CN109306405B - Method for industrially producing 6N ultra-pure copper - Google Patents

Method for industrially producing 6N ultra-pure copper Download PDF

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CN109306405B
CN109306405B CN201811267334.XA CN201811267334A CN109306405B CN 109306405 B CN109306405 B CN 109306405B CN 201811267334 A CN201811267334 A CN 201811267334A CN 109306405 B CN109306405 B CN 109306405B
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ion exchange
copper
copper sulfate
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陈东升
邵志成
邵帅
杨彦春
王栓
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Henan Guoxi Super Pure New Material Co ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • C22B15/0086—Treating solutions by physical methods
    • 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
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention provides a method for industrially producing 6N ultra-pure copper, which comprises the steps of adsorbing copper ions by SuCu inorganic ion exchange resin with high selectivity on the copper ions, eluting other unadsorbed metal ions by deionized water, desorbing the copper ions by using a sulfuric acid solution to obtain an ultra-pure copper sulfate solution, and finally electrolyzing and vacuum casting to obtain the 6N ultra-pure copper. The SuCu inorganic ion exchange resin is used, so that the adsorption rate of copper ions can be improved, the production efficiency and the product percent of pass are improved, and the product percent of pass of the obtained 6N ultra-pure copper is more than 95%. The method has simple production process, can obtain the ultra-pure copper with the purity higher than 6N only by one electrolysis process, and can reduce energy consumption, thereby greatly reducing the cost.

Description

Method for industrially producing 6N ultra-pure copper
Technical Field
The invention belongs to the field of metal purification, and particularly relates to a method for industrially producing 6N ultra-pure copper.
Background
The metal copper is one of the metals widely used by nonferrous metals, and with the continuous progress and development of the industry, people have greater and greater demand on the metal copper, particularly on high-purity and ultra-pure metal copper.
Generally, copper with purity of 4N (99.99%) to 5N (99.999%) is defined as high-purity copper, and copper with purity higher than 6N (99.9999%) is ultra-pure copper. When the purity of the copper is higher than 6N, the heat conduction and the electric conduction of the copper are greatly improved, and the ultra-pure copper has low softening temperature and good ductility, so that the quality of electronic products can be improved by utilizing the ultra-pure copper. In the microelectronics industry, ultrapure copper can completely replace the use of gold (e.g., bond wires).
At present, the production of the ultra-pure copper mainly adopts a zone melting method, a secondary (or tertiary) electrolysis method and a reduction method production process. The zone melting method has low production efficiency and is difficult to form large-scale production capacity; the secondary electrolysis method relates to two dissolving processes of sulfuric acid and nitric acid, needs two or even three times of electrolysis, has complex production process and low product qualification rate (generally between 65 and 75 percent); the production process of the reduction method is also complex, hydrogen is used for reduction in the production process, and the production safety problem is prominent. All the three methods for producing the ultra-pure copper have the defects of high energy consumption and complex production process, so that the ultra-pure copper has high price and is greatly limited in industrial application.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for industrially producing 6N ultra-pure copper. The method provided by the invention can improve the production efficiency and the product qualification rate of 6N ultra-pure copper, and can reduce energy consumption, thereby reducing the cost and making the use of ultra-pure copper to replace copper elements in more fields possible.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for industrially producing 6N ultra-pure copper comprises the following steps:
(1) dissolving anhydrous copper sulfate in water to obtain a copper sulfate solution, and adjusting the pH value of the copper sulfate solution to 4-5.5;
(2) pumping the copper sulfate solution with the pH value adjusted in the step (1) from the bottom of the ion exchange column until the ion exchange tree column is saturated and adsorbed; the ion exchange column is filled with SuCu inorganic ion exchange resin;
(3) washing the saturated and adsorbed ion exchange column in the step (2) by water, and then pumping a sulfuric acid solution from the bottom of the ion exchange column to desorb copper sulfate from the ion exchange column to obtain a copper sulfate desorption solution;
(4) electrolyzing the copper sulfate desorption solution to obtain an electrolytic copper plate;
(5) and carrying out vacuum casting on the electrolytic copper plate to obtain 6N ultra-pure copper.
Preferably, the mass concentration of the copper sulfate solution obtained by dissolving anhydrous copper sulfate in water in the step (1) is 5-10 g/L.
Preferably, the pH regulator for regulating the pH value of the copper sulfate solution in the step (1) is a sulfuric acid solution or a sodium hydroxide solution.
Preferably, the nucleus of the SuCu inorganic ion exchange resin in the step (2) is silica gel, and the active molecules are polyethylene polyamine molecules grafted with pyridine functional groups; the crosslinking degree of the SuCu inorganic ion exchange resin is 40-50%; the particle size of the SuCu inorganic ion exchange resin is 4-100 meshes; the average adsorption capacity of the SuCu inorganic ion exchange resin is 19.7-23.1 g/mol.
Preferably, the amount of the SuCu inorganic type ion exchange resin used in the step (2) is 0.07m 3.
Preferably, the ion exchange column in the step (2) comprises a first ion exchange column and a second ion exchange column which are adsorbed in series.
Preferably, the pumping pressure of the copper sulfate solution in the step (2) is 1-1.2 MPa, and the flow rate is 6 column volumes per hour.
Preferably, the pumping pressure of the sulfuric acid solution in the step (3) is 1-1.2 MPa, the flow rate is 4 column volumes per hour, and the mass concentration of the sulfuric acid solution is 25-35%.
Preferably, the voltage of the electrolysis in the step (4) is 2V, and the current density is 300A/m2。
Preferably, the rated temperature of vacuum casting in the step (5) is 1700 ℃, the melting rate of vacuum casting is 120kg/h, and the vacuum degree of vacuum casting is 6.7 × 10-1Pa。
The invention provides a method for industrially producing 6N ultra-pure copper, which comprises the steps of adsorbing copper ions by SuCu inorganic ion exchange resin with high selectivity on the copper ions, eluting other unadsorbed metal ions by deionized water, desorbing the copper ions by using a sulfuric acid solution to obtain an ultra-pure copper sulfate solution, and finally electrolyzing and vacuum casting to obtain the 6N ultra-pure copper. The SuCu inorganic ion exchange resin is used, so that the adsorption rate of copper ions can be improved, the production efficiency and the product percent of pass are improved, and the product percent of pass of the obtained 6N ultra-pure copper is more than 95%. The method has simple production process, can obtain the ultra-pure copper with the purity higher than 6N only by one electrolysis process, and can reduce energy consumption, thereby greatly reducing the cost.
Detailed Description
The invention provides a method for industrially producing 6N ultra-pure copper, which comprises the following steps:
(1) dissolving anhydrous copper sulfate in water to obtain a copper sulfate solution, and adjusting the pH value of the copper sulfate solution to 4-5.5;
(2) pumping the copper sulfate solution with the pH value adjusted in the step (1) from the bottom of the ion exchange column until the ion exchange tree column is saturated and adsorbed; the ion exchange column is filled with SuCu inorganic ion exchange resin;
(3) washing the saturated and adsorbed ion exchange column in the step (2) by water, and then pumping a sulfuric acid solution from the bottom of the ion exchange column to desorb copper sulfate from the ion exchange column to obtain a copper sulfate desorption solution;
(4) electrolyzing the copper sulfate desorption solution to obtain an electrolytic copper plate;
(5) and carrying out vacuum casting on the electrolytic copper plate to obtain 6N ultra-pure copper.
The invention dissolves anhydrous copper sulfate in water to obtain copper sulfate solution. In the invention, the mass concentration of the copper sulfate solution is preferably 5-10 g/L, and more preferably 6-8 g/L. The invention preferably dissolves the anhydrous copper sulfate under the condition of stirring, has no requirement on stirring operation, and can completely dissolve the anhydrous copper sulfate.
After the copper sulfate solution is obtained, the pH value of the copper sulfate solution is adjusted to 4-5.5. In the present invention, the pH adjuster that adjusts the pH of the copper sulfate solution is preferably a sulfuric acid solution or a sodium hydroxide solution, and the concentration of the sulfuric acid solution or the sodium hydroxide solution is preferably 10%.
After the pH value of the copper sulfate solution is adjusted, the copper sulfate solution with the adjusted pH value is pumped from the bottom of an ion exchange column until the ion exchange tree column is saturated and adsorbed, wherein the ion exchange column is an ion exchange column filled with SuCu inorganic type ion exchange resin. In the present invention, the ion exchange column preferably comprises a first ion exchange column and a second ion exchange column adsorbed in series; the present invention also preferably includes a third, spare ion exchange column, preferably in series with the first and second ion exchange columns, preferably in place of the failed ion exchange column when either the first or second ion exchange column fails. In the invention, the pumping pressure of the copper sulfate solution is preferably 1-1.2 MPa, more preferably 1.05-1.1 MPa, and the flow rate is preferably 6 column volumes/hour.
In the invention, the base nucleus of the SuCu inorganic ion exchange resin is preferably silica gel, and the active molecule is preferably polyethylene polyamine molecule grafted with pyridine functional groups; the crosslinking degree of the SuCu inorganic ion exchange resin is preferably 40-50%, and more preferably 42-48%; the particle size of the SuCu inorganic ion exchange resin is preferably 4-100 meshes, and more preferably 20-80 meshes; the average adsorption capacity of the SuCu inorganic ion exchange resin is preferably 19.7-23.1 g/mol, and more preferably 21-22.5 g/mol. In the present invention, the amount of the SuCu inorganic type ion exchange resin used is preferably 0.07m 3. In the present invention, the SuCu inorganic type ion exchange resin has high selectivity for copper ions, and can adsorb copper ions in an ion exchange column. In a specific embodiment of the present invention, it is preferable to use a SuCu inorganic type ion exchange resin manufactured by environmental protection technologies, Inc. of Loyang Dingli.
After the ion exchange tree column is saturated and adsorbed, the saturated and adsorbed ion exchange column is washed by water. The present invention preferably uses deionized water for cleaning. The invention has no specific requirement on the cleaning frequency, and can elute trace amount of other unadsorbed metal ions.
After the ion exchange column is washed by water, the invention pumps the sulfuric acid solution from the bottom of the ion exchange column to desorb the copper sulfate from the ion exchange column, thus obtaining the copper sulfate desorption solution. In the invention, the mass concentration of the sulfuric acid solution is preferably 25-35%, more preferably 28-32%, the pumping pressure of the sulfuric acid solution is preferably 1-1.2 MPa, more preferably 1.05-1.1 MPa, and the flow rate is preferably 4 column volumes/hour.
After the copper sulfate desorption solution is obtained, the invention carries out electrolysis on the copper sulfate desorption solution to obtain the electrolytic copper plate. The invention preferably uses a cyclone electrolyzer to desorb the copper sulfateThe liquid is electrolyzed. In the present invention, the voltage of the electrolysis is preferably 2V, and the current density is preferably 300A/m2。
After the electrolytic copper plate is obtained, the electrolytic copper plate is subjected to vacuum casting to obtain 6N ultra-pure copper. In the invention, the rated temperature of the vacuum casting is preferably 1700 ℃, the melting rate of the vacuum casting is preferably 120kg/h, and the vacuum degree of the vacuum casting is preferably 6.7 x 10-1Pa. In the invention, the total power of the vacuum casting equipment is preferably 360kW, and the rated power is preferably 250 kW; the power voltage of the vacuum casting is preferably 380V, and the rated voltage is preferably 375V; the power frequency of the vacuum casting is preferably 50Hz, and the rated frequency is preferably 1000 Hz.
After the vacuum casting is finished, the invention preferably performs inspection operation on the vacuum casting product. The purity of the vacuum casting product is preferably checked, when the purity is higher than 99.9999%, the vacuum casting product is a qualified 6N ultrapure copper product, and when the purity is lower than 99.9999%, the vacuum casting product is an unqualified 6N ultrapure copper product; the invention has no specific requirements on the detection mode, and the detection mode well known in the field can be used; after the inspection is completed, the present invention preferably packages 6N ultra pure copper.
The method for industrially producing 6N ultra-pure copper according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The 6N ultra-pure copper is industrially produced by the following method:
(1) dissolving 50kg of anhydrous copper sulfate in 5000L of deionized water to obtain 10g/L of copper sulfate solution, and then adjusting the pH value of the copper sulfate solution to be 4 by using a sulfuric acid solution;
(2) 0.07m3Filling SuCu inorganic ion exchange resin in an ion exchange column, pumping the copper sulfate solution prepared in the step (1) from the bottom of the ion exchange column, and reversely flowing until the ion exchange tree column is saturated and adsorbed, wherein the pumping pressure of the copper sulfate solution is 1MPa, and the flow rate is 6 column volumes/hour;
(3) washing the ion exchange column obtained in the step (2) by using deionized water, pumping 1000L of sulfuric acid solution with the mass concentration of 25% from the bottom of the ion exchange column, and removing copper sulfate adsorbed on the ion exchange column to obtain copper sulfate desorption solution, wherein the pumping pressure of the sulfuric acid solution is 1MPa, and the flow rate is 4 column volumes per hour;
(4) adding the copper sulfate desorption solution into a cyclone electrolyzer for electrolysis, stripping an electrolytic copper plate from the cathode of the cyclone electrolyzer after the electrolysis is finished, wherein the voltage of the electrolysis is 2V, and the current density is 300A/m2；
(5) Vacuum casting the electrolytic copper plate to obtain 6N ultra-pure copper, wherein the rated temperature of the vacuum casting is 1700 ℃, the melting rate is 120kg/h, and the vacuum degree is 6.7 multiplied by 10-1Pa。
The inspection proves that the product percent of pass of the 6N ultra-pure copper is 95.5 percent.
Example 2
The 6N ultra-pure copper is industrially produced by the following method:
(1) dissolving 50kg of anhydrous copper sulfate in 10000L of deionized water to obtain 5g/L of copper sulfate solution, and then adjusting the pH value of the copper sulfate solution to be 5 by using a sodium hydroxide solution;
(2) 0.07m3Filling SuCu inorganic ion exchange resin in an ion exchange column, pumping the copper sulfate solution prepared in the step (1) from the bottom of the ion exchange column, and reversely flowing until the ion exchange tree column is saturated and adsorbed, wherein the pumping pressure of the copper sulfate solution is 1MPa, and the flow rate is 6 column volumes/hour;
(3) washing the ion exchange column obtained in the step (2) by using deionized water, pumping 1000L of sulfuric acid solution with the mass concentration of 30% from the bottom of the ion exchange column, and removing copper sulfate adsorbed on the ion exchange column to obtain copper sulfate desorption solution, wherein the pumping pressure of the sulfuric acid solution is 1MPa, and the flow rate is 4 column volumes per hour;
(4) adding the copper sulfate desorption solution into a cyclone electrolyzer for electrolysis, stripping an electrolytic copper plate from the cathode of the cyclone electrolyzer after the electrolysis is finished, wherein the voltage of the electrolysis is 2V, and the current density is 300A/m2；
(5) Vacuum casting the electrolytic copper plate to obtain 6N ultra-pure copper,wherein the rated temperature of vacuum casting is 1700 ℃, the melting rate is 120kg/h, and the vacuum degree is 6.7 multiplied by 10-1Pa。
The inspection proves that the product percent of pass of the 6N ultra-pure copper is 95.1 percent.
Example 3
The 6N ultra-pure copper is industrially produced by the following method:
(1) dissolving 75kg of anhydrous copper sulfate in 10000L of deionized water to obtain 7.5g/L of copper sulfate solution, and then adjusting the pH value of the copper sulfate solution to be 5.5 by using a sulfuric acid solution;
(2) 0.07m3Filling SuCu inorganic ion exchange resin in an ion exchange column, pumping the copper sulfate solution prepared in the step (1) from the bottom of the ion exchange column, and reversely flowing until the ion exchange tree column is saturated and adsorbed, wherein the pumping pressure of the copper sulfate solution is 1MPa, and the flow rate is 6 column volumes/hour;
(3) washing the ion exchange column obtained in the step (2) by using deionized water, pumping 1000L of sulfuric acid solution with the mass concentration of 35% from the bottom of the ion exchange column, and removing copper sulfate adsorbed on the ion exchange column to obtain copper sulfate desorption solution, wherein the pumping pressure of the sulfuric acid solution is 1MPa, and the flow rate is 4 column volumes per hour;
(4) adding the copper sulfate desorption solution into a cyclone electrolyzer for electrolysis, stripping an electrolytic copper plate from the cathode of the cyclone electrolyzer after the electrolysis is finished, wherein the voltage of the electrolysis is 2V, and the current density is 300A/m2；
(5) Vacuum casting the electrolytic copper plate to obtain 6N ultra-pure copper, wherein the rated temperature of the vacuum casting is 1700 ℃, the melting rate is 120kg/h, and the vacuum degree is 6.7 multiplied by 10-1Pa。
The inspection proves that the product percent of pass of the 6N ultra-pure copper is 95.4 percent.
Comparative example
1 ton of 6N ultrapure copper is produced by using a zone melting method, a secondary electrolysis method and a reduction method respectively, and the method of the embodiment 1 of the invention, the production time, the production cost and the product yield of the zone melting method, the secondary electrolysis method and the reduction method are counted respectively, and the obtained results are listed in Table 1.
TABLE 1 comparison of production efficiency and cost for the main production process for producing 1 ton of 6N ultrapure copper
Figure BDA0001845196420000061
Figure BDA0001845196420000071
As can be seen from the data in Table 1, the time required for producing 1 ton of 6N copper is significantly reduced and the product yield is significantly improved, as compared with the zone melting method, the secondary electrolysis method and the reduction method. In summary, the method of the invention can obviously reduce the production cost of the ultra-pure copper, make the substitution of the ultra-pure copper for copper components in more fields possible, and is beneficial to the development of high-end manufacturing industry.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. A method for industrially producing 6N ultra-pure copper comprises the following steps:
(1) dissolving anhydrous copper sulfate in water to obtain a copper sulfate solution, and adjusting the pH value of the copper sulfate solution to 4-5.5;
(2) pumping the copper sulfate solution with the pH value adjusted in the step (1) from the bottom of the ion exchange column until the ion exchange tree column is saturated and adsorbed; the ion exchange column is filled with SuCu inorganic ion exchange resin; the SuCu inorganic ion exchange resin is characterized in that a basal nucleus is silica gel, and active molecules are polyethylene polyamine molecules grafted with pyridine functional groups; the crosslinking degree of the SuCu inorganic ion exchange resin is 40-50%; the particle size of the SuCu inorganic ion exchange resin is 4-100 meshes; the average adsorption capacity of the SuCu inorganic ion exchange resin is 19.7-23.1 g/mol;
(3) washing the saturated and adsorbed ion exchange column in the step (2) by water, and then pumping a sulfuric acid solution from the bottom of the ion exchange column to desorb copper sulfate from the ion exchange column to obtain a copper sulfate desorption solution; the mass concentration of the sulfuric acid solution is 25-35%;
(4) electrolyzing the copper sulfate desorption solution to obtain an electrolytic copper plate;
(5) carrying out vacuum casting on the electrolytic copper plate to obtain 6N ultra-pure copper; the rated temperature of the vacuum casting is 1700 ℃, the melting rate of the vacuum casting is 120kg/h, and the vacuum degree of the vacuum casting is 6.7 multiplied by 10-1Pa。
2. The method as claimed in claim 1, wherein the mass concentration of the copper sulfate solution obtained after dissolving anhydrous copper sulfate in water in the step (1) is 5-10 g/L.
3. The method as claimed in claim 1 or 2, wherein the pH regulator for regulating the pH of the copper sulfate solution in the step (1) is a sulfuric acid solution or a sodium hydroxide solution.
4. The process according to claim 1, wherein the amount of the SuCu inorganic type ion exchange resin used in the step (2) is 0.07m3。
5. The method of claim 1, wherein the ion exchange column in step (2) comprises a first ion exchange column and a second ion exchange column adsorbed in series.
6. The method according to claim 1, wherein the pumping pressure of the copper sulfate solution in the step (2) is 1 to 1.2MPa, and the flow rate is 6 column volumes/hour.
7. The method according to claim 1, wherein the sulfuric acid solution in the step (3) is pumped at a pressure of 1 to 1.2MPa and a flow rate of 4 column volumes/hour.
8. Root of herbaceous plantThe method as claimed in claim 1, wherein the voltage of the electrolysis in the step (4) is 2V, and the current density is 300A/m2。
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Denomination of invention: A method for industrial production of 6N ultra pure copper

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