CN113774432A - Continuous electrolytic refining process for high-purity copper - Google Patents
Continuous electrolytic refining process for high-purity copper Download PDFInfo
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- CN113774432A CN113774432A CN202110956451.2A CN202110956451A CN113774432A CN 113774432 A CN113774432 A CN 113774432A CN 202110956451 A CN202110956451 A CN 202110956451A CN 113774432 A CN113774432 A CN 113774432A
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a continuous electrolytic refining process for high-purity copper. It comprises the following steps: (1) adding concentrated sulfuric acid, pure water and an additive into a copper sulfate solution obtained after impurity removal treatment of PCB waste liquid to obtain an electrolytic solution; in the electrolytic solution, the concentration of copper sulfate is 12-18g/ml, the weight percentage concentration of concentrated sulfuric acid is 9% -12%, and the weight percentage concentration of concentrated nitric acid is 0.05% -0.07%; the raw materials for preparing the additive comprise thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin; (2) and (4) continuously electrolyzing. According to the continuous electrolytic refining process for high-purity copper, 99.9935% of cathode copper can be prepared through the continuous electrolytic process, and the obtained high-purity copper is good in quality, high in purity and high in utilization rate.
Description
Technical Field
The invention belongs to the field of refining of high-purity copper, and particularly relates to a continuous electrolytic refining process for high-purity copper.
Background
PCB, i.e. printed circuit board, manufacturing technology is a very complex and comprehensive process technology. A qualified PCB is subjected to the processing processes of copper deposition, electroplating, developing, etching and the like, various heavy metal wastewater and organic wastewater are discharged in the processing process, the components are complex, and the processing difficulty is high. Calculated according to the utilization rate of the PCB copper foil of 30-40%, the copper content in the waste liquid and the waste water is considerable. Calculated according to ten thousand square meters of double-sided boards (the thickness of each copper foil is 35 microns), the copper content in the waste liquid and the waste water is about 4500 kilograms, and other heavy metals and noble metals are contained. The metal in the waste liquid and the waste water is discharged without being treated, which causes waste and pollutes the environment.
In the prior art, the electrolytic method is adopted for treating the PCB waste liquid to recover the copper in the PCB waste liquid, but in the prior art, the waste liquid is directly introduced into an electrolytic cell for electrolysis, a plurality of large-particle impurities in the waste liquid are not pretreated, the electrolysis efficiency is influenced, and meanwhile, the impurities in the waste liquid can pollute the environment. In addition, the copper prepared by recovery in the prior art has low purity and low utilization rate.
Disclosure of Invention
The invention aims to provide a continuous electrolytic refining process for high-purity copper. The technical problems that the purity of copper prepared by the PCB waste liquid is not high and the utilization rate is not high in the prior art are solved.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a continuous electrolytic refining process of high-purity copper, which comprises the following steps:
(1) adding concentrated sulfuric acid, pure water and an additive into a copper sulfate solution obtained after impurity removal treatment of PCB waste liquid to obtain an electrolytic solution; the raw materials for preparing the additive comprise thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin; in the electrolytic solution, the concentration of copper ions is 30-50g/L, the weight percentage concentration of concentrated sulfuric acid is 5% -10%, the concentration of thiourea is 1.5-4mg/L, the concentration of PAM is 2-5mg/L, the concentration of bone glue is 1.2-3.8mg/L, the concentration of triethanolamine is 1.5-2.5mg/L, the concentration of sodium nitrite is 1.0-2.0mg/L, and the concentration of gelatin is 2.2-4.6 mg/L;
(2) continuous electrolysis with a current density of 100-300A/m2Controlling the voltage of the single bath to be 0.4-0.8V, and obtaining the high-purity copper after the continuous electrolysis is finished.
Further, in the electrolytic solution of the step (1): the concentration of copper ions is 35-45g/l, and the weight percentage concentration of the concentrated sulfuric acid is 6% -9%.
Further, in the electrolytic solution of the step (1): the concentration of copper ions is 35g/l, and the concentration of concentrated sulfuric acid in percentage by weight is 8%.
Further, in the electrolytic solution of the step (1): the concentration of thiourea is 2-3mg/L, the concentration of PAM is 3-4mg/L, the concentration of bone glue is 2-3mg/L, the concentration of triethanolamine is 2-2.5mg/L, the concentration of sodium nitrite is 1.2-1.8mg/L, and the concentration of gelatin is 3-4 mg/L.
Further, in the step (2), the current density is controlled to 200A/m when the continuous electrolysis is performed2And controlling the voltage of the single groove to be 0.6V.
Further, in the step (2), a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte during continuous electrolysis.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
according to the continuous electrolytic refining process for high-purity copper, provided by the invention, the high-purity electrolyte is obtained by adding the impurity removal additive and continuously filtering and removing impurities of the electrolyte at high precision, and then continuous electrolysis is carried out on the electrolyte additive which is added and is beneficial to the quality of copper on electrolysis, so that the obtained high-purity copper is good in quality, high in purity and high in utilization rate.
Detailed Description
First, preparation example:
example 1:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 35g/L, the weight percentage concentration of concentrated sulfuric acid is 8%, the concentration of thiourea is 3mg/L, the concentration of PAM is 3.6mg/L, the concentration of bone glue is 2.5mg/L, the concentration of triethanolamine is 2.0mg/L, the concentration of sodium nitrite is 1.5mg/L, and the concentration of gelatin is 3.5 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 200A/m2And controlling the voltage of a single tank to be 0.6V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 2:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 50g/L, the weight percentage concentration of concentrated sulfuric acid is 5%, the concentration of thiourea is 4mg/L, the concentration of PAM is 2mg/L, the concentration of bone glue is 1.2mg/L, the concentration of triethanolamine is 2.5mg/L, the concentration of sodium nitrite is 2.0mg/L, and the concentration of gelatin is 2.2 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 100A/m2And controlling the voltage of a single tank to be 0.8V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 3:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 30g/L, the weight percentage concentration of concentrated sulfuric acid is 10%, the concentration of thiourea is 1.5mg/L, the concentration of PAM is 5mg/L, the concentration of bone glue is 3.8mg/L, the concentration of triethanolamine is 1.5mg/L, the concentration of sodium nitrite is 1.0mg/L, and the concentration of gelatin is 4.6 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 300A/m2And controlling the voltage of a single tank to be 0.4V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 4:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 40g/L, the weight percentage concentration of concentrated sulfuric acid is 7%, the concentration of thiourea is 3mg/L, the concentration of PAM is 3mg/L, the concentration of bone glue is 3mg/L, the concentration of triethanolamine is 2.2mg/L, the concentration of sodium nitrite is 1.2mg/L, and the concentration of gelatin is 4 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 250A/m2And controlling the voltage of a single tank to be 0.5V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 5:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from the PCB waste liquid in an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, and adding concentrated sulfuric acid, pure water and an additive into the filtrate to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 45g/L, the weight percentage concentration of concentrated sulfuric acid is 9%, the concentration of thiourea is 2mg/L, the concentration of PAM is 4mg/L, the concentration of bone glue is 2mg/L, the concentration of triethanolamine is 1.8mg/L, the concentration of sodium nitrite is 1.8mg/L, and the concentration of gelatin is 3 mg/L;
(2) continuous electrolysis, wherein during continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and meanwhile, the control is carried outThe current density is 150A/m2And controlling the voltage of a single tank to be 0.7V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 6:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 31g/L, the weight percentage concentration of concentrated sulfuric acid is 9%, the concentration of thiourea is 1.8mg/L, the concentration of PAM is 4.8mg/L, the concentration of bone glue is 1.5mg/L, the concentration of triethanolamine is 2.5mg/L, the concentration of sodium nitrite is 1.2mg/L, and the concentration of gelatin is 2.5 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 110A/m2And controlling the voltage of a single tank to be 0.7V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 7:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 42g/L, the weight percentage concentration of concentrated sulfuric acid is 5%, the concentration of thiourea is 4mg/L, the concentration of PAM is 2.5g/L, the concentration of bone glue is 1.2mg/L, the concentration of triethanolamine is 1.5mg/L, the concentration of sodium nitrite is 2.0mg/L, and the concentration of gelatin is 4.2 mg/L;
(2) continuous electrolysis, wherein during continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 150A/m2And controlling the voltage of a single tank to be 0.8V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 8:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 43g/L, the weight percentage concentration of concentrated sulfuric acid is 10%, the concentration of thiourea is 1.5mg/L, the concentration of PAM is 4mg/L, the concentration of bone glue is 1.5mg/L, the concentration of triethanolamine is 2.2mg/L, the concentration of sodium nitrite is 1.0mg/L, and the concentration of gelatin is 2.8 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 270A/m2And controlling the voltage of a single tank to be 0.6V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 9:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 38g/L, the weight percentage concentration of concentrated sulfuric acid is 8%, the concentration of thiourea is 2mg/L, the concentration of PAM is 4mg/L, the concentration of bone glue is 2.5mg/L, the concentration of triethanolamine is 2.5mg/L, the concentration of sodium nitrite is 2mg/L, and the concentration of gelatin is 3 mg/L;
(2) continuous electrolysis, wherein during the continuous electrolysis, a high-precision filter is adopted to continuously filter and remove impurities from the electrolyte, and the current density is controlled to be 260A/m2Control sheetThe bath voltage is 0.6V, and cathode copper with the content of more than 99.99 percent is obtained after the continuous electrolysis is finished.
Example 10:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 46g/L, the weight percentage concentration of concentrated sulfuric acid is 5%, the concentration of thiourea is 4mg/L, the concentration of PAM is 3mg/L, the concentration of bone glue is 1.2mg/L, the concentration of triethanolamine is 2.5mg/L, the concentration of sodium nitrite is 1.8mg/L, and the concentration of gelatin is 2.2 mg/L;
(2) continuous electrolysis, controlling the current density to 240A/m2And controlling the voltage of a single tank to be 0.5V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Example 11:
a continuous electrolytic refining process for high-purity copper comprises the following steps:
(1) removing impurities from PCB waste liquid by an extraction mode to obtain a copper sulfate solution, filtering to obtain a filtrate, adding concentrated sulfuric acid, pure water and an additive into the filtrate, wherein the additive is prepared from thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin to obtain an electrolytic solution;
in the electrolytic solution, the concentration of copper ions is 35g/L, the weight percentage concentration of concentrated sulfuric acid is 10%, the concentration of thiourea is 1.5mg/L, the concentration of PAM is 5mg/L, the concentration of bone glue is 3.8mg/L, the concentration of triethanolamine is 1.5mg/L, the concentration of sodium nitrite is 1.0mg/L, and the concentration of gelatin is 3.5 mg/L;
(2) continuous electrolysis, controlling the current density to be 300A/m2And controlling the voltage of a single tank to be 0.6V, and obtaining cathode copper with the content of more than 99.99 percent after the continuous electrolysis is finished.
Second, Experimental example
1. The purity content of the electrolytic cathode copper obtained in the step (2) in the examples 1 to 11 is detected by using GB/T467-2010A-level copper, and the results are shown in the following table 1:
TABLE 1 test results
| Purity of | |
| Example 1 | ≥99.9945％ |
| Example 2 | ≥99.9967％ |
| Example 3 | ≥99.9955％ |
| Example 4 | ≥99.9965％ |
| Example 5 | ≥99.9945％ |
| Example 6 | ≥99.9947％ |
| Example 7 | ≥99.9963％ |
| Example 8 | ≥99.9935％ |
| Practice ofExample 9 | ≥99.9954％ |
| Example 10 | ≥99.9966％ |
| Example 11 | ≥99.9959％ |
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (7)
1. The continuous electrolytic refining process of high-purity copper is characterized by comprising the following steps of:
(1) adding concentrated sulfuric acid, pure water and an additive into a copper sulfate solution obtained after impurity removal treatment of PCB waste liquid to obtain an electrolytic solution; the raw materials for preparing the additive comprise thiourea, PAM, bone glue, triethanolamine, sodium nitrite and gelatin; in the electrolytic solution, the concentration of copper ions is 30-50g/L, the weight percentage concentration of concentrated sulfuric acid is 5% -10%, the concentration of thiourea is 1.5-4mg/L, the concentration of PAM is 2-5mg/L, the concentration of bone glue is 1.2-3.8mg/L, the concentration of triethanolamine is 1.5-2.5mg/L, the concentration of sodium nitrite is 1.0-2.0mg/L, and the concentration of gelatin is 2.2-4.6 mg/L;
(2) continuous electrolysis with a current density of 100-300A/m2Controlling the voltage of the single bath to be 0.4-0.8V, and obtaining the high-purity copper after the continuous electrolysis is finished.
2. The continuous electrorefining process of high purity copper according to claim 1, wherein in the electrolytic solution of step (1): the concentration of copper ions is 35-45g/l, and the weight percentage concentration of the concentrated sulfuric acid is 6% -9%.
3. The continuous electrorefining process of high purity copper according to claim 2, characterized in that in the electrolytic solution of step (1): the concentration of copper ions is 35g/l, and the concentration of concentrated sulfuric acid in percentage by weight is 8%.
4. The continuous electrorefining process of high purity copper according to claim 1, wherein in the electrolytic solution of step (1): the concentration of thiourea is 2-3mg/L, the concentration of PAM is 3-4mg/L, the concentration of bone glue is 2-3mg/L, the concentration of triethanolamine is 2-2.5mg/L, the concentration of sodium nitrite is 1.2-1.8mg/L, and the concentration of gelatin is 3-4 mg/L.
5. The continuous electrorefining process of high purity copper according to claim 4, characterized in that in the electrolytic solution of step (1): the concentration of thiourea is 3mg/L, the concentration of PAM is 3.6mg/L, the concentration of bone glue is 2.5mg/L, the concentration of triethanolamine is 2.0mg/L, the concentration of sodium nitrite is 1.5mg/L, and the concentration of gelatin is 3.5 mg/L.
6. The continuous electrorefining process for high purity copper according to claim 1, wherein in the step (2), the current density is controlled to 200A/m while the continuous electrolysis is performed2And controlling the voltage of the single groove to be 0.6V.
7. The continuous electrorefining process of high purity copper according to claim 1, wherein in the step (2), the electrolyte is continuously filtered and purified by a high precision filter during continuous electrolysis.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114293227A (en) * | 2021-12-16 | 2022-04-08 | 虹华科技股份有限公司 | Processing technology of high-purity copper product for aerospace |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550488A (en) * | 2009-05-13 | 2009-10-07 | 中南大学 | Method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550488A (en) * | 2009-05-13 | 2009-10-07 | 中南大学 | Method of preparing high pure cathode copper by using PCB acid chlorine copper etching solution sewage |
Non-Patent Citations (1)
| Title |
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| 程静: "碱性蚀刻液中铜的回收", 《山东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114293227A (en) * | 2021-12-16 | 2022-04-08 | 虹华科技股份有限公司 | Processing technology of high-purity copper product for aerospace |
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Application publication date: 20211210 |