JP2005042161A - Refining method for copper - Google Patents

Refining method for copper Download PDF

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JP2005042161A
JP2005042161A JP2003277439A JP2003277439A JP2005042161A JP 2005042161 A JP2005042161 A JP 2005042161A JP 2003277439 A JP2003277439 A JP 2003277439A JP 2003277439 A JP2003277439 A JP 2003277439A JP 2005042161 A JP2005042161 A JP 2005042161A
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copper
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JP4140470B2 (en
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Tadanori Sano
忠徳 佐野
Taichiro Nishikawa
太一郎 西川
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Sumitomo Electric Industries Ltd
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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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Abstract

<P>PROBLEM TO BE SOLVED: To provide a refining method for copper, which effectively removes Fe without employing an electrolytic refining step, and to provide a method for manufacturing a copper wire rod with the use of the molten copper obtained through the refining method. <P>SOLUTION: This refining method comprises a melting step of melting copper containing Fe, and a refining step of removing Fe from the molten metal while controlling the concentration of oxygen in the molten metal containing the molten copper to 1,000 to 3,000 ppm by weight ratio. The concentration of Fe in the molten copper metal containing Fe becomes lowest in an oxygen concentration range of 1,000 to 3,000 wt. ppm. Accordingly, Fe can be efficiently removed from the molten copper metal containing Fe, by controlling the concentration of oxygen in the molten metal to the above range. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、銅の精錬方法、及びこの精錬方法により得られた溶銅を用いた銅荒引線の製造方法に関するものである。   The present invention relates to a copper refining method and a method for producing a copper roughing wire using molten copper obtained by the refining method.

従来、電線の導体などに使用される銅線は、主に連続鋳造圧延によって製造された銅荒引線に伸線加工などを施すことによって製造される。このとき、電気伝導度(導電率)の高い銅荒引線を得るべく、上記銅線に用いられる銅荒引線の銅原料には、電解によって精錬(精製)された電気銅が一般に使用されている。   Conventionally, the copper wire used for the conductor of an electric wire etc. is manufactured by performing a wire drawing etc. to the copper rough drawing wire mainly manufactured by continuous casting rolling. At this time, in order to obtain a copper rough drawn wire having a high electrical conductivity (conductivity), electrolytic copper refined (purified) by electrolysis is generally used as the copper raw material for the copper rough drawn wire used in the copper wire. .

銅荒引線に用いる銅原料中に不純物元素が多量に含有されている場合、銅荒引線に必要な特性である導電率が悪化したり、熱間圧延の際に割れなどが発生する原因となる。そこで、電解精錬により不純物を低減した、具体的には不純物の総量を重量比で100ppm以下にした電気銅を用いて、導電率の悪化や圧延時の割れなどの防止を図っている。   When a large amount of impurity elements are contained in the copper raw material used for the copper roughing wire, the electrical conductivity, which is a characteristic required for the copper roughing wire, may be deteriorated, or cracking may occur during hot rolling. . In view of this, the use of electrolytic copper in which impurities are reduced by electrolytic refining, specifically, the total amount of impurities is 100 ppm or less by weight, is used to prevent deterioration of conductivity and cracking during rolling.

一方、銅や銅合金は、一般に、鉄やアルミニウムなどと同様に需要の大きい金属である。そのため、市場より発生した銅を含有する銅スクラップを回収して再利用することは、資源保護の立場から重要なことである。しかし、市場から回収された銅線屑をはじめとする銅スクラップには、銅以外の不純物元素が含まれる場合が多い。このような不純物元素を多く含む銅スクラップ、いわゆる低品位銅スクラップは、反射炉などで溶解して酸化還元による精錬を行った後、更に電解精錬を行って電気銅を銅荒引線用の原料として再生させている。また、近年、銅スクラップの精錬において、スラグを用いた精錬方法が検討されている(非特許文献1参照)。   On the other hand, copper and copper alloys are generally metals in great demand like iron and aluminum. For this reason, it is important from the standpoint of resource protection to collect and reuse copper scrap containing copper generated from the market. However, copper scraps including copper wire scraps collected from the market often contain impurity elements other than copper. Copper scrap containing a large amount of impurity elements, so-called low-grade copper scrap, is melted in a reflection furnace and refined by oxidation-reduction, and then further electrolytically refined to use electrolytic copper as a raw material for copper roughing wire. You are playing. In recent years, a refining method using slag has been studied in refining copper scrap (see Non-Patent Document 1).

藤澤敏治、『銅のリサイクルプロセス』、「まてりあ」第35巻12月号(1996)、社団法人 日本金属学会、1294〜1297ページToshiharu Fujisawa, “Copper Recycling Process”, “Materia” Vol. 35, December (1996), Japan Institute of Metals, pp. 1294-1297

上記のように不純物元素を多く含むいわゆる低品位銅スクラップを再生させる際、電解精錬やスラグによる精錬を行うことで、不純物元素を効果的に除去することができる。しかし、近年、リサイクル関連法の整備に伴って低品位銅スクラップが増大する傾向にあり、低品位銅スクラップの使用比率の拡大を図るべく、より簡便な精錬方法が望まれる。   When regenerating so-called low-grade copper scrap containing a large amount of impurity elements as described above, the impurity elements can be effectively removed by performing refining by electrolytic refining or slag. However, in recent years, there is a tendency for low-grade copper scrap to increase with the establishment of recycling-related laws, and a simpler refining method is desired in order to increase the usage ratio of low-grade copper scrap.

そこで、本発明の目的は、電解精製やスラグによる精錬を行うことなく、不純物元素であるFeを効果的に除去可能な銅の精錬方法を提供することにある。また、本発明の他の目的は、上記銅の精錬方法により得られた溶銅を用いて銅荒引線を製造する方法を提供することにある。   Accordingly, an object of the present invention is to provide a copper refining method capable of effectively removing Fe as an impurity element without performing electrolytic refining or refining by slag. Moreover, the other object of this invention is to provide the method of manufacturing a copper rough drawing wire using the molten copper obtained by the said copper refining method.

本発明は、酸素濃度を特定の範囲に調整することで、上記目的を達成する。即ち、本発明銅の精錬方法は、Feを含有する銅を溶解する溶解工程と、前記溶解された銅を含有する溶湯の酸素濃度を重量比で1000ppm以上3000ppm以下にして、Feを溶湯中から除去する精錬工程とを具えることを特徴とする。   The present invention achieves the above object by adjusting the oxygen concentration to a specific range. That is, in the copper refining method of the present invention, the melting step of melting Fe-containing copper, and the oxygen concentration of the molten copper-containing molten metal is 1000 ppm or more and 3000 ppm or less by weight ratio, and Fe is contained in the molten metal. And a refining process to be removed.

従来、いわゆる低品位銅スクラップと呼ばれるものには、Pb、Si、Sn、Zn、Ni、Feなどの少なくとも1種を不純物元素として含むものが多い。そこで、発明者らは、電解精錬を行わないでこれら不純物元素の含有量を低減するべく、酸素濃度を変化させ、このときの各元素の挙動を調べてみた。不純物元素を含む銅を酸化させる際、溶湯中の不純物元素が優先的に酸化されると、不純物元素の酸化物が銅との比重差により溶湯表面に浮上する。従って、浮上した酸化物を除去することで溶湯中の不純物濃度を低下させることができる。この現象を利用して、酸素濃度を変化させた際の各元素の濃度を測定したところ、ある特定範囲の酸素濃度では、Fe濃度を極めて低下できるとの知見を得た。本発明は、この知見に基づき、規定するものである。以下、本発明をより詳しく説明する。   Conventionally, many so-called low-grade copper scraps contain at least one of Pb, Si, Sn, Zn, Ni, Fe and the like as an impurity element. Therefore, the inventors changed the oxygen concentration in order to reduce the content of these impurity elements without performing electrolytic refining, and examined the behavior of each element at this time. When copper containing an impurity element is oxidized, if the impurity element in the molten metal is preferentially oxidized, the oxide of the impurity element floats on the surface of the molten metal due to a difference in specific gravity from copper. Therefore, the impurity concentration in the molten metal can be reduced by removing the floating oxide. Utilizing this phenomenon, the concentration of each element when the oxygen concentration was changed was measured, and it was found that the Fe concentration could be extremely reduced within a certain range of oxygen concentration. The present invention is defined based on this finding. Hereinafter, the present invention will be described in more detail.

本発明精錬方法では、溶解材料としてFeが含まれる銅を対象とし、酸素濃度の調整による精錬にてFeを含む銅からFeを除去するものとする。従って、本発明精錬方法は、一度利用された銅材、即ち、銅スクラップを溶解原料の少なくとも一部に使用する場合に適する。もちろん、溶解原料の全部が銅スクラップの場合でも本発明精錬方法を利用することができる。また、いわゆる低品位銅スクラップの精錬にも利用することができる。更に、Fe以外の不純物元素を除去するために、Feを含むスラグを用いて精錬を行うことでFe濃度が高められた場合の後精錬としても利用することができる。   In the refining method of the present invention, copper containing Fe as a melting material is targeted, and Fe is removed from copper containing Fe by refining by adjusting the oxygen concentration. Therefore, the refining method of the present invention is suitable when the copper material once used, that is, copper scrap is used as at least a part of the melting raw material. Of course, the refining method of the present invention can be used even when the entire melting raw material is copper scrap. It can also be used for refining so-called low-grade copper scrap. Furthermore, in order to remove impurity elements other than Fe, it can utilize also as post-refining when the Fe concentration is increased by refining using slag containing Fe.

本発明において溶湯の酸素濃度は、重量比で1000ppm以上3000ppm以下とする。本発明者らが検討した結果、酸素を含む溶湯中におけるFe濃度は、溶湯中の酸素濃度が低くても、逆に高くても大きくなり、重量比で1000ppm〜3000ppmのとき最低となる、即ち、Feが安定に存在できる濃度の最低値は、重量比で1000ppm〜3000ppmであるとの知見を得た。この知見により、Feを含む銅からFeの除去に最適な酸素濃度として、上記の範囲を規定する。酸素濃度が1000重量ppm未満でもまた3000重量ppm超でも、Feの除去が不十分で溶湯中のFe濃度が20重量ppm超となる恐れがある。より好ましくは、重量比で1500ppm以上2500ppm以下とすることである。酸素濃度を上記範囲に制御することで、本発明精錬方法により精錬された溶銅は、Fe濃度を20重量ppm以下とすることができ、銅荒引線の要求特性を十分満たすことができる。   In the present invention, the oxygen concentration of the molten metal is 1000 ppm to 3000 ppm by weight. As a result of the study by the present inventors, the Fe concentration in the molten metal containing oxygen increases even when the oxygen concentration in the molten metal is low or high, and becomes the lowest when the weight ratio is 1000 ppm to 3000 ppm. The minimum value of the concentration at which Fe can stably exist was found to be 1000 ppm to 3000 ppm by weight. Based on this knowledge, the above range is defined as the optimum oxygen concentration for removing Fe from copper containing Fe. Even if the oxygen concentration is less than 1000 ppm by weight or more than 3000 ppm by weight, the removal of Fe may be insufficient and the Fe concentration in the molten metal may exceed 20 ppm by weight. More preferably, the weight ratio is 1500 ppm or more and 2500 ppm or less. By controlling the oxygen concentration within the above range, the molten copper refined by the refining method of the present invention can have an Fe concentration of 20 ppm by weight or less, and can sufficiently satisfy the required characteristics of the copper drawn wire.

上記酸素濃度の調整は、溶湯に酸素或いは空気を吹き込む量を調整することで行うことが挙げられる。その他、例えば、Fe以外の不純物元素を除去するために酸素濃度を3000重量ppm超に高めて精錬を行った場合、還元剤を用いて還元することでFe除去に適した酸素濃度に調整してもよい。還元剤は、例えば、重油などが挙げられる。   The oxygen concentration may be adjusted by adjusting the amount of oxygen or air blown into the molten metal. In addition, for example, when refining is performed by increasing the oxygen concentration to over 3000 ppm by weight in order to remove impurity elements other than Fe, the oxygen concentration is adjusted to a suitable oxygen removal by reducing with a reducing agent. Also good. Examples of the reducing agent include heavy oil.

なお、銅荒引線の酸素濃度は、通常、重量比で100〜500ppm程度である。本発明精錬方法を行うと、溶銅中の酸素濃度が高くなっている。従って、本発明精錬方法により得られた溶銅を銅荒引線の材料として用いる場合、銅荒引線に適した酸素濃度となるように、本発明精錬方法を施した後は、還元剤などを用いて還元し、酸素濃度を重量比で100〜500ppm程度にすることが好ましい。還元剤としては、重油などが挙げられる。   Note that the oxygen concentration of the copper rough wire is usually about 100 to 500 ppm by weight. When the refining method of the present invention is performed, the oxygen concentration in the molten copper is high. Therefore, when the molten copper obtained by the refining method of the present invention is used as a material for the copper roughing wire, a reducing agent is used after the refining method of the present invention so that the oxygen concentration is suitable for the copper roughing wire. It is preferable to reduce the oxygen concentration to about 100 to 500 ppm by weight. Examples of the reducing agent include heavy oil.

上記本発明精錬方法により得られた溶銅は、銅荒引線の製造に利用することが最適である。特に、連続鋳造圧延により銅荒引線を製造する際にも利用することができる。本発明精錬方法により溶銅中のFe濃度が低減されているため、圧延時に割れが発生することを防止することができる。また、得られた銅荒引線は、優れた導電性を具える。   The molten copper obtained by the above-described refining method of the present invention is optimally used for producing a copper roughing wire. In particular, it can also be used when producing a copper roughing wire by continuous casting and rolling. Since the Fe concentration in the molten copper is reduced by the refining method of the present invention, it is possible to prevent cracks from occurring during rolling. Moreover, the obtained copper rough wire has excellent conductivity.

なお、溶解材料にFe以外の不純物元素、例えば、Sn、Pb、Ni、Znなどが含まれる場合は、別途スラグを用いた精錬などを合わせて行うとよい。   Note that when the dissolved material contains an impurity element other than Fe, for example, Sn, Pb, Ni, Zn, etc., it may be performed together with refining using slag separately.

上記構成を具える本発明精錬方法は、溶湯の酸素濃度を特定範囲に制御して精錬を行うことで、電解精錬やスラグによる精錬を行うことなく、溶湯中からFeを効果的に除去することができるという優れた効果を奏し得る。また、酸素濃度の調整による精錬は、溶解を行う反射炉などの溶解炉を用いて行うことができるため、溶解から精錬への作業を連続的に行うことができ、作業効率を向上させることもできる。更に、酸素濃度の調整による精錬は、上記のように溶解炉において行うことができることから、従来の設備をそのまま利用することができ、更なる設備の増加が不要である。   The refining method of the present invention having the above configuration effectively removes Fe from the molten metal by performing refining by controlling the oxygen concentration of the molten metal within a specific range without performing refining by electrolytic refining or slag. It is possible to achieve an excellent effect of being able to. In addition, since refining by adjusting the oxygen concentration can be performed using a melting furnace such as a reflective furnace that performs melting, work from melting to refining can be performed continuously, which can improve work efficiency. it can. Furthermore, since refining by adjusting the oxygen concentration can be performed in the melting furnace as described above, conventional equipment can be used as it is, and further increase in equipment is unnecessary.

従って、本発明精錬方法を適用すれば、Feを多く含む銅材を溶解原料の一部又は全部に使用しても、連続鋳造圧延にて製造される銅荒引線の導電率の悪化や、熱間圧延時の割れの発生などが生じることがなく、良好な製品を製造することが可能である。   Therefore, if the refining method of the present invention is applied, even if a copper material containing a large amount of Fe is used as a part or all of the melting raw material, the conductivity of the copper roughing wire produced by continuous casting and rolling is reduced. It is possible to produce a good product without causing cracks during hot rolling.

以下、本発明の実施の形態を説明する。
重量比でFe：約120ppmを含有させた銅材1kgを溶解し、Feを含む銅の溶湯の酸素濃度を変化させてFeの除去を行い、このときの溶湯中のFe濃度を測定してみた。 Embodiments of the present invention will be described below.
1 kg of copper material containing about 120 ppm of Fe by weight was dissolved, Fe was removed by changing the oxygen concentration of the copper melt containing Fe, and the Fe concentration in the melt at this time was measured .

酸素濃度は、ノズルを溶湯に浸漬させて、200〜400cm3/minの範囲で流量を変化させて空気を溶湯に吹き込むことで変化させた。このとき、溶湯の温度は、1150℃に保持した。試験の結果を図1のグラフに示す。 The oxygen concentration was changed by immersing the nozzle in the molten metal, changing the flow rate in the range of 200 to 400 cm 3 / min, and blowing air into the molten metal. At this time, the temperature of the molten metal was maintained at 1150 ° C. The test results are shown in the graph of FIG.

図1に示すように溶湯中の酸素濃度を変化させることで、溶湯中のFe濃度が変化していることがわかる。そして、溶湯中の酸素濃度が1000〜3000重量ppmの範囲、特に、1500〜2500重量ppmにあるとき、Fe濃度が最も低下していることがわかる。具体的には、10重量ppm以下にすることができた。   As shown in FIG. 1, it can be seen that the Fe concentration in the molten metal is changed by changing the oxygen concentration in the molten metal. And when the oxygen concentration in a molten metal exists in the range of 1000-3000 weight ppm, especially in 1500-2500 weight ppm, it turns out that Fe concentration has fallen most. Specifically, it could be 10 ppm by weight or less.

上記試験結果から、本発明精錬方法を行うことで、従来のように電解精錬を行うことなく、Feを効果的に除去できることが確認された。   From the above test results, it was confirmed that by performing the refining method of the present invention, Fe can be effectively removed without performing electrolytic refining as in the past.

上記精錬により得られた溶銅を用いて、連続鋳造圧延により銅荒引線を作製し、銅荒引線の特性(引張強さ(MPa)、伸び(％)、導電率(％IACS))を調べてみた。また、上記銅荒引線に伸線加工を施して硬銅線を作製し、硬銅線の特性(引張強さ(MPa)、伸び(％)、導電率(％IACS))を調べてみた。   Using the molten copper obtained by the above refining, copper roughing wire was produced by continuous casting and rolling, and the characteristics of copper roughing wire (tensile strength (MPa), elongation (%), conductivity (% IACS)) were investigated. I tried. Moreover, the copper rough drawing wire was drawn to produce a hard copper wire, and the properties of the hard copper wire (tensile strength (MPa), elongation (%), conductivity (% IACS)) were examined.

連続鋳造圧延の条件、伸線加工の条件は、公知の条件とした。試験の結果を表1に示す。表1において試料No.1〜4が上記酸素濃度の調整による精錬を行ったものである。また、試料No.5は、比較として、Feを含有させていない銅材を用いたものである。具体的には、Feを含有させていない銅材を溶解し、得られた溶湯を用いて、試料No.1〜4と同様の条件で連続鋳造圧延を行って銅荒引線を作製し、同様に銅荒引線の特性を調べた。また、この銅荒引線に同様の条件で伸線加工を施して硬銅線を作製し、同様に硬銅線の特性を調べた。   The conditions for continuous casting and rolling and the conditions for wire drawing were known conditions. The test results are shown in Table 1. In Table 1, sample Nos. 1 to 4 were refined by adjusting the oxygen concentration. Sample No. 5 uses, as a comparison, a copper material that does not contain Fe. Specifically, a copper material not containing Fe is melted, and using the obtained molten metal, continuous casting and rolling is performed under the same conditions as in Sample Nos. 1 to 4, and a copper rough drawn wire is produced. The characteristics of the copper rough wire were investigated. Moreover, the copper rough drawing wire was drawn under the same conditions to produce a hard copper wire, and the characteristics of the hard copper wire were similarly examined.

Figure 2005042161
Figure 2005042161

その結果、酸素濃度1000〜3000重量ppmにて精錬を行った試料No.2及び3は、連続鋳造圧延による熱間圧延を行っている際に割れなどが生じることがなかった。また、表1に示すように、試料No.2及び3は、高い導電率を有する銅荒引線であった。従って、Feを含有した銅材を用いても、酸素濃度の調整による精錬によりFeの除去を行うことで、Feを含有していない銅材を用いた場合と同程度の品位の銅荒引線を提供できることがわかる。以上から、本発明精錬方法を適用すれば、いわゆる低品位銅スクラップを溶解原料として用いても、電解精錬を行うことなく、要求特性を十分に満たす銅荒引線を提供することが可能であると推測される。   As a result, Sample Nos. 2 and 3 that were refined at an oxygen concentration of 1000 to 3000 ppm by weight did not cause cracks during hot rolling by continuous casting rolling. Further, as shown in Table 1, Sample Nos. 2 and 3 were copper rough drawn wires having high conductivity. Therefore, even if a copper material containing Fe is used, by removing Fe by refining by adjusting the oxygen concentration, a rough copper wire with the same grade as when using a copper material not containing Fe is obtained. You can see that it can be provided. From the above, if the refining method of the present invention is applied, even if so-called low-grade copper scrap is used as a melting raw material, it is possible to provide a copper roughing wire that sufficiently satisfies the required characteristics without performing electrolytic refining. Guessed.

本発明銅の精錬方法は、特に、Feを含有する銅スクラップを再利用する際に最適である。また、この精錬方法により得られた溶銅は、銅荒引線の製造に用いることができる。   The copper refining method of the present invention is particularly suitable when recycling copper scrap containing Fe. Moreover, the molten copper obtained by this refining method can be used for manufacture of a copper roughing wire.

酸素濃度の調整による精錬を行った際のFe濃度及び酸素濃度の変化を表すグラフである。It is a graph showing the change of Fe concentration and oxygen concentration at the time of refining by adjustment of oxygen concentration.

Claims (2)

Feを含有する銅を溶解する溶解工程と、
前記溶解された銅を含有する溶湯の酸素濃度を重量比で1000ppm以上3000ppm以下にして、Feを溶湯中から除去する精錬工程とを具えることを特徴とする銅の精錬方法。 A dissolution process for dissolving copper containing Fe;
And a refining step of removing Fe from the molten metal by setting the oxygen concentration of the molten metal containing dissolved copper to 1000 ppm to 3000 ppm by weight. 請求項1に記載の銅の精錬方法により得られた溶銅を用いて、連続鋳造圧延により銅荒引線を製造することを特徴とする銅荒引線の製造方法。   2. A method for producing a rough copper drawn wire, wherein the copper rough drawn wire is produced by continuous casting and rolling using the molten copper obtained by the copper refining method according to claim 1.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106086444A (en) * 2016-08-10 2016-11-09 安徽晋源铜业有限公司 A kind of up-drawing method prepares the method for high-purity oxygen-free copper bar
CN116984573A (en) * 2023-08-14 2023-11-03 湖南展卓新材料科技有限公司 Process for producing low-oxygen copper rod based on reclaimed copper modified continuous casting and rolling

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106086444A (en) * 2016-08-10 2016-11-09 安徽晋源铜业有限公司 A kind of up-drawing method prepares the method for high-purity oxygen-free copper bar
CN106086444B (en) * 2016-08-10 2018-09-14 安徽晋源铜业有限公司 A kind of method that up-drawing method prepares high-purity oxygen-free copper bar
CN116984573A (en) * 2023-08-14 2023-11-03 湖南展卓新材料科技有限公司 Process for producing low-oxygen copper rod based on reclaimed copper modified continuous casting and rolling
CN116984573B (en) * 2023-08-14 2024-04-30 湖南展卓新材料科技有限公司 Process for producing low-oxygen copper rod based on reclaimed copper modified continuous casting and rolling

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