FR2611689A1 - NEPTUNIUM SEPARATION PROCESS - Google Patents
NEPTUNIUM SEPARATION PROCESS Download PDFInfo
- Publication number
- FR2611689A1 FR2611689A1 FR8802788A FR8802788A FR2611689A1 FR 2611689 A1 FR2611689 A1 FR 2611689A1 FR 8802788 A FR8802788 A FR 8802788A FR 8802788 A FR8802788 A FR 8802788A FR 2611689 A1 FR2611689 A1 FR 2611689A1
- Authority
- FR
- France
- Prior art keywords
- neptunium
- solution
- extraction
- acid
- phosphoric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052781 Neptunium Inorganic materials 0.000 title claims abstract description 24
- LFNLGNPSGWYGGD-UHFFFAOYSA-N neptunium atom Chemical compound [Np] LFNLGNPSGWYGGD-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000000926 separation method Methods 0.000 title claims description 9
- 238000000605 extraction Methods 0.000 claims abstract description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- IAONKHJEAQWGBJ-UHFFFAOYSA-N bis(8-methylnonyl) hydrogen phosphate Chemical compound CC(C)CCCCCCCOP(O)(=O)OCCCCCCCC(C)C IAONKHJEAQWGBJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 5
- 239000010452 phosphate Substances 0.000 claims abstract description 5
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 229910000478 neptunium(IV) oxide Inorganic materials 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 3
- 229940094933 n-dodecane Drugs 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- LFNLGNPSGWYGGD-IGMARMGPSA-N neptunium-237 Chemical compound [237Np] LFNLGNPSGWYGGD-IGMARMGPSA-N 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 101150033364 cnp-4 gene Proteins 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- TXBBUSUXYMIVOS-UHFFFAOYSA-N thenoyltrifluoroacetone Chemical compound FC(F)(F)C(=O)CC(=O)C1=CC=CS1 TXBBUSUXYMIVOS-UHFFFAOYSA-N 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G56/00—Compounds of transuranic elements
- C01G56/001—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
PROCEDE DE SEPARATION DU NEPTUNIUM UTILISANT UN REACTIF D'EXTRACTION A BASE DE PHOSPHATE ACIDE TEL QUE L'ACIDE DI-ISODECYL PHOSPHORIQUE, L'ACIDE DI-2-ETHYL-HEXYL PHOSPHORIQUE, ETC., CARACTERISE PAR LA PRESENCE DE PEROXYDE D'HYDROGENE DANS LA SOLUTION. COMME LE MONTRE LA FIGURE, LE TAUX D'EXTRACTION DE NPO AUGMENTE DU FAIT DE LA PRESENCE DU PEROXYDE D'AZOTE.PROCESS FOR SEPARATING NEPTUNIUM USING AN EXTRACTION REAGENT BASED ON ACID PHOSPHATE SUCH AS DI-ISODECYL PHOSPHORIC ACID, DI-2-ETHYL-HEXYL PHOSPHORIC ACID, ETC., CHARACTERIZED BY THE PRESENCE OF HYDROGEN PEROXIDE IN THE SOLUTION. AS SHOWN IN THE FIGURE, THE NPO EXTRACTION RATE INCREASES DUE TO THE PRESENCE OF NITROGEN PEROXIDE.
Description
PROCEDE DE SEPARATION DU NEPTUNIUM
La présente invention concerne un procédé de séparation du neptunium. PLus précisément, la
présente invention concerne un procédé de séparation
du neptunium par extraction en utiLisant un réactif
d'extraction à base de phosphate acide tel que
L'acide di-isodécyL phosphorique, L'acide di-2-éthyLhexyl
phosphorique, etc.NEPTUNIUM SEPARATION PROCESS
The present invention relates to a process for separating neptunium. More precisely, the
present invention relates to a separation process
neptunium by extraction using a reagent
extraction based on acid phosphate such as
Di-isodecyL phosphoric acid, Di-2-ethylhexyl acid
phosphoric, etc.
Le neptunium est un élément contenu en quantités relativement importantes dans des combustibles nucléaires épuisés et dont La récupération est recherchée
dans un processus de retraitement des combustibles pour l'extraction d'uranium et de plutonium à partir de
combustibles nucléaires épuisés, dans Le but d'une
utilisation effective du neptunium. Depuis peu, le
neptunium est considéré comme un élément très dangereux
du point de vue de l'élimination des déchets radio
actifs, et il s'est avéré nécessaire de développer un
procédé pour séparer de façon plus efficace le neptunium
d'une solution radio-active telle qu'une solution de
combustible épuisé, une solution de déchets retraités
à haute concentration, etc.Neptunium is an element contained in relatively large quantities in spent nuclear fuels and whose recovery is sought
in a reprocessing process of fuels for the extraction of uranium and plutonium from
spent nuclear fuels, with the aim of
effective use of neptunium. Recently, the
neptunium is considered a very dangerous element
from the point of view of radio waste disposal
assets, and it was necessary to develop a
process for more efficient separation of neptunium
of a radioactive solution such as a solution of
spent fuel, a reprocessed waste solution
at high concentration, etc.
Comme procédé de séparation, il est considéré
qu'une méthode d'extraction utilisant un solvant
organique est très satisfaisante car elle est capable
de séparer en continu le neptunium d'une importante
quantité de solution radio-active. Cependant, dans le
cas de l'extraction de l'art antérieur, le neptunium
existant à L'état de NpO2 sous la forme d'un ion
de valence V en solution était en général précédemment 2+
transformé en valence VI (ni02 ) ou en valence IV
(Np4+) par utilisation d'un agent d'oxydation ou d'un
agent réducteur, puis il était extrait par un solvant
organique. As a separation process, it is considered
than an extraction method using a solvent
organic is very satisfactory because it is capable
to continuously separate neptunium from a large
amount of radioactive solution. However, in the
case of the extraction of the prior art, neptunium
existing in the state of NpO2 as an ion
of valence V in solution was generally previously 2+
transformed into valence VI (ni02) or valence IV
(Np4 +) by using an oxidizing agent or a
reducing agent, then it was extracted with a solvent
organic.
Ce procédé présente l'inconvénient de poser le problème de la conservation de l'état d'oxydation et de réduction en solution afin d'améliorer La récupération par séparation du neptunium, et nécessite une opération compliquée puisqu'on utilise un agent d'oxydation ou un agent réducteur, ce qui entraîne la production d'une nouvelle solution de déchets contenant ces réactifs. This method has the drawback of posing the problem of preserving the state of oxidation and reduction in solution in order to improve the recovery by separation of neptunium, and requires a complicated operation since an oxidizing agent is used. or a reducing agent, which results in the production of a new waste solution containing these reagents.
Pour remédier à ces inconvénients, il est très souhaitable d'utiliser un solvant organique qui soit capable d'extraire directement le neptunium à l'état de valence V (ni02 ). Comme procédé de séparation du neptunium satisfaisant à cette exigence, un procédé d'extraction du neptunium utilisant de
L'acide di-isodécyl phosphorique a été inventé et a fait l'objet d'une demande de brevet (Journal des publications de brevets japonais nO 30799/86). Ce procédé demande à être amélioré car le taux d'extraction décroit lorsque la concentration en acide augmente, celle-ci étant limitée à environ 2N.To remedy these drawbacks, it is very desirable to use an organic solvent which is capable of directly extracting the neptunium in the state of valence V (ni02). As a method of separating neptunium satisfying this requirement, a method of extracting neptunium using
Di-isodecyl phosphoric acid was invented and has been the subject of a patent application (Journal of Japanese Patent Publication No. 30799/86). This process needs to be improved because the extraction rate decreases when the acid concentration increases, the latter being limited to about 2N.
Un but de la présente invention est de fournir un procédé de séparation du neptunium dans lequel la vitesse d'extraction a été améliorée par résolution de ce problème. An object of the present invention is to provide a process for the separation of neptunium in which the extraction rate has been improved by solving this problem.
La figure 1 est un graphique représentant un résultat de l'Exemple. Fig. 1 is a graph showing a result of Example.
Après avoir mené une recherche approfondie dans le but d'atteindre ce but, les présents inventeurs ont découvert que, lors de la séparation du neptunium dans un état de valence V < NpO2+) en utilisant de
L'acide di-isodécyl phosphorique, l'addition de peroxyde d'hydrogène augmentait le taux d'extraction.After conducting extensive research for the purpose of achieving this goal, the present inventors have found that when separating neptunium in a valence state V <NpO2 +) using
Di-isodecyl phosphoric acid, addition of hydrogen peroxide increased the extraction rate.
Lors de l'addition de peroxyde d'hydrogène, pour L'extraction de neptunium à l'état de valence V (NP02 ), en association avec un autre réactif d'extraction à base de phosphate acide tel que L'acide di-2éthylhexyl phosphorique, etc., on augmente le taux d'extraction et, alors que ce réactif d'extraction ne pouvait être utilisé jusqu'à présent à haute concentration qu'en solution acide, il est devenu possible de l'utiliser pour séparer par extraction le neptunium à L'état de valence V (NpO2 ). When adding hydrogen peroxide, for the extraction of neptunium in the valence state V (NP02), in combination with another extraction reagent based on acid phosphate such as di-2ethylhexyl acid phosphoric acid, etc., the rate of extraction is increased and, while this extraction reagent could heretofore only be used in high concentration in acidic solution, it has become possible to use it for separating by extraction neptunium in the valence state V (NpO2).
Par addition de peroxyde d'hydrogène, on entend la réduction du neptnium de la valence V (NpO2+) à la valence IV CNp4+). Cependant, cette réaction de réduction s'effectue difficilement dans une solution acide de faible concentration, par exemple d'environ 0,5 N mais ne se déroule qu'en présence d'un réactif d'extraction à base de phosphate acide. By addition of hydrogen peroxide is meant the reduction of neptnium from valence V (NpO2 +) to valence IV (CNp4 +). However, this reduction reaction is hardly carried out in an acid solution of low concentration, for example of about 0.5 N, but only takes place in the presence of an extraction reagent based on acid phosphate.
L'exemple non limitatif suivant est donné à titre d'illustration de l'invention. The following non-limiting example is given by way of illustration of the invention.
Après introduction d'acide nitrique et d'une solution de neptunium 237 converti en valence V dans un tube à essai muni d'un bouchon rodé, une solution de peroxyde d'hydrogène ou d'eau y a été introduite jusqu'à ce qu'un volume total de 2 000 l ait été atteint. 2 ml d'un solvant organique constitué de 0,5 M d'acide di-isodécyl phosphorique + n-dodécane, ou de 0,5 M d'acide di-2-éthylhexyl phosphorique + ndodécane, y ont été ajoutés et la solution a été agitée pendant un certain temps. After introducing nitric acid and a solution of neptunium 237 converted to valence V in a test tube fitted with a ground-glass stopper, a solution of hydrogen peroxide or water was introduced into it until a total volume of 2000 l was reached. 2 ml of an organic solvent consisting of 0.5 M di-isodecyl phosphoric acid + n-dodecane, or 0.5 M di-2-ethylhexyl phosphoric acid + ndodecane, were added thereto and the solution has been restless for a while.
Après séparation en une phase organique et en une phase aqueuse par centrifugation, des échantillons de 1 ml ont été prélevés dans les deux phases pour effectuer des mesures de radio-activité. After separation into an organic phase and an aqueous phase by centrifugation, 1 ml samples were taken from the two phases to carry out radioactivity measurements.
Les rayons y de 29 KeV émis par le neptunium 237 ont été détectés à l'aide d'un détecteur Ge afin d'obtenir un rapport de distribution du neptunium. The 29 KeV y-rays emitted by neptunium 237 were detected using a Ge detector in order to obtain a neptunium distribution ratio.
Une solution de conversion du neptunium en valence V utilisé ici, a été préparée, après extraction du neptunium d'une solution réduite en valence IV, par addition de chlorhydrate d'hydroxylamine et d'acide sulfamique ferreux, avec 0,5 M d'une solution de thénoyltrifluoracétone + xylène, réextraction par 10 M d'acide nitrique, puis dilution à L'eau pour donner une solution d'acide nitrique à 0,5 M, et chauffage sur un bain chaud afin d'obtenir une solution d'acide nitrique à 0,1 M. A solution for converting neptunium into valency V used here, was prepared, after extracting the neptunium from a solution reduced to valence IV, by addition of hydroxylamine hydrochloride and ferrous sulfamic acid, with 0.5 M of a solution of thenoyltrifluoroacetone + xylene, reextraction with 10 M of nitric acid, then dilution with water to give a solution of nitric acid at 0.5 M, and heating on a hot bath in order to obtain a solution of 0.1 M nitric acid.
Le résultat est illustré Figure 1. Dans cette figure, les abscisses représentent la durée d'agitation en minute et les ordonnées, le rapport de distribution du neptunium. Dans tous Les cas, l'extraction a été une extraction de la valence V (NpO2+) à partir de la solution d'acide nitrique à 0,5 M, (A) et (C) représentent l'extraction obtenue avec la solution d'acide di-isodécyl phosphorique + n-dodécane à 0,5 M et (B) et (D) représentent l'extraction avec de L'acide di-2-éthylhexyl phosphorique + n-dodécane à 0,5 M. De plus, (A) et (B) contiennent du peroxyde d'hydrogène à la concentration de 0,4 M et (C) et (D) ne contiennent pas de peroxyde d'hydrogène. The result is illustrated in Figure 1. In this figure, the abscissas represent the stirring time in minutes and the ordinates the neptunium distribution ratio. In all cases, the extraction was an extraction of the valence V (NpO2 +) from the 0.5 M nitric acid solution, (A) and (C) represent the extraction obtained with the solution of '0.5 M di-isodecyl phosphoric acid + n-dodecane and (B) and (D) represent the extraction with 0.5 M di-2-ethylhexyl phosphoric acid + n-dodecane. , (A) and (B) contain hydrogen peroxide at a concentration of 0.4 M and (C) and (D) do not contain hydrogen peroxide.
Comme le montre la figure, quel que soit le réactif d'extraction, le taux d'extraction de NpO2 augmente du fait de la présence du peroxyde d'hydrogène. As shown in the figure, whatever the extraction reagent, the NpO2 extraction rate increases due to the presence of hydrogen peroxide.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62048754A JP2561831B2 (en) | 1987-03-05 | 1987-03-05 | Separation method of neptunium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| FR2611689A1 true FR2611689A1 (en) | 1988-09-09 |
| FR2611689B1 FR2611689B1 (en) | 1991-11-08 |
Family
ID=12812070
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR8802788A Expired - Lifetime FR2611689B1 (en) | 1987-03-05 | 1988-03-04 | PROCESS FOR SEPARATING NEPTUNIUM |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2561831B2 (en) |
| FR (1) | FR2611689B1 (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2847276A (en) * | 1955-04-15 | 1958-08-12 | John P Butler | Solvent extraction of neptunium |
| US2907628A (en) * | 1949-06-22 | 1959-10-06 | Lyle R Dawson | Neptunium solvent extraction process |
| US3004823A (en) * | 1959-07-15 | 1961-10-17 | Donald F Peppard | Method of separating neptunium by liquid-liquid extraction |
| US4341743A (en) * | 1980-12-29 | 1982-07-27 | E. I. Du Pont De Nemours And Company | Simultaneous oxidation and extraction of vanadium from wet-process phosphoric acid |
| FR2551745A1 (en) * | 1983-09-13 | 1985-03-15 | Kernforschungsz Karlsruhe | PROCESS FOR THE SEPARATION OF NEPTUNIUM FORMING FROM AN ORGANIC PHASE DURING THE RETIREMENT OF IRRADIATED COMBUSTIBLE AND / OR FERTILIZED MATERIALS |
| FR2573061A1 (en) * | 1984-07-24 | 1986-05-16 | Japan Atomic Energy Res Inst | Process for the separation of neptunium |
-
1987
- 1987-03-05 JP JP62048754A patent/JP2561831B2/en not_active Expired - Fee Related
-
1988
- 1988-03-04 FR FR8802788A patent/FR2611689B1/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2907628A (en) * | 1949-06-22 | 1959-10-06 | Lyle R Dawson | Neptunium solvent extraction process |
| US2847276A (en) * | 1955-04-15 | 1958-08-12 | John P Butler | Solvent extraction of neptunium |
| US3004823A (en) * | 1959-07-15 | 1961-10-17 | Donald F Peppard | Method of separating neptunium by liquid-liquid extraction |
| US4341743A (en) * | 1980-12-29 | 1982-07-27 | E. I. Du Pont De Nemours And Company | Simultaneous oxidation and extraction of vanadium from wet-process phosphoric acid |
| FR2551745A1 (en) * | 1983-09-13 | 1985-03-15 | Kernforschungsz Karlsruhe | PROCESS FOR THE SEPARATION OF NEPTUNIUM FORMING FROM AN ORGANIC PHASE DURING THE RETIREMENT OF IRRADIATED COMBUSTIBLE AND / OR FERTILIZED MATERIALS |
| FR2573061A1 (en) * | 1984-07-24 | 1986-05-16 | Japan Atomic Energy Res Inst | Process for the separation of neptunium |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63218510A (en) | 1988-09-12 |
| FR2611689B1 (en) | 1991-11-08 |
| JP2561831B2 (en) | 1996-12-11 |
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| Date | Code | Title | Description |
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| ST | Notification of lapse |