CN113088722A - Method for electrolytically recovering copper from copper sulfide ore - Google Patents
Method for electrolytically recovering copper from copper sulfide ore Download PDFInfo
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- CN113088722A CN113088722A CN202110284469.2A CN202110284469A CN113088722A CN 113088722 A CN113088722 A CN 113088722A CN 202110284469 A CN202110284469 A CN 202110284469A CN 113088722 A CN113088722 A CN 113088722A
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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
- C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
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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
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0073—Leaching or slurrying with acids or salts thereof containing nitrogen
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- 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
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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
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a method for recovering copper from copper sulfide ores, which comprises the following steps: (1) grinding the copper ore into 100-120 meshes by using a ball mill; (2) putting the ground copper ore into a stirring barrel, and adding hydrochloric acid, sulfuric acid, nitric acid, water and a medicament to perform chlorination reaction; (3) carrying out solid-liquid separation on the solution obtained after the reaction in the step (2) to obtain a copper chloride solution and filter residues; (4) pumping the copper chloride solution into an electrolytic bath for electrolysis, adding a flocculating agent, and controlling voltage, current and copper concentration to separate out copper in the electrolyte from a negative plate; (5) and returning the circulating solution after copper recovery to leaching. The whole process is reasonable in design, low in energy consumption and cost, and high in dissolution leaching rate and electrolysis recovery rate of copper in the copper ore, experiments show that the recovery rate of copper is more than 95%, comprehensive utilization of copper resources can be realized, and the method is applicable to both low-grade copper ore and high-grade copper ore, can reduce environmental pollution, and has important significance in protecting the environment.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a method for recovering copper from copper sulfide ore by acid electrolysis.
Background
At present, the copper content in the metal copper is generally more than 15%, and the copper content in the waste residue after the process equipment falls behind is more than 3%. Namely, the copper slag after comprehensive treatment often contains a certain amount of heavy metals such as arsenic, lead and the like. Not only wastes resources, but also generates great pollution to the environment.
In the prior art, no report exists on the recovery of copper by using copper sulfide ore as a raw material and adopting an acid method electrolysis method. The invention can avoid the waste of a large amount of copper resources, can also reduce environmental pollution, and has important application value.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to overcome the defects of the prior art and provide a method for recovering copper from copper sulfide ore by adopting the flow of an acid electrolysis process and reasonable process design. The invention has important significance for saving resources and protecting environment.
The technical scheme is as follows: in order to realize the purpose, the invention adopts the technical scheme that:
a method for recovering copper from copper sulphide ores, comprising the steps of:
(1) grinding the copper ore into 80-120 meshes by using a ball mill;
(2) putting the ground copper ore into a stirring barrel, and adding hydrochloric acid, sulfuric acid, nitric acid, water and a medicament to perform chlorination reaction;
(3) carrying out solid-liquid separation on the solution obtained after the reaction in the step (2) to obtain a copper chloride solution and filter residues;
(4) pumping the copper chloride solution obtained in the step (3) into an electrolytic bath of an electrolytic plant for electrolysis, adding a flocculating agent, and controlling the concentration of copper and the voltage and current magnitude to separate out copper in the electrolyte from a negative plate;
(5) and returning the circulating solution after copper recovery to leaching.
Preferably, in the method for recovering copper from copper sulphide ore, the filter residue obtained in the step (3) is added with ammonia water and dechlorinated to obtain the cement production raw material.
Preferably, in the above method for recovering copper from copper sulfide ore, in the step (2), 0.8 to 2.4 tons of hydrochloric acid with a volume concentration of 30 to 35 percent, 0.2 to 0.4 tons of concentrated sulfuric acid with a volume concentration of 95 percent or more, 100 to 200 kilograms of nitric acid, 0.2 to 0.4 tons of underground water and 60 to 120 kilograms of reagent are added to each ton of copper ore based on 20 percent of copper content for chlorination reaction. Particularly preferably, 0.8 to 1.2 tons of hydrochloric acid having a volume concentration of 30 to 35%, 0.2 tons of concentrated sulfuric acid having a volume concentration of 95% or more, 100 kg of nitric acid, 0.2 tons of groundwater, and 60 kg of chemical are added to carry out chlorination reaction.
Preferably, in the method for recovering copper from copper sulfide ore, the chemical in step (2) is hydrogen peroxide.
Preferably, in the method for recovering copper from copper sulfide ore, in the step (2), the hydrochloric acid, the sulfuric acid, the nitric acid and the reagent are reacted in a stirring barrel for 2-4 hours. The reaction is particularly preferably stirred for 3 hours.
Preferably, in the method for recovering copper from copper sulphide ore described above, the electrolysis time in the electrolytic cell in the step (4) is 24 hours.
Preferably, in the above method for recovering copper from copper sulphide ore, caustic soda and ammonium bicarbonate are added in step (3) to remove chloride in the filter residue by washing.
Preferably, in the method for recovering copper from copper sulfide ore, the flocculating agent added in the step (4) is industrial bone glue, and the concentration is controlled to be 5 g/L; the concentration of copper is controlled to be 100-150 g/L.
Preferably, in the above method for recovering copper from copper sulfide ore, the electrolysis voltage in step (4) is controlled to be 1.9V-2.0V, and the current is: 280-300A.
Preferably, in the above method for recovering copper from copper sulfide ore, the copper ore is low-grade copper sulfide ore or high-grade copper sulfide ore.
The process principle of the invention is as follows:
after the copper sulfide ore is dissolved by the reaction of hydrochloric acid and a catalyst, most of copper generated into copper chloride is dissolved in the solution, and most of other insoluble impurities are removed in a solid state. And putting the copper chloride solution into an electrolytic bath for electrolysis and collecting a 2# copper product.
As a further preferable scheme, the filter residue obtained in the step (3) is added with caustic soda and ammonium bicarbonate for dechlorination to obtain cement production raw materials or other fillers, so that the full utilization of resources is realized.
Preferably, the copper ore is low-grade copper sulfide or high-grade copper sulfide ore.
The method for recovering copper from copper sulfide ore provided by the invention specifically comprises the following chemical reactions:
Cu+H2SO4+1/2O2 = CuSO4+ H2O
CuO +2HCl=CuCl2+ H2O
the following reactions take place at the cathode:
Cu2++2e= Cu E°（Cu2+/Cu）=+0.34V
the total reaction is as follows: CuSO4+ H2O= Cu+ H2SO4+ 1/2O2
Has the advantages that: compared with the prior art, the invention has the following advantages:
the invention screens out the optimal copper electrolysis recovery process steps by an acid method through a large number of experiments, and the optimal copper electrolysis recovery process steps comprise the optimal copper acidification treatment and electrolysis process steps. The whole process is reasonable in design, low in energy consumption and cost, and high in dissolving leaching rate and electrolytic recovery rate of copper in the copper sulfide ore, and experiments show that the recovery rate of copper is more than 95%, so that the high-efficiency utilization of copper resources can be realized, the environment can be protected, and the method has important significance.
Drawings
FIG. 1 is a process flow diagram for recovering copper from copper sulphide ore according to the invention.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the specific material ratios, process conditions and results thereof described in the examples are illustrative only and should not be taken as limiting the invention as detailed in the claims.
Example 1
As shown in fig. 1, a method for recovering copper from copper sulphide ores, comprising the steps of:
(1) 500g of dried copper sulphide ore (Cu 37.73%, S4.80%, Fe 28.10%) was weighed and ground to 100 mesh using a ball mill.
(2) Putting the ground copper ore powder into a stirring barrel, adding 450 g of hydrochloric acid with the volume concentration of 30%, 150 g of sulfuric acid with the volume concentration of more than 95%, 60 g of nitric acid, 150 ml of underground water and 35 g of hydrogen peroxide, and carrying out chlorination reaction for 3 hours;
(3) and carrying out solid-liquid separation on the reacted solution to obtain a copper chloride solution and filter residue.
(4) Pumping the copper chloride solution into an electrolytic bath for electrolysis for 24 hours, adding 7.5 g of flocculant, controlling the concentration of copper to be 80 g/L, controlling the electrolysis voltage to be 1.9V, and controlling the current to be: 280A, copper was precipitated in the cathode to obtain 215.5 g of electrolytic copper containing 83.67% copper. The recovery of copper in this example was 95.6%
Example 2
A method for recovering copper from copper sulphide ores comprising the steps of:
(1) 500g of dried copper sulphide ore (Cu 29.58%, S11.17%, Fe 38.74%) was weighed out and ground to 120 mesh using a ball mill.
(2) The ground copper ore powder is put into a stirring barrel, 700 g of hydrochloric acid with the volume concentration of 35%, 160 g of sulfuric acid with the volume concentration of more than 95%, 60 g of nitric acid, 160 ml of underground water and 40 g of medicament (hydrogen peroxide) are added for chlorination reaction for 3 hours.
(3) And carrying out solid-liquid separation on the reacted solution to obtain a copper chloride solution and filter residue.
(4) Pumping the copper chloride solution into an electrolytic bath for electrolysis for 24 hours, adding 7.5 g of flocculant (bone glue), controlling the concentration of copper to be 80 g/L, controlling the electrolysis voltage to be 2.0V, and controlling the current to be: 300A. Copper is precipitated on the cathode plate to obtain 158.5 g of electrolytic copper with the content of 93.31 percent. The copper recovery of this example was 96.10%.
Comparative example 1
A method for recovering copper from copper sulphide ores comprising the steps of:
(1) 500g of dried copper sulphide ore (Cu 29.58%, S11.17%, Fe 38.74%) was weighed out and ground to 120 mesh using a ball mill.
(2) And putting the ground copper ore powder into a stirring barrel, and adding 700 g of hydrochloric acid with the volume concentration of 35%, 220 g of nitric acid and 160 ml of underground water to perform chlorination reaction for 3 hours.
(3) And carrying out solid-liquid separation on the reacted solution to obtain a copper chloride solution and filter residue.
(4) Pumping the copper chloride solution into an electrolytic bath for electrolysis for 24 hours, adding 7.5 g of flocculant (bone glue), controlling the concentration of copper to be 80 g/L, controlling the electrolysis voltage to be 2.0V, and controlling the current to be: 300A. Copper was precipitated at the cathode plate to obtain 137.53 g of electrolytic copper with a content of 87.52%. The copper recovery of this example was 81.38%.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various modifications and changes may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents may fall within the scope of the invention as defined in the claims appended hereto.
Claims (10)
1. A method for recovering copper from copper sulphide ores, comprising the steps of:
(1) grinding the copper ore into powder by using a ball mill;
(2) putting the ground copper ore into a stirring barrel, and adding different acids, water and medicaments for chlorination reaction;
(3) carrying out solid-liquid separation on the solution obtained after the reaction in the step (2) to obtain a copper chloride solution and filter residues;
(4) pumping the copper chloride solution obtained in the step (3) into an electrolytic bath of an electrolytic plant for electrolysis, adding a flocculating agent, and controlling the concentration of copper and the voltage and current magnitude to separate out copper in the electrolyte from a negative plate;
(5) and returning the circulating solution after copper recovery to leaching.
2. A method for recovering copper from copper sulphide ores, comprising the steps of:
(1) grinding the copper ore into 80-120 meshes by using a ball mill;
(2) putting the ground copper ore into a stirring barrel, and adding hydrochloric acid, sulfuric acid, nitric acid, water and a medicament to perform chlorination reaction;
(3) carrying out solid-liquid separation on the solution obtained after the reaction in the step (2) to obtain a copper chloride solution and filter residues;
(4) pumping the copper chloride solution obtained in the step (3) into an electrolytic bath of an electrolytic plant for electrolysis, adding a flocculating agent, and controlling the concentration of copper and the voltage and current magnitude to separate out copper in the electrolyte from a negative plate;
(5) and returning the circulating solution after copper recovery to leaching.
3. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: and (4) adding ammonia water into the filter residue obtained in the step (3) and dechlorinating to obtain a cement production raw material.
4. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: and (2) adding 0.8-2.4 tons of hydrochloric acid with the volume concentration of 30% -35%, 0.2-0.4 tons of concentrated sulfuric acid with the volume concentration of more than 95%, 100-200 kilograms of nitric acid, 0.2-0.4 tons of underground water and 60-120 kilograms of medicament into each ton of copper ore according to the content of 20% copper for chlorination reaction.
5. A method for recovering copper from copper sulphide ores as claimed in claim 1 or claim 3 in which: the medicament in the step (2) is hydrogen peroxide.
6. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: in the step (2), the hydrochloric acid, the sulfuric acid, the nitric acid and the medicament are reacted in a stirring barrel for 2-4 hours.
7. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: and (4) electrolyzing in the electrolytic bath for 24-48 hours.
8. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: and (3) adding caustic soda and ammonium bicarbonate to remove chloride in the filter residue by washing.
9. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: adding a flocculating agent which is industrial bone glue into the step (4), and controlling the concentration to be 5 g/L; the concentration of copper is controlled to be 100-150 g/L.
10. A method of recovering copper from copper sulphide ores as claimed in claim 1 in which: controlling the electrolytic voltage to be 1.9V-2.0V and the current to be: 280-300A; the copper ore is low-grade copper sulfide ore or high-grade copper sulfide ore.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110284469.2A CN113088722A (en) | 2021-03-17 | 2021-03-17 | Method for electrolytically recovering copper from copper sulfide ore |
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| CN202110284469.2A CN113088722A (en) | 2021-03-17 | 2021-03-17 | Method for electrolytically recovering copper from copper sulfide ore |
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| CN113088722A true CN113088722A (en) | 2021-07-09 |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094460A (en) * | 1993-04-24 | 1994-11-02 | 王绍和 | Directly electrolytic extraction of electrolytic copper by copper sulfide ore |
| CN1407120A (en) * | 2001-09-03 | 2003-04-02 | 贾建立 | Process for oxidation leaching-out, cuprous chloride and refining copper from cupric sulfide |
| CN1500892A (en) * | 2002-11-18 | 2004-06-02 | 住友金属矿山株式会社 | Refined method for copper materials containing copper sulphide minerals |
| CN101792864A (en) * | 2009-11-17 | 2010-08-04 | 灵宝市金源矿业有限责任公司 | Hyperbaric oxygen acid leaching process for cogenerating calcium sulfate whiskers from copper-sulphide ores |
| CN102418099A (en) * | 2011-12-12 | 2012-04-18 | 嘉兴科菲冶金科技股份有限公司 | Process for recovering copper by processing acidic copper chloride etchant through rotational flow electrolysis |
| CN103936081A (en) * | 2013-01-21 | 2014-07-23 | 解付兵 | Method and system for preparing ferric chloride, electrodeposited copper and copper powder from copper-containing hydrochloric acid waste liquid |
| CN105039989A (en) * | 2015-06-26 | 2015-11-11 | 无锡市瑞思科环保科技有限公司 | Electrodeposition decoppering and regenerating method of waste copper-bearing etching liquor of acidic chlorination system |
| CN106587105A (en) * | 2016-12-15 | 2017-04-26 | 明高电路版（赣州）有限公司 | Method for recovering copper chloride acid etching liquid in printed circuit board |
| CN109161895A (en) * | 2018-08-27 | 2019-01-08 | 安徽绿洲危险废物综合利用有限公司 | Acid copper chloride etching liquid copper reclaiming system and reclaiming method |
| CN112458280A (en) * | 2020-11-30 | 2021-03-09 | 江西睿锋环保有限公司 | Method for extracting valuable metals by leaching low grade nickel matte with acidic etching solution |
-
2021
- 2021-03-17 CN CN202110284469.2A patent/CN113088722A/en active Pending
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| CN1094460A (en) * | 1993-04-24 | 1994-11-02 | 王绍和 | Directly electrolytic extraction of electrolytic copper by copper sulfide ore |
| CN1407120A (en) * | 2001-09-03 | 2003-04-02 | 贾建立 | Process for oxidation leaching-out, cuprous chloride and refining copper from cupric sulfide |
| CN1500892A (en) * | 2002-11-18 | 2004-06-02 | 住友金属矿山株式会社 | Refined method for copper materials containing copper sulphide minerals |
| CN101792864A (en) * | 2009-11-17 | 2010-08-04 | 灵宝市金源矿业有限责任公司 | Hyperbaric oxygen acid leaching process for cogenerating calcium sulfate whiskers from copper-sulphide ores |
| CN102418099A (en) * | 2011-12-12 | 2012-04-18 | 嘉兴科菲冶金科技股份有限公司 | Process for recovering copper by processing acidic copper chloride etchant through rotational flow electrolysis |
| CN103936081A (en) * | 2013-01-21 | 2014-07-23 | 解付兵 | Method and system for preparing ferric chloride, electrodeposited copper and copper powder from copper-containing hydrochloric acid waste liquid |
| CN105039989A (en) * | 2015-06-26 | 2015-11-11 | 无锡市瑞思科环保科技有限公司 | Electrodeposition decoppering and regenerating method of waste copper-bearing etching liquor of acidic chlorination system |
| CN106587105A (en) * | 2016-12-15 | 2017-04-26 | 明高电路版（赣州）有限公司 | Method for recovering copper chloride acid etching liquid in printed circuit board |
| CN109161895A (en) * | 2018-08-27 | 2019-01-08 | 安徽绿洲危险废物综合利用有限公司 | Acid copper chloride etching liquid copper reclaiming system and reclaiming method |
| CN112458280A (en) * | 2020-11-30 | 2021-03-09 | 江西睿锋环保有限公司 | Method for extracting valuable metals by leaching low grade nickel matte with acidic etching solution |
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Application publication date: 20210709 |