JP2019157240A - REMOVAL METHOD OF Sn AND MANUFACTURING METHOD OF Pb - Google Patents

REMOVAL METHOD OF Sn AND MANUFACTURING METHOD OF Pb Download PDF

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JP2019157240A
JP2019157240A JP2018048466A JP2018048466A JP2019157240A JP 2019157240 A JP2019157240 A JP 2019157240A JP 2018048466 A JP2018048466 A JP 2018048466A JP 2018048466 A JP2018048466 A JP 2018048466A JP 2019157240 A JP2019157240 A JP 2019157240A
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JP6959169B2 (en
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拓也 横田
Takuya Yokota
拓也 横田
瑛基 小野
Eiki Ono
瑛基 小野
琢真 武井
Takuma Takei
琢真 武井
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JX Nippon Mining and Metals Corp
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Abstract

To provide a removal method of Sn and a manufacturing method of Pb, capable of suppressing impurities contamination amount to Sn scum.SOLUTION: A removal method of Sn includes a Harris treatment process for repeating one or more of a series of a process for conducting a soda treatment on a melting crude Pb metal in a Harris furnace, a process for separating a Sd scum generated by the soda treatment; and a recovery process for recovering a part of purified Pb metal obtained in the Harris treatment process with remaining a part of the purified Pb metal, in which the soda treatment is conducted on the melting crude Pb metal obtained by mixing the remaining purified Pb metal and crude Pb metal in the Harris furnace when next Harris treatment process is initiated.SELECTED DRAWING: Figure 1

Description

本件は、Ｓｎの除去方法およびＰｂの製造方法に関する。   This case relates to a method for removing Sn and a method for producing Pb.

例えば、銅製錬などで発生する鉛（Ｐｂ）滓などの鉛原料から製品Ｐｂを製造する鉛製錬において、溶融粗Ｐｂメタルに対してソーダ処理を行うことで、錫（Ｓｎ）スカムが発生する。Ｓｎスカムを回収することでＳｎを除去することができる（例えば、特許文献１参照）。   For example, in lead smelting that produces product Pb from lead raw materials such as lead (Pb) soot generated in copper smelting, etc., tin (Sn) scum is generated by performing a soda treatment on the molten crude Pb metal. . Sn can be removed by collecting the Sn scum (see, for example, Patent Document 1).

特開２０１３−２３４３５６号公報JP 2013-234356 A

しかしながら、Ｐｂなどの不純物もＳｎスカムに混入してしまう。Ｓｎスカムへの不純物混入量が多いと、Ｓｎスカムの浸出残渣を鉛製錬工程に繰り返す際に当該不純物の繰り返し量が増え、処理コストが増加するおそれがあり、歩留まりが悪化するおそれがある。   However, impurities such as Pb are also mixed in the Sn scum. If the amount of impurities mixed in Sn scum is large, when the Sn scum leaching residue is repeated in the lead smelting process, the amount of the impurities repeated increases, the processing cost may increase, and the yield may deteriorate.

本件は上記の課題に鑑み、Ｓｎスカムへの不純物混入量を抑制することができるＳｎの除去方法およびＰｂの製造方法を提供することを目的とする。   In view of the above-described problems, an object of the present invention is to provide a method for removing Sn and a method for producing Pb that can suppress the amount of impurities mixed into Sn scum.

１つの態様では、Ｓｎの除去方法は、ハリス炉において、溶融粗Ｐｂメタルに対してソーダ処理を行う行程と、前記ソーダ処理で発生するＳｎスカムを分離する工程と、を含む一連の工程を１以上繰り返すハリス処理工程と、前記ハリス処理工程で得られる精製Ｐｂメタルの一部を前記ハリス炉に残して回収する回収工程と、を含み、次回のハリス処理工程を開始する際に、前記ハリス炉に残った精製Ｐｂメタルと粗Ｐｂメタルとを混合して得られる溶融粗Ｐｂメタルに対してソーダ処理を行うことを特徴とする。   In one aspect, the Sn removal method includes a series of steps including a step of performing a soda treatment on the molten crude Pb metal in a Harris furnace and a step of separating Sn scum generated in the soda treatment. A Harris treatment step that repeats the above, and a recovery step in which a part of the refined Pb metal obtained in the Harris treatment step is collected while remaining in the Harris furnace, and when the next Harris treatment step is started, the Harris furnace The soda treatment is performed on the molten crude Pb metal obtained by mixing the refined Pb metal and the crude Pb metal remaining in the substrate.

１つの態様では、Ｓｎの除去方法は、ハリス炉において、溶融粗Ｐｂメタルに対してソーダ処理を行う行程と、前記ソーダ処理で発生するＳｎスカムを分離する工程と、を含む一連の工程を１以上繰り返すハリス処理工程と、前記ハリス処理工程で得られる精製Ｐｂメタルを前記ハリス炉から回収する回収工程と、を含み、前記ハリス処理工程を開始する際の前記溶融粗ＰｂメタルのＳｎ品位を６．０ｍａｓｓ％以下に調整することを特徴とする。   In one aspect, the Sn removal method includes a series of steps including a step of performing a soda treatment on the molten crude Pb metal in a Harris furnace and a step of separating Sn scum generated in the soda treatment. Including a repeating Harris treatment step and a recovery step of recovering the purified Pb metal obtained in the Harris treatment step from the Harris furnace, and the Sn quality of the molten crude Pb metal at the start of the Harris treatment step is 6 It is characterized by adjusting to 0.0 mass% or less.

１つの態様では、Ｐｂの製造方法は、上記いずれかのＳｎの除去方法の回収工程で回収された精製Ｐｂメタルに対して電解工程を行うことで、Ｐｂを製造することを特徴とする。   In one aspect, the method for producing Pb is characterized in that Pb is produced by performing an electrolysis step on the purified Pb metal collected in any of the above-described methods for removing Sn.

本発明によれば、Ｓｎスカムへの不純物混入量を抑制することができる。   According to the present invention, the amount of impurities mixed into Sn scum can be suppressed.

ＳｎおよびＰｂを製造する工程の一例について説明する図である。It is a figure explaining an example of the process of manufacturing Sn and Pb. （ａ）および（ｂ）はハリス処理工程について例示する図である。(A) And (b) is a figure illustrated about a Harris processing process. 溶融粗Ｐｂメタル中のＳｎ品位と、ＳｎスカムへのＰｂ混入量（Ｐｂ／Ｓｎ比）との関係を例示する図である。It is a figure which illustrates the relationship between Sn quality in a molten rough Pb metal, and Pb mixing amount (Pb / Sn ratio) to Sn scum.

以下、本発明を実施するための実施形態について説明する。   Hereinafter, an embodiment for carrying out the present invention will be described.

図１は、製品Ｓｎおよび製品Ｐｂを製造する製造工程の一例について説明する図である。図１で例示するように、銅製錬工程などで発生する鉛滓、排バッテリー等の鉛原料に対して脱銅および炭酸化が行われる。脱銅および炭酸化によって得られた炭酸鉛は、Ｐｂ原料としてＰｂ電気炉に投入される。炭酸鉛は、Ｐｂ電気炉で１０００℃〜１２００℃で溶融することによって、粗Ｐｂメタルとスラグとに分離する。   FIG. 1 is a diagram illustrating an example of a manufacturing process for manufacturing the product Sn and the product Pb. As illustrated in FIG. 1, copper removal and carbonation are performed on lead raw materials such as lead soot generated in a copper smelting process and the like, an exhaust battery, and the like. Lead carbonate obtained by copper removal and carbonation is put into a Pb electric furnace as a Pb raw material. Lead carbonate is separated into crude Pb metal and slag by melting at 1000 ° C. to 1200 ° C. in a Pb electric furnace.

粗Ｐｂメタルには、不純物としてＳｎが含まれている。例えば、粗ＰｂメタルにおけるＳｎ品位は、６．０ｍａｓｓ％を上回り、８．０ｍａｓｓ％以上となることもある。以下で説明する工程では、Ｓｎを効果的に除去することができるため、粗ＰｂメタルにおけるＳｎ品位が１０．０ｍａｓｓ％を上回るような場合に特に有効となる。   The crude Pb metal contains Sn as an impurity. For example, the Sn quality in the rough Pb metal may exceed 6.0 mass% and may be 8.0 mass% or more. In the process described below, Sn can be effectively removed, and thus is particularly effective when the Sn quality in the crude Pb metal exceeds 10.0 mass%.

冷却した粗Ｐｂメタルは、ハリス炉に投入される。ハリス炉では、粗Ｐｂメタルを溶融することで得られる溶融粗Ｐｂメタルに対してソーダ処理が行われる。ソーダ処理とは、５００℃程度に加熱して溶融した溶融粗Ｐｂメタルに、例えば苛性ソーダを添加し、さらに場合により追加の苛性ソーダおよび硝酸ソーダを添加して、Ｓｎをソーダ塩（Ｎａ２ＳｎＯ３）化して、溶湯表面において固形化させる処理のことである。固形化したＳｎのソーダ塩は、一般にＳｎスカムと呼ばれる。Ｓｎスカムを掬い取る等して分離することでＳｎスカムを除去することができる。溶融粗Ｐｂメタル中のＳｎ品位を十分に低くするために、ソーダ処理を行う行程と、Ｓｎスカムを分離する工程と、を含む一連の工程を１以上繰り返す。当該一連の工程を１以上繰り返す工程を、ハリス処理工程と称する。 The cooled crude Pb metal is put into a Harris furnace. In the Harris furnace, soda treatment is performed on the molten crude Pb metal obtained by melting the crude Pb metal. In the soda treatment, for example, caustic soda is added to the molten crude Pb metal melted by heating to about 500 ° C., and additional caustic soda and sodium nitrate are added in some cases, so that Sn is a soda salt (Na 2 SnO 3 ). It is a process of solidifying on the surface of the molten metal. Solidified soda salt of Sn is generally called Sn scum. Sn scum can be removed by scraping and separating the Sn scum. In order to sufficiently lower the Sn quality in the molten crude Pb metal, one or more of a series of steps including the process of performing the soda process and the step of separating the Sn scum are repeated. A step of repeating the series of steps one or more times is referred to as a Harris processing step.

Ｓｎスカムは、Ｓｎ製造用のＳｎ原料として利用される。具体的には、Ｓｎスカムは、Ｓｎを浸出するＳｎ浸出工程に供される。得られた浸出後液は、電解採取工程に供され、製品Ｓｎが製造される。Ｓｎ浸出工程の浸出残渣は、鉛電気炉または炭酸化工程に繰り返される。一方、ハリス処理工程によって、Ｓｎ品位が低くなった精製Ｐｂメタルが得られる。この精製Ｐｂメタルは、電解精製工程に供され、製品Ｐｂが製造される。   Sn scum is used as an Sn raw material for producing Sn. Specifically, the Sn scum is subjected to a Sn leaching process for leaching Sn. The obtained post-leaching solution is subjected to an electrowinning process to produce a product Sn. The leaching residue of the Sn leaching process is repeated in the lead electric furnace or the carbonation process. On the other hand, a refined Pb metal having a low Sn quality is obtained by the Harris treatment process. This purified Pb metal is subjected to an electrolytic purification process to produce a product Pb.

図２（ａ）は、ハリス処理工程について例示する図である。図２（ａ）で例示するように、ハリス炉１０内に冷却した粗Ｐｂメタルが投入される。この粗Ｐｂメタルをハリス炉１０で加熱することで、溶融粗Ｐｂメタル２０が得られる。なお、黒丸は、含有されるＳｎ成分を表している。溶融粗Ｐｂメタル２０に対してソーダ処理を行うことで、溶湯表面においてＳｎスカム３０が発生する。このＳｎスカム３０を掬い取る等して分離することで、Ｓｎスカム３０を除去することができる。さらに溶融粗Ｐｂメタル２０に対してソーダ処理を行うことで、溶湯表面においてＳｎスカム３０が発生する。このＳｎスカム３０を掬い取る等して分離することで、Ｓｎスカム３０をさらに除去することができる。ハリス処理工程では、溶融粗Ｐｂメタル２０中のＳｎ濃度が十分に低くなるまで、ソーダ処理を行う行程とＳｎスカム３０を分離する工程とが繰り返されることになる。溶融粗Ｐｂメタル２０中のＳｎ濃度が十分に低くなれば、当該溶融粗Ｐｂメタル２０をメタルポンプによって吸引することで、ハリス炉１０から精製Ｐｂメタル４０を回収することができる。   FIG. 2A is a diagram illustrating the Harris processing step. As illustrated in FIG. 2A, the cooled coarse Pb metal is put into the Harris furnace 10. By heating the crude Pb metal in the Harris furnace 10, the molten crude Pb metal 20 is obtained. In addition, the black circle represents the Sn component contained. By performing a soda treatment on the molten coarse Pb metal 20, Sn scum 30 is generated on the surface of the molten metal. The Sn scum 30 can be removed by scraping or separating the Sn scum 30. Furthermore, Sn scum 30 is generated on the surface of the molten metal by performing a soda treatment on the molten rough Pb metal 20. The Sn scum 30 can be further removed by, for example, scraping and separating the Sn scum 30. In the Harris treatment process, the process of performing the soda process and the process of separating the Sn scum 30 are repeated until the Sn concentration in the molten coarse Pb metal 20 becomes sufficiently low. If the Sn concentration in the molten crude Pb metal 20 becomes sufficiently low, the purified Pb metal 40 can be recovered from the Harris furnace 10 by sucking the molten crude Pb metal 20 with a metal pump.

ここで、ソーダ処理によってＳｎスカムを形成する際に、Ｐｂ、Ｂｉ（ビスマス）などの不純物もＳｎスカムに巻き込まれてＳｎスカムに混入してしまう。図１で例示したように、混入した不純物は、Ｓｎ浸出工程で浸出残渣として回収され、鉛製錬工程に繰り返される。鉛製錬工程への不純物の繰返し量が増えると、処理コストが増加するおそれがあり、歩留まりが悪化するおそれがある。したがって、Ｓｎスカムへの不純物混入量を抑制することが望まれる。   Here, when the Sn scum is formed by the soda process, impurities such as Pb and Bi (bismuth) are also caught in the Sn scum and mixed into the Sn scum. As illustrated in FIG. 1, the mixed impurities are recovered as a leaching residue in the Sn leaching process and are repeated in the lead smelting process. If the repetition amount of impurities in the lead smelting process increases, the processing cost may increase and the yield may deteriorate. Therefore, it is desired to suppress the amount of impurities mixed into the Sn scum.

図３は、溶融粗Ｐｂメタル中のＳｎ品位と、ＳｎスカムへのＰｂ混入量（Ｐｂ／Ｓｎ比）との関係を例示する図である。本発明者らの鋭意研究により、図３で例示するように、溶融粗Ｐｂメタル中のＳｎ品位が高いと、ＳｎスカムへのＰｂ混入量が多くなることが突き止められた。Ｂｉについても、図３と同様の結果が得られる。   FIG. 3 is a diagram illustrating the relationship between the Sn quality in the molten coarse Pb metal and the amount of Pb mixed in the Sn scum (Pb / Sn ratio). As illustrated in FIG. 3, it has been found out that the amount of Pb mixed into the Sn scum increases when the Sn quality in the molten crude Pb metal is high as a result of diligent research by the present inventors. For Bi, the same results as in FIG. 3 are obtained.

そこで、本実施形態においては、ハリス炉１０から精製Ｐｂメタル４０を回収する際に、精製Ｐｂメタル４０の一部をハリス炉１０に残す。なお、メタルポンプによって精製Ｐｂメタル４０を全て回収しようとしても一部の精製Ｐｂメタル４０がハリス炉１０内に残る場合もある。そこで、ここでの「一部を残す」とは、メタルポンプによって回収可能な精製Ｐｂメタル４０の一部を意図的に残すことを意味する。例えば、ハリス炉１０内の精製Ｐｂメタル４０の１／１０〜１／２を残すようにしてもよい。   Therefore, in the present embodiment, when the purified Pb metal 40 is recovered from the Harris furnace 10, a part of the purified Pb metal 40 is left in the Harris furnace 10. Note that some of the purified Pb metal 40 may remain in the Harris furnace 10 even if all of the purified Pb metal 40 is to be recovered by the metal pump. Therefore, “leaving a part” here means intentionally leaving a part of the purified Pb metal 40 that can be recovered by the metal pump. For example, 1/10 to 1/2 of the purified Pb metal 40 in the Harris furnace 10 may be left.

この場合、図２（ｂ）で例示するように、ハリス炉１０内に冷却した粗Ｐｂメタルを投入する際に、精製Ｐｂメタル４０がハリス炉１０内に残存していることになる。ハリス炉１０内に残存している精製Ｐｂメタル４０のＳｎ濃度は十分に低くなっているため、ソーダ処理を行う時点での溶融粗Ｐｂメタル２０中のＳｎ濃度は低くなる。したがって、ソーダ処理を行う際に発生するＳｎスカム中の不純物混入量を抑制することができる。   In this case, as illustrated in FIG. 2B, the purified Pb metal 40 remains in the Harris furnace 10 when the cooled crude Pb metal is charged into the Harris furnace 10. Since the Sn concentration of the refined Pb metal 40 remaining in the Harris furnace 10 is sufficiently low, the Sn concentration in the molten crude Pb metal 20 at the time of performing the soda treatment is low. Therefore, it is possible to suppress the amount of impurities mixed in the Sn scum generated when performing the soda process.

図３の結果から、ＳｎスカムにおけるＰｂ／Ｓｎ比を１．５未満に抑制するためには、ハリス炉１０内に残存する精製Ｐｂメタル４０と、新たにハリス炉１０内に投入する粗Ｐｂメタルとを混合して得られる溶融粗Ｐｂメタル２０（ハリス処理開始時の溶融粗Ｐｂメタル）におけるＳｎ品位を６．０ｍａｓｓ％以下に調整することが好ましい。なお、ＳｎスカムへのＰｂ混入量を十分に抑制する観点から、ハリス処理開始時の溶融粗Ｐｂメタル２０におけるＳｎ品位を４．０ｍａｓｓ％以下とすることが好ましく、２．０ｍａｓｓ％以下とすることがより好ましい。   From the results shown in FIG. 3, in order to suppress the Pb / Sn ratio in Sn scum to less than 1.5, the refined Pb metal 40 remaining in the Harris furnace 10 and the crude Pb metal newly introduced into the Harris furnace 10 are used. It is preferable to adjust the Sn quality in the molten crude Pb metal 20 (melted rough Pb metal at the start of the Harris process) obtained by mixing to 6.0 mass% or less. In addition, from the viewpoint of sufficiently suppressing the amount of Pb mixed into the Sn scum, it is preferable that the Sn quality in the molten crude Pb metal 20 at the start of the Harris process is 4.0 mass% or less, and 2.0 mass% or less. Is more preferable.

ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位Ｃ３は、下記式（１）で表すことができる。
Ｃ３＝（Ｃ１×Ｗ１＋Ｃ２×Ｗ２）／（Ｗ１＋Ｗ２） （１）
Ｃ１：精製Ｐｂメタル４０中のＳｎ品位（１ｍａｓｓ％以下で一定）
Ｃ２：粗Ｐｂメタル中のＳｎ品位（５ｍａｓｓ％〜２０ｍａｓｓ％程度）
Ｃ３：ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位
Ｗ１：ハリス炉１０内に残す精製Ｐｂメタル４０の重量
Ｗ２：粗Ｐｂメタルの重量 The Sn quality C3 in the molten crude Pb metal 20 at the start of the Harris process can be expressed by the following formula (1).
C3 = (C1 × W1 + C2 × W2) / (W1 + W2) (1)
C1: Sn quality in purified Pb metal 40 (constant at 1 mass% or less)
C2: Sn grade in crude Pb metal (about 5 mass% to 20 mass%)
C3: Sn grade W1 in molten crude Pb metal 20 at the start of the Harris process W1: Weight of purified Pb metal 40 left in Harris furnace 10 W2: Weight of crude Pb metal

粗Ｐｂメタル中のＳｎ品位Ｃ２に応じて、ハリス炉１０内に残す精製Ｐｂメタル４０の重量Ｗ１を調整することで、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位を６ｍａｓｓ％以下に調整することができる。粗Ｐｂメタル中のＳｎ品位が高い場合には、精製Ｐｂメタル４０をハリス炉１０内に多く残すことで、希釈を行う。粗Ｐｂメタル中のＳｎ品位が低い場合には、ハリス炉１０内に残す精製Ｐｂメタル４０の量を少なくすることができる。この場合、ハリス炉１０からメタルポンプによって回収可能な精製Ｐｂメタル４０の量が多くなり、工程を簡略化することができるとともに、コストを抑制することができる。   By adjusting the weight W1 of the purified Pb metal 40 remaining in the Harris furnace 10 according to the Sn grade C2 in the crude Pb metal, the Sn grade in the molten crude Pb metal 20 at the start of the Harris process is reduced to 6 mass% or less. Can be adjusted. When the Sn quality in the crude Pb metal is high, dilution is performed by leaving a large amount of the purified Pb metal 40 in the Harris furnace 10. When the Sn quality in the crude Pb metal is low, the amount of the purified Pb metal 40 left in the Harris furnace 10 can be reduced. In this case, the amount of the purified Pb metal 40 that can be recovered from the Harris furnace 10 by the metal pump increases, and the process can be simplified and the cost can be suppressed.

例えば、粗Ｐｂメタル中のＳｎ品位Ｃ２が１８ｍａｓｓ％の場合には、ハリス炉１０内に残す精製Ｐｂメタル４０の重量Ｗ１を６ｔ以上とし、粗Ｐｂメタルの重量Ｗ２を３ｔ以下とすれば、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位Ｃ３を６ｍａｓｓ％以下とすることができる。例えば、粗Ｐｂメタル中のＳｎ品位Ｃ２が１２ｍａｓｓ％の場合には、ハリス炉１０内に残す精製Ｐｂメタル４０の重量Ｗ１を４．５ｔ以上とし、粗Ｐｂメタルの重量Ｗ２を４．５ｔ以下とすれば、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位Ｃ３を６ｍａｓｓ％以下とすることができる。   For example, if the Sn grade C2 in the crude Pb metal is 18 mass%, the weight W1 of the purified Pb metal 40 left in the Harris furnace 10 is set to 6 t or more, and the weight P2 of the crude Pb metal is set to 3 t or less. The Sn quality C3 in the molten crude Pb metal 20 at the start of the treatment can be set to 6 mass% or less. For example, when the Sn grade C2 in the crude Pb metal is 12 mass%, the weight W1 of the purified Pb metal 40 left in the Harris furnace 10 is 4.5 t or more, and the weight P2 of the crude Pb metal is 4.5 t or less. If so, the Sn grade C3 in the molten crude Pb metal 20 at the start of the Harris process can be made 6 mass% or less.

（実施例）
実施形態に従って、ハリス処理工程を行った。ハリス炉１０から精製Ｐｂメタル４０を回収する際に、一部の精製Ｐｂメタル４０をハリス炉１０内に残した。精製Ｐｂメタル４０が残存するハリス炉１０に粗Ｐｂメタルを投入した。ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位は、５．１ｍａｓｓ％であった。ハリス処理工程によってＳｎスカムを発生させ、掬い取った。掬い取ったＳｎスカムの各成分品位を表１に示す。

Figure 2019157240
(Example)
According to the embodiment, a Harris treatment process was performed. When recovering the refined Pb metal 40 from the Harris furnace 10, a part of the refined Pb metal 40 was left in the Harris furnace 10. Crude Pb metal was charged into the Harris furnace 10 where the purified Pb metal 40 remained. The Sn quality in the molten crude Pb metal 20 at the start of the Harris treatment was 5.1 mass%. Sn scum was generated and scraped off by the Harris treatment process. Table 1 shows the quality of each component of the Sn scum thus obtained.
Figure 2019157240

（比較例）
比較例では、ハリス炉１０から精製Ｐｂメタル４０を回収する際に、メタルポンプの回収能力で回収可能な精製Ｐｂメタル４０を全て回収した。その後、ハリス炉１０に粗Ｐｂメタルを投入した。ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位は、８．９ｍａｓｓ％であった。ハリス処理工程によってＳｎスカムを発生させ、掬い取った。掬い取ったＳｎスカムの各成分品位を表２に示す。

Figure 2019157240
(Comparative example)
In the comparative example, when the purified Pb metal 40 was recovered from the Harris furnace 10, all of the purified Pb metal 40 that could be recovered with the recovery capability of the metal pump was recovered. Thereafter, crude Pb metal was charged into the Harris furnace 10. The Sn quality in the molten crude Pb metal 20 at the start of the Harris treatment was 8.9 mass%. Sn scum was generated and scraped off by the Harris treatment process. Table 2 shows the quality of each component of the Sn scum scooped up.
Figure 2019157240

精製Ｐｂメタル４０の一部を残存させることによって、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位を低くすることができた。表１および表２の結果から、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位を低くすることで、Ｓｎスカムに取り込まれる不純物混入量を抑制できることがわかった。また、ハリス処理開始時の溶融粗Ｐｂメタル２０中のＳｎ品位を６ｍａｓｓ％以下とすることで、Ｓｎスカムへの不純物混入量を十分に抑制できることがわかった。   By leaving a part of the purified Pb metal 40, the Sn quality in the molten crude Pb metal 20 at the start of the Harris process could be lowered. From the results of Tables 1 and 2, it was found that the amount of impurities incorporated into the Sn scum can be suppressed by lowering the Sn quality in the molten crude Pb metal 20 at the start of the Harris process. It was also found that the amount of impurities mixed into the Sn scum can be sufficiently suppressed by setting the Sn quality in the molten crude Pb metal 20 at the start of the Harris process to 6 mass% or less.

以上、本発明の実施例について詳述したが、本発明は係る特定の実施例に限定されるものではなく、特許請求の範囲に記載された本発明の要旨の範囲内において、種々の変形・変更が可能である。   Although the embodiments of the present invention have been described in detail above, the present invention is not limited to such specific embodiments, and various modifications and changes can be made within the scope of the gist of the present invention described in the claims. It can be changed.

１０ ハリス炉
２０ 溶融粗Ｐｂメタル
３０ Ｓｎスカム
４０ 精製Ｐｂメタル 10 Harris furnace 20 Molten rough Pb metal 30 Sn scum 40 Refined Pb metal

Claims (6)

ハリス炉において、溶融粗Ｐｂメタルに対してソーダ処理を行う行程と、前記ソーダ処理で発生するＳｎスカムを分離する工程と、を含む一連の工程を１以上繰り返すハリス処理工程と、
前記ハリス処理工程で得られる精製Ｐｂメタルの一部を前記ハリス炉に残して回収する回収工程と、を含み、
次回のハリス処理工程を開始する際に、前記ハリス炉に残った精製Ｐｂメタルと粗Ｐｂメタルとを混合して得られる溶融粗Ｐｂメタルに対してソーダ処理を行うことを特徴とするＳｎの除去方法。 In a Harris furnace, a Harris treatment step that repeats one or more of a series of steps including a step of performing a soda treatment on the molten coarse Pb metal and a step of separating Sn scum generated in the soda treatment;
A recovery step of recovering a part of the refined Pb metal obtained in the Harris treatment step while leaving it in the Harris furnace,
Removal of Sn characterized by performing a soda treatment on the molten crude Pb metal obtained by mixing the refined Pb metal remaining in the Harris furnace and the crude Pb metal when starting the next Harris treatment process. Method. 粗Ｐｂメタルを前記ハリス炉に残った精製Ｐｂメタルと混合することで、Ｓｎ品位を６．０ｍａｓｓ％以下に調整することを特徴とする請求項１記載のＳｎの除去方法。   The method for removing Sn according to claim 1, wherein the Sn quality is adjusted to 6.0 mass% or less by mixing the crude Pb metal with the refined Pb metal remaining in the Harris furnace. ハリス炉において、溶融粗Ｐｂメタルに対してソーダ処理を行う行程と、前記ソーダ処理で発生するＳｎスカムを分離する工程と、を含む一連の工程を１以上繰り返すハリス処理工程と、
前記ハリス処理工程で得られる精製Ｐｂメタルを前記ハリス炉から回収する回収工程と、を含み、
前記ハリス処理工程を開始する際の前記溶融粗ＰｂメタルのＳｎ品位を６．０ｍａｓｓ％以下に調整することを特徴とするＳｎの除去方法。 In a Harris furnace, a Harris treatment step that repeats one or more of a series of steps including a step of performing a soda treatment on the molten coarse Pb metal and a step of separating Sn scum generated in the soda treatment;
A recovery step of recovering the purified Pb metal obtained in the Harris treatment step from the Harris furnace,
A method for removing Sn, characterized in that the Sn quality of the molten crude Pb metal at the start of the Harris treatment step is adjusted to 6.0 mass% or less. 前記回収工程において、前記ハリス処理工程で得られる精製Ｐｂメタルの一部を前記ハリス炉に残し、前記ハリス炉に残った精製Ｐｂメタルを粗Ｐｂメタルと混合することで、前記ハリス処理工程を開始する際の前記溶融粗ＰｂメタルのＳｎ品位を６．０ｍａｓｓ％以下に調整することを特徴とする請求項３記載のＳｎの除去方法。   In the recovery step, a part of the refined Pb metal obtained in the Harris treatment step is left in the Harris furnace, and the refined Pb metal remaining in the Harris furnace is mixed with the crude Pb metal to start the Harris treatment step. 4. The method for removing Sn according to claim 3, wherein the Sn grade of the molten crude Pb metal is adjusted to 6.0 mass% or less. 前記粗ＰｂメタルのＳｎ品位は、８．０ｍａｓｓ％以上であることを特徴とする請求項２または４に記載のＳｎの除去方法。   The Sn removal method according to claim 2 or 4, wherein Sn quality of the rough Pb metal is 8.0 mass% or more. 請求項１〜５のいずれか一項に記載のＳｎの除去方法の回収工程で回収された精製Ｐｂメタルに対して電解工程を行うことで、Ｐｂを製造することを特徴とするＰｂの製造方法。   A method for producing Pb, characterized in that Pb is produced by performing an electrolysis step on the purified Pb metal recovered in the recovery step of the Sn removal method according to any one of claims 1 to 5. .
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JP2020147813A (en) * 2019-03-14 2020-09-17 Ｊｘ金属株式会社 METHOD OF REMOVING Sn AND METHOD OF MANUFACTURING Pb
JP7126972B2 (en) 2019-03-14 2022-08-29 Ｊｘ金属株式会社 Method for removing Sn and method for producing Pb

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