JP2011208249A - Method for separating platinum group element - Google Patents
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Abstract
Description
本発明は、溶液中の白金族金属を共存金属から効率良く溶媒抽出によって分離する方法に関する。本発明の方法は貴金属の製錬工程などにおいて副生する処理物から白金族元素を分離回収する方法として利用することができる。 The present invention relates to a method for efficiently separating a platinum group metal in a solution from a coexisting metal by solvent extraction. The method of the present invention can be used as a method for separating and recovering a platinum group element from a processed product by-produced in a precious metal smelting step or the like.
白金族金属は希少な元素であり、白金族金属を高品位で含む天然鉱物の産出は少ないので、工業的には非鉄金属製錬の副産物や使用済み触媒などから回収されている。例えば、銅やニッケルの精練工程で生じる陽極スライムあるいはニッケルの精練工程で生じる抽出残渣には、金、銀、白金、パラジウムなどが含まれており、従来、これらの製錬残渣から白金や金などの貴金属が回収されている。 Platinum group metals are rare elements, and since there are few productions of natural minerals containing platinum group metals in high quality, they are industrially recovered from non-ferrous metal smelting byproducts and spent catalysts. For example, anodic slime produced in the copper and nickel scouring process or extraction residue produced in the nickel scouring process contains gold, silver, platinum, palladium, etc. Of precious metals have been recovered.
従来、このような製錬残渣等から白金族元素が分離回収されている。例えば、脱銅スライムを塩化浸出し、浸出滓から銀や鉛を回収する一方、浸出液から溶媒抽出によって金を回収した後に、この金抽出後液には白金族元素やセレン等が含まれているので、金抽出後液から白金族元素を回収している。 Conventionally, platinum group elements have been separated and recovered from such smelting residues and the like. For example, leaching copper-free slime and recovering silver and lead from the leachate, while recovering gold from the leachate by solvent extraction, the gold-extracted solution contains platinum group elements and selenium. Therefore, platinum group elements are recovered from the solution after gold extraction.
白金族元素を含む溶液から白金族元素を回収する方法として、ジアルキルスルフィド(DAS)やトリブチル燐酸(TBP)を用いた溶媒抽出方法が知られている（特許文献１：特開昭６３−１４８２４号公報、特許文献２：特開２０００−１７８６６４号公報）。特許文献２の方法は、ＴＢＰと共にオクチルメチルアンモニウムを併用することによって白金族元素を集合して抽出分離できることが記載されている。 As a method for recovering a platinum group element from a solution containing a platinum group element, a solvent extraction method using dialkyl sulfide (DAS) or tributyl phosphoric acid (TBP) is known (Patent Document 1: Japanese Patent Laid-Open No. 63-14824). Gazette, patent document 2: JP 2000-178664 A). The method of Patent Document 2 describes that platinum group elements can be collected and extracted and separated by using octylmethylammonium together with TBP.
白金族元素をイオン交換樹脂に吸着させて分離回収する方法も知られている（特許文献３：特開平２００４−１３１７４５号公報、特許文献４：特開２００７−３０２９４４号公報）。特許文献３にはポリアミン型アニオン交換樹脂を用いることによって比較的低濃度の白金族元素を吸着分離できることが記載されている。また、特許文献４には、白金族元素を吸着したイオン交換樹脂を酸化還元雰囲気下で焙焼して白金族元素を合金化し、焙焼物を酸化剤の存在下で塩酸浸出し、浸出液に塩化カリウムを添加して白金族元素のクロロ錯塩結晶を生成させて分離することによって不純物の少ない白金族元素を回収する方法が記載されている。 Methods for separating and recovering platinum group elements by adsorbing them on ion exchange resins are also known (Patent Document 3: Japanese Patent Laid-Open No. 2004-131745, Patent Document 4: Japanese Patent Laid-Open No. 2007-302944). Patent Document 3 describes that a relatively low concentration of a platinum group element can be adsorbed and separated by using a polyamine type anion exchange resin. Patent Document 4 discloses that an ion exchange resin adsorbing a platinum group element is roasted in an oxidation-reduction atmosphere to alloy the platinum group element, and the roasted product is leached with hydrochloric acid in the presence of an oxidizing agent, and chlorinated in the leachate. A method is described in which platinum group elements with few impurities are recovered by adding potassium to form and separate platinum group element chloro complex crystals.
白金族元素と共に他の金属（不純物金属）を含む溶液から、イオン交換法によって白金族元素を選択的に分離するときに、白金族元素を選択的に吸着するイオン交換樹脂として一般的な弱塩基型イオン交換樹脂を用いた場合、不純物金属の種類によっては、該不純物金属の濃度が高いとイオン交換樹脂の官能基に不純物金属が吸着して白金族元素の吸着を妨げ、さらに不純物金属がイオン交換樹脂に蓄積して吸着能力を低下させ、寿命を短くすると云う問題がある。 A weak base commonly used as an ion exchange resin that selectively adsorbs platinum group elements when the platinum group elements are selectively separated by ion exchange from a solution containing platinum group elements and other metals (impurity metals). When the type ion exchange resin is used, depending on the type of the impurity metal, if the concentration of the impurity metal is high, the impurity metal is adsorbed on the functional group of the ion exchange resin and hinders the adsorption of the platinum group element. There is a problem that it accumulates in the exchange resin to reduce the adsorption capacity and shorten the life.
イオン交換樹脂による白金族元素の分離が不十分になると、溶液中に白金族元素が残留し、抽出後液からセレンなどを回収するときに、回収したセレン中に白金族元素が混入し、セレンの純度を低下させる問題を引き起こす。 If the separation of the platinum group element by the ion exchange resin becomes insufficient, the platinum group element remains in the solution, and when recovering selenium etc. from the liquid after extraction, the platinum group element is mixed in the recovered selenium, Cause the problem of reducing the purity of.
本発明は、白金族元素を含む溶液から、イオン交換法によって白金族元素を分離する際の上記問題を解決したものであり、イオン交換樹脂による白金族元素の吸着を妨げる不純物金属の種類を特定し、その濃度を制限することによって、白金族元素のイオン交換による分離効果を高めた白金族元素の分離方法を提供する。 The present invention solves the above-mentioned problem when the platinum group element is separated from the solution containing the platinum group element by an ion exchange method, and identifies the type of impurity metal that hinders the adsorption of the platinum group element by the ion exchange resin. And the density | concentration is restrict | limited, The separation method of the platinum group element which improved the separation effect by ion exchange of a platinum group element is provided.
本発明は、以下の構成によって上記課題を解決した、白金族元素の分離方法に関する。
〔１〕白金族元素を含む溶液から、イオン交換樹脂を用いて白金族元素を選択的に吸着分離するときに、共存金属のＢｉ、Ｓｎ、Ｐｂの合計モル濃度(Ｍ１)と、白金族元素の合計モル濃度(Ｍ２)の比(Ｍ１/Ｍ２)を１以下に調整して白金族元素を吸着分離することを特徴とする白金族元素の分離方法。
〔２〕白金族元素を含む溶液が、銅電解スライムを塩酸浸出し、この浸出液から金を分離した後液に亜硫酸ガスを導入して還元処理し、生じた固形物を酸と酸化剤によって浸出した液である上記[１]に記載する方法。
The present invention relates to a platinum group element separation method that solves the above problems by the following configuration.
[1] When the platinum group element is selectively adsorbed and separated from the solution containing the platinum group element using an ion exchange resin, the total molar concentration (M1) of the coexisting metals Bi, Sn, and Pb and the platinum group element A platinum group element separation method comprising adsorbing and separating a platinum group element by adjusting a ratio (M1 / M2) of the total molar concentration (M2) to 1 or less.
[2] A solution containing a platinum group element leaches copper electrolytic slime with hydrochloric acid, separates gold from the leached solution, introduces sulfurous acid gas into the solution, and reduces the resulting solid. The resulting solid is leached with an acid and an oxidizing agent. The method according to [1] above, which is a liquid obtained.
本発明の分離方法によれば、イオン交換樹脂による白金族元素の吸着を妨げる影響の大きい共存金属としてＢｉ、Ｓｎ、Ｐｂを特定し、これらの合計モル濃度(Ｍ１)を制限してイオン交換を行うので、白金族元素の吸着分離効果が高い。 According to the separation method of the present invention, Bi, Sn, and Pb are specified as coexisting metals having a large influence on hindering the adsorption of platinum group elements by the ion exchange resin, and the total molar concentration (M1) thereof is limited to perform ion exchange. As a result, the effect of adsorption and separation of platinum group elements is high.
具体的には、白金族元素（Pt、Pd、Ru、Rh、Ir）の合計モル濃度(Ｍ２)に対して、Ｂｉ、Ｓｎ、Ｐｂの合計モル濃度(Ｍ１)の比(Ｍ１/Ｍ２)を１以下にすることによって、Ｂｉ等がイオン交換樹脂の官能基に吸着する量を制限して、白金族元素に対するイオン交換樹脂の吸着能力を確保し、さらに吸着後の溶離洗浄工程におけるイオン交換樹脂への残留が少ない。 Specifically, the ratio (M1 / M2) of the total molar concentration (M1) of Bi, Sn, and Pb to the total molar concentration (M2) of the platinum group elements (Pt, Pd, Ru, Rh, Ir). By limiting the amount to 1 or less, the amount of Bi or the like adsorbed to the functional group of the ion exchange resin is limited to ensure the adsorption ability of the ion exchange resin to the platinum group element, and the ion exchange resin in the elution washing process after the adsorption There is little residue in
また、本発明の分離方法は白金族元素の吸着効果が高いので、イオン交換樹脂に使用量が比較的少量で済み、またイオン交換樹脂に吸着される白金族元素の濃度が高いので、回収率が向上する。 Further, since the separation method of the present invention has a high adsorption effect for the platinum group element, the amount used for the ion exchange resin is relatively small, and the concentration of the platinum group element adsorbed to the ion exchange resin is high, so that the recovery rate is high. Will improve.
以下、本発明を実施形態に基づいて具体的に説明する。
本発明の方法は、〔１〕白金族元素を含む溶液から、イオン交換樹脂を用いて白金族元素を選択的に吸着分離するときに、共存金属のＢｉ、Ｓｎ、Ｐｂの合計モル濃度(Ｍ１)と、白金族元素の合計モル濃度(Ｍ２)の比(Ｍ１/Ｍ２)を１以下に調整して白金族元素を吸着分離することを特徴とする白金族元素の分離方法である。
Hereinafter, the present invention will be specifically described based on embodiments.
In the method of the present invention, [1] when the platinum group element is selectively adsorbed and separated from the solution containing the platinum group element using an ion exchange resin, the total molar concentration of the coexisting metals Bi, Sn, and Pb (M1 ) And the total molar concentration (M2) of platinum group elements (M1 / M2) is adjusted to 1 or less, and the platinum group elements are adsorbed and separated.
白金族元素と共に他の金属（不純物金属）を含む溶液から、イオン交換法によって白金族元素を選択的に吸着分離するときに、白金族元素を吸着する一般的なイオン交換樹脂（弱塩基型イオン交換樹脂）を用いた場合、不純物金属の種類によっては白金族元素の吸着が大きく妨げられる。特にＢｉ、Ｓｎ、Ｐｂの影響が大きい。Ｃｕ、Ｓe、Ａｓなどは影響が少ない。 General ion exchange resin (weak base ion) that adsorbs platinum group elements when the platinum group elements are selectively adsorbed and separated by ion exchange from a solution containing other metals (impurity metals) together with platinum group elements. When an exchange resin is used, the adsorption of platinum group elements is greatly hindered depending on the type of impurity metal. In particular, the influence of Bi, Sn, and Pb is large. Cu, Se, As, etc. have little influence.
そこで、本発明の分離方法は、白金族元素と共存する不純物金属について、Ｂｉ、Ｓｎ、Ｐｂの濃度を制限し、Ｂｉ、Ｓｎ、Ｐｂの合計モル濃度(Ｍ１)を、白金族元素（Pt、Pd、Ru、Rh、Ir）の合計モル濃度(Ｍ２)に対して、Ｍ１/Ｍ２比を１以下に制御してイオン交換を行う。 Therefore, in the separation method of the present invention, the concentration of Bi, Sn, and Pb is limited for impurity metals that coexist with the platinum group element, and the total molar concentration (M1) of Bi, Sn, and Pb is changed to the platinum group element (Pt, Ion exchange is performed by controlling the M1 / M2 ratio to 1 or less with respect to the total molar concentration (M2) of Pd, Ru, Rh, Ir).
上記モル濃度比(Ｍ１/Ｍ２)を１以下に制御してイオン交換を行うことによって、図１に示すように、８５％以上の白金族元素の吸着率を得ることができる。モル濃度比(Ｍ１/Ｍ２)が概ね１を上回ると、このモル濃度比に比例して白金族元素の吸着率が低下し、Ｍ１/Ｍ２比が１.５では白金族元素の吸着率は約４０％に低下し、Ｍ１/Ｍ２比が２.０では白金族元素の吸着率は約１０％以下である。 By performing ion exchange while controlling the molar concentration ratio (M1 / M2) to 1 or less, as shown in FIG. 1, a platinum group element adsorption rate of 85% or more can be obtained. When the molar concentration ratio (M1 / M2) exceeds about 1, the adsorption rate of the platinum group element decreases in proportion to the molar concentration ratio. When the M1 / M2 ratio is 1.5, the adsorption rate of the platinum group element is about When the M1 / M2 ratio is 2.0, the platinum group element adsorption rate is about 10% or less.
白金族元素を含む溶液として、銅電解スライムを塩酸浸出し、この浸出液から金を分離した後液に亜硫酸ガスを導入して還元処理し、生じた固形物を酸と酸化剤によって浸出した液を用いることができる。 As a solution containing a platinum group element, copper electrolytic slime is leached with hydrochloric acid, gold is separated from the leached solution, sulfur dioxide gas is introduced into the solution, reduction treatment is performed, and the resulting solid is leached with an acid and an oxidizing agent. Can be used.
具体的には、例えば、脱銅精錬スライムは次のように処理される。まず、脱銅精錬スライムを塩酸および過酸化水素によってスラリーにし、これを濾過して主に銀を含む浸出滓と、金や白金族元素およびセレン、テルルを含む浸出液とに分離する。次に、この浸出液の液性を調整し、ＤＢＣ等を用いた溶媒抽出によって浸出液から金を分離する。このようにして金を分離した抽出残液には白金族元素やセレン、テルル、さらにはＢｉ、Ｓｎ、およびＰｂなどが液中に溶存している。そこで、この抽出残液に亜硫酸ガスを導入しセレンを還元沈殿させ、抽出残液から分離する。セレンを分離した濾液にさらに亜硫酸ガスを導入し、残りのセレンと共にテルルを還元して沈澱させる。なお、白金族元素はセレンやテルルと共に沈殿し、Ｂｉ、Ｓｎ、およびＰｂは液中に残る。これを濾別してセレンテルル白金族含有物を得ることができる。 Specifically, for example, the copper removal refining slime is processed as follows. First, the decopper refining slime is slurried with hydrochloric acid and hydrogen peroxide, and is filtered to separate into a leach cake containing mainly silver and a leach solution containing gold, platinum group elements, selenium and tellurium. Next, the liquid property of the leachate is adjusted, and gold is separated from the leachate by solvent extraction using DBC or the like. In the extraction residual liquid from which gold is thus separated, platinum group elements, selenium, tellurium, Bi, Sn, Pb, and the like are dissolved in the liquid. Therefore, sulfurous acid gas is introduced into the extraction residual liquid to reduce and precipitate selenium and separate from the extraction residual liquid. Sulfurous acid gas is further introduced into the filtrate from which selenium has been separated, and tellurium is reduced and precipitated together with the remaining selenium. The platinum group element is precipitated together with selenium and tellurium, and Bi, Sn, and Pb remain in the liquid. This can be filtered off to obtain a platinum group containing selenium tellurium.
このセレンテルル白金族含有物に酸化剤の存在下で塩酸を加えて白金族元素を溶解した後に固液分離し、濾別した白金族含有溶液から本発明の分離方法によって、白金族元素を選択的に分離することができる。この白金族含有溶液は、前段階で亜硫酸ガスを導入して白金族元素を沈澱化するときに、Ｂｉ、Ｓｎ、およびＰｂは液中に残るので、Ｍ１/Ｍ２＜１にすることができる。 To this selenium tellurium group-containing material, hydrochloric acid is added in the presence of an oxidant to dissolve the platinum group element, followed by solid-liquid separation and selective separation of the platinum group element from the filtered platinum group-containing solution by the separation method of the present invention. Can be separated. In this platinum group-containing solution, Bi, Sn, and Pb remain in the liquid when sulfurous acid gas is introduced in the previous step to precipitate the platinum group element, so that M1 / M2 <1.
以下、本発明の実施例を比較例と共に示す。
〔実施例１〜２〕
白金族元素と共に不純物としてＢｉ、Ｓｎ、およびＰｂを含む溶液について、イオン交換によって白金族元素を分離した。イオン交換樹脂として、弱塩基型イオン交換樹脂（商品名：ダイアイオンＷＡ−３０）を用いた。白金族元素含有溶液をイオン交換樹脂にＳＶ＝１の流速で通液し、吸着操作１０ＢＤの後に吸着率を調べた。
Ｂｉ＋Ｓｎ＋Ｐｂの合計モル濃度(Ｍ１)と白金族（Ｐｔ＋Ｐｄ＋Ｒｈ＋Ｒｕ＋Ｉｒ）の合計モル濃度(Ｍ２)の比（Ｍ１/Ｍ２）が約０.１、約０.８の試料について、Ｍ１/Ｍ２比に対する白金族元素の吸着率を図１に示した。
Examples of the present invention are shown below together with comparative examples.
[Examples 1-2]
For a solution containing Bi, Sn, and Pb as impurities together with the platinum group element, the platinum group element was separated by ion exchange. As the ion exchange resin, a weak base type ion exchange resin (trade name: Diaion WA-30) was used. The platinum group element-containing solution was passed through the ion exchange resin at a flow rate of SV = 1, and the adsorption rate was examined after the adsorption operation 10BD.
Platinum group element with respect to M1 / M2 ratio for samples with a ratio (M1 / M2) of the total molar concentration (M1) of Bi + Sn + Pb to the total molar concentration (M2) of platinum group (Pt + Pd + Rh + Ru + Ir) (M1 / M2) of about 0.1 The adsorption rate is shown in FIG.
〔比較例１〜２〕
Ｍ１/Ｍ２比が１.５、２.０の試料について、実施例１〜２と同様にしてイオン交換を行い、Ｍ１/Ｍ２比に対する白金族元素の吸着率を図１に示した。
[Comparative Examples 1-2]
Samples having an M1 / M2 ratio of 1.5 and 2.0 were subjected to ion exchange in the same manner as in Examples 1 and 2, and the adsorption rate of platinum group elements with respect to the M1 / M2 ratio is shown in FIG.
図１に示すように、実施例１および実施例２の試料は、Ｍ１/Ｍ２比が１より小さく、白金族元素の吸着率は約９５％〜約８５％であり、高い抽出効果が得られ。一方、比較例１および比較例２の試料は、Ｍ１/Ｍ２比が１より大きく、この比の増加に比例して白金族元素の吸着率は急激に低下し、Ｍ１/Ｍ２比が１.５では吸着率は約４０％以下であり、Ｍ１/Ｍ２比が２.０では白金族元素の吸着率は約１０％以下である。 As shown in FIG. 1, the samples of Example 1 and Example 2 have an M1 / M2 ratio smaller than 1, and the adsorption rate of platinum group elements is about 95% to about 85%, so that a high extraction effect is obtained. . On the other hand, the samples of Comparative Example 1 and Comparative Example 2 have an M1 / M2 ratio larger than 1, and the adsorption rate of the platinum group element rapidly decreases in proportion to the increase of this ratio, and the M1 / M2 ratio is 1.5. Then, the adsorption rate is about 40% or less, and when the M1 / M2 ratio is 2.0, the adsorption rate of the platinum group element is about 10% or less.
Claims (2)
When the platinum group element is selectively adsorbed and separated from the solution containing the platinum group element using an ion exchange resin, the total molar concentration (M1) of the coexisting metals Bi, Sn, and Pb and the total mole of the platinum group element A platinum group element separation method, wherein the ratio (M1 / M2) of the concentration (M2) is adjusted to 1 or less to adsorb and separate platinum group elements.
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Cited By (3)
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|---|---|---|---|---|
| JP2011208248A (en) * | 2010-03-30 | 2011-10-20 | Mitsubishi Materials Corp | Method for separating platinum group element |
| JP2016121399A (en) * | 2014-12-25 | 2016-07-07 | 三菱マテリアル株式会社 | Leaching method of valuable metal contained in copper removal slime |
| CN108085499A (en) * | 2017-12-13 | 2018-05-29 | 长沙汇聚环境技术有限公司 | A kind of separation and recovery method of tin bismuth waste material |
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| JPH03253524A (en) * | 1990-03-02 | 1991-11-12 | Tanaka Kikinzoku Kogyo Kk | Extracting agent and recovering method of palladium and platinum |
| JPH11229052A (en) * | 1998-02-19 | 1999-08-24 | Mitsubishi Materials Corp | Method of separating and removing platinum and palladium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2011208248A (en) * | 2010-03-30 | 2011-10-20 | Mitsubishi Materials Corp | Method for separating platinum group element |
| JP2016121399A (en) * | 2014-12-25 | 2016-07-07 | 三菱マテリアル株式会社 | Leaching method of valuable metal contained in copper removal slime |
| CN108085499A (en) * | 2017-12-13 | 2018-05-29 | 长沙汇聚环境技术有限公司 | A kind of separation and recovery method of tin bismuth waste material |
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