JP2017031468A - METHOD FOR SEPARATING Ru, Rh AND Ir FROM SUBSTANCE CONTAINING SELENIUM AND PLATINUM GROUP ELEMENTS - Google Patents

METHOD FOR SEPARATING Ru, Rh AND Ir FROM SUBSTANCE CONTAINING SELENIUM AND PLATINUM GROUP ELEMENTS Download PDF

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JP2017031468A
JP2017031468A JP2015152393A JP2015152393A JP2017031468A JP 2017031468 A JP2017031468 A JP 2017031468A JP 2015152393 A JP2015152393 A JP 2015152393A JP 2015152393 A JP2015152393 A JP 2015152393A JP 2017031468 A JP2017031468 A JP 2017031468A
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JP6585955B2 (en
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裕貴 有吉
Yuki Ariyoshi
裕貴 有吉
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JX Nippon Mining and Metals Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a method for efficiently separating Ru, Rh and Ir from a substance containing selenium and platinum group elements.SOLUTION: The method for separating Ru, Rh and Ir from a substance containing selenium and platinum group elements comprises: an alkali treatment step of adding a flux being a mixture of sodium hydroxide and sodium nitrate to a substance containing selenium and platinum group elements composed mainly of Se, Pt, Pd, Ru, Rh and Ir in which Pt, Pd and Ru are bonded mainly to Se to form a selenium compound and melting the substance to produce a melt; and an acid leaching step of subjecting the melt to acid leaching treatment and after that performing solid-liquid separation to produce a solid including Ru, Rh and Ir and a liquid including Se, Pt and Pd.SELECTED DRAWING: None

Description

本発明はセレン白金族元素含有物からＲｕ、ＲｈおよびＩｒを分離する方法に関する。   The present invention relates to a method for separating Ru, Rh and Ir from a selenium platinum group element-containing material.

銅製錬の銅電解工程で発生する電解殿物には貴金属が含まれており、王水や塩酸等の薬剤により溶解した後に元素ごとに分離回収される。貴金属には白金族元素も含まれており、白金族元素とともにセレンが共存しているセレン白金族元素含有物として存在している。このセレン白金族元素含有物は王水や塩酸等の薬剤で溶解しにくいため湿式処理が困難である。
これに関連して、従来、特許文献１に記載の方法が提案されている。
特許文献１には、セレン白金族元素含有物に苛性ソーダと硝酸ソーダの混合物からなるフラックスを添加し、該フラックスの共晶温度以上に加熱して溶融し、この溶融物を水浸出して固液分離し、亜セレン酸ソーダを含む液分と白金族元素を含む残渣とに分離することを特徴とするセレン白金族元素含有物の溶解処理方法が記載されており、このような方法によれば、セレンを効率よく浸出して白金族元素と分離することができると記載されている。 Electrolytic deposits generated in the copper electrolysis process of copper smelting contain precious metals, which are separated and recovered for each element after being dissolved by chemicals such as aqua regia and hydrochloric acid. The noble metal includes a platinum group element, and exists as a selenium platinum group element-containing material in which selenium coexists with the platinum group element. This selenium platinum group element-containing material is difficult to be wet-treated because it is difficult to dissolve with chemicals such as aqua regia and hydrochloric acid.
In relation to this, a method described in Patent Document 1 has been proposed.
In Patent Document 1, a flux composed of a mixture of caustic soda and sodium nitrate is added to a selenium platinum group element-containing material, heated to a temperature equal to or higher than the eutectic temperature of the flux and melted, and the melt is leached into a solid liquid. A method for dissolving a selenium platinum group element-containing material, characterized in that it is separated and separated into a liquid component containing sodium selenite and a residue containing a platinum group element, is described. Selenium can be efficiently leached and separated from platinum group elements.

特開２００３−２６８４５７号公報JP 2003-268457 A

しかしながら、セレン白金族元素含有物が、特にＲｕ、ＲｈおよびＩｒを多く含む場合に、これらの元素成分を、その他の元素（特にＳｅ、ＰｔおよびＰｄ）と効率よく分離する方法については、従来、検討されていなかった。
すなわち、特許文献１に記載の方法のようにＳｅと白金族元素とを分離するのではなく、Ｒｕ、ＲｈおよびＩｒと、その他の元素とを分離する方法は、従来、提案されていない。 However, when the selenium platinum group element-containing material contains a large amount of Ru, Rh and Ir in particular, a method for efficiently separating these element components from other elements (especially Se, Pt and Pd) has been conventionally known. It was not examined.
That is, a method of separating Ru, Rh, and Ir from other elements has not been proposed conventionally, instead of separating Se and platinum group elements as in the method described in Patent Document 1.

本発明者は上記課題を解決するため鋭意検討し、Ｒｕ、ＲｈおよびＩｒを多く含むセレン白金族元素含有物から、Ｒｕ、ＲｈおよびＩｒを効率よく分離する方法を見出し、本発明を完成させた。
本発明は以下の（１）〜（４）である。
（１）Ｓｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒを主成分として含み、Ｐｔ、ＰｄおよびＲｕは主にＳｅと結合してセレン化合物を形成しているセレン白金族元素含有物に、苛性ソーダおよび硝酸ソーダの混合物であるフラックスを添加し、溶融して、溶融物を得るアルカリ処理工程と、
前記溶融物に酸浸出処理を施した後、固液分離し、Ｒｕ、ＲｈおよびＩｒを含む固体と、Ｓｅ、ＰｔおよびＰｄを含む液体とを得る酸浸出工程と、
を備える、セレン白金族元素含有物からＲｕ、ＲｈおよびＩｒを分離する分離方法。
（２）前記酸浸出工程において、前記溶融物を１．０〜３．５ｍｏｌ／Ｌの塩酸水溶液に浸漬する前記酸浸出処理を施す、上記（１）に記載の分離方法。
（３）前記酸浸出工程において、前記溶融物に水浸出処理を施した後、固液分離し、固体として得られた残渣を、前記塩酸水溶液と過酸化水素とを含む溶液に浸漬する前記酸浸出処理を施す、上記（１）または（２）に記載の分離方法。
（４）アルカリ処理工程において、苛性ソーダと硝酸ソーダとを７０：３０〜８９：１１のモル比で含む前記フラックスを用いる、上記（１）〜（３）のいずれかに記載の分離方法。 The present inventors diligently studied to solve the above problems, and found a method for efficiently separating Ru, Rh and Ir from a selenium platinum group element-containing material containing a large amount of Ru, Rh and Ir, and completed the present invention. .
The present invention includes the following (1) to (4).
(1) A selenium platinum group element containing se, Pt, Pd, Ru, Rh and Ir as main components, wherein Pt, Pd and Ru are mainly bonded to Se to form a selenium compound. An alkali treatment step of adding a flux that is a mixture of sodium nitrate and melting to obtain a melt;
An acid leaching step of subjecting the melt to an acid leaching treatment followed by solid-liquid separation to obtain a solid containing Ru, Rh and Ir, and a liquid containing Se, Pt and Pd;
A separation method for separating Ru, Rh and Ir from a selenium platinum group element-containing material.
(2) The separation method according to (1), wherein in the acid leaching step, the acid leaching treatment is performed in which the melt is immersed in a 1.0 to 3.5 mol / L hydrochloric acid aqueous solution.
(3) In the acid leaching step, the melt is subjected to a water leaching treatment and then separated into solid and liquid, and the residue obtained as a solid is immersed in a solution containing the hydrochloric acid aqueous solution and hydrogen peroxide. The separation method according to (1) or (2) above, wherein a leaching process is performed.
(4) The separation method according to any one of (1) to (3), wherein in the alkali treatment step, the flux containing caustic soda and sodium nitrate at a molar ratio of 70:30 to 89:11 is used.

本発明によれば、Ｒｕ、ＲｈおよびＩｒを多く含むセレン白金族元素含有物から、Ｒｕ、ＲｈおよびＩｒを効率よく分離する方法を提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the method of isolate | separating Ru, Rh, and Ir efficiently from the selenium platinum group element containing material containing many Ru, Rh, and Ir can be provided.

実施例２の結果を示すグラフである。10 is a graph showing the results of Example 2. 実施例３の結果を示すグラフである。10 is a graph showing the results of Example 3. 実施例３のもう一つの結果を示すグラフである。10 is a graph showing another result of Example 3.

本発明について説明する。
本発明は、Ｓｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒを主成分として含み、Ｐｔ、ＰｄおよびＲｕは主にＳｅと結合してセレン化合物を形成しているセレン白金族元素含有物に、苛性ソーダおよび硝酸ソーダの混合物であるフラックスを添加し、溶融して、溶融物を得るアルカリ処理工程と、前記溶融物に酸浸出処理を施した後、固液分離し、Ｒｕ、ＲｈおよびＩｒを含む固体と、Ｓｅ、ＰｔおよびＰｄを含む液体とを得る酸浸出工程と、を備える、セレン白金族元素含有物からＲｕ、ＲｈおよびＩｒを分離する分離方法である。
このような分離方法を、以下では「本発明の分離方法」ともいう。 The present invention will be described.
The present invention relates to a selenium platinum group element-containing material containing Se, Pt, Pd, Ru, Rh and Ir as main components, wherein Pt, Pd and Ru are mainly combined with Se to form a selenium compound. And an alkali treatment step of adding a flux that is a mixture of sodium nitrate and melting to obtain a melt, and subjecting the melt to an acid leaching treatment, followed by solid-liquid separation, and a solid containing Ru, Rh, and Ir And an acid leaching step for obtaining a liquid containing Se, Pt, and Pd, and a separation method for separating Ru, Rh, and Ir from a selenium platinum group element-containing material.
Hereinafter, such a separation method is also referred to as “the separation method of the present invention”.

＜セレン白金族元素含有物＞
初めにセレン白金族元素含有物について説明する。
本発明の分離方法においてセレン白金族元素含有物は、Ｓｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒを主成分として含んでいる。また、それらの中でＰｔ、ＰｄおよびＲｕは主にＳｅと結合してセレン化合物を形成し、セレン白金族元素含有物の少なくとも一部を構成している。 <Selenium platinum group element-containing material>
First, the selenium platinum group element-containing material will be described.
In the separation method of the present invention, the selenium platinum group element-containing material contains Se, Pt, Pd, Ru, Rh and Ir as main components. Among them, Pt, Pd, and Ru are mainly bonded to Se to form a selenium compound, and constitute at least a part of the selenium platinum group element-containing material.

本発明において主成分とは、含有率が６０質量％以上であることを意味するものとする。すなわち、本発明の分離方法においてセレン白金族元素含有物におけるＳｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒの合計含有率は６０質量％以上である。
この合計含有率は７０質量％以上であることが好ましく、７５質量％以上であることがより好ましく、８０質量％以上であることがより好ましく、８５質量％以上であることがさらに好ましい。 In the present invention, the main component means that the content is 60% by mass or more. That is, in the separation method of the present invention, the total content of Se, Pt, Pd, Ru, Rh and Ir in the selenium platinum group element-containing material is 60% by mass or more.
The total content is preferably 70% by mass or more, more preferably 75% by mass or more, more preferably 80% by mass or more, and further preferably 85% by mass or more.

セレン白金族元素含有物においてＳｅ含有率は、４０〜８０質量％であることが好ましく、５０〜７０質量％であることがより好ましい。   In the selenium platinum group element-containing material, the Se content is preferably 40 to 80% by mass, and more preferably 50 to 70% by mass.

セレン白金族元素含有物においてＰｔ含有率は、０．１〜１０質量％であることが好ましい。   In the selenium platinum group element-containing material, the Pt content is preferably 0.1 to 10% by mass.

セレン白金族元素含有物においてＰｄ含有率は、０．１〜１５質量％であることが好ましい。   In the selenium platinum group element-containing material, the Pd content is preferably 0.1 to 15% by mass.

セレン白金族元素含有物においてＲｕ含有率は、１〜４５質量％であることが好ましく、５〜４０質量％であることがより好ましく、１０〜３５質量％であることがさらに好ましい。   In the selenium platinum group element-containing material, the Ru content is preferably 1 to 45% by mass, more preferably 5 to 40% by mass, and still more preferably 10 to 35% by mass.

セレン白金族元素含有物においてＲｈ含有率は、０．１〜８質量％であることが好ましい。   In the selenium platinum group element-containing material, the Rh content is preferably 0.1 to 8% by mass.

セレン白金族元素含有物においてＩｒ含有率は、０．１〜８質量％であることが好ましい。   In the selenium platinum group element-containing material, the Ir content is preferably 0.1 to 8% by mass.

なお、セレン白金族元素含有物が含むＳｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒの各成分ならびにその他成分の含有率は、ＩＣＰ発光分析装置を用いて測定して得られる値を意味するものとする。   The contents of each component of Se, Pt, Pd, Ru, Rh, and Ir contained in the selenium platinum group element-containing material and other components mean values obtained by measurement using an ICP emission analyzer. To do.

上記のような成分のうち、少なくともＰｔ、ＰｄおよびＲｕは、主にＳｅと結合してセレン化合物を形成している。
Ｐｔ、ＰｄおよびＲｕがＳｅと結合してなるセレン化合物としては、ＰｔＲｕＳｅ4、ＰｄＳｅ2、ＰｔＳｅ2が挙げられる。 Among the components as described above, at least Pt, Pd, and Ru are mainly bonded to Se to form a selenium compound.
Examples of the selenium compound in which Pt, Pd and Ru are bonded to Se include PtRuSe 4 , PdSe 2 and PtSe 2 .

ここで「主に」とは、他の形態の化合物（例えばＰｔ、ＰｄまたはＲｕを含む酸化物）や単体（例えばＰｔ、ＰｄおよびＲｕの各々の単体）と比較して、その含有率が１０倍以上であることを意味するものとする。すなわち、Ｐｔ、ＰｄおよびＲｕがＳｅと結合してなるセレン化合物の含有率は、その他の形態の化合物および単体の合計含有率の１０倍以上、好ましくは１００倍以上である。   Here, “mainly” means that the content rate is 10% compared to other forms of compounds (for example, oxides containing Pt, Pd, or Ru) or simple substances (for example, single elements of Pt, Pd, and Ru). It means to be more than double. That is, the content of the selenium compound formed by bonding Pt, Pd, and Ru with Se is 10 times or more, preferably 100 times or more, of the total content of other forms of compounds and simple substances.

なお、Ｐｔ、ＰｄおよびＲｕがＳｅと結合してなるセレン化合物や、他の形態の化合物（例えばＰｔ、ＰｄまたはＲｕを含む酸化物）や単体（例えばＰｔ、ＰｄおよびＲｕの各々の単体）のセレン白金族元素含有物における含有率は、鉱物粒子解析装置（ＭＬＡ解析装置）を用いて測定して得られる値を意味するものとする。   In addition, selenium compounds in which Pt, Pd and Ru are bonded to Se, compounds of other forms (for example, oxides containing Pt, Pd or Ru) and simple substances (for example, simple substances of Pt, Pd and Ru) The content rate in a selenium platinum group element containing material shall mean the value obtained by measuring using a mineral particle analyzer (MLA analyzer).

セレン白金族元素含有物において、Ｐｔ、ＰｄおよびＲｕがＳｅと結合してなるセレン化合物の合計含有率（例えば、ＰｔＲｕＳｅ4、ＰｄＳｅ2およびＰｔＳｅ2の合計含有率）は、６５〜９９質量％であることが好ましい。 In the selenium platinum group element-containing material, the total content of selenium compounds formed by combining Pt, Pd and Ru with Se (for example, the total content of PtRuSe 4 , PdSe 2 and PtSe 2 ) is 65 to 99% by mass. Preferably there is.

セレン白金族元素含有物においてＰｔＲｕＳｅ4の含有率は、５０〜９０質量％であることが好ましく、６０〜８０質量％であることがより好ましい。 In the selenium platinum group-containing material, the content of PtRuSe 4 is preferably 50 to 90% by mass, and more preferably 60 to 80% by mass.

セレン白金族元素含有物においてＰｄＳｅ2の含有率は、５〜４０質量％であることが好ましい。 In the selenium platinum group-containing material, the content of PdSe 2 is preferably 5 to 40% by mass.

セレン白金族元素含有物においてＰｔＳｅ2の含有率は、１〜１５質量％であることが好ましい。 In the selenium platinum group-containing material, the content of PtSe 2 is preferably 1 to 15% by mass.

また、銅電解殿物を酸浸出して脱銅した後、固液分離する脱銅工程と、前記脱銅工程において固液分離することで固体として得られる酸浸出後の銅電解殿物を塩化浸出し、その後、固液分離する塩化浸出工程と、前記塩化浸出工程において固液分離することで液体として得られる塩化浸出液から溶媒抽出によって金を分離する金抽出工程と、前記金抽出工程において金を分離した後に得られる金抽出後液に二酸化硫黄を添加してセレンとテルルを順に還元して沈殿分離させ、その後、沈殿物からセレンを蒸留分離して蒸留残渣を得る還元工程と、を備える操作によって得られる前記蒸留残渣を、前記セレン白金族元素含有物として用いることが好ましい。   In addition, after the copper electrolytic deposit is acid leached to remove copper, the copper removal step for solid-liquid separation and the copper electrolytic deposit after acid leaching obtained as a solid by solid-liquid separation in the copper removal step are chlorinated. Chloride leaching step for leaching, followed by solid-liquid separation, gold extraction step for separating gold by solvent extraction from chlorinated leachate obtained as a liquid by solid-liquid separation in the chloride leaching step, and gold in the gold extraction step A reduction step in which sulfur dioxide is added to the gold-extracted solution obtained after the separation of selenium to reduce selenium and tellurium in order to precipitate separation, and then selenium is separated from the precipitate by distillation to obtain a distillation residue. The distillation residue obtained by the operation is preferably used as the selenium platinum group element-containing material.

ここで銅電解殿物は、例えば以下のようにして得られるものである。
銅の電解精製においては、転炉からの粗銅を精製炉において９９．５％程度に精製し、鋳造した陽極（アノード）と陰極としての種板を電解槽に交互に数十枚一組で吊し、電解精製が実施される。種板上に電着した銅は電気銅と呼ばれ、周知の態様で爾後処理されて商品化される。電解槽の底には陽極に含まれる不純物が泥状で沈積し、これは銅電解殿物（アノードスライム）と呼ばれている。銅電解殿物には、銅に加えて、金を始め、原料中の貴金属が濃縮しており、貴金属回収の主要原料である。この他、セレン及びテルルも含まれている。 Here, the copper electrolytic product is obtained, for example, as follows.
In the electrolytic refining of copper, the crude copper from the converter is refined to about 99.5% in the refining furnace, and the cast anode (anode) and the seed plate as the cathode are suspended in pairs in the electrolytic cell alternately. Then, electrolytic purification is performed. The copper electrodeposited on the seed plate is called electrolytic copper and is post-treated in a well-known manner and commercialized. Impurities contained in the anode are deposited in a muddy state at the bottom of the electrolytic cell, which is called a copper electrolytic deposit (anode slime). In addition to copper, noble metals in the raw materials are concentrated in the copper electrolytic deposit, and it is the main raw material for precious metal recovery. In addition, selenium and tellurium are also included.

＜アルカリ処理工程＞
本発明の分離方法におけるアルカリ処理工程について説明する。
アルカリ処理工程では、前記セレン白金族元素含有物に、苛性ソーダおよび硝酸ソーダの混合物であるフラックスを添加し、溶融して、溶融物を得る。 <Alkali treatment process>
The alkali treatment process in the separation method of the present invention will be described.
In the alkali treatment step, a flux that is a mixture of caustic soda and sodium nitrate is added to the selenium platinum group element-containing material and melted to obtain a melt.

セレン白金族元素含有物と、苛性ソーダ（ＮａＯＨ）および硝酸ソーダ（ＮａＮＯ3）の混合物からなるフラックスとを、例えば坩堝などの容器へ装入し、これをフラックスの共晶温度以上に加熱して溶融する。具体的には３５０〜４５０℃に加熱して溶融することが好ましい。
加熱溶融によってＳｅが主に４価となり亜セレン酸ソーダ（Ｎａ2ＳｅＯ3）となる。 A selenium platinum group element-containing material and a flux composed of a mixture of caustic soda (NaOH) and sodium nitrate (NaNO 3 ) are charged into a vessel such as a crucible, for example, and heated to a temperature equal to or higher than the eutectic temperature of the flux. To do. Specifically, it is preferable to melt by heating to 350 to 450 ° C.
By heating and melting, Se becomes mainly tetravalent and becomes sodium selenite (Na 2 SeO 3 ).

ここで、苛性ソーダと硝酸ソーダとを７０：３０〜８９：１１のモル比（Ｎａモル比）とすることが好ましく、７５：２５〜８５：１５のモル比（Ｎａモル比）とすることがより好ましく、７５：２５〜８０：２０のモル比（Ｎａモル比）とすることがさらに好ましい。このような範囲であると、Ｒｕ、ＲｈおよびＩｒをより効率よく分離できるからである。
苛性ソーダと硝酸ソーダのモル比が７０：３０よりも硝酸ソーダ比率が高まると溶融物のＳｅが６価の割合が高くなる傾向がある。苛性ソーダと硝酸ソーダのモル比が８９：１１よりも苛性ソーダ比率が高まるとＰｔ,Ｐｄの浸出率が低くなる傾向がある。
なお、本発明において浸出率は、原料として用いるセレン白金族元素含有物に対する各元素の質量ベースの比率（百分率）を意味するものとする。 Here, it is preferable to make caustic soda and sodium nitrate into a molar ratio (Na molar ratio) of 70:30 to 89:11, more preferably 75:25 to 85:15 (Na molar ratio). Preferably, the molar ratio (Na molar ratio) is 75:25 to 80:20. This is because within such a range, Ru, Rh and Ir can be more efficiently separated.
When the molar ratio of caustic soda to sodium nitrate is higher than 70:30, the ratio of hexavalent Se to the melt tends to increase. When the molar ratio of caustic soda and sodium nitrate is higher than 89:11, the leaching rate of Pt and Pd tends to decrease.
In the present invention, the leaching rate means the mass-based ratio (percentage) of each element to the selenium platinum group element-containing material used as a raw material.

また、苛性ソーダと硝酸ソーダとを８６：１４〜８９：１１のモル比（Ｎａモル比）とすることが好ましい。６価のＳｅの存在率を低くすることができるからである。
また、苛性ソーダと硝酸ソーダとを７０：３０〜７４：２６のモル比（Ｎａモル比）とすることが好ましい。後述する酸浸出工程におけるＰｔおよびＰｄの浸出率を概ね９０％以上とすることができるからである。
さらに、苛性ソーダと硝酸ソーダとを７０：３０〜８５：１５のモル比（Ｎａモル比）とすることが好ましく、７４：２６〜８０：２０のモル比（Ｎａモル比）とすることがより好ましい。後述する酸浸出工程における金の浸出率を高めることができるからである。 Moreover, it is preferable to make caustic soda and sodium nitrate into the molar ratio (Na molar ratio) of 86: 14-89: 11. This is because the abundance ratio of hexavalent Se can be lowered.
Moreover, it is preferable to make caustic soda and sodium nitrate into a molar ratio (Na molar ratio) of 70:30 to 74:26. This is because the leaching rate of Pt and Pd in the acid leaching step described later can be approximately 90% or more.
Furthermore, caustic soda and sodium nitrate are preferably in a molar ratio (Na molar ratio) of 70:30 to 85:15, and more preferably in a molar ratio (Na molar ratio) of 74:26 to 80:20. . This is because the gold leaching rate in the acid leaching step described later can be increased.

このようなアルカリ処理工程を行って、溶融物を得る。   Such an alkali treatment process is performed to obtain a melt.

＜酸浸出工程＞
本発明の分離方法における酸浸出工程について説明する。
酸浸出工程では、前記溶融物に酸浸出処理を施した後、固液分離し、Ｒｕ、ＲｈおよびＩｒを含む固体と、Ｓｅ、ＰｔおよびＰｄを含む液体とを得る。 <Acid leaching process>
The acid leaching process in the separation method of the present invention will be described.
In the acid leaching step, the melt is subjected to an acid leaching treatment and then subjected to solid-liquid separation to obtain a solid containing Ru, Rh and Ir and a liquid containing Se, Pt and Pd.

ここで酸浸出処理は、塩酸を用いることが好ましい。また、前記溶融物を１．０〜３．５ｍｏｌ／Ｌ、好ましくは２．０〜３．０ｍｏｌ／Ｌ、より好ましくは２．０〜２．９ｍｏｌ／Ｌの塩酸水溶液に浸漬して酸浸出処理を施すことが好ましい。このような範囲であると、Ｒｕ、ＲｈおよびＩｒをより効率よく分離できるからである。
また、前記溶融物を２．０〜３．０ｍｏｌ／Ｌ（好ましくは２．０〜２．９ｍｏｌ／Ｌ）の塩酸水溶液に浸漬して酸浸出処理を施すと、酸浸出工程における金の浸出率を高めることができるので好ましい。 Here, hydrochloric acid is preferably used for the acid leaching treatment. The melt is immersed in an aqueous hydrochloric acid solution of 1.0 to 3.5 mol / L, preferably 2.0 to 3.0 mol / L, and more preferably 2.0 to 2.9 mol / L. It is preferable to apply. This is because within such a range, Ru, Rh and Ir can be more efficiently separated.
Moreover, when the said melt is immersed in 2.0-3.0 mol / L (preferably 2.0-2.9 mol / L) hydrochloric acid aqueous solution and an acid leaching process is performed, the leaching rate of gold in the acid leaching step Can be increased, which is preferable.

また、塩酸に過酸化水素を加えた溶液を用いて前記溶融物に酸浸出処理を施すことが好ましい。ここで塩酸に過酸化水素を加えた溶液における過酸化水素の濃度は３０〜６０質量％であることが好ましい。   Moreover, it is preferable to subject the melt to an acid leaching treatment using a solution obtained by adding hydrogen peroxide to hydrochloric acid. Here, the concentration of hydrogen peroxide in a solution obtained by adding hydrogen peroxide to hydrochloric acid is preferably 30 to 60% by mass.

さらに、酸浸出工程では、前記溶融物に水浸出処理を施した後、固液分離し、固体として得られた残渣について、上記のような酸浸出処理を施すことが好ましい。また、その残渣について、前記塩酸水溶液と過酸化水素とを含む溶液に浸漬する、上記のような酸浸出処理を施すことが好ましい。   Furthermore, in the acid leaching step, it is preferable to subject the molten material to a water leaching treatment, followed by solid-liquid separation and subjecting the residue obtained as a solid to the acid leaching treatment as described above. The residue is preferably subjected to the acid leaching treatment as described above in which the residue is immersed in a solution containing the hydrochloric acid aqueous solution and hydrogen peroxide.

このような酸浸出工程によって、Ｒｕ、ＲｈおよびＩｒを含む固体と、Ｓｅ、ＰｔおよびＰｄを含む液体とを得ることができる。
ここでＳｅ、ＰｔおよびＰｄの液体への浸出率は極めて高い。
具体的にはＳｅの浸出率は９０％以上、好ましくは９５％以上、より好ましくは９８％以上である。
また、ＰｔまたはＰｄの浸出率は６０％以上、好ましくは８０％以上、より好ましくは８８％以上である。
そして、Ｒｕ、ＲｈおよびＩｒの液体への浸出率は低く、固体への残存率が高い。
具体的にはＲｕ、Ｒｈ、Ｉｒのいずれか１種の浸出率は４５％以下、好ましくは３８％以下、より好ましくは３５％以下である。
したがって、Ｒｕ、ＲｈおよびＩｒをより効率よく分離することができる。 By such an acid leaching step, a solid containing Ru, Rh and Ir and a liquid containing Se, Pt and Pd can be obtained.
Here, the leaching rate of Se, Pt and Pd into the liquid is extremely high.
Specifically, the leaching rate of Se is 90% or more, preferably 95% or more, more preferably 98% or more.
The leaching rate of Pt or Pd is 60% or more, preferably 80% or more, more preferably 88% or more.
The leaching rate of Ru, Rh and Ir into the liquid is low, and the residual rate in the solid is high.
Specifically, the leaching rate of any one of Ru, Rh, and Ir is 45% or less, preferably 38% or less, more preferably 35% or less.
Therefore, Ru, Rh and Ir can be separated more efficiently.

上記の酸浸出工程において固液分離することで回収した固体を、例えば特開２００４−３３２０４１号に記載の方法で処理して、Ｒｕ、ＲｈおよびＩｒを得ることができる。   The solid recovered by solid-liquid separation in the acid leaching step can be processed by, for example, a method described in JP-A No. 2004-332041 to obtain Ru, Rh, and Ir.

＜実施例１＞
一般的な成分を備える銅電解殿物を用意し、これを硫酸溶液を用いて脱銅浸出処理した。得られた脱銅浸出残渣を塩酸と過酸化水素で溶解した。得られた溶液をＤＢＣ（ジブチルカルビトール）を用いて金抽出した。得られた金抽出後液を亜硫酸ガスを用いて還元し白金族含有還元物を分離した。この還元後液に対してさらに亜硫酸ガスを用いて還元してセレン含有還元物を得た。このセレン含有還元物を蒸留してセレンと蒸留残渣を得た。得られた蒸留残渣の分析結果を第1表に示す。 <Example 1>
A copper electrolytic product having general components was prepared and subjected to a copper removal leaching process using a sulfuric acid solution. The obtained decopper leaching residue was dissolved with hydrochloric acid and hydrogen peroxide. The resulting solution was gold extracted using DBC (dibutyl carbitol). The resulting gold-extracted solution was reduced using sulfurous acid gas to separate the platinum group-containing reduced product. The reduced solution was further reduced using sulfurous acid gas to obtain a selenium-containing reduced product. This selenium-containing reduced product was distilled to obtain selenium and a distillation residue. The analysis results of the obtained distillation residue are shown in Table 1.

また、蒸留残渣に含まれる成分の形態を鉱物粒子解析装置（ＭＬＡ解析装置）により求めた。
測定結果を第２表に示す。 Moreover, the form of the component contained in the distillation residue was calculated | required with the mineral particle analyzer (MLA analyzer).
The measurement results are shown in Table 2.

第１表、第２表に示すように、蒸留残渣はＲｕ、Ｒｈ、Ｉｒを多く含み、特にＲｕの含有率が２２質量％と高い。また、ＲｕはＰｔＲｕＳｅ4の形態で含まれることが分かった。 As shown in Tables 1 and 2, the distillation residue contains a lot of Ru, Rh, and Ir, and the content of Ru is particularly high at 22% by mass. It was also found that Ru is contained in the form of PtRuSe 4 .

上記のような蒸留残渣をアルカリ処理および酸浸出処理を行った。具体的には、坩堝内へ５ｇの蒸留残渣とフラックス（ＮａＯＨ：１０ｇ＋ＮａＮＯ3：５ｇ）とを装入し、４００℃で２時間の処理を行った後、１ｍｏｌ／Ｌの塩酸水溶液に浸漬し、８０℃で２時間の処理を行った。その後、メンブレンフィルターを用いて真空ろ過することによって固液分離を行った。
そして、浸出液に含まれる各成分の含有率を測定し、浸出率（対原料（質量％））を求めた。第３表に示す。 The distillation residue as described above was subjected to alkali treatment and acid leaching treatment. Specifically, 5 g of distillation residue and flux (NaOH: 10 g + NaNO 3 : 5 g) were charged into the crucible, treated at 400 ° C. for 2 hours, then immersed in a 1 mol / L hydrochloric acid aqueous solution, The treatment was performed at 80 ° C. for 2 hours. Then, solid-liquid separation was performed by vacuum filtration using a membrane filter.
And the content rate of each component contained in the leachate was measured, and the leach rate (vs. raw material (mass%)) was determined. It is shown in Table 3.

第３表に示すように、Ｒｕ、Ｒｈ、Ｉｒの大半は固体中に残存させることが可能であることが確認された。
したがって、この固体からＲｕ、Ｒｈ、Ｉｒを回収し、一方で、浸出液は、例えば金抽出後液の還元工程へ戻し、白金族・金含有還元物と共に従来法によって処理してパラジウム、金等を回収することができる。 As shown in Table 3, it was confirmed that most of Ru, Rh, and Ir can remain in the solid.
Therefore, Ru, Rh, and Ir are recovered from this solid. On the other hand, the leachate is returned to the reduction step of the solution after gold extraction, for example, and treated with a platinum group / gold-containing reduced product by a conventional method to remove palladium, gold, etc. It can be recovered.

＜実施例２＞
実施例１で用いた蒸留残渣についてアルカリ処理を行った。具体的には、坩堝内へ２０ｇの蒸留残渣とフラックス（ＮａＯＨとＮａＮＯ3とを８６ｍｏｌ：１４ｍｏｌで混合したもの）とを装入し、４００℃で２時間の処理を行った。
その後、塩酸濃度を変更した複数のパターンの酸浸出処理を行った。具体的には、上記のアルカリ処理後の残留残渣を８０℃に調整した蒸留水内で２ｈ撹拌した後、固液分離し、得られた残渣を、１ｍｏｌ／Ｌ、２ｍｏｌ／Ｌ、３ｍｏｌ／Ｌ、４ｍｏｌ／Ｌ、６ｍｏｌ／Ｌの各々に調整した塩酸水溶液に浸漬し、６０℃で３時間の処理を行った。なお、塩酸水溶液には３０％Ｈ2Ｏ2を初期液量に対し７５％の体積量を添加した。
そして、その後、メンブレンフィルターを用いて真空ろ過することによって固液分離を行い、浸出液に含まれる各成分の含有率を測定し、浸出率を求めた。
結果を図１および第４表に示す。 <Example 2>
The distillation residue used in Example 1 was subjected to alkali treatment. Specifically, 20 g of distillation residue and flux (mixed with NaOH and NaNO 3 at a ratio of 86 mol: 14 mol) were charged into the crucible and treated at 400 ° C. for 2 hours.
Thereafter, acid leaching treatment was performed in a plurality of patterns with different hydrochloric acid concentrations. Specifically, the residual residue after the alkali treatment was stirred in distilled water adjusted to 80 ° C. for 2 h, and then solid-liquid separation was performed. The obtained residue was 1 mol / L, 2 mol / L, 3 mol / L. It was immersed in a hydrochloric acid aqueous solution adjusted to 4 mol / L and 6 mol / L, respectively, and treated at 60 ° C. for 3 hours. In addition, 75% of the initial volume of 30% H 2 O 2 was added to the aqueous hydrochloric acid solution.
And after that, solid-liquid separation was performed by carrying out vacuum filtration using a membrane filter, the content rate of each component contained in the leachate was measured, and the leach rate was obtained.
The results are shown in FIG. 1 and Table 4.

図１および第４表に示すように、塩酸濃度が２ｍｏｌ／Ｌ以上である場合にＰｔおよびＰｄの浸出率が７０％以上となり、Ａｕの浸出率が６９％以上となった。また、塩酸濃度が４ｍｏｌ／Ｌ以上であると、Ｒｕ、Ｒｈ、Ｉｒの浸出率が高くなることがわかった。
これより、塩酸濃度が好ましくは１〜３．５ｍｏｌ／Ｌ（より好ましくは２〜３ｍｏｌ／Ｌ）である場合にＰｔ、Ｐｄの浸出率を高く、かつ、Ｒｕ、Ｒｈ、Ｉｒの浸出率を低くすることができることがわかった。
したがって、塩酸濃度を上記の範囲とした酸浸出処理を行い、その後、固液分離して得られる固体としてＲｕ、Ｒｈ、Ｉｒを効率よく回収し、一方で、浸出液は、例えば金抽出後液の還元工程へ戻し、白金族・金含有還元物と共に従来法によって処理してパラジウム、金等を回収することができる。 As shown in FIG. 1 and Table 4, when the hydrochloric acid concentration was 2 mol / L or more, the leaching rate of Pt and Pd was 70% or more, and the leaching rate of Au was 69% or more. It was also found that the leaching rate of Ru, Rh, and Ir was increased when the hydrochloric acid concentration was 4 mol / L or more.
Accordingly, when the hydrochloric acid concentration is preferably 1 to 3.5 mol / L (more preferably 2 to 3 mol / L), the leaching rate of Pt and Pd is high, and the leaching rate of Ru, Rh, and Ir is low. I found out that I can do it.
Therefore, an acid leaching treatment with a hydrochloric acid concentration in the above range is performed, and then Ru, Rh, and Ir are efficiently recovered as solids obtained by solid-liquid separation, while the leachate is, for example, a solution after gold extraction Returning to the reduction step, palladium, gold and the like can be recovered by treating with a platinum group / gold-containing reduced product by a conventional method.

＜実施例３＞
実施例１で用いた蒸留残渣について、ＮａＯＨとＮａＮＯ3との混合比を変更した複数のパターンのフラックスを用いたアルカリ処理を行った。具体的には、坩堝内へ２０ｇの蒸留残渣とＮａＮＯ3の混合比を０〜２６ｍｏｌ％（Ｎａモル比）の範囲で変更したフラックスとを装入し、４００℃で２時間の処理を行った。
そして、上記のアルカリ処理後の残留残渣を８０℃に調整した蒸留水内で２ｈ撹拌した後、固液分離し、得られた残渣を１ｍｏｌ／Ｌの塩酸水溶液に浸漬し、６０℃で３時間の処理を行い、さらにメンブレンフィルターを用いて真空ろ過することによって固液分離を行った。なお、塩酸水溶液には３０％Ｈ2Ｏ2を初期液量に対し７５％の体積量を添加した。
そして、その後、メンブレンフィルターを用いて真空ろ過することによって固液分離を行い、浸出液に含まれる各成分の含有率を測定し、浸出率を求めた。結果を図２および第５表に示す。
また、上記のアルカリ処理後の残留残渣を８０℃に調整した蒸留水内で２ｈ撹拌した後に固液分離して得られた水に含まれる４価Ｓｅおよび６価Ｓｅの割合を測定した。結果を図３および第６表に示す。 <Example 3>
The distillation residue used in Example 1 was subjected to alkali treatment using a plurality of patterns of flux in which the mixing ratio of NaOH and NaNO 3 was changed. Specifically, 20 g of distillation residue and a flux in which the mixing ratio of NaNO 3 was changed in the range of 0 to 26 mol% (Na molar ratio) were charged into the crucible, and the treatment was performed at 400 ° C. for 2 hours. .
The residual residue after the alkali treatment was stirred in distilled water adjusted to 80 ° C. for 2 h, then solid-liquid separated, and the resulting residue was immersed in a 1 mol / L aqueous hydrochloric acid solution at 60 ° C. for 3 hours. The solid-liquid separation was performed by vacuum filtration using a membrane filter. In addition, 75% of the initial volume of 30% H 2 O 2 was added to the aqueous hydrochloric acid solution.
And after that, solid-liquid separation was performed by carrying out vacuum filtration using a membrane filter, the content rate of each component contained in the leachate was measured, and the leach rate was obtained. The results are shown in FIG. 2 and Table 5.
Further, the ratio of tetravalent Se and hexavalent Se contained in the water obtained by solid-liquid separation after stirring for 2 h in distilled water adjusted to 80 ° C. was measured for the residual residue after the alkali treatment. The results are shown in FIG. 3 and Table 6.

図２および第５表に示すように、フラックスに含まれるＮａＮＯ3の割合が１０ｍｏｌ％（Ｎａモル比）以下であると、ＰｔおよびＰｄの浸出率が低くなることが分かった。また、フラックスに含まれるＮａＮＯ3の割合が高くても、Ｒｕ、Ｒｈ、Ｉｒの浸出率は高くならないことがわかった。
これより、フラックスに含まれるＮａＮＯ3の割合が１１〜３０ｍｏｌ％（Ｎａモル比）とすると、Ｐｔ、Ｐｄの浸出率を高く、かつ、Ｒｕ、Ｒｈ、Ｉｒの浸出率を低くすることができることがわかった。
したがって、フラックスに含まれるＮａＮＯ3の割合を上記の範囲としたアルカリ処理を行い、その後、固液分離して得られる固体としてＲｕ、Ｒｈ、Ｉｒを効率よく回収し、一方で、浸出液は、例えば金抽出後液の還元工程へ戻し、白金族・金含有還元物と共に従来法によって処理してパラジウム、金等を回収することができる。 As shown in FIG. 2 and Table 5, it was found that when the proportion of NaNO 3 contained in the flux was 10 mol% (Na molar ratio) or less, the leaching rate of Pt and Pd was lowered. It was also found that even if the ratio of NaNO 3 contained in the flux was high, the leaching rate of Ru, Rh, and Ir did not increase.
From this, when the ratio of NaNO 3 contained in the flux is 11 to 30 mol% (Na molar ratio), the leaching rate of Pt and Pd can be increased and the leaching rate of Ru, Rh, and Ir can be decreased. all right.
Therefore, an alkali treatment is performed with the ratio of NaNO 3 contained in the flux within the above range, and then Ru, Rh, and Ir are efficiently recovered as solids obtained by solid-liquid separation, while leachate is, for example, It can return to the reduction | restoration process of the liquid after gold extraction, and can process palladium and gold | metal | money containing reduction products with a conventional method, and can collect | recover palladium, gold | metal | money, etc.

また、図３および第６表に示すように、フラックスに含まれるＮａＮＯ3の割合が高くなると水浸出によるＳｅ浸出率が高くなることが分かった。また、フラックスに含まれるＮａＮＯ3の割合が高くなるほど、４価Ｓｅの割合が減り、６価Ｓｅの割合が増えることが分かった。 Further, as shown in FIG. 3 and Table 6, it was found that the Se leaching rate due to water leaching increases as the proportion of NaNO 3 contained in the flux increases. It was also found that the higher the proportion of NaNO 3 contained in the flux, the lower the proportion of tetravalent Se and the higher the proportion of hexavalent Se.

Claims (4)

Ｓｅ、Ｐｔ、Ｐｄ、Ｒｕ、ＲｈおよびＩｒを主成分として含み、Ｐｔ、ＰｄおよびＲｕは主にＳｅと結合してセレン化合物を形成しているセレン白金族元素含有物に、苛性ソーダおよび硝酸ソーダの混合物であるフラックスを添加し、溶融して、溶融物を得るアルカリ処理工程と、
前記溶融物に酸浸出処理を施した後、固液分離し、Ｒｕ、ＲｈおよびＩｒを含む固体と、Ｓｅ、ＰｔおよびＰｄを含む液体とを得る酸浸出工程と、
を備える、セレン白金族元素含有物からＲｕ、ＲｈおよびＩｒを分離する分離方法。 It contains Se, Pt, Pd, Ru, Rh, and Ir as main components, and Pt, Pd, and Ru are mainly combined with Se to form a selenium compound. An alkali treatment step of adding and melting a flux as a mixture to obtain a melt;
An acid leaching step of subjecting the melt to an acid leaching treatment followed by solid-liquid separation to obtain a solid containing Ru, Rh and Ir, and a liquid containing Se, Pt and Pd;
A separation method for separating Ru, Rh and Ir from a selenium platinum group element-containing material. 前記酸浸出工程において、前記溶融物を１．０〜３．５ｍｏｌ／Ｌの塩酸水溶液に浸漬する前記酸浸出処理を施す、請求項１に記載の分離方法。   The separation method according to claim 1, wherein in the acid leaching step, the acid leaching treatment is performed in which the melt is immersed in a 1.0 to 3.5 mol / L hydrochloric acid aqueous solution. 前記酸浸出工程において、前記溶融物に水浸出処理を施した後、固液分離し、固体として得られた残渣を、前記塩酸水溶液と過酸化水素とを含む溶液に浸漬する前記酸浸出処理を施す、請求項１または２に記載の分離方法。   In the acid leaching step, the melt is subjected to a water leaching treatment, followed by solid-liquid separation, and the acid leaching treatment in which the residue obtained as a solid is immersed in a solution containing the hydrochloric acid aqueous solution and hydrogen peroxide. The separation method according to claim 1 or 2, which is performed. アルカリ処理工程において、苛性ソーダと硝酸ソーダとを７０：３０〜８９：１１のモル比で含む前記フラックスを用いる、請求項１〜３のいずれかに記載の分離方法。   The separation method according to any one of claims 1 to 3, wherein in the alkali treatment step, the flux containing caustic soda and sodium nitrate at a molar ratio of 70:30 to 89:11 is used.
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