JP2014019898A - Method for recovering rhenium - Google Patents

Method for recovering rhenium Download PDF

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JP2014019898A
JP2014019898A JP2012159070A JP2012159070A JP2014019898A JP 2014019898 A JP2014019898 A JP 2014019898A JP 2012159070 A JP2012159070 A JP 2012159070A JP 2012159070 A JP2012159070 A JP 2012159070A JP 2014019898 A JP2014019898 A JP 2014019898A
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rhenium
iron ions
containing liquid
recovery method
precipitate
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JP5881551B2 (en
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Shohei Kanemura
祥平 金村
Koji Mizuguchi
浩司 水口
Yuya Takahashi
優也 高橋
Takeo Yamashita
雄生 山下
Yumi Yaita
由美 矢板
Tetsuo Osato
哲夫 大里
Takashi Omori
孝 大森
Takashi Yazawa
孝 矢澤
Reiko Fujita
玲子 藤田
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Toshiba Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a method for recovering rhenium not using an ion exchange resin or a solvent extraction method.SOLUTION: The method for recovering rhenium comprises: a step (S11) of adding bivalent iron ions (Fe)to a rhenium-containing liquid 1a; a step (S12) of adding a Ph regulator 3 to precipitate rhenium; a step (S13) of recovering precipitates 5 from a mother liquid 4 by solid-liquid separation; and a step of adding acid to the precipitates 5 to dissolve rhenium (S14) and producing a rhenium-concentrated liquid 6.

Description

本発明は、含有濃度が低いレニウムの回収方法に関する。   The present invention relates to a method for recovering rhenium having a low content concentration.

近年、航空機タービンに用いられ耐高温材料であるＮｉ基スーパーアロイの原料として、レニウムの需要が高まっている。
一般的にレニウムは、モリブデンや銅鉱石中に微少量含まれており、鉱石溶解後のレニウムは、過レニウム酸イオン（ＲｅＯ4-)として他の不純物元素と共に溶液中に存在している。
従来の回収プロセスは、溶媒抽出法やイオン交換法を用い、これら他の不純物元素からレニウムを分離し、精製濃縮を行っていた。
そして、この精製濃縮させた過レニウム酸イオン溶液に塩化カリウムを加え、析出させた過レニウム酸カリウムを、ろ過して水素還元を行うことで金属レニウムを得ることができる。 In recent years, demand for rhenium has been increasing as a raw material for Ni-based superalloys, which are high-temperature resistant materials used in aircraft turbines.
Generally, rhenium is contained in a very small amount in molybdenum or copper ore, and rhenium after ore dissolution is present in the solution together with other impurity elements as perrhenate ion (ReO 4− ).
Conventional recovery processes used solvent extraction and ion exchange methods to separate rhenium from these other impurity elements and perform purification and concentration.
Then, rhenium metal can be obtained by adding potassium chloride to the purified perrhenate ion solution and filtering the precipitated potassium perrhenate to perform hydrogen reduction.

昨今、レアメタルの需要が急増しており、レアメタル濃度の高い高品位鉱石からだけでなく、レアメタル濃度の低い低品位鉱石や従来は廃棄していた残渣から、レアメタルを回収することが試みられている。
また、レニウムを含むタービンや触媒からのリサイクルも行われている。このような含有濃度が低いレアメタルを回収するためには、レアメタルの濃縮が必須であり、濃縮方法としてイオン交換法や溶媒抽出法が用いられている（例えば、非特許文献１）。 In recent years, the demand for rare metals has increased rapidly, and attempts have been made to recover rare metals not only from high-grade ores with a high concentration of rare metals, but also from low-grade ores with a low concentration of rare metals and residues that were previously discarded. .
Recycling from rhenium-containing turbines and catalysts is also performed. In order to recover such a rare metal having a low content concentration, it is essential to concentrate the rare metal, and an ion exchange method or a solvent extraction method is used as a concentration method (for example, Non-Patent Document 1).

原子力学会Ｖｏ１２４．Ｎｏ２，ｐ１５０（１９８２）Atomic Energy Society Vo124. No2, p150 (1982)

従来では廃棄されるような低品位鉱石や廃液から低濃度のレニウムを回収する場合、不純物の影響によりイオン交換樹脂や溶媒抽出法を適用できず、濃縮が困難であった。   Conventionally, when low-level rhenium is recovered from low-grade ore or waste liquid that is discarded, ion exchange resins and solvent extraction methods cannot be applied due to the influence of impurities, making concentration difficult.

本発明はこのような事情を考慮してなされたもので、イオン交換樹脂又は溶媒抽出法を用いないレニウムの回収方法を提供することを目的とする。   The present invention has been made in view of such circumstances, and an object thereof is to provide a method for recovering rhenium without using an ion exchange resin or a solvent extraction method.

レニウム回収方法は、レニウム含有液に二価鉄イオンを添加する工程と、ｐＨ調整剤を添加してレニウムを沈殿させる工程と、固液分離により沈殿物を回収する工程と、前記沈殿物に酸を添加してレニウムを溶解しレニウム濃縮液を生成する工程と、を含むことを特徴とする。   The rhenium recovery method includes a step of adding divalent iron ions to a rhenium-containing liquid, a step of adding rhedium to precipitate a rhenium, a step of recovering the precipitate by solid-liquid separation, and an acid in the precipitate. And a step of dissolving rhenium to produce a rhenium concentrate.

本発明により、イオン交換樹脂又は溶媒抽出法を用いないレニウムの回収方法が提供される。   According to the present invention, a method for recovering rhenium without using an ion exchange resin or a solvent extraction method is provided.

本発明に係るレニウムの回収方法の第１実施形態を示す工程図。1 is a process diagram showing a first embodiment of a rhenium recovery method according to the present invention. レニウム含有溶液において調整された水素イオン濃度（ｐＨ）に対するレニウムの沈殿率を示すグラフ。The graph which shows the precipitation rate of rhenium with respect to the hydrogen ion concentration (pH) adjusted in the rhenium containing solution. 本発明に係るレニウムの回収方法の第２実施形態を示す工程図。Process drawing which shows 2nd Embodiment of the collection | recovery method of rhenium based on this invention. 本発明に係るレニウムの回収方法の第３実施形態を示す工程図。Process drawing which shows 3rd Embodiment of the collection | recovery method of rhenium based on this invention. 第３実施形態に適用される電解槽の構成図。The block diagram of the electrolytic cell applied to 3rd Embodiment.

（第１実施形態）
以下、本発明の実施形態を添付図面に基づいて説明する。
図１に示すように、第１実施形態に係るレニウムの回収方法は、レニウム含有液１ａに二価鉄イオン（Ｆｅ2+）を添加する工程（Ｓ１１）と、ｐＨ調整剤３を添加してレニウムを沈殿させる工程（Ｓ１２）と、固液分離により母液４から沈殿物５を回収する工程（Ｓ１３）と、この沈殿物５に酸を添加してレニウムを溶解し（Ｓ１４）、レニウム濃縮液６を生成する工程と、を含んでいる。 (First embodiment)
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings.
As shown in FIG. 1, the rhenium recovery method according to the first embodiment includes a step (S11) of adding divalent iron ions (Fe 2+ ) to the rhenium-containing liquid 1a and a pH adjuster 3 added. A step of precipitating rhenium (S12), a step of recovering the precipitate 5 from the mother liquor 4 by solid-liquid separation (S13), an acid is added to the precipitate 5 to dissolve rhenium (S14), and a rhenium concentrate 6 is generated.

鉄イオン添加工程（Ｓ１１）において、レニウム含有液１ａに添加される二価の鉄イオンＦｅ2+の形態としては、硫酸鉄(II)や塩化鉄(II)などの２価のＦｅ塩が挙げられる。
レニウム沈殿工程（Ｓ１２）において、Ｆｅ2+が添加されたレニウム含有液１ａの水素イオン濃度を、ｐＨ調整剤３の添加によりｐＨ７よりも大きく設定する。このように、溶液をアルカリ性に設定すると、イオンとして存在するレニウム（VII）が、Ｆｅ2+により還元されて酸化レニウム(IVまたはVI)に変化し、水酸化鉄とともに共沈し沈殿物５に移行する。
ｐＨ調整剤３としては、一般的に用いられる水酸化ナトリウムやアンモニア水が使用可能であるが、特に限定はない。 In the iron ion addition step (S11), examples of the form of the divalent iron ion Fe 2+ added to the rhenium-containing liquid 1a include divalent Fe salts such as iron (II) sulfate and iron (II) chloride. It is done.
In the rhenium precipitation step (S12), the hydrogen ion concentration of the rhenium-containing liquid 1a to which Fe 2+ is added is set to be higher than pH 7 by the addition of the pH adjuster 3. Thus, when the solution is set to be alkaline, rhenium (VII) existing as ions is reduced by Fe 2+ to change to rhenium oxide (IV or VI), and coprecipitated with iron hydroxide to precipitate 5. Transition.
As the pH adjuster 3, commonly used sodium hydroxide or aqueous ammonia can be used, but there is no particular limitation.

固液分離工程（Ｓ１３）において母液から分離回収された沈殿物５は、さらに酸溶解工程（Ｓ１４）において添加される少量の酸（例えば、硝酸、塩酸、硫酸の中から選択される少なくとも１種の化合物）に溶解し、レニウム濃縮液６を得る。   The precipitate 5 separated and recovered from the mother liquor in the solid-liquid separation step (S13) is at least one selected from a small amount of acid (for example, nitric acid, hydrochloric acid, sulfuric acid) added in the acid dissolution step (S14). To obtain rhenium concentrate 6.

図２のグラフは、レニウム含有溶液において調整された水素イオン濃度（ｐＨ）に対するレニウムの沈殿率を示している。
この図２より、二価鉄イオン（Ｆｅ2+）を含むレニウム（Ｒｅ）含有溶液では、水素イオン濃度をｐＨ７以上に設定することにより、レニウム（Ｒｅ）の沈殿回収が可能であることが示される。 The graph of FIG. 2 shows the rhenium precipitation rate versus the adjusted hydrogen ion concentration (pH) in the rhenium-containing solution.
FIG. 2 shows that in the rhenium (Re) -containing solution containing divalent iron ions (Fe 2+ ), the precipitation recovery of rhenium (Re) is possible by setting the hydrogen ion concentration to pH 7 or higher. It is.

（第２実施形態）
図３に示すように第２実施形態に係るレニウムの回収方法は、レニウム含有液１ｂは、鉄イオンを固有に含有し、二価鉄イオン（Ｆｅ2+）の添加工程（Ｓ１１；図１）は、このレニウム含有液１ｂに還元剤７を投入し含有する鉄イオンの価数調整を行う工程（Ｓ２１）で実行される。
なお、図２において図１と共通の工程は、同一符号で示し、重複する説明を省略する。 (Second Embodiment)
As shown in FIG. 3, in the method for recovering rhenium according to the second embodiment, the rhenium-containing liquid 1b inherently contains iron ions, and a divalent iron ion (Fe 2+ ) addition step (S11; FIG. 1). Is performed in the step (S21) of adjusting the valence of the iron ions contained in the rhenium-containing liquid 1b by introducing the reducing agent 7 therein.
In FIG. 2, steps common to FIG. 1 are denoted by the same reference numerals, and redundant description is omitted.

図２のグラフで示されるように、レニウム（Ｒｅ）の沈殿は三価鉄イオン（Ｆｅ3+）の存在下では、ほとんど生じない。
しかし、金属製品からレニウム（Ｒｅ）を回収すると、この三価鉄イオン（Ｆｅ3+）が含まれている場合が多分にある。 As shown in the graph of FIG. 2, the precipitation of rhenium (Re) hardly occurs in the presence of trivalent iron ions (Fe 3+ ).
However, when rhenium (Re) is recovered from a metal product, this trivalent iron ion (Fe 3+ ) is often included.

そこで、鉄イオン価数調整工程（Ｓ２１）において、鉄を含むレニウム含有液１ｂに、例えばヒドラジンなどの還元剤７を添加し、含まれる三価鉄イオン（Ｆｅ3+）を二価鉄イオン（Ｆｅ2+）に調整する。
これにより、その後のレニウム沈殿工程（Ｓ１２）において、イオンとして存在するレニウム（VII）を、酸化レニウム(IVまたはVI)として沈殿物５に移行させることが可能となる。 Therefore, in the iron ion valence adjusting step (S21), a reducing agent 7 such as hydrazine is added to the rhenium-containing liquid 1b containing iron, and the contained trivalent iron ions (Fe 3+ ) are converted to divalent iron ions (Fe 3+ ). To Fe 2+ ).
Thereby, in the subsequent rhenium precipitation step (S12), rhenium (VII) existing as ions can be transferred to the precipitate 5 as rhenium oxide (IV or VI).

（第３実施形態）
図４に示すように第３実施形態に係るレニウムの回収方法は、レニウム含有液１ｂは、鉄イオンを固有に含有し、二価鉄イオン（Ｆｅ2+）の添加（図１；Ｓ１１）は、レニウム含有液１ｂを電解して含有する鉄イオンの価数調整を行う工程（Ｓ３１）で実行される。
なお、図２において図３と共通の工程は、同一符号で示し、重複する説明を省略する。 (Third embodiment)
As shown in FIG. 4, in the rhenium recovery method according to the third embodiment, the rhenium-containing liquid 1b inherently contains iron ions, and the addition of divalent iron ions (Fe 2+ ) (FIG. 1; S11) This is carried out in the step (S31) of adjusting the valence of the iron ion containing the rhenium-containing liquid 1b by electrolysis.
In FIG. 2, steps common to FIG. 3 are denoted by the same reference numerals, and redundant description is omitted.

鉄を含むレニウム含有液１ｂがレニウムの回収対象として多量に存在するときは、第２実施形態のように還元剤７を添加することが困難である。
このような場合には、鉄イオン電解価数調整工程（Ｓ３１）において、含まれる三価鉄イオン（Ｆｅ3+）を二価鉄イオン（Ｆｅ2+）に還元するとよい。 When the rhenium-containing liquid 1b containing iron is present in a large amount as a rhenium recovery target, it is difficult to add the reducing agent 7 as in the second embodiment.
In such a case, in the iron ion electrolytic valence adjustment step (S31), the contained trivalent iron ions (Fe 3+ ) may be reduced to divalent iron ions (Fe 2+ ).

図５に示すように、この鉄イオン電解価数調整工程（Ｓ３１）に適用される電解槽１０は、隔膜１５により隔離された陰極１１と陽極１２が、それぞれ直流電源１３の両端に接続されている。   As shown in FIG. 5, the electrolytic cell 10 applied to the iron ion electrolytic valence adjusting step (S31) has a cathode 11 and an anode 12 separated by a diaphragm 15 connected to both ends of a DC power supply 13, respectively. Yes.

陰極１１に鉄を含むレニウム含有液１６（１ｂ）を装荷した状態で、直流電源１３から電圧を印加し電解すると、陰極１１及び陽極１２において、それぞれ次の電解反応が起きる。
陰極：Ｆｅ3+ ＋ ｅ- → Ｆｅ2+
陽極：２Ｈ2Ｏ → ２Ｈ2 + Ｏ2 + ４ｅ- When the rhenium-containing liquid 16 (1b) containing iron is loaded on the cathode 11 and a voltage is applied from the DC power source 13 to perform electrolysis, the following electrolytic reaction occurs at the cathode 11 and the anode 12, respectively.
Cathode: Fe 3+ + e − → Fe 2+
Anode: 2H 2 O → 2H 2 + O 2 + 4e −

なお、この電解反応は、参照電極１４と陰極１１との間の陰極電位が０．７７Ｖ ｖｓ ＳＨＥより卑な電位に設定することにより、陰極１１において三価鉄イオン（Ｆｅ3+）を二価鉄イオン（Ｆｅ2+）に還元することができる。
さらに、この陰極電位を水素発生が起きる電位よりも貴な電位に設定することにより、高い電流効率で三価鉄イオン（Ｆｅ3+）を二価鉄イオン（Ｆｅ2+）に還元することができる。 In this electrolytic reaction, the cathode potential between the reference electrode 14 and the cathode 11 is set to a potential lower than 0.77 V vs SHE, whereby trivalent iron ions (Fe 3+ ) are divalently converted at the cathode 11. It can be reduced to iron ions (Fe 2+ ).
Furthermore, by setting this cathode potential to a potential more noble than the potential at which hydrogen generation occurs, trivalent iron ions (Fe 3+ ) can be reduced to divalent iron ions (Fe 2+ ) with high current efficiency. it can.

このように電解反応を利用することにより、還元剤７等を用いることなく、三価鉄イオン（Ｆｅ3+）を二価鉄イオン（Ｆｅ2+）に還元することができる。
そして、その後のレニウム沈殿工程（Ｓ１２）において、イオンとして存在するレニウム（VII）を、酸化レニウム(IVまたはVI)として沈殿物５に移行させることが可能となる。 By using the electrolytic reaction in this way, trivalent iron ions (Fe 3+ ) can be reduced to divalent iron ions (Fe 2+ ) without using the reducing agent 7 or the like.
In the subsequent rhenium precipitation step (S12), rhenium (VII) existing as ions can be transferred to the precipitate 5 as rhenium oxide (IV or VI).

以上述べた少なくともひとつの実施形態のレニウムの回収方法によれば、レニウム含有液に二価鉄イオンを存在させることにより、イオン交換樹脂又は溶媒抽出法を用いずに、低濃度のレニウムを溶液から高効率的で回収することが可能となる。   According to the method for recovering rhenium of at least one embodiment described above, by allowing divalent iron ions to be present in the rhenium-containing liquid, a low concentration of rhenium can be removed from the solution without using an ion exchange resin or a solvent extraction method. It is highly efficient and can be recovered.

本発明のいくつかの実施形態を説明したが、これらの実施形態は、例として提示したものであり、発明の範囲を限定することは意図していない。これら実施形態は、その他の様々な形態で実施されることが可能であり、発明の要旨を逸脱しない範囲で、種々の省略、置き換え、変更、組み合わせを行うことができる。これら実施形態やその変形は、発明の範囲や要旨に含まれると同様に、特許請求の範囲に記載された発明とその均等の範囲に含まれるものである。   Although several embodiments of the present invention have been described, these embodiments are presented by way of example and are not intended to limit the scope of the invention. These embodiments can be implemented in various other forms, and various omissions, replacements, changes, and combinations can be made without departing from the scope of the invention. These embodiments and their modifications are included in the scope and gist of the invention, and are also included in the invention described in the claims and the equivalents thereof.

１ａ，１ｂ…レニウム含有液、３…ｐＨ調整剤、４…母液、５…沈殿物、６…レニウム濃縮液、７…還元剤、１０…電解槽、１１…陰極、１２…陽極、１３…直流電源、１４…参照電極、１５…隔膜、１６…鉄を含むレニウム含有液。   DESCRIPTION OF SYMBOLS 1a, 1b ... Rhenium containing liquid, 3 ... pH adjuster, 4 ... Mother liquor, 5 ... Precipitate, 6 ... Rhenium concentrate, 7 ... Reducing agent, 10 ... Electrolyzer, 11 ... Cathode, 12 ... Anode, 13 ... DC Power source, 14 ... reference electrode, 15 ... diaphragm, 16 ... rhenium-containing liquid containing iron.

Claims (7)

レニウム含有液に二価鉄イオンを添加する工程と、
ｐＨ調整剤を添加してレニウムを沈殿させる工程と、
固液分離により母液から沈殿物を回収する工程と、
前記沈殿物に酸を添加してレニウムを溶解しレニウム濃縮液を生成する工程と、を含むことを特徴とするレニウム回収方法。 Adding divalent iron ions to the rhenium-containing liquid;
adding a pH adjuster to precipitate rhenium;
Collecting the precipitate from the mother liquor by solid-liquid separation;
Adding an acid to the precipitate to dissolve rhenium to form a rhenium concentrate, and a method for recovering rhenium. 前記レニウム含有液は、鉄イオンを固有に含有し、
前記二価鉄イオンの添加は、前記レニウム含有液に還元剤を投入し含有する前記鉄イオンの価数調整を行うことによる請求項１に記載のレニウム回収方法。 The rhenium-containing liquid inherently contains iron ions,
The rhenium recovery method according to claim 1, wherein the addition of the divalent iron ion is performed by adjusting the valence of the iron ion contained in the rhenium-containing liquid by introducing a reducing agent. 前記レニウム含有液は、鉄イオンを固有に含有し、
前記二価鉄イオンの添加は、前記レニウム含有液を電解して含有する前記鉄イオンの価数調整を行うことによる請求項１に記載のレニウム回収方法。 The rhenium-containing liquid inherently contains iron ions,
The rhenium recovery method according to claim 1, wherein the addition of the divalent iron ions is performed by adjusting the valence of the iron ions contained by electrolyzing the rhenium-containing liquid. 前記ｐＨ調整剤は、水素イオン濃度がｐＨ７以上になるように添加される請求項１から請求項３のいずれか１項に記載のレニウム回収方法。   The rhenium recovery method according to any one of claims 1 to 3, wherein the pH adjuster is added so that a hydrogen ion concentration becomes pH 7 or more. 前記酸は、塩酸、硝酸及び硫酸の中から選択される少なくとも１種の化合物である請求項１から請求項４のいずれか１項に記載のレニウム回収方法。   The rhenium recovery method according to any one of claims 1 to 4, wherein the acid is at least one compound selected from hydrochloric acid, nitric acid, and sulfuric acid. 前記電解は、隔膜により陰極と陽極が隔離された電解槽を用い、前記陰極室において前記鉄イオンの価数調整を行う請求項３から請求項５のいずれか１項に記載のレニウム回収方法。   The rhenium recovery method according to any one of claims 3 to 5, wherein the electrolysis uses an electrolytic cell in which a cathode and an anode are separated by a diaphragm, and valence adjustment of the iron ions is performed in the cathode chamber. 前記電解は、陰極電位が０．７７Ｖ ｖｓ ＳＨＥより卑かつ水素発生が起きる電位よりも貴な電位で行う請求項３から請求項６のいずれか１項に記載のレニウム回収方法。   The rhenium recovery method according to any one of claims 3 to 6, wherein the electrolysis is performed at a cathode potential lower than 0.77V vs SHE and a potential higher than a potential at which hydrogen generation occurs.
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