EP2564394B1 - Verfahren zur oberflächen-dekontamination - Google Patents

Verfahren zur oberflächen-dekontamination Download PDF

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Publication number
EP2564394B1
EP2564394B1 EP11721251.4A EP11721251A EP2564394B1 EP 2564394 B1 EP2564394 B1 EP 2564394B1 EP 11721251 A EP11721251 A EP 11721251A EP 2564394 B1 EP2564394 B1 EP 2564394B1
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EP
European Patent Office
Prior art keywords
solution
oxidation step
oxide layer
decontamination
oxidation
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
EP11721251.4A
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German (de)
English (en)
French (fr)
Other versions
EP2564394A1 (de
Inventor
Rainer Gassen
Bertram Zeiler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Areva GmbH
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Areva GmbH
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Publication date
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Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • 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

Definitions

  • the invention relates to a method for surface decontamination of components or systems of a nuclear power plant, for example a pressurized water reactor (PWR).
  • a nuclear power plant for example a pressurized water reactor (PWR).
  • the core of a nuclear power plant is a reactor pressure vessel in which nuclear fuel-containing fuel elements are arranged.
  • a coolant circuit forming tube system is connected, which is connected in the case of a PWR with at least one coolant pump and a steam generator.
  • the oxide layers contain iron oxide with di- and tri-valent iron and oxides of other metals, especially chromium and nickel, which are present as alloying constituents in the steels mentioned above, depending on the type of alloy used for a component.
  • Nickel is always present in divalent form (Ni 2+ ), chromium in trivalent (Cr 3+ ) form.
  • the oxide layer present on the surfaces of the components is removed as completely as possible by means of a decontamination process.
  • a decontamination process either the entire coolant system or a part separated therefrom by valves is filled with an aqueous cleaning solution or individual components of the system are treated in a separate container containing the cleaning solution.
  • the oxide layer is first treated oxidatively (oxidation step) and then the oxide layer is dissolved under acidic conditions.
  • decontamination step which is referred to below as a decontamination step (or shorter than decontamination step)
  • decontamination step is also often worked under reductive conditions.
  • the oxidizing agent used in the preceding oxidation step is therefore removed or neutralized, as will be shown below.
  • the oxidative treatment of the oxide layer is required because chromium-III oxides and trivalent chromium-containing mixed oxides, especially of the spinel type, in the for decontamination in question coming Decontamination acids, eg in oxalic acid, difficult to solve.
  • the oxide layer is first treated with an aqueous solution of an oxidizing agent such as Ce 4+ , HMnO 4 , H 2 S 2 O 8 , KMnO 4 or O 3 .
  • an oxidizing agent such as Ce 4+ , HMnO 4 , H 2 S 2 O 8 , KMnO 4 or O 3 .
  • the result of this treatment is that Cr-III is oxidized to Cr-VI, which goes into solution as CrO 4 2- .
  • the cleaning solution present at the end of an oxidative treatment is either discarded or processed so that it can be used in the decontamination step. If the latter is the case, a remaining residual content of oxidizing agent must be removed or neutralized by a reducing agent, for example by using a corresponding excess of deconic acid.
  • the decontamination step subsequent to the oxidation serves to dissolve the previously oxidatively treated oxide layer with the aid of one or mixtures of complex-forming organic acid.
  • a deconic acid can simultaneously also serve for the neutralization of the oxidizing agent used in the oxidation step.
  • an oxidizing agent such as HMnO 4
  • a reducing agent added in addition to the deconic acid for example ascorbic acid, citric acid or hydrogen peroxide.
  • the Cr-VI formed in the oxidation step is also reduced again to Cr-III.
  • the cleaning solution contains Cr-III, Fe-II, Fe-III, Ni-II and radioactive isotopes such as Co-60. These metal ions can be removed from the cleaning solution with an ion exchanger.
  • the decontact factor is the ratio of the initial value measured prior to the execution of a cleaning cycle and the final value of the radioactive radiation present at the end of the cleaning cycle, starting from a component or system surface or the oxide layer present thereon.
  • the object of the invention is to provide a method for surface decontamination with improved effectiveness.
  • This object is achieved according to claim 1 by a method of the type mentioned, in which at least one oxidation step in acidic and at least one oxidation step are carried out in alkaline solution. It has been found that a change in the pH of the oxidation solution from the acidic to the alkaline region or vice versa - such a change is referred to below as a pH change - causes an increase in the decontactor.
  • the pH change can take place in one and the same cleaning cycle.
  • an oxidation step in acidic or alkaline solution and in a subsequent cleaning cycle an oxidation step in alkaline or acidic solution is carried out in a cleaning cycle.
  • the oxidizing agent are preferably O 3 , in dissolved or gaseous form, S 2 O 8 2- , for example, used as Na salt and cerium-IV compound, but especially in (preferably nitric) acid solution HMnO 4 and KMnO 4 and in alkaline solution KMnO 4 , especially with NaOH, as alkalizing agent.
  • an oxide layer located on a component of a nuclear power plant is at least partially removed by treating this oxide layer or the component with several cleaning cycles.
  • this oxide layer For a decontamination of an entire system, such as a coolant system of a pressurized or boiling water reactor, this is filled with the respective cleaning solutions.
  • the system acts as its own container. If, on the other hand, individual components are decontaminated, a container is used in which the component is treated with the appropriate cleaning solutions.
  • oxidation of the oxide layer is made to oxidize chromium III contained therein to chromium VI.
  • oxidizing agents which are capable of oxidizing chromium-III to chromium-VI, for example ozone, peroxodisulfate, cerium-IV-oxide and permanganic acid or permanganate, could be used as the oxidizing agent.
  • the oxidation is conveniently carried out at elevated temperature, for example from 80-95 ° C.
  • the cleaning solution is exchanged or, as described above, treated so that it can be used in the subsequent decontamination step.
  • organic acids such as oxalic acid, citric acid, ascorbic acid and the like are used.
  • a residual oxidizing agent remaining in the solution of the oxidation step is neutralized by a corresponding excess of deconic acid.
  • the metal ions dissolved out of the oxide layer are removed, likewise in a manner known per se, with the aid of an ion exchanger. If this is the case to a sufficient extent, a renewed cleaning cycle is started, whereby a change in the pH of the oxidation solution from acidic to alkaline or vice versa already takes place during this or a subsequent cleaning cycle.
  • pH values of less than 6, preferably less than 4 are maintained.
  • the pH values are greater than 8, preferably greater than 10.
  • the attached diagram shows the result of an experiment in which a sample has been decontaminated in the manner according to the invention.
  • the sample came from a coolant tube that was in use for several years.
  • a radial cylinder was taken from the pipe and its former pipe outside forming side and its peripheral surface were provided with a protective layer, so that only the front side of the radial cylinder, which corresponds to the earlier pipe inside, are accessible to the cleaning solutions.
  • the tube or sample consisted of steel of the type AISI 316 L.
  • the oxide layer contained about 50% iron, 40% chromium and 10% nickel, based on the total content of metals.
  • the radioactivity, which was based essentially on the presence of cobalt-60 in the oxide layer, was 2.4 * 10 5 becquerels.
  • the oxide layer or the end face of the sample carrying it had an area of 5.3 cm 2 .
  • a total of 9 cleaning cycles were performed.
  • oxidation was carried out in acidic medium using permanganic acid at a concentration of 0.3 g / l and at a temperature of 95 ° C. This resulted in a pH of about 3 a.
  • the duration of the oxidation was about 17 hours.
  • the remaining reaction solution was replaced with an oxalic acid solution having a concentration of 2 g / l, and thus the oxide layer was treated at a temperature of 95 ° C for about 5 hours.
  • two more cycles of the type described were performed.

Landscapes

  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Chemical Treatment Of Metals (AREA)
EP11721251.4A 2010-04-30 2011-04-26 Verfahren zur oberflächen-dekontamination Active EP2564394B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010028457A DE102010028457A1 (de) 2010-04-30 2010-04-30 Verfahren zur Oberflächen-Dekontamination
PCT/EP2011/056580 WO2011134958A1 (de) 2010-04-30 2011-04-26 Verfahren zur oberflächen-dekontamination

Publications (2)

Publication Number Publication Date
EP2564394A1 EP2564394A1 (de) 2013-03-06
EP2564394B1 true EP2564394B1 (de) 2013-12-11

Family

ID=44521403

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11721251.4A Active EP2564394B1 (de) 2010-04-30 2011-04-26 Verfahren zur oberflächen-dekontamination

Country Status (9)

Country Link
US (1) US20130220366A1 (ko)
EP (1) EP2564394B1 (ko)
JP (1) JP2013529299A (ko)
KR (1) KR20130014494A (ko)
CN (1) CN102667958A (ko)
DE (1) DE102010028457A1 (ko)
ES (1) ES2441589T3 (ko)
TW (1) TW201201221A (ko)
WO (1) WO2011134958A1 (ko)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5787588B2 (ja) * 2011-04-18 2015-09-30 三菱重工業株式会社 化学洗浄方法
KR101523763B1 (ko) * 2013-06-19 2015-06-01 한국원자력연구원 금속 표면 고착성 방사능 오염 산화막 제거를 위한 산화 제염제 및 이를 이용한 산화 제염방법
JP6547224B2 (ja) * 2015-01-30 2019-07-24 三菱重工業株式会社 化学除染方法
HUE047725T2 (hu) 2015-02-05 2020-05-28 Framatome Gmbh Eljárás fém felületek szennyezõdés-mentesítésére nukleáris reaktor hûtõrendszerében
DE102016104846B3 (de) * 2016-03-16 2017-08-24 Areva Gmbh Verfahren zur Behandlung von Abwasser aus der Dekontamination einer Metalloberfläche, Abwasserbehandlungsvorrichtung und Verwendung der Abwasserbehandlungsvorrichtung
JP6580509B2 (ja) * 2016-03-31 2019-09-25 三菱重工業株式会社 固形物除去方法
US10830093B2 (en) * 2017-06-13 2020-11-10 General Electric Company System and methods for selective cleaning of turbine engine components
DE102017115122B4 (de) * 2017-07-06 2019-03-07 Framatome Gmbh Verfahren zum Dekontaminieren einer Metalloberfläche in einem Kernkraftwerk
JP6901947B2 (ja) * 2017-09-29 2021-07-14 三菱重工業株式会社 化学除染方法
CN108560003A (zh) * 2018-01-08 2018-09-21 绵阳科大久创科技有限公司 一种金属表面放射性污染去污剂及其使用方法
CN113105955A (zh) * 2021-03-31 2021-07-13 山东核电有限公司 一种用于ap1000反应堆一回路部件放射性污染沉积氧化物的去污配方和去污方法

Family Cites Families (14)

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Publication number Priority date Publication date Assignee Title
US4587043A (en) * 1983-06-07 1986-05-06 Westinghouse Electric Corp. Decontamination of metal surfaces in nuclear power reactors
SE451915B (sv) * 1984-03-09 1987-11-02 Studsvik Energiteknik Ab Forfarande for dekontaminering av tryckvattenreaktorer
DE3413868A1 (de) * 1984-04-12 1985-10-17 Kraftwerk Union AG, 4330 Mülheim Verfahren zur chemischen dekontamination von metallischen bauteilen von kernreaktoranlagen
JPH0631867B2 (ja) * 1984-07-09 1994-04-27 石川島播磨重工業株式会社 脱硝濃縮器付着クラッドの溶解方法
JPH0664191B2 (ja) * 1986-05-07 1994-08-22 科学技術庁原子力局長 放射性クラッドを化学的に溶解するための汚染除去方法
CH673545A5 (ko) * 1987-10-02 1990-03-15 Industrieorientierte Forsch
DE58906153D1 (de) * 1988-08-24 1993-12-16 Siemens Ag Verfahren zur chemischen Dekontamination der Oberfläche eines metallischen Bauteils einer Kernreaktoranlage.
JPH0699193A (ja) * 1992-09-24 1994-04-12 Ebara Kogyo Senjo Kk 化学除染方法
JP3859902B2 (ja) * 1998-06-23 2006-12-20 株式会社東芝 放射線取扱施設の構造部品の化学除染方法及びその装置
US20030139047A1 (en) * 2002-01-24 2003-07-24 Thomas Terence M. Metal polishing slurry having a static etch inhibitor and method of formulation
CA2633626C (en) * 2005-11-29 2010-05-04 Areva Np Gmbh Method for the decontamination of an oxide layer-containing surface of a component or a system of a nuclear facility
JP4204596B2 (ja) * 2006-02-09 2009-01-07 株式会社東芝 化学除染装置およびその除染方法
FR2897786B1 (fr) * 2006-02-24 2008-06-27 Commissariat Energie Atomique Procede de nettoyage d'un substrat contamine par des contaminants inorganiques particulaires, a l'aide d'un fluide dense sous pression
FR2937054B1 (fr) * 2008-10-13 2010-12-10 Commissariat Energie Atomique Procede et dispositif de decontamination d'une surface metallique.

Also Published As

Publication number Publication date
JP2013529299A (ja) 2013-07-18
WO2011134958A1 (de) 2011-11-03
CN102667958A (zh) 2012-09-12
KR20130014494A (ko) 2013-02-07
TW201201221A (en) 2012-01-01
US20130220366A1 (en) 2013-08-29
EP2564394A1 (de) 2013-03-06
DE102010028457A1 (de) 2011-11-03
ES2441589T3 (es) 2014-02-05

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