raffinate is adjusted to be = 3.5-5.0, and returning the obtained filtrate C to a sewage treatment system of the copper smelting plant.
2. The method for recovering copper in the copper smelting waste acid and the gypsum slag according to claim 1, which is characterized by comprising the following steps: the method comprises the step of enabling the using amount of the water to be 3-6 times of the mass of the copper smelting neutralization gypsum slag.
3. The method for recovering copper in the copper smelting waste acid and the gypsum slag according to claim 1, which is characterized by comprising the following steps: the acid in the step II is sulfuric acid with the volume concentration of 10-20%.
4. The method for recovering copper in the copper smelting waste acid and the gypsum slag according to claim 1, which is characterized by comprising the following steps: the extraction condition in the fourth step is room temperature, and the organic phase is composed of a LIX-based extractant and kerosene; the ratio of the filtrate B to the extractant is 1: 1-1: 3.
5. the method for recovering copper in the copper smelting waste acid and the gypsum slag according to claim 1, which is characterized by comprising the following steps: and adding a sodium hydroxide solution with the mass concentration of 30% into the raffinate in the step fifthly to adjust the pH value.
6. The method for recovering copper in the copper smelting waste acid and the gypsum slag according to claim 1, which is characterized by comprising the following steps: and fifthly, the addition amount of the sodium sulfide is 2-3 times of the arsenic content in the solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111442400.4A CN114231746A (en) | 2021-11-30 | 2021-11-30 | Method for recovering copper from copper smelting waste acid and gypsum slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111442400.4A CN114231746A (en) | 2021-11-30 | 2021-11-30 | Method for recovering copper from copper smelting waste acid and gypsum slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114231746A true CN114231746A (en) | 2022-03-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111442400.4A Pending CN114231746A (en) | 2021-11-30 | 2021-11-30 | Method for recovering copper from copper smelting waste acid and gypsum slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114231746A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4231993A (en) * | 1979-06-11 | 1980-11-04 | The United States Of America As Represented By The Secretary Of The Interior | Recovery of metal values from lead smelter matte |
| CN108754148A (en) * | 2018-06-08 | 2018-11-06 | 陕西中环信环保科技有限公司 | A kind of processing method of cupric, manganese, cobalt, zinc, nickel heavy metal waste slag recycling |
| CN112609082A (en) * | 2020-11-30 | 2021-04-06 | 江西睿锋环保有限公司 | Method for preparing high-purity cathode copper by using copper-containing soot and acidic waste liquid |
| CN113088708A (en) * | 2021-03-30 | 2021-07-09 | 中南大学 | Method for recycling polymetallic through resource synergistic treatment of copper smelting white smoke and dirty acid |
-
2021
- 2021-11-30 CN CN202111442400.4A patent/CN114231746A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4231993A (en) * | 1979-06-11 | 1980-11-04 | The United States Of America As Represented By The Secretary Of The Interior | Recovery of metal values from lead smelter matte |
| CN108754148A (en) * | 2018-06-08 | 2018-11-06 | 陕西中环信环保科技有限公司 | A kind of processing method of cupric, manganese, cobalt, zinc, nickel heavy metal waste slag recycling |
| CN112609082A (en) * | 2020-11-30 | 2021-04-06 | 江西睿锋环保有限公司 | Method for preparing high-purity cathode copper by using copper-containing soot and acidic waste liquid |
| CN113088708A (en) * | 2021-03-30 | 2021-07-09 | 中南大学 | Method for recycling polymetallic through resource synergistic treatment of copper smelting white smoke and dirty acid |
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