CN111364059A - Method for treating copper separating liquid in electrolytic liquid cleaning process - Google Patents
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Abstract
The invention discloses a method for treating a copper separating liquid in an electrolysis liquid purification process, which adopts an electrolysis liquid purification workshop to treat the copper separating liquid generated in a copper anode mud treatment workshop, does not influence the normal treatment requirement of the electrolysis liquid purification workshop, and effectively treats the copper separating liquid. The copper liquid treatment process of a copper anode mud treatment workshop is reduced, and the equipment investment is reduced; the copper electrode waste residues in the electrolytic solution cleaning workshop are adopted to replace iron powder to replace selenium and tellurium in the copper separating solution, so that the replacement rate is high, the investment of the iron powder is reduced, the cost is reduced, and the resource recovery rate is high; the return smelting of the sponge copper is avoided, and the energy consumption is reduced; the sewage treatment process is reduced, and the treatment cost is saved; the copper-separating displacement liquid is treated by the electrolytic cleaning liquid, the treatment effect is good, the treated black acid returns to the system, no pollution waste is generated in the treatment process, and the environment-friendly effect of the treatment process is good; the electrolytic solution cleaning workshop adopts a three-section electrolysis mode, the copper content of the first-section cathode copper is more than 99.95 percent, the copper content of the second-section cathode copper is more than 99.9 percent, the copper electrode has high quality and high economic benefit.
Description
Technical Field
The invention relates to the technical field of copper smelting, in particular to a method for treating a copper separating liquid in an electrolysis liquid purifying process.
Background
The copper smelting plant comprises a plurality of workshop processes, wherein the workshop processes comprise a copper anode slime treatment workshop and an electrolysis liquid purification workshop, the copper anode slime treatment workshop is used for treating copper anode slime which is an intermediate product generated in the copper electrolysis refining process, the electrolysis liquid purification workshop is used for purifying electrolyte generated in the copper smelting process, and the two workshops respectively carry out respective process treatment and do not interfere with each other. The conventional treatment process of the copper anode mud comprises roasting, acid leaching and copper separating, gold chloride separating, sodium sulfite separating and silver separating and gold and silver refining. During the roasting process, a series of sulfation reactions can occur to copper, selenium and tellurium in the anode mud, the copper is converted into copper sulfate, the selenium is converted into selenium dioxide, most of the selenium dioxide is reduced into selenium by sulfur dioxide in flue gas and is discharged along with the flue gas, and the tellurium is converted into tellurate. And leaching copper and most impurities in the roasted slag into a solution by adopting a low-acid leaching liquid. The copper separating liquid is the leaching liquid after acid leaching, contains a large amount of copper, and needs to be subjected to copper recovery and impurity removal treatment. At present, in the prior art, an iron powder replacement method is mostly adopted to replace copper into sponge copper, the sponge copper returns to a smelting system, and the replaced copper separating liquid is used for sewage treatment. The method consumes a large amount of iron powder, generates a large amount of waste water, and has high smelting energy consumption and treatment cost of the sponge copper. The existing electrolytic cleaning liquid workshop mostly adopts secondary copper removal electrolysis, namely, the concentration of copper ions is reduced to 40-20g/L in the primary copper removal electrolysis to produce a copper electrode, the secondary electrolytic copper removal is carried out to remove impurities such as arsenic, antimony and bismuth in the electrolyte to produce black copper, and the black copper is returned to a smelting system. The produced copper electrode has unstable copper content, low electrode quality and low economic benefit.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for treating copper separating liquid in an electrolysis liquid purification process. The use of iron powder and sewage treatment processes are reduced, the equipment cost is reduced, the resource recovery rate is high, the sponge copper is prevented from being melted back, the energy consumption is reduced, the generation of waste water is reduced, and the environment-friendly effect is good; meanwhile, three-section electrolysis is adopted in the electrolysis liquid cleaning workshop, the copper content of the first-section cathode copper is more than 99.95%, the copper content of the second-section cathode copper is more than 99.9%, the copper electrode quality is high, and the economic benefit is high.
The aim of the invention is achieved by the following technical measures: a method for treating gold, silver and copper separating liquid in an electrolytic liquid purifying process comprises the following steps:
(1) copper liquid separation and replacement: adding excessive copper sheets into the copper separating liquid, removing selenium and tellurium in the copper separating liquid by displacement, and carrying out solid-liquid separation after the reaction is finished to obtain selenium-tellurium slag and copper separating displacement liquid;
(2) and (3) electrolytic solution purification: the electrolyte in the electrolyte cleaning workshop is subjected to first-stage electrolysis, copper ions are subjected to a cathode reaction in the first-stage electrolysis to generate first-stage cathode copper which can be sold as a product, the electrolyte subjected to the first-stage electrolysis is subjected to second-stage electrolysis, a copper separation replacement solution is added into the second-stage electrolysis, the copper ions are subjected to a cathode reaction in the second-stage electrolysis to generate second-stage cathode copper which can be sold as a product, the electrolyte subjected to the second-stage electrolysis is subjected to third-stage electrolysis, the copper ions and arsenic, antimony and bismuth in the electrolyte are subjected to a cathode reaction in the third-stage electrolysis to generate black copper, the black copper is returned to a smelting system for smelting, the electrolyte subjected to the third-stage electrolysis is subjected to evaporation concentration, nickel in the electrolyte is crystallized to form a crude nickel product which can.
Further, when the concentration of copper ions in the electrolyte of the first-stage electrolysis is reduced to 30g/L, the electrolyte is conveyed to the second-stage electrolysis, when the concentration of copper ions in the electrolyte of the second-stage electrolysis is reduced to 18g/L, the electrolyte is conveyed to the third-stage electrolysis, and the concentration of copper ions in the electrolyte of the third-stage electrolysis is reduced to be less than 0.5 g/L.
Further, the volume ratio of the copper-separating replacement liquid added in the second-stage electrolysis to the electrolyte entering the second-stage electrolysis is less than 10%.
Further, the flow rate of the copper separation displacement liquid added with the two-stage electrolysis is 0.4-0.8m3/h。
Further, the temperature of the copper separating liquid displacement reaction is 80-100 ℃.
Further, the copper sheet is a waste material of an original copper electrode sheet in an electrolysis workshop.
Compared with the prior art, the invention has the beneficial effects that: according to the method for treating the copper separating liquid in the electrolytic liquid cleaning process, the copper separating liquid generated in the copper anode mud treatment workshop is treated in the electrolytic liquid cleaning workshop, so that the normal treatment requirement of the electrolytic liquid cleaning workshop is not influenced, the copper separating liquid is effectively treated, the copper separating liquid treatment process in the copper anode mud treatment workshop is reduced, and the equipment investment is reduced; the copper electrode waste residues in the electrolytic solution cleaning workshop are adopted to replace iron powder to replace selenium and tellurium in the copper separating solution, so that the replacement rate is high, the investment of the iron powder is reduced, the cost is reduced, and the resource recovery rate is high; the return smelting of the sponge copper is avoided, and the energy consumption is reduced; the generation of waste water is reduced, the environment-friendly treatment is realized, the sewage treatment process is reduced, and the treatment cost is saved; the copper-separating displacement liquid is treated by the electrolytic cleaning liquid, the treatment effect is good, the treated black acid returns to the system, no pollution waste is generated in the treatment process, and the environment-friendly effect of the treatment process is good; the electrolytic solution cleaning workshop adopts a three-section electrolysis mode, the copper content of the first-section cathode copper is more than 99.95 percent, the copper content of the second-section cathode copper is more than 99.9 percent, the copper electrode has high quality and high economic benefit.
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Drawings
FIG. 1 is a process flow chart of the method for treating the gold, silver and copper separating liquid in the electrolytic liquid purifying process.
Detailed Description
As shown in fig. 1, a method for treating gold, silver and copper separating liquid in an electrolytic liquid purifying process comprises the following steps:
(1) copper liquid separation and replacement: and adding excessive copper sheets into the copper separating liquid, wherein the copper sheets are waste scraps of original copper electrode plates of the electrolytic plant. The reaction temperature is controlled at 80-100 ℃, selenium and tellurium in the copper separating liquid are removed by displacement, selenium-tellurium slag and the copper separating displacement liquid are obtained by solid-liquid separation after the reaction is finished, and the selenium-tellurium slag can be subjected to subsequent selenium-tellurium purification treatment.
(2) And (3) electrolytic solution purification: the electrolyte in the electrolyte cleaning workshop is subjected to first-stage electrolysis, the current intensity of the first-stage electrolysis is 4900-6500A, and the current density is 190-250A/m3The temperature of the electrolyte is 50-70 ℃, a lead electrode is used as an anode, gelatin and thiourea are added into the electrolyte as additives, the addition amount of the gelatin is 400g/t Cu, and the addition amount of the thiourea is 400-900 g/L. The copper ions are reacted in the cathode of the first-stage electrolysis to generate first-stage cathode copper which can be sold as a product, and the copper content in the first-stage cathode copper exceeds 99.95 percent. When the concentration of copper ions is reduced to 30g/L, the electrolyte after the first-stage electrolysis is conveyed to the second-stage electrolysis, and meanwhile, copper separation replacement liquid is added into the second-stage electrolysis, the volume ratio of the copper separation replacement liquid to the electrolyte entering the second-stage electrolysis is less than 10%, and the adding flow rate of the copper separation replacement liquid is 0.4-0.8m3The current intensity of the two-stage electrolysis is 4900-6500A, and the current density is 190-250A/m3The temperature of the electrolyte is 50-70 ℃, a lead electrode is used as an anode, gelatin and thiourea are added into the electrolyte as additives, the addition amount of the gelatin is 200-500g/t Cu, and the addition amount of the thiourea is 400-900 g/L. The copper ions are reacted in the cathode of the second-stage electrolysis to generate second-stage cathode copper which can be sold as a product, and the copper content in the second-stage cathode copper exceeds 99.9 percent. When the concentration of copper ions is reduced to 18g/L, the electrolyte is conveyed to three-stage electrolysis, the current intensity of the three-stage electrolysis is 5000-6600A, and the current density is 200-264A/m3The temperature of the electrolyte is 40-60 ℃, a lead electrode is used as an anode, copper ions and arsenic, antimony and bismuth in the electrolyte react in a cathode of three-stage electrolysis to generate black copper, the black copper returns to a smelting system for smelting, and the copper ions in the electrolyte after the three-stage electrolysis are concentratedThe degree is reduced to below 0.5 g/L. And evaporating and concentrating the electrolyte after three-stage electrolysis, crystallizing nickel in the electrolyte to form a crude nickel product which can be sold, and returning the concentrated black acid to the system for recycling.
Example 1
The main chemical components (g/L) of the copper separating liquid are as follows: cu 49.5, Te 2.96, Se 3.78, As 3.62, Bi 2.76, Sb0.60, Ni 1.6, Fe 1.43, oriented at 280m3Adding 200g/L of copper sheets into the copper separating solution, wherein the reaction temperature is 80 ℃, and filtering after the reaction is finished to obtain the copper separating replacement solution, wherein the copper separating replacement solution mainly comprises the following chemical components in percentage by weight (g/L): cu 58.4, Te 0.0084, Se 0.0044, As3.63, Bi 2.76, Sb 0.59, Ni 1.61 and Fe 1.42.
Main chemical components (g/L) of the electrolyte: cu 54, Te<0.0001，Se<0.0001, As2.8, Bi 0.660, Sb0.178, Ni 6.4, Fe 1.562, 4500m3The electrolyte is subjected to first-stage electrolysis, the current intensity of the first-stage electrolysis is 4900A, and the current density is 190A/m3The temperature of the electrolyte is 50 ℃, the addition amount of gelatin is 200g/t Cu, the addition amount of thiourea is 400g/L, and copper ions react at a cathode of the first-stage electrolysis to generate first-stage cathode copper. The main chemical components (g/L) of the electrolyte after the first-stage electrolysis are as follows: cu 31, Te 0.0002, Se 0.00366, As 3.02, Bi 0.98, Sb 0.181, Ni 6.32 and Fe 1.47. The ratio of the first section of cathode copper to the standard cathode copper is as follows:
TABLE 1 comparison of standard chemical composition of first stage cathode copper and standard cathode copper
After the first-stage electrolysis, the electrolyte is conveyed to the second-stage electrolysis, and simultaneously copper separation replacement liquid is added into the second-stage electrolysis, the volume ratio of the copper separation replacement liquid to the electrolyte entering the second-stage electrolysis is 6.2 percent, and the adding flow rate of the copper separation replacement liquid is 0.4m3The current intensity of the two-stage electrolysis is 4900A, and the current density is 190A/m3The temperature of the electrolyte is 50 ℃, the addition amount of gelatin is 200g/t Cu, the addition amount of thiourea is 400g/L, and copper ions react at the cathode of the two-stage electrolysis to generate two-stage cathode copper. The main chemical components (g/L) of the electrolyte after the second-stage electrolysis are as follows: cu16.2, Te 0.0001, Se 0.00342, As3, Bi 0.97, Sb0.178, Ni6.31 and Fe 1.46. The comparison of the two-stage cathode copper with the No. 2 cathode copper standard is as follows:
TABLE 2 comparison of standard chemical composition of two-stage cathode copper and No. 2 cathode copper
After the second-stage electrolysis, the electrolyte is conveyed to the third-stage electrolysis, the current intensity of the third-stage electrolysis is 5000A, and the current density is 200A/m3The temperature of the electrolyte is 40 ℃, black copper is formed by the cathode of the three-stage electrolysis, and the black copper is returned to the smelting system for smelting. The main chemical components (g/L) of the electrolyte after three-stage electrolysis are as follows: cu 0.0045, Te<0.0001，Se<0.0001, As 0.0008, Bi 0.002, Sb 0.0001, Ni 12.84 and Fe 1.45. And evaporating and concentrating the electrolyte after three-stage electrolysis, crystallizing nickel in the electrolyte to form a crude nickel product which can be sold, and returning the concentrated black acid to the system for recycling.
Example 2
The main chemical components (g/L) of the copper separating liquid are as follows: cu 52.4, Te 2.58, Se 3.24, As 2.54, Bi 0.55, Sb0.24, Ni 1.61, Fe 1.17, up to 330m3Adding 220g/L of copper sheets into the copper separating solution, wherein the reaction temperature is 100 ℃, and filtering after the reaction is finished to obtain the copper separating replacement solution, wherein the copper separating replacement solution mainly comprises the following chemical components in percentage by weight (g/L): cu 62.7, Te 0.016, Se 0.0015, As2.56, Bi 0.55, Sb 0.22, Ni 1.62 and Fe 1.18.
Main chemical components (g/L) of the electrolyte: cu 53, Te<0.0001，Se<0.0001, As3.57, Bi 0.42, Sb0.14, Ni6.31, Fe 2.03, and 4460m3The electrolyte is subjected to first-stage electrolysis, the current intensity of the first-stage electrolysis is 6500A, and the current density is 250A/m3The temperature of the electrolyte is 70 ℃, the addition amount of gelatin is 500g/t Cu, the addition amount of thiourea is 900g/L, and copper ions react at the cathode of the first-stage electrolysis to generate first-stage cathode copper. The main chemical components (g/L) of the electrolyte after the first-stage electrolysis are as follows: cu 30.5, Te 0.0003, Se 0.00396, As 3.25, Bi 0.52, Sb 0.191, Ni 6.32 and Fe 1.77. The ratio of the first section of cathode copper to the standard cathode copper is as follows:
TABLE 3 comparison of standard chemical composition of cathode copper with standard cathode copper
After the first-stage electrolysis, the electrolyte is conveyed to the second-stage electrolysis, and simultaneously copper separation replacement liquid is added into the second-stage electrolysis, the volume ratio of the copper separation replacement liquid to the electrolyte entering the second-stage electrolysis is 7.3 percent, and the adding flow rate of the copper separation replacement liquid is 0.8m3The current intensity of the two-stage electrolysis is 6500A, and the current density is 250A/m3The temperature of the electrolyte is 70 ℃, the addition amount of gelatin is 400g/t Cu, the addition amount of thiourea is 900g/L, and copper ions react at the cathode of the two-stage electrolysis to generate two-stage cathode copper. The main chemical components (g/L) of the electrolyte after the second-stage electrolysis are as follows: cu 16.1, Te 0.0001, Se 0.0008, As 3.22, Bi 0.49, Sb0.185, Ni 6.33 and Fe 1.76. The comparison of the two-stage cathode copper with the No. 2 cathode copper standard is as follows:
TABLE 4 comparison of standard chemical compositions of two-stage cathode copper and No. 2 copper electrode
| The ingredients are% | Cu | Bi | Pb | Ag | Total amount of impurities |
| Copper electrode standard No. 2 | 99.9 | 0.0006 | 0.002 | 0.001 | 0.03 |
| Two-stage cathode copper | 99.9 | 0.0004 | 0.0012 | 0.00075 | <0.03 |
After the second-stage electrolysis, the electrolyte is conveyed to the third-stage electrolysis, the current intensity of the third-stage electrolysis is 6600A, and the current density is 264A/m3And the temperature of the electrolyte is 60 ℃, black copper is formed by the cathode of the three-stage electrolysis, and the black copper returns to the smelting system for smelting. The main chemical components (g/L) of the electrolyte after three-stage electrolysis are as follows: cu 0.0039, Te<0.0001，Se<0.0001, As 0.0007, Bi 0.001, Sb 0.0003, Ni 11.84 and Fe 1.73. And evaporating and concentrating the electrolyte after three-stage electrolysis, crystallizing nickel in the electrolyte to form a crude nickel product which can be sold, and returning the concentrated black acid to the system for recycling.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for treating gold, silver and copper separating liquid in an electrolytic liquid purifying process is characterized by comprising the following steps:
(1) copper liquid separation and replacement: adding excessive copper sheets into the copper separating liquid, removing selenium and tellurium in the copper separating liquid by displacement, and carrying out solid-liquid separation after the reaction is finished to obtain selenium-tellurium slag and copper separating displacement liquid;
(2) and (3) electrolytic solution purification: the electrolyte in the electrolyte cleaning workshop is subjected to first-stage electrolysis, copper ions are subjected to a cathode reaction in the first-stage electrolysis to generate first-stage cathode copper which can be sold as a product, the electrolyte subjected to the first-stage electrolysis is subjected to second-stage electrolysis, a copper separation replacement solution is added into the second-stage electrolysis, the copper ions are subjected to a cathode reaction in the second-stage electrolysis to generate second-stage cathode copper which can be sold as a product, the electrolyte subjected to the second-stage electrolysis is subjected to third-stage electrolysis, the copper ions and arsenic, antimony and bismuth in the electrolyte are subjected to a cathode reaction in the third-stage electrolysis to generate black copper, the black copper is returned to a smelting system for smelting, the electrolyte subjected to the third-stage electrolysis is subjected to evaporation concentration, nickel in the electrolyte is crystallized to form a crude nickel product which can.
2. The method for treating gold, silver and copper separating liquid in the electrolytic liquid purifying process according to claim 1, which is characterized in that: and when the concentration of copper ions in the electrolyte of the first-stage electrolysis is reduced to 30g/L, the electrolyte is conveyed to the second-stage electrolysis, when the concentration of copper ions in the electrolyte of the second-stage electrolysis is reduced to 18g/L, the electrolyte is conveyed to the third-stage electrolysis, and the concentration of copper ions in the electrolyte of the third-stage electrolysis is reduced to be below 0.5 g/L.
3. The method for treating gold, silver and copper separating liquid in the electrolytic liquid purifying process according to claim 1, which is characterized in that: the volume ratio of the copper-separating replacement liquid added in the second-stage electrolysis to the electrolyte entering the second-stage electrolysis is less than 10%.
4. The method for treating gold, silver and copper separating liquid in the electrolytic liquid purifying process according to claim 1, which is characterized in that: the flow rate of the copper-separating replacement liquid added with the two-stage electrolysis is 0.4-0.8m3/h。
5. The method for treating gold, silver and copper separating liquid in the electrolytic liquid purifying process according to claim 1, which is characterized in that:
the temperature of the copper separating liquid displacement reaction is 80-100 ℃.
6. The method for treating gold, silver and copper separating liquid in the electrolytic liquid purifying process according to claim 1, which is characterized in that:
the copper sheet is a waste material of an original copper electrode plate in an electrolysis workshop.
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| CN112210790A (en) * | 2020-09-17 | 2021-01-12 | 中南大学 | Treatment method of copper anode slime copper separating liquid |
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| CN112210790A (en) * | 2020-09-17 | 2021-01-12 | 中南大学 | Treatment method of copper anode slime copper separating liquid |
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