CN113025829B - Method for treating copper ore smelting waste residues by applying bipolar membrane electrodialysis - Google Patents

Method for treating copper ore smelting waste residues by applying bipolar membrane electrodialysis Download PDF

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CN113025829B
CN113025829B CN202110454254.0A CN202110454254A CN113025829B CN 113025829 B CN113025829 B CN 113025829B CN 202110454254 A CN202110454254 A CN 202110454254A CN 113025829 B CN113025829 B CN 113025829B
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waste residue
chamber
bipolar membrane
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CN113025829A (en
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刘耀兴
戴丽萍
柯雄
丁建国
陈日耀
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Fujian Normal University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4693Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses a method for treating copper ore smelting waste residue by applying bipolar membrane electrodialysis, which combines an electrolytic bath with an anion-cation exchange membrane and a bipolar membrane, uses a ruthenium iridium titanium plate as an electrode to form a bipolar membrane electrodialysis device, and firstly utilizes the H production of the bipolar membrane electrodialysis device + The performance is that the waste residue is in a strong acid environment, so that heavy metal in the waste residue is dissociated from the waste residue; then, separating a solid phase part and a liquid phase part of the waste residue by using a solid-liquid separation device, namely separating the residue in the waste residue from the acidic heavy metal solution; and finally, removing heavy metals in the separated supernatant, namely the acidic heavy metal solution, by using bipolar membrane electrodialysis. By adopting the method, the total time for waste residue treatment is 90-100, the removal rate of all heavy metals can reach more than 90%, and when the treatment unit in the step C is 2-5 units, the energy consumption can be reduced by 30-50%, the current efficiency can be improved by 40-60%, and the cost can be saved.

Description

Method for treating copper ore smelting waste residues by applying bipolar membrane electrodialysis
Technical Field
The invention relates to the technical field of treatment of copper ore smelting waste residues, in particular to a method for treating copper ore smelting waste residues by using bipolar membrane electrodialysis.
Background
Copper has excellent ductility and thermal conductivity, and is widely used in the fields of electricity, construction, national defense, mechanical manufacturing and the like. China now becomes the second largest economy of the world and the country with the greatest demand for copper, and in order to meet the ever-increasing demand for copper, mining of copper ores is required to obtain the required copper. Hydrometallurgical copper smelting has the advantages of low energy consumption and cost, small environmental pollution and the like, and is often used for extracting copper from low-grade copper ores (the low grade accounts for 56% in Chinese copper ore reserves). But a large amount of waste residues are generated in the process of copper ore hydrometallurgy, the components of the waste residues are complex, the waste residues are rich in a large amount of heavy metal ions and toxic and harmful substances, and the particles of the waste residues are small and dust is easy to form. If these residues are directly discharged without effective treatment, they will ultimately pose a significant risk to the environmental ecosystem, to the survival of living organisms and to human health.
At present, the waste residue treatment modes comprise backfilling and reclamation, valuable metal extraction, functional material preparation, building material production and the like, but all have the inevitable defects. The backfilling and the reclamation can effectively reduce the collapse and landslide risks of a mining area, but the backfilled waste residues have secondary pollution risks to the environment, and harmful substances such as heavy metals in the reclaimed waste residues can still influence the survival of animals, plants and microorganisms. The valuable metal can be extracted to effectively reduce the harm of heavy metal in the waste residue to the ecological environment, and the method can be used for recycling and generating economic value, but the method is suitable for the tailing waste residue rich in valuable metal and has no universal applicability. The functional material prepared by the waste residue can effectively improve the functionality of the material and generate social and economic values, but the requirement of the tailing waste residue is low and the utilization rate is low. The storage amount of the tailing waste residue in the environment can be effectively reduced by using the waste residue to produce the building material, but the air pollution is generated in the resource recycling process. The application of the methods has the problems of secondary pollution, high cost, long operation period, resource waste and the like. Therefore, there is a need to develop a green and environment-friendly process for treating waste residues.
The Electrodialysis (ED) method is a membrane separation technique, which uses potential difference as driving force to make the anions and cations in the pollutant pass through selectively permeable anion and cation membranes under the action of electric field force, so as to realize the purposes of desalination, purification, refining and concentration of the solution. The bipolar membrane (BPM) is a new type of ion exchange membrane, which is mainly composed of cation exchange membrane layer, anion exchange membrane layer and intermediate interface layer, and is characterized in that under the action of external electric field, water in the intermediate interface layer can be dissociated into H + And OH - And the hydrolysis voltage is only 0.828V, which is much less than the electrode hydrolysis voltage of 2.057V. In recent years, a method combining bipolar membrane and electrodialysis(bipolar membrane electrodialysis, BMED) is widely applied in the field of acid and alkali recovery, and meanwhile, with the development of bipolar membrane technology, BMED technology is also widely applied in the fields of chemical industry, pollution control, energy industry and the like.
Disclosure of Invention
The invention aims to design an energy-saving, environment-friendly and efficient method for treating copper ore smelting waste residues by using bipolar membrane electrodialysis, and realize harmless and resource utilization of the waste residues.
The technical scheme adopted for realizing the purpose of the invention is as follows: the method combines an electrolytic bath with an anion-cation exchange membrane and a bipolar membrane, takes a ruthenium iridium titanium plate as an electrode to form a bipolar membrane electrodialysis device, and treats the copper ore smelting waste residues, and comprises the following steps: leaching heavy metal in waste residue A: h production using bipolar membrane electrodialysis device + The performance is that the waste residue is in a strong acid environment, so that heavy metal in the waste residue is dissociated from the waste residue; b, separating residue from solution: separating the solid phase part (residue) and the liquid phase part (acidic heavy metal solution) of the waste residue by using a solid-liquid separation device; c acid heavy metal solution (supernatant) treatment: and removing heavy metals in the separated supernatant by using bipolar membrane electrodialysis.
The whole processing device of the invention is composed of three processing units, and the processing device adopted in the step A is as follows: the electrolytic bath is of a nylon material cuboid groove-shaped structure, the left end and the right end of the electrolytic bath are respectively provided with an anode and a cathode which are respectively connected with a positive pole line and a negative pole line of a direct current stabilized voltage power supply, and a waste residue treatment unit which consists of a bipolar membrane, a cation exchange membrane and the bipolar membrane is arranged between the anode and the cathode from the anode end at the left end to the cathode end at the right end; the space where the anode at the left end is located is an anode chamber, the space where the cathode at the right end is located is a cathode chamber, the space between the bipolar membrane and the cation exchange membrane on the right side of the anode chamber is a waste residue chamber, and the space between the cation exchange membrane and the bipolar membrane on the right side of the waste residue chamber is a heavy metal chamber; the solid-liquid separation device in the step B is composed of a water circulation multifunctional vacuum pump and a suction filtration device; the processing device adopted in the step C is as follows: the electrolytic tank is of a nylon material cuboid groove-shaped structure, the left end and the right end of the electrolytic tank are respectively provided with an anode and a cathode which are respectively connected with a positive electrode and a negative electrode of a direct current stabilized voltage power supply, and a supernatant processing unit which consists of an anion exchange membrane, a cation exchange membrane and a bipolar membrane is arranged between the anode and the cathode from the anode end at the left end to the cathode end at the right end; the space where the anode at the left end is positioned is an anode chamber, the space where the cathode at the right end is positioned is a cathode chamber, and the space between an anion exchange membrane and a cation exchange membrane on the right side of the anode chamber is a supernatant chamber; the space between the cation exchange membrane and the bipolar membrane on the right side of the supernatant chamber is a heavy metal chamber.
And the waste residue chamber and the supernatant chamber are both provided with electric stirrers, and the uniformity of the waste residue and the supernatant is kept through stirring.
When the supernatant processing unit is 2-5 units, the arrangement of the membranes is formed by sequentially spacing 2-5 groups of anion exchange membranes, cation exchange membranes and bipolar membranes from the anode end to the cathode end.
While the step C is used for treating, SO in the solution is treated 4 2- With H 2 SO 4 The recovery is performed in the manner described above.
The anode and the cathode adopt ruthenium iridium titanium plates.
The bipolar membrane adopts BP-1E type bipolar membrane of Astom company of Japan, wherein the cathode membrane layer faces to the anode, and the anode membrane layer faces to the cathode.
The specific application process of the BMED treatment system of the invention is as follows: adding the copper ore smelting waste residue into a waste residue chamber of the treatment device in the step A, and adding 1-2 mol/L Na into an anode chamber, a heavy metal chamber and a cathode chamber 2 SO 4 Starting an electric stirrer arranged in the waste residue chamber, stirring to keep the uniformity of the waste residue liquid, providing constant current by a direct current stabilized power supply, wherein the current density is 3.0-4.0 mA/cm 2 After 50-60 h of treatment, carrying out solid-liquid separation on the waste residue liquid by adopting the solid-liquid separation device in the step B; adding the supernatant into a supernatant chamber of the treatment device in the step C, and adding 1-2 mol/L Na into the anode chamber, the supernatant chamber and the cathode chamber 2 SO 4 Starting an electric stirrer arranged in the supernatant fluid chamber, stirring to keep the uniformity of the wastewater, and stirring to keep the uniformity of the supernatant fluidThe current stabilized power supply provides constant current with the current density of 2.0-3.0 mA/cm 2 And finishing the removal of heavy metals in the supernatant through treatment for 40-50 h.
The invention applies BMED technology to treat waste residues generated by copper ore hydrometallurgy, and aims to remove most heavy metals in the waste residues, thereby achieving the harmless treatment effect of the waste residues, and residual liquid in the treatment process can be used as acid leaching liquid in the copper ore hydrometallurgy process. The BMED system has the characteristics of small occupied area, high treatment efficiency, no secondary pollution and the like.
The invention has the following beneficial effects:
1. the heavy metal content of the waste residue after treatment is greatly reduced, and the waste residue can reach the harmless standard after a series of treatments.
2. The treated supernatant has low Cu concentration and small pH value, and can be used as acid leaching solution in copper ore hydrometallurgy.
3. The characteristic that the theoretical water dissociation voltage of the bipolar membrane is far lower than the water electrolysis voltage is utilized, the plurality of processing units are alternately connected in series, the unit energy consumption is reduced, the current efficiency is improved, and the cost is saved.
Drawings
FIG. 1 is a schematic view of the flow of waste residue treatment by the BMED technology of the present invention.
1: an electrolytic cell; 2: a ruthenium iridium titanium plate anode; 3: bipolar membrane; 4: a cation exchange membrane; 5: a bipolar membrane; 6: a ruthenium iridium titanium plate cathode; i: an anode chamber; II: a waste residue chamber; III: a heavy metal chamber; IV: a cathode chamber; 7: a suction filtration device; 8: filtering the membrane; 9: an electrolytic cell; 10: a ruthenium iridium titanium plate anode; 11: an anion exchange membrane; 12: a cation exchange membrane; 13: a bipolar membrane; 14: a ruthenium iridium titanium plate cathode; v: an anode chamber; VI, a supernatant chamber; VII: a heavy metal chamber; VIII: a cathode chamber.
FIG. 2 is a schematic diagram of a plurality of units in step C in the process of treating waste residues by the BMED technology.
AEM: an anion exchange membrane; CEM: a cation exchange membrane; BPM: a bipolar membrane; AC: an anode chamber; SFC: a waste residue chamber; HMC: a heavy metal chamber; CC: a cathode chamber.
Detailed Description
For a better understanding of the present invention, reference will now be made to the following descriptions taken in conjunction with the accompanying drawings.
In the step A, an anode 2, a bipolar membrane 3, a cation exchange membrane 4, a bipolar membrane 5 and a cathode 6 are sequentially arranged at intervals from an anode end to a cathode end to form a waste residue treatment unit.
And in the step B, the water circulation multifunctional vacuum pump and the suction filtration device form a solid-liquid separation device.
In the step C, the anode 10, the anion exchange membrane 11, the cation exchange membrane 12, the bipolar membrane 13 and the cathode 14 are sequentially arranged at intervals from the anode end to the cathode end to form a supernatant processing unit.
Example 1
The experimental setup used in this example is shown in FIG. 1.
When in use, the waste residue is added into a waste residue chamber of the device A shown in figure 1, and 1mol/L of Na is added into an anode chamber, a heavy metal chamber and a cathode chamber 2 SO 4 The solution plays a role of electrolyte, and both the initial cathode and anode adopt ruthenium-iridium-titanium plates as electrodes; stirring by using an electric stirrer to keep the uniformity of the solution in the waste residue chamber; the DC stabilized power supply provides constant current with the current density of 3.5mA/cm 2 And after running for 50 hours, separating heavy metals from the waste residues. Through determination, the removal rate of all heavy metals in the waste residue is more than 90%, and the purpose of harmlessness of the waste residue is achieved.
And then adding the waste residue liquid after the treatment in the step A into a filtering device shown as a step B in the figure 1, and then providing separation power by using a water circulation multifunctional vacuum pump, controlling the temperature to be room temperature and preventing water from evaporating. The treatment target is to separate the waste residue liquid into two parts of dry waste residue and supernatant. After the dry waste residue is subjected to morphological determination, the content of heavy metal in the dry waste residue is found to be low, the dry waste residue is in an inert state, and the dry waste residue can be directly discharged or comprehensively utilized. The supernatant contains a large amount of heavy metals, has high concentration and is acidic, and needs further treatment.
Finally, the supernatant is added into a supernatant chamber of the device shown as C in figure 1, and 1mol/L of Na is added into the anode chamber, the supernatant chamber and the cathode chamber 2 SO 4 The solution acts as electrolyte, and ruthenium is adopted for both the initial anode and the initial cathodeThe iridium titanium plate is used as an electrode; stirring by an electric stirrer to keep the solution uniformity in the supernatant chamber; the DC stabilized power supply provides constant current with the current density of 3.0mA/cm 2 The treatment time was 45h. Through determination, the removal rate of all heavy metals in the supernatant is over 95 percent. The concentration of all heavy metals in the treated supernatant is less than or equal to 100mg/L, the pH value is less than or equal to 1.0, and the treated supernatant can be used as acid leaching solution in copper ore hydrometallurgy.
The waste slag used in the embodiment is solid waste produced in hydrometallurgy of certain copper mine in Fujian province.
The bipolar membrane used in this example was a BP-1E type bipolar membrane from Astom corporation, japan, with the cathode layer facing the anode and the anode layer facing the cathode.
As the cation exchange membrane used in this example, nafion cation exchange membrane model NRE212 from Dupont, USA was used.
The anion exchange membrane used in this example was the ion exchange membrane of iosep EDI, hangzhou ael environmental protection technologies ltd.
Electrolyte Na used in this example 2 SO 4 Purchased from Shanghai national drug group chemical reagent Co., ltd, and is analytically pure.
The filter membrane used in this example, with a pore size of 0.45um, was purchased from Shanghai New Asian purification device factories.
The multifunctional vacuum pump for water circulation used in this example was purchased from shanghai rejie instruments ltd.
The suction filtration device used in this example was purchased from glass instrument factories of Feida of Jiangsu.
The anode and the cathode described in this embodiment are ruthenium-iridium-titanium plates with the specification of 30mm × 80mm × 3mm, which are purchased from metal material purchasing sites of Mingxuan in Qinghe county, hebei.
Example 2
The experimental setup used in this example is shown in FIG. 2.
When the processing unit of the step C is 2-5 units, the arrangement of the films from the anode end to the cathode end is as follows in sequence: 2-5 groups of anion exchange membrane, cation exchange membrane and bipolar membrane are formed at intervals in sequence.
At the start of the treatment, the supernatant was added to all supernatant compartments in FIG. 2. 1mol/L of Na is added into all the anode chamber, the supernatant chamber and the cathode chamber 2 SO 4 The solution plays a role of electrolyte, and ruthenium iridium titanium plates are adopted as electrodes for the initial anode and cathode; stirring by an electric stirrer to keep the solution uniformity in the supernatant chamber; the DC stabilized power supply provides constant current with the current density of 3.0mA/cm 2 The treatment time was 45h. Through determination, the removal rate of all heavy metals in the supernatant is over 90 percent. The current efficiency is increased by 40-60% and the energy consumption is reduced by 30-50% when one group of current is added. The concentration of all heavy metals in the treated supernatant is less than or equal to 100mg/L, the pH value is less than or equal to 1.0, and the treated supernatant can be used as acid leaching solution in copper ore hydrometallurgy.
The bipolar membrane used in this example was a BP-1E type bipolar membrane from Astom corporation, japan, with the cathode layer facing the anode and the anode layer facing the cathode.
As the cation exchange membrane used in this example, nafion cation exchange membrane model NRE212 from Dupont, USA was used.
The anion exchange membrane used in this example was the ion exchange membrane IONSEP EDI, an environmental protection technologies Inc. of Hangzhou El.
Electrolyte Na used in this example 2 SO 4 Purchased from Shanghai national drug group chemical reagent, inc., and is analytically pure.
The anode and the cathode described in this embodiment are ruthenium-iridium-titanium plates with the specification of 30mm × 80mm × 3mm, which are purchased from metal material purchasing sites of Mingxuan in Qinghe county, hebei.

Claims (5)

1. A method for treating copper ore smelting waste residue by applying bipolar membrane electrodialysis is characterized in that an electrolytic bath is combined with an anion-cation exchange membrane and a bipolar membrane, a bipolar membrane electrodialysis device is formed by taking a ruthenium-iridium-titanium plate as an electrode, and the copper ore smelting waste residue is treated, and the method comprises the following steps:
a: h production using bipolar membrane electrodialysis device + The performance is that the waste residue is in a strong acid environment, so that heavy metal in the waste residue is dissociated from the waste residue;
b: separating the solid phase part and the liquid phase part of the waste residue by using a solid-liquid separation device, namely separating the residue in the waste residue from the acidic heavy metal solution;
c: removing heavy metals in the separated supernatant, namely the acidic heavy metal solution, by using bipolar membrane electrodialysis;
the processing device adopted in the step A is as follows: the electrolytic bath is of a nylon material cuboid groove-shaped structure, the left end and the right end of the electrolytic bath are respectively provided with an anode and a cathode which are respectively connected with a positive pole line and a negative pole line of a direct current stabilized voltage power supply, and a waste residue treatment unit which consists of a bipolar membrane, a cation exchange membrane and the bipolar membrane is arranged between the anode and the cathode from the anode end at the left end to the cathode end at the right end; the space where the anode at the left end is positioned is an anode chamber, the space where the cathode at the right end is positioned is a cathode chamber, the space between the bipolar membrane and the cation exchange membrane on the right side of the anode chamber is a waste residue chamber, and the space between the cation exchange membrane and the bipolar membrane on the right side of the waste residue chamber is a heavy metal chamber;
the solid-liquid separation device in the step B is composed of a water circulation multifunctional vacuum pump and a suction filtration device;
the processing device adopted in the step C is as follows: the electrolytic bath is of a nylon material cuboid groove-shaped structure, the left end and the right end of the electrolytic bath are respectively provided with an anode and a cathode which are respectively connected with a positive pole and a negative pole of a direct current stabilized voltage power supply, and a supernatant processing unit which is composed of an anion exchange membrane, a cation exchange membrane and a bipolar membrane is arranged between the anode and the cathode from the anode end at the left end to the cathode end at the right end; the space where the anode at the left end is positioned is an anode chamber, the space where the cathode at the right end is positioned is a cathode chamber, and the space between an anion exchange membrane and a cation exchange membrane on the right side of the anode chamber is a supernatant chamber; a space between the cation exchange membrane and the bipolar membrane on the right side of the supernatant chamber is a heavy metal chamber;
adding the copper ore smelting waste residue into a waste residue chamber of the treatment device in the step A, and adding Na into an anode chamber, a heavy metal chamber and a cathode chamber of the treatment device in the step A 2 SO 4 The solution and a direct current stabilized power supply provide constant current, and the current density is 3.0 to 4.0mA/cm 2 After 50 to 60 hours of treatment, carrying out solid-liquid separation on the waste residue liquid by adopting the solid-liquid separation device in the step BSeparating, adding the supernatant into the supernatant chamber of the treating device in the step C, and adding Na into the anode chamber, the supernatant chamber and the cathode chamber 2 SO 4 The solution and a direct current stabilized power supply provide constant current, and the current density is 2.0 to 3.0mA/cm 2 Finishing the removal of heavy metals in the supernatant after 40-50h of treatment;
when the supernatant processing unit is 2 to 5 units, the arrangement of the membranes is formed by sequentially spacing 2 to 5 groups of anion exchange membranes, cation exchange membranes and bipolar membranes from an anode end to a cathode end.
2. The method for treating the copper ore smelting waste residue by using bipolar membrane electrodialysis as claimed in claim 1, wherein said Na is 2 SO 4 The concentration of the solution is 1 to 2 mol/L.
3. The method for treating the waste residue from copper ore smelting by using bipolar membrane electrodialysis as claimed in claim 1, wherein step C is performed while SO in the solution is treated 4 2- With H 2 SO 4 The recovery is performed in the manner described above.
4. The method for treating the copper ore smelting waste residue by using the bipolar membrane electrodialysis as claimed in claim 1, wherein the waste residue chamber and the supernatant chamber are provided with electric stirrers.
5. The method for treating the waste residue from copper ore smelting by bipolar membrane electrodialysis according to claim 1, wherein said bipolar membrane is BP-1E type bipolar membrane from Astom corporation of Japan, and the cathode membrane layer is anode and the anode membrane layer is cathode.
CN202110454254.0A 2021-04-26 2021-04-26 Method for treating copper ore smelting waste residues by applying bipolar membrane electrodialysis Active CN113025829B (en)

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