CN111057981A - Low-purity copper rod purification method - Google Patents
Low-purity copper rod purification method Download PDFInfo
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- CN111057981A CN111057981A CN201911294286.8A CN201911294286A CN111057981A CN 111057981 A CN111057981 A CN 111057981A CN 201911294286 A CN201911294286 A CN 201911294286A CN 111057981 A CN111057981 A CN 111057981A
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- copper rod
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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Abstract
The invention belongs to the technical field of copper rod purification, and particularly relates to a low-purity copper rod purification method, which comprises the following specific purification steps: s1: primary heat treatment: placing the copper rod in an electrically heated container, connecting an external suction pump to the electrically heated container, vacuumizing the electrically heated container, starting an electrical heating assembly in the electrically heated container to heat the copper rod to 190-210 ℃, continuously heating at the temperature, and taking out the copper rod subjected to preliminary heat treatment; s2: carrying out heat treatment again; s3: repelling anions in oxygen to the surface of the copper rod; s4: and (5) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen, thereby improving the product quality and purity of the copper rod.
Description
Technical Field
The invention relates to the technical field of copper rod purification, in particular to a low-purity copper rod purification method.
Background
The electrolytic copper is generally used for production, and the resistivity is lower than that of the low-oxygen copper rod, so that the oxygen-free copper rod is more economic in the production of products with strict requirements on resistance; the manufacturing of oxygen-free copper rods requires raw materials with higher quality; oxygen-free copper rods appear to be even more advantageous when drawing copper wire with a diameter of <0.5 mm. The 6MM oxygen-free copper rod is used for producing a copper flat wire.
After the copper rod is produced, due to the problems of product batches and different technical parameters, the oxygen content in the copper rod is easily different, so that the product quality of the copper rod is influenced.
Disclosure of Invention
The invention aims to provide a low-purity copper rod purification method, which aims to solve the problem that after copper rods are produced, the quality of the copper rods is affected due to different oxygen contents in the copper rods caused by different product batches and different technical parameters.
In order to achieve the purpose, the invention provides the following technical scheme: a low-purity copper rod purification method comprises the following specific purification steps:
s1: primary heat treatment: placing the copper rod in an electrically heated container, connecting an external suction pump to the electrically heated container, vacuumizing the electrically heated container, starting an electrical heating assembly in the electrically heated container to heat the copper rod to 190-210 ℃, continuously heating at the temperature, and taking out the copper rod subjected to preliminary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, and heating the copper rod to ensure that the temperature of the copper rod is heated to 500-600 ℃;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: acid washing to remove anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
Preferably, the temperature at which the copper rod is heated in the step S1 is 195-205 ℃.
Preferably, the temperature at which the copper rod is heated in step S1 is 200 ℃.
Preferably, the copper rod is heated in step S1, and the heating time is 30 min.
Preferably, the diameter of the copper rod is set to 7 to 9 mm.
Preferably, the temperature of the copper rod in the step S2 is heated to 550 ℃, and then the copper rod is subjected to heat preservation for 20-30 min.
Preferably, the direct current introduced in step S3 is supplied from a 12V battery, and the 12V battery is connected in series with the copper rod through a lead.
Compared with the prior art, the invention has the beneficial effects that:
1) impurity anions are discharged, and the product quality of the copper rod is remarkably improved;
2) after processing, the oxygen content of each batch of copper rods is close, and the product quality and purity of the copper rods are improved.
Drawings
FIG. 1 is a flow diagram of the purification process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution: a low-purity copper rod purification method comprises the following specific purification steps:
s1: primary heat treatment: placing the copper rod in an electrically heated container, connecting an external suction pump to the electrically heated container, vacuumizing the electrically heated container, starting an electrical heating assembly in the electrically heated container to heat the copper rod to 190-210 ℃, continuously heating at the temperature, and taking out the copper rod subjected to preliminary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, and heating the copper rod to ensure that the temperature of the copper rod is heated to 500-600 ℃;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: removing anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
Further, the temperature at which the copper rod is heated in step S1 is 195-.
Further, the temperature at which the copper rod is heated in step S1 is 200 degrees celsius.
Further, the copper rod is heated in step S1, and the heating is continued for 30 min.
Further, the diameter of the copper rod was set to 7 to 9 mm.
Further, in the step S2, the temperature of the copper rod is heated to 550 ℃, and then the copper rod is subjected to heat preservation for 20-30 min.
Further, the dc power supplied in step S3 is supplied from a 12V battery, and the 12V battery is connected in series to the copper rod via a lead.
The first embodiment is as follows:
the specific purification steps of the low-purity copper rod purification method are as follows:
s1: primary heat treatment: placing a copper rod in an electrically heated container, setting the diameter of the copper rod to be 7mm, connecting a suction pump to the electrically heated container externally, vacuumizing the electrically heated container, starting an electric heating assembly in the electrically heated container, heating the copper rod at 195 ℃, continuously heating at the temperature, heating the copper rod for 30min, and taking out the copper rod after primary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, heating the copper rod to enable the temperature of the copper rod to be 500 ℃, and carrying out heat preservation treatment on the copper rod for 20 min;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, connecting the 12V storage battery and the copper rod in series through a lead by using the 12V storage battery as a power supply through the introduced direct current, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: removing anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
Example two:
the specific purification steps of the low-purity copper rod purification method are as follows:
s1: primary heat treatment: placing a copper rod in an electrically heated container, setting the diameter of the copper rod to be 8mm, connecting a suction pump to the electrically heated container externally, vacuumizing the electrically heated container, starting an electric heating assembly in the electrically heated container, heating the copper rod at 200 ℃, continuously heating at the temperature, heating the copper rod for 30min, and taking out the copper rod after primary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, heating the copper rod to the temperature of 550 ℃, and carrying out heat preservation treatment on the copper rod for 25 min;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, connecting the 12V storage battery and the copper rod in series through a lead by using the 12V storage battery as a power supply through the introduced direct current, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: removing anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
Example three:
the specific purification steps of the low-purity copper rod purification method are as follows:
s1: primary heat treatment: placing a copper rod in an electrically heated container, setting the diameter of the copper rod to be 9mm, externally connecting a suction pump to the electrically heated container, vacuumizing the electrically heated container, starting an electric heating assembly in the electrically heated container, heating the copper rod at 205 ℃, continuously heating at the temperature, heating the copper rod for 30min, and taking out the copper rod after primary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, heating the copper rod to enable the temperature of the copper rod to be 600 ℃, and carrying out heat preservation treatment on the copper rod for 30 min;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, connecting the 12V storage battery and the copper rod in series through a lead by using the 12V storage battery as a power supply through the introduced direct current, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: removing anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
The copper rods processed in the three embodiments are detected, and the detection result is obtained: the purity of the three copper rods reaches 99.9999 percent.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A low-purity copper rod purification method is characterized in that: the specific purification steps of the low-purity copper rod purification method are as follows:
s1: primary heat treatment: placing the copper rod in an electrically heated container, connecting an external suction pump to the electrically heated container, vacuumizing the electrically heated container, starting an electrical heating assembly in the electrically heated container to heat the copper rod to 190-210 ℃, continuously heating at the temperature, and taking out the copper rod subjected to preliminary heat treatment;
s2: and (4) secondary heat treatment: filling nitrogen-argon mixed gas into the electrically heated container in the step S1, then starting an electric heating assembly of the electrically heated container, and heating the copper rod to ensure that the temperature of the copper rod is heated to 500-600 ℃;
s3: repelling anions in oxygen to the copper rod surface: introducing direct current into the copper rod, and repelling anions in oxygen onto the surface of the copper rod under the driving action of the direct current;
s4: removing anions in oxygen on the surface of the copper rod: and (4) introducing a nitrogen-hydrogen mixed gas into the copper rod treated in the step S3, and removing oxygen ions on the surface of the copper rod by using a method of combining hydrogen and oxygen.
2. The purification method of the low-purity copper rod as claimed in claim 1, wherein the purification method comprises the following steps: the temperature at which the copper rod is heated in the step S1 is 195-205 ℃.
3. The purification method of the low-purity copper rod as claimed in claim 2, wherein: the temperature at which the copper rod is heated in the step S1 is 200 ℃.
4. The purification method of the low-purity copper rod as claimed in claim 1, wherein the purification method comprises the following steps: in the step S1, the copper rod is heated, and the heating time is 30 min.
5. The purification method of the low-purity copper rod as claimed in claim 1, wherein the purification method comprises the following steps: the diameter of the copper rod is set to 7-9 mm.
6. The purification method of the low-purity copper rod as claimed in claim 1, wherein the purification method comprises the following steps: and in the step S2, the temperature of the copper rod is heated to 550 ℃, and then the copper rod is subjected to heat preservation for 20-30 min.
7. The purification method of the low-purity copper rod as claimed in claim 1, wherein the purification method comprises the following steps: the direct current introduced in the step S3 uses a 12V storage battery as a power supply, and the 12V storage battery and the copper rod are connected in series through a lead.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007046102A (en) * | 2005-08-09 | 2007-02-22 | Furukawa Electric Co Ltd:The | Oxygen-free copper wire with low-temperature softening property, and its manufacturing method |
CN102312184A (en) * | 2011-08-29 | 2012-01-11 | 杭州富通昭和铜业有限公司 | Method for producing bright and oxygen-free copper rod |
CN108962860A (en) * | 2018-08-15 | 2018-12-07 | 芜湖长润特种铜线有限公司 | A kind of preparation method of resistance to oxidation bonding brass wire material |
CN109465414A (en) * | 2018-12-28 | 2019-03-15 | 江阴华瑞电工科技股份有限公司 | A method of preparing oxygen-free copper bar |
CN110382743A (en) * | 2017-06-01 | 2019-10-25 | 三菱综合材料株式会社 | High-purity electrolytic copper |
-
2019
- 2019-12-16 CN CN201911294286.8A patent/CN111057981A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007046102A (en) * | 2005-08-09 | 2007-02-22 | Furukawa Electric Co Ltd:The | Oxygen-free copper wire with low-temperature softening property, and its manufacturing method |
CN102312184A (en) * | 2011-08-29 | 2012-01-11 | 杭州富通昭和铜业有限公司 | Method for producing bright and oxygen-free copper rod |
CN110382743A (en) * | 2017-06-01 | 2019-10-25 | 三菱综合材料株式会社 | High-purity electrolytic copper |
CN108962860A (en) * | 2018-08-15 | 2018-12-07 | 芜湖长润特种铜线有限公司 | A kind of preparation method of resistance to oxidation bonding brass wire material |
CN109465414A (en) * | 2018-12-28 | 2019-03-15 | 江阴华瑞电工科技股份有限公司 | A method of preparing oxygen-free copper bar |
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Application publication date: 20200424 |