JP2013253816A - Solid extractant and method for extracting platinum group element - Google Patents
Solid extractant and method for extracting platinum group element Download PDFInfo
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Abstract
Description
本発明は、固体抽出剤及び白金族元素の抽出方法に係り、特に高レベル放射性廃液等の溶液から白金族元素を効率良く抽出する際に適用して好適な固体抽出剤及び白金族元素の抽出方法に関する。 The present invention relates to a solid extractant and a platinum group element extraction method, and particularly suitable for extraction of a platinum group element from a solution such as a high-level radioactive liquid waste, and suitable for extraction of the solid extractant and platinum group element. Regarding the method.
使用済み核燃料の再処理工程等で発生する高レベル放射性廃液は、最終的にガラス固化体として処理されることになっている。 The high-level radioactive liquid waste generated in the spent nuclear fuel reprocessing step or the like is finally treated as a glass solid.
このような高レベル放射性廃液中には、有用金属であるパラジウム（Ｐｄ）をはじめとする白金族元素（金属）が多く含まれているが、これら白金族元素は該廃液からガラス固化体を作製する際堆積し、ガラス固化を阻害する要因となっているために、該廃液から白金族元素を分離・回収する技術の開発が望まれていた。 Such high-level radioactive liquid waste contains a large amount of platinum group elements (metals), including palladium (Pd), which is a useful metal, and these platinum group elements produce a glass solid from the liquid waste. Therefore, development of a technique for separating and recovering the platinum group element from the waste liquid has been desired because it accumulates and becomes a factor that hinders vitrification.
このような要望に応える技術としては、例えば特許文献１に開示されているポリジフェニルビニルホスフィンオキシド（ＰＤＰＶＰＯ）や特許文献２に開示されているポリジアルキルビニルホスフィンオキシド（ＰＤＡＶＰＯ）からなるポリマー型抽出剤を利用し、高レベル放射性廃液から白金族元素を分離・回収することが考えられる。
As a technique that meets such a demand, for example, a polymer-type extractant comprising polydiphenylvinylphosphine oxide (PDPVPO) disclosed in
しかしながら、特許文献１に開示されているＰＤＰＶＰＯや特許文献２に開示されているＰＤＡＶＰＯは抽出剤として有効ではあるものの、粉末状のポリマーであるために比重が小さいことから、水溶液等の溶液を混合等により接触させる際には、有機溶媒に溶かして液−液抽出を採用する必要があるため、抽出後に有機溶媒を分離・回収しなければならないという問題があった。
However, although PDPVPO disclosed in
本発明は、前記従来の問題点を解決するべくなされたもので、有機溶媒を使用しない液−固抽出ができるために有機溶媒を分離・回収する必要がない上に、白金族元素に対する抽出性能にも優れた固体抽出剤及び白金族元素の抽出方法を提供することを課題とする。 The present invention has been made to solve the above-mentioned conventional problems. Since liquid-solid extraction without using an organic solvent can be performed, it is not necessary to separate and recover the organic solvent, and extraction performance with respect to platinum group elements. It is another object of the present invention to provide a solid extractant and a method for extracting a platinum group element which are excellent.
本発明者等は、有機溶媒を使用しない液−固抽出ができ、白金族元素に対する抽出性能にも優れた技術を提供するべく、ポリマー型抽出剤をビーズ化したポリマービーズ型抽出剤とポリマー型抽出剤をシリカに適正な範囲に担持したシリカ担持ポリマー型抽出剤を検討した。この結果シリカ担持ポリマー型抽出剤であるポリフェニルビニルスルフィド（ＰＰＶＳ）が、有機溶媒を使用しない液−固抽出ができる上に、優れた抽出特性を備えていることを知見した。 In order to provide a technique capable of performing liquid-solid extraction without using an organic solvent and having excellent extraction performance for platinum group elements, the present inventors have provided a polymer bead type extractant and a polymer type in which a polymer type extractant is beaded. A silica-supported polymer-type extractant in which the extractant was supported on silica in an appropriate range was investigated. As a result, it was found that polyphenyl vinyl sulfide (PPVS), which is a silica-supported polymer type extractant, can be liquid-solid extracted without using an organic solvent and has excellent extraction characteristics.
本発明は、上記知見に基づいてなされたもので、溶液から白金族元素を抽出する際に使用する固体抽出剤であって、ポリフェニルビニルスルフィドをシリカに０．１質量％〜５０質量％の割合に担持した構成とすることにより、前記課題を解決したものである。 The present invention has been made on the basis of the above knowledge, and is a solid extractant used when extracting a platinum group element from a solution, and 0.1% by mass to 50% by mass of polyphenylvinyl sulfide on silica. The above-mentioned problem is solved by adopting a configuration in which the ratio is supported.
本発明は、又、前記固体抽出剤に溶液を接触させ、該溶液から白金族元素を抽出することにより、同様に前記課題を解決したものである。 The present invention also solves the above problem by bringing a solution into contact with the solid extractant and extracting a platinum group element from the solution.
ここで、前記白金族元素をパラジウムとすることができる。 Here, the platinum group element may be palladium.
本発明によれば、固体抽出剤を、ポリフェニルビニルスルフィドをシリカに０．１質量％〜５０質量％の割合に担持して調製したことにより、該固体抽出剤に溶液を混合等により接触させ、該溶液から白金族元素を分離・回収する際、有機溶媒を使用せずに液−固抽出できる上に、優れた抽出率を得ることができた。 According to the present invention, the solid extractant was prepared by supporting polyphenylvinyl sulfide on silica at a ratio of 0.1% by mass to 50% by mass, whereby the solution was brought into contact with the solid extractant by mixing or the like. When separating and recovering the platinum group element from the solution, liquid-solid extraction was possible without using an organic solvent, and an excellent extraction rate could be obtained.
以下、図面を参照して、本発明の実施の形態について詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
本発明に係る固体抽出剤は、構造式
このＰＰＶＳは、（１）式の置換反応と（２）式の脱離反応により生成されるフェニルビニルスルフィド（モノマー）を、（３）式の重合反応により生成することができ、その後（４）式に示すように、シリカゲル（シリカ）：ＳｉＯ2に担持させることにより前記固体抽出剤を生成することができる。 This PPVS can produce phenyl vinyl sulfide (monomer) produced by the substitution reaction of the formula (1) and the elimination reaction of the formula (2) by the polymerization reaction of the formula (3), and then (4) As shown in the formula, the solid extractant can be produced by supporting silica gel (silica): SiO 2 .
（１）式、（２）式により合成したモノマーを（３）式により重合させ、質量平均分子量（Ｍｗ）が３６，９００、分子量分布（Ｍｗ／Ｍｎ）が１．６６のＰＰＶＳを得た。 The monomers synthesized by the formulas (1) and (2) were polymerized by the formula (3) to obtain PPVS having a mass average molecular weight (Mw) of 36,900 and a molecular weight distribution (Mw / Mn) of 1.66.
分子量は、カラムとして、Ｔｏｓｏｈ社製、商品名「ＧＭＨＨＲ−Ｈ＊２」を、溶媒としてＮ−メチル―２−ピロリドンを用い、ポリスチレンをスタンダードとしたゲルパーミエーションクロマトグラフィにより測定した。 The molecular weight was measured by gel permeation chromatography using Tosoh's product name “GMHHR-H * 2” as a column and N-methyl-2-pyrrolidone as a solvent and polystyrene as a standard.
次いで得られたＰＰＶＳを、異なる割合でシリカに担持させた複数の固体抽出剤を調製し、パラジウムに対する抽出率の評価を行った。 Next, a plurality of solid extractants in which the obtained PPVS was supported on silica at different ratios were prepared, and the extraction rate with respect to palladium was evaluated.
担持方法は、シリカとして、関東化学株式会社製 slica gel 60（シリカゲル，particle size 40-50μｍ）を使用し、前記（４）式に従ってＰＰＶＳのクロロホルム溶液に該シリカゲルを加え、室温で一晩攪拌した後、真空下で溶媒を除去して、ＰＰＶＳが担持されたシリカゲルを得た。 As the loading method, slica gel 60 (silica gel, particle size 40-50 μm) manufactured by Kanto Chemical Co., Inc. was used as silica, and the silica gel was added to a PPVS chloroform solution according to the formula (4) and stirred overnight at room temperature. Thereafter, the solvent was removed under vacuum to obtain silica gel carrying PPVS.
シリカに対するＰＰＶＳの担持割合が異なる９．１質量％と１６．７質量％の各固体抽出剤について、１モルの硝酸溶液に金属量０．０３ｍｍｏlの硝酸パラジウムを溶解したサンプル溶液を、抽出剤量同等条件の０．０３ｍｍｏlのイオウを含有する固体抽出剤と混合し、室温で１２時間攪拌した後ろ別し、ろ液中のパラジウム濃度をＩＰＣ発光分光分析装置（ＨＯＲＩＢＡ ＵＬＴＭＡ２）により測定して抽出率を求めた。 For each of the 9.1% by mass and 16.7% by mass solid extractants having different PPVS loading ratios on silica, a sample solution in which 0.03 mmol of palladium nitrate was dissolved in 1 mol of nitric acid solution was used as the extractant amount. The mixture was mixed with a solid extractant containing 0.03 mmol sulfur under the same conditions, stirred at room temperature for 12 hours, separated, and the palladium concentration in the filtrate was measured by an IPC emission spectrophotometer (HORIBA ULTMA2). Asked.
その結果を表１と図１のグラフに示す。 The results are shown in Table 1 and the graph of FIG.
なお、この固体抽出剤は、１原子のパラジウムに２原子のイオウが配位する錯形成により該パラジウムを捕捉し、抽出するものと考えられる。 This solid extractant is considered to capture and extract palladium by complex formation in which 2 atoms of sulfur coordinate to 1 atom of palladium.
この図１から、ＰＰＶＳをシリカに担持した固体抽出剤（以下、シリカ担持型抽出剤ともいう）としては、０．１質量％〜５０質量％の範囲の担持割合が有効であることがわかる。 As can be seen from FIG. 1, as the solid extractant having PPVS supported on silica (hereinafter also referred to as silica-supported extractant), a supported ratio in the range of 0.1% by mass to 50% by mass is effective.
担持割合が９．１質量％の固体抽出剤について、金属量０．００５ｍｍｏlのパラジウムイオンを含む１モルの硝酸酸性のサンプル溶液に対して０．０３ｍｍｏlのイオウを含有する抽出剤量を使用する、６０倍の抽出剤量過剰条件の下で、実施例１と同様の方法で抽出し、求めた抽出率を非担持のポリマー型抽出剤による結果と対比して表２に示す。 For a solid extractant with a loading ratio of 9.1% by weight, use an extractant amount containing 0.03 mmol sulfur with respect to a 1 mol nitric acid acidic sample solution containing 0.005 mmol metal palladium ions. Extraction was performed in the same manner as in Example 1 under the condition that the amount of the extractant was 60 times excessive, and the obtained extraction rate is shown in Table 2 in comparison with the result obtained with the unsupported polymer type extractant.
この表２は、次の構造式で表されるＰＶＳ−Ｃｏ−５ＭＭＡとＰＤＰＶＰＯの各ポリマーについてシリカ担持したものと非担持のものについて同様に抽出した結果をも併記してある。 Table 2 also shows the results of the same extraction of PVS-Co-5MMA and PDPVPO polymers supported by silica and those not supported by the following structural formula.
表２より、シリカ担持ポリマー型抽出剤（ＰＰＶＳ，ＰＶＳ−Ｃｏ−５ＭＭＡ）は、
非担持のポリマー型抽出剤と同等以上の抽出率を示している。
From Table 2, the silica-supported polymer type extractant (PPVS, PVS-Co-5MMA) is
The extraction rate is equal to or higher than that of the unsupported polymer type extractant.
表３には、前記表２に示したシリカ担持型と非担持のポリマー型の各ＰＰＶＳについて、放射線（γ線）照射による抽出率への影響を評価した結果を示す。照射した線量は１．０ＭＧｙである。 Table 3 shows the results of evaluating the influence of the radiation (γ-ray) irradiation on the extraction rate for each of the silica-supported and non-supported PPVSs shown in Table 2. The irradiated dose is 1.0 MGy.
この表より、いずれの抽出剤もγ線照射による悪影響は認められず高い抽出率を示し、高レベル放射線廃液を処理する過酷な条件でも使用可能であることがわかる。 From this table, it can be seen that any of the extractants shows a high extraction rate without any adverse effects due to γ-ray irradiation, and can be used even under severe conditions for treating high-level radioactive waste liquid.
なお、表３には、次式により得られるポリマービーズ型のＰＴＰＰＳ（Ｐoly Ｔri Ｐhenyl Ｐhosphine Ｓulfide）についての結果も併記してある。 Table 3 also shows the results of polymer bead type PPPPS (Poly Tri Phenyl Phosphine Sulfide) obtained by the following formula.
図２には、同様の抽出剤量過剰条件で測定した抽出速度をポリマービーズ型ＰＴＰＰＳと対比して示した。 FIG. 2 shows the extraction rate measured under the same condition of excess amount of the extractant in comparison with the polymer bead type PTPPS.
この図２より、ポリマービーズ型ＰＴＰＰＳの抽出速度は非常に緩やかで５時間でもパラジウムの抽出率が４０％であったのに対し、シリカ担持型ＰＰＶＳの抽出速度は非常に速く、１時間以内で抽出率が１００％となった。 From FIG. 2, the extraction rate of the polymer bead type PTPPS was very slow, and the extraction rate of palladium was 40% even in 5 hours, whereas the extraction rate of the silica-supported PPVS was very fast and within 1 hour. The extraction rate was 100%.
また、表４には、ポリマービーズ型ＰＴＰＰＳとシリカ担持型ＰＰＶＳによる抽出率と逆抽出率をそれぞれ示す。 Table 4 shows the extraction rate and back extraction rate of the polymer bead type PTPPS and the silica-supported type PPVS, respectively.
逆抽出率は、抽出後の抽出剤と溶液の混合系から水相を除去し、その抽出剤に３ｍｌの１モル尿酸（１モル硝酸溶液）を加え、室温で２４時間攪拌して溶解した後、その溶液のパラジウム濃度を測定して求めた。 The reverse extraction rate is obtained by removing the aqueous phase from the mixed system of extractant and solution after extraction, adding 3 ml of 1 molar uric acid (1 molar nitric acid solution) to the extractant, and stirring and dissolving at room temperature for 24 hours. The palladium concentration of the solution was measured and determined.
パラジウムに対する抽出率は、いずれの抽出剤でも１００％であった。パラジウムの逆抽出については、シリカ担持型ＰＰＶＳは１００％であったが、ポリマービーズ型ＰＴＰＰＳは約７７％と低かった。 The extraction ratio with respect to palladium was 100% for any of the extraction agents. Regarding the back extraction of palladium, the silica-supported PPVS was 100%, whereas the polymer bead type PTPPS was as low as about 77%.
表４には、逆抽出後のポリマー型抽出剤を硝酸で洗浄した後、再度抽出を行った繰り返し抽出の結果についても併記してある。この繰り返し抽出率は、いずれの抽出剤も１００％を示し、抽出剤の繰り返し使用が可能であることがわかった。以上の図２、表４の結果については、非特許文献１にも記載されている。
Table 4 also shows the results of repeated extraction in which the polymer-type extractant after back extraction was washed with nitric acid and then extracted again. This repeated extraction rate showed 100% for any extractant, and it was found that the extractant can be used repeatedly. The results shown in FIG. 2 and Table 4 are also described in
また表５には、同じ固体抽出剤について、他の白金族元素としてルテニウム（Ｒｕ）とロジウム（Ｒｈ）を含む溶液を、同様の条件により抽出率を測定した結果を示す。 Table 5 shows the results of measuring the extraction rate of a solution containing ruthenium (Ru) and rhodium (Rh) as other platinum group elements under the same conditions for the same solid extractant.
これにより、シリカ担持型ＰＰＶＳ及びポリマービーズ型ＰＴＰＰＳは、パラジウム抽出について高い選択性を備えていることがわかる。 Thereby, it turns out that silica carrying type PPVS and polymer bead type PTPPS have high selectivity about palladium extraction.
以上詳述したように、シリカにポリマー型抽出剤のＰＰＶＳを担持したシリカ担持型ＰＰＶＳは、０．１質量％〜５０質量％の範囲の担持割合において、優れた抽出特性を有し、特にパラジウムに対して有効な抽出剤であることがわかった。 As described in detail above, silica-supported PPVS in which PPVS as a polymer-type extractant is supported on silica has excellent extraction characteristics at a loading ratio in the range of 0.1% by mass to 50% by mass, particularly palladium. It was found that this is an effective extractant.
また、シリカ担持型ＰＰＶＳは、抽出速度がポリマービーズ型ＰＴＰＰＳと比較して非常に速い上に、逆抽出率と繰り返し抽出率は共に１００％を示し、しかもパラジウムに対して優れた選択性を示すことからパラジウムに対しては最適な抽出剤であることもわかった。 Silica-supported PPVS has a very high extraction rate compared to polymer bead type PTPPS, and both the back extraction rate and the repeat extraction rate are 100%, and it exhibits excellent selectivity for palladium. Therefore, it was also found that it is an optimum extractant for palladium.
なお、以上詳述したポリマー型抽出剤に関しては非特許文献３に、ポリマービーズ型抽出剤とシリカ担持ポリマー型抽出剤に関しては非特許文献２にも記載されている。
The polymer type extractant detailed above is described in
Claims (4)
ポリフェニルビニルスルフィドをシリカに０．１質量％〜５０質量％の割合に担持したことを特徴とする固体抽出剤。 A solid extractant used to extract a platinum group element from a solution,
A solid extractant characterized in that polyphenylvinyl sulfide is supported on silica in a proportion of 0.1% by mass to 50% by mass.
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| CN112206750A (en) * | 2020-09-07 | 2021-01-12 | 中南大学 | Material for selectively adsorbing palladium and preparation method and application thereof |
| CN112206749A (en) * | 2020-09-07 | 2021-01-12 | 中南大学 | Material for selectively adsorbing platinum and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112206750A (en) * | 2020-09-07 | 2021-01-12 | 中南大学 | Material for selectively adsorbing palladium and preparation method and application thereof |
| CN112206749A (en) * | 2020-09-07 | 2021-01-12 | 中南大学 | Material for selectively adsorbing platinum and preparation method and application thereof |
| CN112206749B (en) * | 2020-09-07 | 2021-10-08 | 中南大学 | Material for selectively adsorbing platinum and preparation method and application thereof |
| CN112206750B (en) * | 2020-09-07 | 2021-10-12 | 中南大学 | Material for selectively adsorbing palladium and preparation method and application thereof |
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