CN111910215A - Method for deeply removing trace nickel by electrodepositing cobalt - Google Patents
Method for deeply removing trace nickel by electrodepositing cobalt Download PDFInfo
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- CN111910215A CN111910215A CN202010702123.5A CN202010702123A CN111910215A CN 111910215 A CN111910215 A CN 111910215A CN 202010702123 A CN202010702123 A CN 202010702123A CN 111910215 A CN111910215 A CN 111910215A
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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
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0476—Separation of nickel from cobalt
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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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Abstract
The invention discloses a method for deeply removing trace nickel by electrodepositing cobalt, which belongs to the technical field of metal purification, and adopts chelate resin CH27 to deeply remove impurity nickel in a cobalt solution by a dynamic ion exchange method, and the electrodeposited cobalt solution is introduced into an electrodeposition tank to carry out insoluble anode electrodeposition purification, so that 99.9995 percent high-purity cobalt with the nickel content lower than 0.00002 percent is prepared. The method is suitable for deep removal of trace nickel in the electrodeposited cobalt solution, is simple in operation, good in stability, low in cost, green and environment-friendly, achieves the purpose of deep removal of nickel, meets the requirement of preparing a 5N5 high-purity cobalt product, and is beneficial to realizing large-scale industrial production of wet-process electrolysis high-purity metal.
Description
Technical Field
The invention belongs to the technical field of metal purification, and particularly relates to a method for deeply removing trace nickel by electrodepositing cobalt.
Background
The high-purity metal material is one of the key supporting materials in the high-end electronic information industry, the high-purity cobalt is an important material for preparing magnetic recording, magnetic recording magnetic heads, photoelectric devices, magnetic sensors, integrated circuits and other components, the high-purity cobalt with the purity of 99.9% -99.99% is widely applied to the manufacture of magnetic materials and super alloys, the high-purity cobalt with the purity of 99.999% is used for 90-180nm target materials for the integrated circuits, and the ultrahigh-purity cobalt with higher purity and low nickel content is mainly applied to the preparation of high-purity cobalt targets for 7nm advanced chip manufacturing processes.
Nickel in the cobalt electrodeposition liquid is one of common impurities, and the nickel is separated out along with cobalt at a cathode in the cobalt electrodeposition preparation process, so that the quality of the cobalt is influenced. The nickel impurities in the cobalt target can affect the service performance of electronic devices and mainly affect the interface performance of semiconductors. Therefore, the deep removal of the impurity Ni in the cobalt electrodeposition liquid and the improvement of the quality of the cobalt target have important significance.
With the development of the ion exchange method, the cobalt solution purification technology is developed. In the prior art, resin is adopted to remove specific metal ions, or the removal or recovery degree of other coexisting ions is not considered, or the coexisting ions are partially or slightly removed; the separation degree of the resin to specific metal ions cannot be well adjusted, the capability of well separating two or more metal ions cannot be achieved, and waste is caused to a certain degree.
At present, 701 resin and 330 resin are also reported to be used for purifying the cobalt solution, but impurity ions such as Cu, Fe, Pb, Zn and the like are preferentially removed, and the processing capacity of the cobalt solution on nickel is low. The high-purity cobalt prepared by the prior art cannot meet the requirement of a high-purity cobalt target for 7nm advanced chip manufacturing process, and the process is too complicated and complicated to operate.
Disclosure of Invention
In order to solve the problems, the invention provides a method for deeply removing trace nickel by electrodepositing cobalt, which comprises the following steps:
a) preparing an electrodeposition solution by using cobalt salt and water;
b) adjusting the pH value of the electrodeposition solution to be less than 1, and selectively removing nickel through an ion exchange column, wherein the exchange resin in the ion exchange column is chelate resin CH 27;
c) carrying out insoluble anode electrodeposition purification on the purified electrodeposition solution to obtain high-purity cobalt after electrodeposition; wherein the purity of cobalt in the high-purity cobalt is more than 99.9995 percent, and the content of nickel is less than 0.00002 percent.
In the electro-deposition solution in the step a), the concentration of cobalt ions is 40-50g/L, and the concentration of nickel is lower than 0.010 g/L.
And in the step b), the ion exchange rate is 2.0-3.0BV/h, and the nickel content in the solution is reduced to be lower than 0.001g/L after the resin exchange is finished.
The electro-deposition purification temperature of the insoluble anode in the step c) is 40-50 ℃, and the current density is 20-30A/m2The voltage is 0.8-1.0V.
The insoluble anode material in the step c) is a titanium-coated iridium electrode, a titanium-coated ruthenium electrode or a titanium-coated ruthenium iridium electrode, and the cathode material is a titanium plate.
The invention has the beneficial effects that:
1. the invention adopts chelate resin CH27 as the exchange resin of the ion exchange column, selectively removes Ni in the electrolyte, prepares high-purity cobalt with the cobalt purity of more than 99.9995 percent and the nickel content of less than 0.00002 percent, and meets the requirement of preparing 5N5 high-purity cobalt products.
2. The method can remove trace Ni with the content lower than 0.010g/L in the electrolyte, achieves the aim of deep nickel removal, and overcomes the defect of low cobalt purity caused by the residual Ni content in the prior art.
3. According to the invention, the pH value of the electrodeposition liquid is adjusted to be less than 1, the CH27 resin has high affinity to nickel and has no influence on cobalt ions, the nickel content in the solution is reduced to be lower than 0.001g/L after the resin exchange is finished, the main ion cobalt is hardly adsorbed, the loss of cobalt is less, the cobalt-nickel separation and cobalt purification processes are highly realized, and the industrial production is facilitated.
4. The method is simple to operate and low in cost, and can realize large-scale industrial production of the high-purity metal by wet electrolysis.
Detailed Description
The present invention is further illustrated in detail by the following specific examples: the invention provides a method for deeply removing trace nickel by electrodepositing cobalt, and the content of the invention is further detailed by combining with an example.
Example 1
2L of cobalt deposition solution with the cobalt ion concentration of 40g/L is prepared, the nickel content is 0.005g/L, the cobalt deposition solution passes through an ion exchange column filled with 1LCH27 chelating resin, the exchange rate with the resin is controlled to be 2.5BV/h, and the nickel content in the purified cobalt deposition solution is 0.001 g/L. Selecting titanium-coated ruthenium iridium electrode to carry out insoluble anode electrolysis, adjusting the pH value of cobalt deposition liquid to 0.8, the temperature to 45 ℃, and the current density to 20A/m2And the voltage is 0.9V, 99.9996 percent of high-purity cobalt with the nickel content of 0.000015 percent is prepared. In order to further determine the purity of the high-purity cobalt product, the content of each element is determined, the determination result is shown in table 1, the content of other impurities is far lower than the application standard, and the prepared high-purity cobalt can be applied to the fine processing aspects such as high-purity cobalt targets in the field of magnetron sputtering.
TABLE 1 determination of the elemental content of the high purity cobalt obtained in example 1
Example 2
Preparing cobalt with cobalt ion concentration of 50g/L2L of the deposition solution, wherein the nickel content is 0.010g/L, the deposition solution passes through an ion exchange column filled with 1LCH27 chelating resin, the exchange rate with the resin is controlled to be 2.0BV/h, and the nickel content in the purified cobalt deposition solution is 0.0008 g/L. Taking a titanium-coated iridium electrode as an anode and a titanium plate as a cathode, carrying out insoluble anode electrolysis, adjusting the pH value of the cobalt deposition solution to 0.5, the temperature to 40 ℃, and the current density to 30A/m2And the voltage is 0.8V, 99.99953 percent of high-purity cobalt with the nickel content of 0.000012 percent is obtained.
Example 3
2L of cobalt sediment liquid with the cobalt ion concentration of 45g/L is prepared, the nickel content is 0.006g/L, the cobalt sediment liquid passes through an ion exchange column filled with 1LCH27 chelating resin, the exchange rate with the resin is controlled to be 3.0BV/h, and the nickel content in the purified cobalt sediment liquid is 0.0005 g/L. Taking a titanium-coated ruthenium electrode as an anode and a titanium plate as a cathode, carrying out insoluble anode electrolysis, adjusting the pH value of the cobalt deposition solution to 0.1, the temperature to 50 ℃, and the current density to 25A/m2And the voltage is 1.0V, 99.99951 percent of high-purity cobalt with the nickel content of 0.000010 percent is prepared.
Claims (5)
1. A method for deeply removing trace nickel by electrodepositing cobalt is characterized by comprising the following steps:
a) preparing an electrodeposition solution by using cobalt salt and water;
b) adjusting the pH value of the electrodeposition solution to be less than 1, and selectively removing nickel through an ion exchange column, wherein the exchange resin in the ion exchange column is chelate resin CH 27;
c) carrying out insoluble anode electrodeposition purification on the purified electrodeposition solution to obtain high-purity cobalt after electrodeposition; wherein the purity of cobalt in the high-purity cobalt is more than 99.9995 percent, and the content of nickel is less than 0.00002 percent.
2. The method of claim 1 wherein the electrodeposition solution of step a) has a cobalt ion concentration of 40 to 50g/L and a nickel concentration of less than 0.010 g/L.
3. The method as claimed in claim 1, wherein in the step b), the ion exchange rate is 2.0 to 3.0BV/h, and the nickel content in the solution is reduced to less than 0.001g/L after the resin exchange is completed.
4. The method as claimed in claim 1, wherein the insoluble anode electrodeposition purification temperature of step c) is 40-50 ℃ and the current density is 20-30A/m2The voltage is 0.8-1.0V.
5. The method of claim 1, wherein the insoluble anode material of step c) is a titanium-coated iridium electrode, a titanium-coated ruthenium electrode or a titanium-coated ruthenium iridium electrode, and the cathode material is a titanium plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010702123.5A CN111910215A (en) | 2020-07-21 | 2020-07-21 | Method for deeply removing trace nickel by electrodepositing cobalt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010702123.5A CN111910215A (en) | 2020-07-21 | 2020-07-21 | Method for deeply removing trace nickel by electrodepositing cobalt |
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| CN111910215A true CN111910215A (en) | 2020-11-10 |
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| CN202010702123.5A Pending CN111910215A (en) | 2020-07-21 | 2020-07-21 | Method for deeply removing trace nickel by electrodepositing cobalt |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538721A (en) * | 2009-03-19 | 2009-09-23 | 金川集团有限公司 | Method for preparing high-purity cobalt |
| CN104862479A (en) * | 2015-04-23 | 2015-08-26 | 金川集团股份有限公司 | Deep purification and nickel removal method for cobalt chloride solutions |
| CN105154672A (en) * | 2015-09-08 | 2015-12-16 | 有研亿金新材料有限公司 | Method for removing nickel ions in cobalt chloride solution |
| CN108560020A (en) * | 2018-05-21 | 2018-09-21 | 金川集团股份有限公司 | A method of preparing ultra-pure cobalt plate |
-
2020
- 2020-07-21 CN CN202010702123.5A patent/CN111910215A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538721A (en) * | 2009-03-19 | 2009-09-23 | 金川集团有限公司 | Method for preparing high-purity cobalt |
| CN104862479A (en) * | 2015-04-23 | 2015-08-26 | 金川集团股份有限公司 | Deep purification and nickel removal method for cobalt chloride solutions |
| CN105154672A (en) * | 2015-09-08 | 2015-12-16 | 有研亿金新材料有限公司 | Method for removing nickel ions in cobalt chloride solution |
| CN108560020A (en) * | 2018-05-21 | 2018-09-21 | 金川集团股份有限公司 | A method of preparing ultra-pure cobalt plate |
Non-Patent Citations (1)
| Title |
|---|
| 翟秀静: "《重金属冶金学》", 30 June 2019, 北京冶金工业出版社 * |
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Address after: 100088 No.2 xinwai street, Xicheng District, Beijing Applicant after: China Youyan Technology Group Co.,Ltd. Address before: 100088 No.2 xinwai street, Xicheng District, Beijing Applicant before: Youyan Technology Group Co.,Ltd. |
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