JP4590585B2 - A method of back-extracting Am (III) and Pu (IV) in an organic solvent into a nitric acid solution with an N, N, N ', N'-tetramethyldiglycolamide (TMDGA) compound - Google Patents
A method of back-extracting Am (III) and Pu (IV) in an organic solvent into a nitric acid solution with an N, N, N ', N'-tetramethyldiglycolamide (TMDGA) compound Download PDFInfo
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- JP4590585B2 JP4590585B2 JP2004172218A JP2004172218A JP4590585B2 JP 4590585 B2 JP4590585 B2 JP 4590585B2 JP 2004172218 A JP2004172218 A JP 2004172218A JP 2004172218 A JP2004172218 A JP 2004172218A JP 4590585 B2 JP4590585 B2 JP 4590585B2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 11
- QLFOOTHTIJUSHB-UHFFFAOYSA-N 2-[2-(dimethylamino)-2-oxoethoxy]-n,n-dimethylacetamide Chemical compound CN(C)C(=O)COCC(=O)N(C)C QLFOOTHTIJUSHB-UHFFFAOYSA-N 0.000 title claims description 3
- 150000001875 compounds Chemical class 0.000 title description 6
- 239000003960 organic solvent Substances 0.000 title description 2
- 229910052768 actinide Inorganic materials 0.000 claims description 10
- -1 actinide ions Chemical class 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- VRZYWIAVUGQHKB-UHFFFAOYSA-N 2-[2-(dioctylamino)-2-oxoethoxy]-n,n-dioctylacetamide Chemical compound CCCCCCCCN(CCCCCCCC)C(=O)COCC(=O)N(CCCCCCCC)CCCCCCCC VRZYWIAVUGQHKB-UHFFFAOYSA-N 0.000 claims description 7
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 229940094933 n-dodecane Drugs 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 description 8
- 239000012074 organic phase Substances 0.000 description 8
- 239000008139 complexing agent Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 5
- 239000002915 spent fuel radioactive waste Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000011165 process development Methods 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- CNDWHJQEGZZDTQ-UHFFFAOYSA-N 2-(2-amino-2-oxoethoxy)acetamide Chemical compound NC(=O)COCC(N)=O CNDWHJQEGZZDTQ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000009918 complex formation Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000002927 high level radioactive waste Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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- Extraction Or Liquid Replacement (AREA)
Description
原子力分野では、使用済み燃料又は高レベル放射性廃液から、３，４価のアクチノイドイオンを抽出した後に効率的に逆抽出することはプロセス開発上重要であり、本発明の方法はこれら金属を逆抽出する方法に関わる。 In the nuclear power field, it is important for process development to extract the trivalent and tetravalent actinide ions from spent fuel or high-level radioactive liquid waste, and it is important for process development. The method of the present invention back-extracts these metals. Involved in how to do.
３，４価のアクチノイドイオンを逆抽出することは、これまでには薄い硝酸溶液などを用いる方法、クエン酸、アミノポリカルボン酸などの水溶性錯形成剤を用いる方法、さらに原子価を変える方法などを用いている。 The back-extraction of trivalent and tetravalent actinide ions can be achieved by a method using a thin nitric acid solution, a method using a water-soluble complexing agent such as citric acid or aminopolycarboxylic acid, and a method of changing the valence. Etc. are used.
プロセス開発において、Ｎｐ（ＩＶ），Ｐｕ（ＩＩＩ）Ｐｕ（ＩＶ），Ａｍ（ＩＩＩ），およびＣｍ（ｍ）のような３，４価のアクチノイドイオンを抽出した後に水相に逆抽出することは使用済み燃料再処理などのプロセス開発において重要な課題である。従来法の主要な課題は次のとおりである。 In process development, extracting trivalent and tetravalent actinide ions such as Np (IV), Pu (III) Pu (IV), Am (III), and Cm (m) and back-extracting them into the aqueous phase is This is an important issue in process development such as spent fuel reprocessing. The main problems of the conventional method are as follows.
（１）酸性度を薄くしすぎた場合、特にＰｕ（ＩＶ）は水酸化物を形成し沈殿を生ずる。
（２）クエン酸、ＥＤＴＡ（エチレンジアミン四酢酸）のような錯形成剤では、使用で
きるｐＨ条件が高く（ｐＨ＞３）、Ｐｕ（ＩＶ）の水酸化物沈殿する可能性がある。硝酸溶液でも使用可能なシュウ酸はＰｕ（ＩＶ）と沈殿を生成し、またＤＴＰＡ（ジエチレントリアミン五酢酸）に関しては硝酸溶液への溶解度が低い（最大５０ｍＭ程度）。これらの錯形成剤は下の参考文献１−３で参照できる（非特許文献１，２及び３）。
(1) When acidity is made too thin, Pu (IV) forms a hydroxide and precipitates.
(2) With complexing agents such as citric acid and EDTA (ethylenediaminetetraacetic acid), the usable pH conditions are high (pH> 3), and there is a possibility that Pu (IV) hydroxide precipitates. Oxalic acid that can also be used in a nitric acid solution forms a precipitate with Pu (IV), and DTPA (diethylenetriaminepentaacetic acid) has low solubility in nitric acid solution (up to about 50 mM). These complexing agents can be referred to in References 1-3 below (
（３）原子価を変える方法をとる場合、強い還元剤を用いることになる上に溶液内反応が複雑になる。また原子価を変える方法はＴＯＤＧＡ抽出剤のようにＡｎ（ＩＩＩ），（ＩＶ）ともに強く錯形成する化合物にはそのままでは使用する事ができない。
（１）本発明の目的の錯形成剤は、０．２Ｍ硝酸濃度条件でもＡｎ（ＩＩＩ），（ＩＶ）の分配比を十分に下げることのできる化合物である。また、３Ｍ程度の硝酸溶液からでもＰｕ（ＩＶ）の分配比を下げる事ができ、逆抽出の際に水酸化物形成を完全に抑制できる。（２）本発明の目的の錯形成剤は０．２Ｍ硝酸溶液に十分溶解可能であり、この時に１Ｍ ＴＭＤＧＡの溶液を調製する事が可能である。また濃硝酸でも十分な溶解度を示し、一方有機相には殆ど溶解しない。（３）本発明の目的の錯形成剤は２次廃棄物発生量を低減できる、炭素、水素、酸素、窒素からなる化合物である。（４）本発明の目的の錯形成剤は中性の化合物であり、錯形成時にＰｕ（ＩＶ）と沈殿を生成しない。 (1) The complexing agent of the present invention is a compound that can sufficiently reduce the distribution ratio of An (III) and (IV) even under a 0.2M nitric acid concentration condition. Moreover, the distribution ratio of Pu (IV) can be lowered even from about 3M nitric acid solution, and hydroxide formation can be completely suppressed during back extraction. (2) The complexing agent of the present invention can be sufficiently dissolved in a 0.2 M nitric acid solution, and at this time, a 1 M TMDGA solution can be prepared. Concentrated nitric acid also shows sufficient solubility, while it hardly dissolves in the organic phase. (3) The complexing agent of the object of the present invention is a compound composed of carbon, hydrogen, oxygen, and nitrogen that can reduce the amount of secondary waste generated. (4) The complexing agent of the object of the present invention is a neutral compound, and does not produce Pu (IV) and precipitates during complex formation.
本発明においては、以上の課題を解決すべき錯形成剤を見出した。即ち、本発明は、ＤＧＡ（ジグリコールアミド）化合物の一つである、ＴＭＤＧＡ（Ｎ，Ｎ，Ｎ’，Ｎ’−テトラメチル−１，３−オキサペンタンジアミド）を開発した。即ち、本発明は、Ｎ，Ｎ，Ｎ'，Ｎ'−テトラメチルジグリコールアミド（ＴＭＤＧＡ）化合物により有機溶媒中のＡｍ（ＩＩＩ），Ｐｕ（ＩＶ）を硝酸溶液に逆抽出する方法である。 In the present invention, the complexing agent which should solve the above-mentioned subject was found. That is, the present invention has developed TMDGA (N, N, N ′, N′-tetramethyl-1,3-oxapentanediamide), which is one of DGA (diglycolamide) compounds. That is, the present invention is a method for back-extracting Am (III) and Pu (IV) in an organic solvent into a nitric acid solution with an N, N, N ′, N′-tetramethyldiglycolamide (TMDGA) compound.
従来の抽出剤使用に起因する欠点に対して、本発明の抽出剤の利点をまとめると、
（１）０．２Ｍ硝酸の条件でＡｍ（ＩＩＩ），Ｐｕ（ＩＶ）の低い分配比を
示し、３Ｍ硝酸でもＰｕ（ＩＶ）の低い分配比を示す。
To summarize the advantages of the extractant of the present invention against the disadvantages caused by the use of conventional extractants,
(1) Low distribution ratio of Am (III) and Pu (IV) under the condition of 0.2M nitric acid, and low distribution ratio of Pu (IV) even with 3M nitric acid.
分配比とは、基本的に「有機相中の金属イオン濃度」／「水相中の金属イオン濃度」を示すが、本発明においては、有機相にある金属イオンをＴＭＤＧＡによって水相に戻すことを意味するので、分配比が低い方がＴＭＤＧＡの働きが強いことを示している。 The distribution ratio basically indicates “metal ion concentration in the organic phase” / “metal ion concentration in the aqueous phase”. In the present invention, the metal ions in the organic phase are returned to the aqueous phase by TMDGA. Therefore, the lower the distribution ratio, the stronger the action of TMDGA.
（２）Ｐｕ（ＩＶ）と沈殿形成しない。
（３）炭素、水素、酸素、窒素からなり構造内にリンを含まない化合物である。
（４）還元剤を加える必要がない。
(2) No precipitate formation with Pu (IV).
(3) A compound composed of carbon, hydrogen, oxygen, and nitrogen and containing no phosphorus in the structure.
(4) There is no need to add a reducing agent.
（５）水への溶解度が高く、最大１Ｍ ＴＭＤＧＡ/３Ｍ硝酸の溶液として使用可能である。 (5) It has high solubility in water and can be used as a solution of 1M TMDGA / 3M nitric acid at maximum.
本発明においては、使用済み燃料（ＳＦ）溶解液あるいは高レベル放射性廃液（ＨＬＬＷ）のような硝酸水溶液から金属イオンを溶媒抽出する際に、抽出した後のＡｎ（ＩＩＩ），（ＩＶ）を水相に逆抽出する事ができ、プロセスに応用できる。また、高い錯形成能力を生かして、現在使用されるＥＤＴＡ等に代わる放射能除染剤としても使用可能である。 In the present invention, when extracting metal ions from an aqueous nitric acid solution such as spent fuel (SF) solution or high-level radioactive waste liquid (HLLW), the extracted An (III) and (IV) are extracted from water. It can be back-extracted into phases and applied to processes. Moreover, it can be used as a radioactive decontamination agent in place of EDTA or the like currently used by making use of its high complexing ability.
又、本発明においては、ＳＦ溶解液あるいはＨＬＬＷから効率的に３，４価アクチノイドイオンを有機相より逆抽出でき、水酸化物沈殿などの問題を解決でき、円滑なプロセス運転を可能とするという本発明に特有な顕著な効果を生ずるものである。 In the present invention, the trivalent and tetravalent actinide ions can be efficiently back-extracted from the organic phase from the SF solution or HLLW, so that problems such as hydroxide precipitation can be solved, and smooth process operation is possible. The remarkable effect peculiar to this invention is produced.
実施例１
ＴＭＤＧＡを用いて、Ｐｕ（ＩＶ）及びＡｍ（ＩＩＩ）の抽出分配比を測定した。水相に各アクチノイドイオンとＴＭＤＧＡを含む０．２Ｍ硝酸溶液を、有機相に０．２Ｍ ＴＯＤＧＡ／ｎ−ドデカン溶媒を用いて、得られた分配比をＴＭＤＧＡ濃度に対してプロットした。その結果を図１に示す。図１に示されるように、ＴＭＤＧＡ濃度が増加するとともにＰｕ（ＩＶ），Ａｍ（ＩＩＩ）分配比は減少し、ＴＭＤＧＡ濃度０．１Ｍで、Ｐｕ（ＩＶ）及びＡｍ（ＩＩＩ）それぞれの分配比は０．０１以下であった。なお、ＴＭＤＧＡが存在しない条件で０．２Ｍ ＴＯＤＧＡ／ｎ−ドデカン−０．２Ｍ硝酸条件での分配比はＰｕ（ＩＶ）が３で、Ａｍ（ＩＩＩ）が１．４６であった。したがって、ＴＭＤＧＡは、その濃度が低くてもＰｕ（ＩＶ）及びＡｍ（ＩＩＩ）の抽出が良好に行われることを示している。
実施例２
ＴＭＤＧＡを用いて、Ｐｕ（ＩＶ），Ａｍ（ＩＩＩ）の抽出分配比を測定した。水相にアクチノイドイオンと０．１Ｍ ＴＭＤＧＡを含む硝酸溶液、有機相に０．２Ｍ ＴＯＤＧＡ／ｎ−ドデカン溶媒を用いて、得られた分配比を硝酸濃度に対してプロットした。その結果を図２に示す。図２に示されるように、０．１Ｍ ＴＭＤＧＡを含む０．６４Ｍ硝酸溶液を用いて、Ｐｕ（ＩＶ），Ａｍ（ＩＩＩ）分配比はそれぞれ０．００２，０．０１７であり、これ以下の酸濃度条件で一括逆抽出が可能である。なお、Ｐｕ（ＩＶ）に対して、３Ｍ ＨＮＯ3の条件でも分配比は０．１以下であり、この条件を用いれば、単独にＰｕ（ＩＶ）のみを逆抽出する事が出来る。
Example 1
The extraction partition ratio of Pu (IV) and Am (III) was measured using TMDGA. Using 0.2M nitric acid solution containing each actinide ion and TMDGA in the aqueous phase and 0.2M TODGA / n-dodecane solvent in the organic phase, the obtained distribution ratio was plotted against the TMDGA concentration. The result is shown in FIG. As shown in FIG. 1, as the TMDGA concentration increases, the Pu (IV), Am (III) distribution ratio decreases, and at the TMDGA concentration of 0.1 M, the distribution ratios of Pu (IV) and Am (III) are as follows. It was 0.01 or less. In the absence of TMDGA, the distribution ratio under the conditions of 0.2M TODGA / n-dodecane-0.2M nitric acid was 3 for Pu (IV) and 1.46 for Am (III). Therefore, TMDGA shows that Pu (IV) and Am (III) are well extracted even at low concentrations.
Example 2
The extraction partition ratio of Pu (IV) and Am (III) was measured using TMDGA. Using a nitric acid solution containing actinide ions and 0.1M TMDGA in the aqueous phase and a 0.2M TODGA / n-dodecane solvent in the organic phase, the obtained distribution ratio was plotted against the nitric acid concentration. The result is shown in FIG. As shown in FIG. 2, using a 0.64M nitric acid solution containing 0.1M TMDGA, Pu (IV) and Am (III) distribution ratios are 0.002 and 0.017, respectively. Batch back extraction is possible under concentration conditions. Note that the distribution ratio is 0.1 or less with respect to Pu (IV) even under the condition of 3M HNO 3 , and using this condition, only Pu (IV) can be back-extracted alone.
即ち、３価のアクチノイドイオン（Ａｍ（ＩＩＩ））と４価のアクチノイドイオン（Ｐｕ（ＩＶ））とが共存する系においては、図２中のプロットでＰｕの分配比が低く、Ａｍの分配比が高い条件下においては、選択的にＰｕのみ水相に分離回収することができることを意味している。 That is, in a system in which a trivalent actinoid ion (Am (III)) and a tetravalent actinoid ion (Pu (IV)) coexist, the distribution ratio of Pu is low in the plot in FIG. This means that under high conditions, only Pu can be separated and recovered in the aqueous phase.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4534000B2 (en) * | 2004-09-02 | 2010-09-01 | 独立行政法人 日本原子力研究開発機構 | A method of back-extracting Am (III) and Pu (IV) in an organic solvent using a nitric acid solution having a concentration of 0.1 M or more in which an N, N-dipropyldiglycolamidic acid (PDGAA) compound is dissolved. |
| JP4604226B2 (en) * | 2005-11-16 | 2011-01-05 | 独立行政法人 日本原子力研究開発機構 | Method for quantitative extraction and back extraction of neptunium in nitric acid solution with DGA (diglycolamide) compound |
| FR2948384B1 (en) * | 2009-07-27 | 2011-09-23 | Commissariat Energie Atomique | INCREASING THE SEPARATION FACTOR BETWEEN AMERICIUM AND CURIUM AND / OR BETWEEN LANTHANIDES IN A LIQUID-LIQUID EXTRACTION OPERATION |
| JP5526434B2 (en) * | 2010-01-20 | 2014-06-18 | 独立行政法人日本原子力研究開発機構 | N, N, N ′, N′-tetraalkyl-3,6-dioxaoctane-1,8-diamide (DOODA) and TADGA (N, N, N ′, N′-tetraalkyl-diglycolamide) Mutual separation of Am, Cm and Sm, Eu, Gd used together |
| CN115522052B (en) * | 2022-06-15 | 2024-06-25 | 济南大学 | Method for recovering rare noble metals in spent fuel post-treatment high-level waste liquid |
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