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EP3607562B1 - Dosage de zinc pour la decontamination des réacteurs à eau légère - Google Patents

Dosage de zinc pour la decontamination des réacteurs à eau légère Download PDF

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Publication number
EP3607562B1
EP3607562B1 EP18712094.4A EP18712094A EP3607562B1 EP 3607562 B1 EP3607562 B1 EP 3607562B1 EP 18712094 A EP18712094 A EP 18712094A EP 3607562 B1 EP3607562 B1 EP 3607562B1
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EP
European Patent Office
Prior art keywords
acid
decontamination
zinc
metal
decontamination solution
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.)
Active
Application number
EP18712094.4A
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German (de)
English (en)
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EP3607562A1 (fr
Inventor
Dietmar NIEDER
David Jordan
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RWE Power AG
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RWE Power AG
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Publication of EP3607562A1 publication Critical patent/EP3607562A1/fr
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/001—Decontamination of contaminated objects, apparatus, clothes, food; Preventing contamination thereof
    • G21F9/002—Decontamination of the surface of objects with chemical or electrochemical processes
    • G21F9/004—Decontamination of the surface of objects with chemical or electrochemical processes of metallic surfaces
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28—Treating solids
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28—Treating solids
    • G21F9/30—Processing

Definitions

  • the present invention relates to a method for the decontamination of radioactive metal surfaces by means of the decontamination solution and the use of the decontamination solution for this purpose.
  • radioactive contamination of metal components occurs. Such contamination occurs regularly in the regular operation of reactors and particularly affects metal components that are in the primary circuit, for example a pressurized water reactor. Radioactive substances are deposited in the oxide layers formed on the surface of the components, causing them to become radioactively contaminated.
  • mechanical means can be used to remove such deposits, in which case, for example, the oxide layers and thus the contaminated areas are abraded. This is particularly disadvantageous in the case of components which, due to their dimensions or their positioning, are difficult to access for the grinding tool.
  • a decontamination of the components with a decontamination solution having a complexing agent including various carboxylic acids, such as oxalic acid
  • a decontamination solution having a complexing agent including various carboxylic acids, such as oxalic acid
  • the sparingly soluble components of the oxide layers are first oxidized or reduced, with Cr-III being oxidized to Cr-VI using permanganates (potassium permanganate, permanganic acid), for example.
  • the oxide layer consisting mainly of iron and nickel ions, is then dissolved with the aid of the complexing agent and the cations released, including 60 Co 2+ or 58 Co 2+ , are removed from the decontamination solution by ion exchange.
  • This decontamination process is usually carried out in several rounds, with the oxide layer being broken down in layers.
  • inactive ions are always released into the decontamination solution, which are also removed from the decontamination solution via the ion exchange resins. Furthermore, the radioactive ions in the decontamination solution cause recontamination of the components during the decontamination process. This reduces the efficiency of the decontamination process, which on the one hand leads to the need for a larger number of decontamination cycles, which are time-consuming and costly, and on the other hand results in an increased amount of contaminated ion exchange resins that have to be disposed of with immense effort .
  • the WO 00/78403 A1 describes a process for the decontamination of radioactively contaminated metal surfaces in which zinc and a complexing agent are used.
  • Diphosphonic acids in particular etidronic acid, are used as complexing agents.
  • this object is achieved by a method having the features specified in claim 1. Furthermore, this object is achieved by the use according to claim 11. Advantageous refinements are given in the subclaims.
  • the method according to the invention is a method for decontaminating a radioactively contaminated metal surface, comprising the step of bringing at least a section of the radioactively contaminated metal surface into contact with a decontamination solution, comprising a complexing agent and a transition metal.
  • a decontamination solution comprising a complexing agent and a transition metal.
  • the transition metal added to the decontamination solution competes with the released radioactive isotopes for (renewed) storage in the metal surface (or the oxide layer on it).
  • a larger amount of radioactive isotopes can advantageously be removed from the decontamination solution via the ion exchange process, which in turn leads to a reduction in the number of rounds of decontamination steps required and / or a reduction in the amount of ion exchange resins to be disposed of.
  • the decontamination solution is preferably an aqueous solution. It contains an ion of a transition metal, more preferably a cation of the transition metal, even more preferably a divalent or trivalent cation of the transition metal. Most preferably the transition metal is a divalent cation of the transition metal.
  • the transition metal is a depleted transition metal, ie a transition metal with a reduced proportion of isotopes that can be easily activated by neutrons compared to the natural occurrence.
  • the use of a depleted transition metal is particularly advantageous if the metal to be decontaminated, for example the component of a reactor, is not to be disposed of after decontamination, but is to be reused and exposed to neutron flux.
  • the transition metal is also preferably selected from the group consisting of zinc, nickel, cobalt or mixtures thereof. More preferably, the transition metal is selected from the group consisting of zinc and nickel. Most preferably the transition metal is zinc. The use of zinc in the decontamination solution surprisingly showed the greatest effect in decontaminating the metal surface.
  • the transition metal in the decontamination solution is preferably in a concentration in the range from 0.5 mg / kg and 15 mg / kg, more preferably 0.5 mg / kg and 10 mg / kg, more preferably 1.5 mg / kg and ⁇ 5 mg / kg or ⁇ 2 mg / kg and ⁇ 5 mg / kg and most preferably about ⁇ 3 mg / kg and ⁇ 4 mg / kg.
  • the mg / kg the mmol / L can also be given, whereby the given mg / kg value has to be divided by the atomic mass of the respective transition metal.
  • the transition metal in the decontamination solution is preferably in a concentration in the range of ⁇ 7 ⁇ mol / L and ⁇ 230 pmol / L, more preferably ⁇ 7 ⁇ mol / L and ⁇ 155 pmol / L, more preferably ⁇ 23 ⁇ mol / L and ⁇ 70 ⁇ mol / L or ⁇ 30 ⁇ mol / L and ⁇ 80 ⁇ mol / L and most preferably approximately ⁇ 46 ⁇ mol / L and ⁇ 62 ⁇ mol / L.
  • the specified concentration ranges for the concentration of the transition metals at the time when the metal surface is brought into contact with the decontamination solution preferably apply.
  • the stated concentrations are likewise preferably the mean concentrations.
  • transition metals instead of “transition metals”, reference is only made to the element zinc as an example. As far as applicable, the statements made also apply analogously to transition metals in general and preferably also to nickel and / or cobalt.
  • zinc should preferably be understood to mean the zinc ions present in the decontamination solution, more preferably Zn 2+. This can, even more preferably, be depleted zinc, in particular zinc depleted in 64 Zn.
  • the zinc is introduced into the decontamination solution by means of a soluble zinc compound.
  • Preferred soluble zinc compounds are selected from the groups of acids used and / or the complexing agents used with zinc, including zinc methanesulfonate (Zn (CH 3 SO 3 ) 2 ), zinc nitrate (Zn (NO 3 ) 2 ), zinc permanganate (Zn (MnO 4 ) 2 ), zinc sulfate (ZnSO 4 ) and / or a soluble zinc complex.
  • the zinc complex is more preferably a complex of zinc and the complexing agent used.
  • decontamination is known to the person skilled in the art. This is to be understood in particular as the reduction and / or removal of radioactivity on the metal surface. In particular, this is to be understood as the removal of a deposited layer of metal oxides on a metal component, the deposited layer having radioactive isotopes, preferably cobalt.
  • radioactive isotopes are removed from the metal surface to be decontaminated by means of the method according to the invention.
  • These radioactive isotopes are preferably selected from the group consisting of 55 Fe ions, 63 Ni ions, 54 Mn ions, 65 Zn ions, 125 Sb ions, 137 Cs ions, 58 Co ions and 60 Co ions.
  • the radioactive isotopes are more preferably selected from the group consisting of 54 Mn ions, 125 Sb ions, 137 Cs ions, 58 Co ions and 60 Co ions. Most preferably, these radioactive isotopes are 58 Co ions and / or 60 Co ions, even more preferably 60 Co ions.
  • the decontamination method of the present invention can preferably also be referred to as chemical decontamination. More preferably, the decontamination process can be a decontamination process for a nuclear reactor to be dismantled or for a nuclear reactor to be continued to operate.
  • the release of solid and liquid substances is regulated according to the Radiation Protection Ordinance (StrlSchV) and is essentially divided according to the unrestricted release and the release for disposal in landfills. After decontamination of the metal surface, it is preferably a component that is released for disposal in landfills. Even more preferably, after the decontamination of the metal surface, it is a component that is suitable for unrestricted release.
  • StrlSchV Radiation Protection Ordinance
  • radioactively contaminated metal surface should preferably be understood to mean the surface of a metal component including the radioactively contaminated deposit layer located on it, which is formed, for example, during normal use of the component in a pressurized water reactor.
  • a deposit layer preferably consists of sparingly soluble metal oxides.
  • the radioactive metal surface to be decontaminated preferably comprises at least one radioactively contaminated layer of sparingly soluble metal oxides arranged on the surface of metal base material.
  • the metal of the metal surface to be decontaminated can in principle be any suitable metal.
  • the metal is a metal selected from the group consisting of iron, nickel, chromium, manganese, titanium, niobium, copper, cobalt and combinations of at least two of these metals. Even more preferably, the metal is selected from the group consisting of iron, chromium, nickel, cobalt, and combinations of at least two of these metals.
  • At least a section of the metal surface is also brought into contact with the decontamination solution.
  • several sections, and even more preferably the entire metal surface are brought into contact with the decontamination solution.
  • the radioactively contaminated metal surface can be brought into contact with the decontamination solution in any suitable manner.
  • the metal surface to be decontaminated is preferably wetted with the decontamination solution.
  • the decontamination solution is more preferably introduced into the primary circuit of a reactor.
  • the decontamination solution can more preferably be circulated. This advantageously avoids concentration gradients in the area of the metal surface and increases the efficiency of the decontamination process.
  • the circulation is more preferably carried out continuously and, likewise preferably, using pumps.
  • the metal surface to be decontaminated is also preferably the inner jacket surface of a metal and cylindrical component (such as a pipe of a recuperator) and the decontamination solution is introduced into the cavity of the cylindrical component.
  • a metal and cylindrical component such as a pipe of a recuperator
  • the method according to the invention preferably has an additional method step for oxidation or reduction of the radioactively contaminated metal surface before the method step of bringing the at least one section of the metal surface into contact with the decontamination solution, i.e. as a first method step.
  • this process step can also be referred to as pre-oxidation of the radioactively contaminated metal surface.
  • Cr-III is oxidized to Cr-VI in the pre-oxidation.
  • the pre-oxidation is preferably carried out by bringing the radioactively contaminated metal surface into contact with nitric acid and potassium permanganate, with sodium hydroxide and potassium permanganate, a vanadium compound (preferably vanadium formate) or with permanganic acid, with permanganic acid treatment being the most preferred.
  • the oxidation layer is preferably reduced with the aid of a vanadium compound.
  • the dissolved products are preferably complexed with picolinic acid.
  • an additional process step for reducing the excess oxidizing agent for example the permanganates (potassium permanganate, permanganic acid), can be carried out.
  • the method according to the invention has the further method step of at least partial removal of the radioactive isotopes or their ions contained in the decontamination solution.
  • These radioactive isotopes are preferred selected from the group consisting of 55 Fe, 63 Ni, 54 Mn, 65 Zn, 125 Sb, 137 Cs, 58 Co and 60 Co. More preferably, the radioactive isotopes are selected from the group consisting of 54 Mn, 125 Sb, 137 Cs , 58 Co and 60 Co. Most preferably these radioactive isotopes are 58 Co and / or 60 Co, more preferably 60 Co.
  • the radioactive isotopes are preferably removed by binding to an ion exchange resin, more preferably a cation exchange resin and / or a synthetic resin ion exchanger.
  • the ion exchanger is a strongly acidic cation exchanger in which protons are exchanged for the bound cations.
  • Such ion exchange resins are sufficiently known to the person skilled in the art.
  • Radioactive isotopes in the decontamination solution More preferably about 50%, even more preferably about 70%, 80%, 90% or 99% of the radioactive isotopes in the decontamination solution are removed. Most preferably, approximately ⁇ 99% and ⁇ 100% of the isotopes in the decontamination solution are removed.
  • the method according to the invention is more preferably carried out cyclically. In other words, at least the method steps of bringing the metal surface into contact with the decontamination solution and the subsequent at least partial removal of the radioactive isotopes in the decontamination solution are repeated at least once. Of course, individual or all of the other method steps listed above can also be repeated here.
  • the method according to the invention is preferably repeated until a decontamination factor has been reached which corresponds to a reduction in the activity of the radioactively contaminated metal surface by 1 to 3 order (s), more preferably approximately 2 orders of magnitude.
  • the The decontamination factor is preferably determined by measuring the activity of the ion exchange resin used to remove the radioactive isotopes in the decontamination solution, or comparing the activity of the ion exchange resin before and after performing the method according to the invention.
  • the method according to the invention is likewise preferably repeated cyclically approximately 1 to 30 times, more preferably 10 to 25 times, even more preferably 13 to 20 times. A range from 13 to 17 cycles showed particularly good results when using oxalic acid.
  • the decontamination solution comprises at least one complexing agent in addition to the transition metal.
  • the complexing agent can also be referred to as a chelating agent.
  • Complexing agents form chelate complexes with metal ions.
  • Exemplary complexing agents include nitriloacetic acid, ethylenediaminetetraacetic acid, hydrofluoric acid, oxalic acid, tartaric acid, citric acid and their salts.
  • the decontamination solution further comprises water, so that the water-soluble constituents of the decontamination solution can be present in their dissolved form.
  • the decontamination solution is an aqueous solution.
  • the acid is selected from the group consisting of carboxylic acid, methanesulfonic acid, oxalic acid, picolinic acid, and citric acid.
  • the acid is preferably a mixture of methanesulfonic acid and oxalic acid. Most preferably the acid is oxalic acid.
  • the decontamination solution also comprises an oxidizing agent, more preferably permanganic acid, or a reducing agent.
  • the decontamination solution comprises zinc methanesulfonate, Zinc nitrate, zinc permanganate, zinc sulfate and / or a zinc complex of the complexing agent used.
  • the complex of the transition metal and the complexing agent used is particularly preferred.
  • Example 1 was repeated, the Ni concentration or the Cr concentration being considered instead of the Zn concentration. In each case, a correlation was also found between the concentration of the transition metal and the activity carried out over 60 Co. The correlation determined tended to decrease from Ni to Cr compared to Zn.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
  • Detergent Compositions (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Claims (11)

  1. Procédé permettant la décontamination d'une surface métallique contaminée par la radioactivité, comprenant l'étape :
    - de mise en contact d'au moins une section de la surface métallique avec une solution de décontamination comprenant un agent complexant choisi parmi l'acide fluorhydrique, l'acide méthanesulfonique et les acides carboxyliques, tels que l'acide nitriloacétique, l'acide éthylènediaminetétraacétique, l'acide oxalique, l'acide tartrique, l'acide citrique et l'acide picolinique et leurs sels et un ion d'un métal de transition.
  2. Procédé selon la revendication 1, dans lequel l'ion du métal de transition est choisi dans le groupe constitué par le zinc, le nickel, le cobalt ou leurs mélanges.
  3. Procédé selon au moins l'une des revendications précédentes, dans lequel la concentration du métal de transition est comprise dans une plage allant de ≥ 0,5 à ≤ 15 mg/kg.
  4. Procédé selon au moins l'une des revendications précédentes, dans lequel l'ion du métal de transition est le zinc et est présent à une concentration comprise dans une plage allant de ≥ 2 à ≤ 5 mg/kg.
  5. Procédé selon au moins l'une des revendications précédentes, dans lequel des ions 58Co et/ou des ions 60Co sont éliminés de la surface métallique.
  6. Procédé selon au moins l'une des revendications précédentes, dans lequel la solution de décontamination est introduite dans le circuit primaire d'un réacteur nucléaire.
  7. Procédé selon au moins l'une des revendications précédentes, dans lequel la solution de décontamination est mise en circulation.
  8. Procédé selon au moins l'une des revendications précédentes, dans lequel le procédé présente comme première étape de procédé une étape de pré-oxydation ou une étape de réduction permettant l'oxydation ou permettant la réduction de la surface métallique contaminée par la radioactivité.
  9. Procédé selon au moins l'une des revendications précédentes, dans lequel le procédé présente en outre l'étape :
    - d'élimination au moins partielle des isotopes radioactifs présents dans la solution de décontamination.
  10. Procédé selon la revendication 9, dans lequel toutes les étapes de procédé sont répétées au moins une fois.
  11. Utilisation d'une solution aqueuse comprenant un agent complexant choisi parmi l'acide fluorhydrique, l'acide méthanesulfonique et les acides carboxyliques tels que l'acide nitriloacétique, l'acide éthylènediaminetétraacétique, l'acide oxalique, l'acide tartrique, l'acide citrique et l'acide picolinique et leurs sels et un ion d'un métal de transition à une concentration comprise dans une plage allant de ≥ 0,5 mg/kg à ≤ 15 mg/kg, permettant la décontamination de surfaces métalliques contaminées par la radioactivité.
EP18712094.4A 2017-04-07 2018-03-05 Dosage de zinc pour la decontamination des réacteurs à eau légère Active EP3607562B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102017107584.4A DE102017107584A1 (de) 2017-04-07 2017-04-07 Zinkdosierung zur Dekontamination von Leichtwasserreaktoren
PCT/EP2018/055374 WO2018184780A1 (fr) 2017-04-07 2018-03-05 Dosage du zinc pour la décontamination de réacteurs à eau légère

Publications (2)

Publication Number Publication Date
EP3607562A1 EP3607562A1 (fr) 2020-02-12
EP3607562B1 true EP3607562B1 (fr) 2021-09-22

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EP18712094.4A Active EP3607562B1 (fr) 2017-04-07 2018-03-05 Dosage de zinc pour la decontamination des réacteurs à eau légère

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US (1) US10998106B2 (fr)
EP (1) EP3607562B1 (fr)
JP (1) JP6858274B2 (fr)
KR (1) KR102246411B1 (fr)
CN (1) CN110494928A (fr)
DE (1) DE102017107584A1 (fr)
ES (1) ES2897688T3 (fr)
RU (1) RU2767977C2 (fr)
UA (1) UA124477C2 (fr)
WO (1) WO2018184780A1 (fr)

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UA124477C2 (uk) 2021-09-22
RU2019134954A3 (fr) 2021-05-07
WO2018184780A1 (fr) 2018-10-11
ES2897688T3 (es) 2022-03-02
DE102017107584A1 (de) 2018-10-11
EP3607562A1 (fr) 2020-02-12
RU2019134954A (ru) 2021-05-07
RU2767977C2 (ru) 2022-03-22
US10998106B2 (en) 2021-05-04
US20200051706A1 (en) 2020-02-13
CN110494928A (zh) 2019-11-22
JP6858274B2 (ja) 2021-04-14
KR20190132374A (ko) 2019-11-27
JP2020516876A (ja) 2020-06-11
KR102246411B1 (ko) 2021-05-03

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