EP1060476B1 - Verfahren und anlage zur dekontamination metallischer oberflächen - Google Patents

Verfahren und anlage zur dekontamination metallischer oberflächen Download PDF

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Publication number
EP1060476B1
EP1060476B1 EP99903548A EP99903548A EP1060476B1 EP 1060476 B1 EP1060476 B1 EP 1060476B1 EP 99903548 A EP99903548 A EP 99903548A EP 99903548 A EP99903548 A EP 99903548A EP 1060476 B1 EP1060476 B1 EP 1060476B1
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EP
European Patent Office
Prior art keywords
decontamination
tank
set forth
solution
ozone
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Expired - Lifetime
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EP99903548A
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English (en)
French (fr)
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EP1060476A1 (de
Inventor
Michel Klein
Mathieu Marie Fernand Ponnet
André Henri Alain Joseph RAHIER
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Centre dEtude de lEnergie Nucleaire CEN
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Centre dEtude de lEnergie Nucleaire CEN
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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

Definitions

  • the subject of the present invention is a method for decontaminating metal surfaces, according to which the latter are treated with an acid solution of cerium with a valence of 4 + , the ceric ion being regenerated with ozone in such a way that continuous in a gas-liquid contactor at substantially the same temperature as that of the aforesaid solution.
  • the metal surfaces to be decontaminated may or may not be covered with a layer of oxides. Decontamination takes place by reaction of the cerium acid with the metal and / or the oxide layer covering the surface of this metal.
  • the metal surfaces in question may be contaminated with both natural and artificial radioisotopes and non-radioactive elements.
  • the surfaces are part of metal parts that can come from nuclear reactors of different types, such as pressurized water reactors, boiling water reactors, gas-cooled reactors or others.
  • the radioactive contamination is either related to the activation of impurities by the reactor core and the deposit and fixation of this contamination on the metal walls, either caused by radioactive leaks at the fuel elements and the fission product deposition. and of fuels on the metal walls.
  • Parts contaminated with radioactive material may also come from nuclear fuel, spent fuel reprocessing facilities, nuclear waste facilities, low, medium and high activity laboratories handling radioactive elements, radioactive waste storage facilities, and any facility in which radioactive products are handled.
  • the metal parts contaminated by non-radioactive elements can be contaminated either by the deposit or by the attachment of a contaminant on the metal or in the oxide layer present on the surface of the metal.
  • the metals may have undergone oxidation at a temperature above room temperature, the layer of corrosion products formed having the particularity of strongly fixing the contaminants.
  • This known method comprises treating the contaminated surfaces with an aqueous oxidizing agent having a pH of less than 7 and containing cerium nitrate, chromic acid and ozone at a temperature below 60 ° C and preferably below 25 ° C.
  • the oxidizing agent is an acidic solution of Ce 4+ saturated with ozone. This solution is sent co-currently in the system to be decontaminated until the total depletion of Ce 4+ / 0 3 before returning to the ozonation reactor and recovering its oxidizing potential ".
  • EP-A-0.180.826 discloses a method as defined in the first paragraph.
  • the treatment of the surface also takes place at low temperature, that is to say a temperature below 50 ° C.
  • the ceric ion is regenerated with ozone in an injection column in which ozone is injected at the lower end while the solution with ceric ion flows up and down.
  • metallic surfaces of a nuclear reactor are decontaminated first by a decontamination composition which is added to the refrigerant and then removed, and then, after cooling the refrigerant to 40 to 100 ° C. C, by a composition comprising ozone dissolved by spraying in water and a soluble compound of Ce 4 .
  • the refrigerant containing this composition is circulated in the reactor cooling system and then heated to at least 100 ° C. Finally this refrigerant is passed through an exchanger comprising an anionic resin, its temperature is adjusted to 60 to 200 ° C and it is re-used.
  • the object of the invention is to overcome the aforementioned drawbacks and to provide a method for decontaminating metal surfaces rapidly and effectively.
  • the metal surface is treated, that is to say oxidized, at a temperature between 60 ° C. and 90 ° C. by an acid solution of cerium containing cerium at the valence 4 + .
  • the cerium being regenerated by injection of ozone into the decontamination solution in a static mixer type gas-liquid contactor in which the ozone and the acidic solution based on cerium are transported in co-current.
  • No. 4,162,229 discloses the treatment of contaminated surfaces with an aqueous solution based on a cerium (4 + ) salt at a temperature between 20 ° C. and 90 ° C. followed by the removal of the solution and No. 4,657,596 discloses the treatment of such surfaces with an aqueous solution containing ceric acid at temperatures between 70 ° C and 200 ° C. None of these documents describes a regeneration of cerium, which suggests that such eventual regeneration takes place in a separate step and at another temperature.
  • the invention also relates to a device particularly intended for carrying out the method according to the aforementioned invention.
  • the invention more particularly relates to a decontamination installation for metal surfaces, comprising a decontamination tank, and a gas-liquid contactor connected to an ozone production system, the tank and the contactor being mounted in a circulation loop of the decontamination solution.
  • gas-liquid contactor is a conctactor with an injector or with an injection column.
  • the gas-liquid regeneration contactor is a gas-liquid contactor of the static mixer type.
  • the installation represented in the figure essentially comprises a decontamination tank 1 filled with decontamination solution, a gas-liquid regeneration contactor 2 connected to an ozone production system 3, and a buffer tank 4, the decontamination tank 1. , the contactor 2 and the buffer tank 4 being mounted in the same circulation loop 5 of the decontamination solution.
  • the decontamination tank 1 is made of zirconium and has for example a content of about 2 m 3 . It is closed by a cover 6 on which ultrasound probes 7 are fixed.
  • This decontamination tank 1 is provided at its upper part with an overflow 8 connected to a discharge pipe 9 opening into the buffer tank 4 located below the decontamination tank 1 and heated by a heating system 10.
  • this heating system 10 is not mounted in the buffer tank 4 but in the decontamination tank 1.
  • the tank 1 has an exhaust duct 11 for gas opening into a gas treatment device 12 comprising in series a condenser 13, a deiciler 14 and a residual ozone destruction unit. 15.
  • the condensates of the condenser 13 are collected in a tank 16 and returned via the conduit 17 to the exhaust duct 9 aforesaid.
  • a basket 18 for the parts to be decontaminated. Like the rest of the installation, it must be made of a material having a high corrosion resistance, although it may be lower than the resistance of the material of the tank 1.
  • This basket 18 and the other components such as the buffer tank 4, loop 5 and contactor 2 can be made of titanium provided that the medium remains oxidizing or coated material such as enamelled materials or materials coated with a fluoropolymer coating.
  • the circulation loop 5 comprises, apart from the evacuation duct 9, also a suction duct 19 connected on the one hand to the bottom of the buffer tank 4 and on the other hand to a pump 20 and a discharge duct 21 between the pump 20 and the bottom of the decontamination tank 1, the gas-liquid contactor 2 being mounted in this duct 21.
  • a duct 22 comprising a valve 23 connects this discharge duct 21, just below the decontamination tank 1 with the buffer tank 4.
  • the ozone production system 3 is connected to the discharge pipe 21, between the pump 20 and the contactor 2, via a pipe 24.
  • This ozone production system 3 comprises an ozonizer 25 connected to an oxygen reservoir 26 by a line 27.
  • the gas-liquid contactor 2 is a co-current contactor formed by a column filled with packing elements providing a high exchange surface, more particularly a static mixer.
  • the buffer tank 4 is also mounted in a filtration loop 28 and comprises a suction duct 29 connected to the bottom of the buffer tank 4 and to a pump 30, and a discharge duct 31 between the pump 30 and the upper part of the tank.
  • buffer 4 a valve 32, a filter 33, a second valve 34 and a third valve 35 being successively mounted in this discharge conduit 31.
  • the filter 33 is short-circuited by a duct 36 with a valve 37.
  • a duct 38 is connected to the duct 31.
  • This duct 38 comprises a valve 39 and is connected to an effluent storage tank 40.
  • the exhaust duct 11 is connected by a duct 41 to the buffer tank 4.
  • the decontamination solution heated to a temperature between 60 ° C and 90 ° C and preferably at a temperature between 80 ° C and 85 ° C, for example at 82 ° C, in the buffer tank 4, is transferred by the pump 20 from the latter into the reservoir of decontamination 1.
  • the solution is heated to the aforesaid temperature in the latter tank.
  • This decontamination solution is an acid solution of cerium sulphate thus containing Ce 4+ .
  • the principle of decontamination is based on the oxidative nature of this 4+ / Ce 3+ couple. When this solution is brought into contact with steels, it leads to their corrosion by oxidation reactions of metals and oxides.
  • electrolyte In order to minimize the consumption of cerium IV and to ensure maximum stability to the solution, the electrolyte must be chosen carefully.
  • the most suitable electrolyte according to the invention is sulfuric acid, although nitric acid is also usable.
  • the total concentration of cerium is between 0.1 and 50 g / l and preferably between 1 and 15 g / l, for example of the order of 0.05 M and the concentration of sulfuric acid between 10 -1 and 2 M, preferably between 1 and 2 M, for example 1 M.
  • the aforementioned decontamination solution circulates continuously through the circulation loop 5, that is to say, the solution overflowing by the overflow 8 returns to the buffer tank 4, from where it is pumped via the conduit of suction 19 by the pump 20.
  • this solution is discharged through the contactor 2 where it is regenerated by means of ozone of the ozone production system 3 and, before returning via the conduit 21 to the decontamination tank 1.
  • the oxygen of the reservoir 26 is charged with ozone, for example with a concentration of 5 to 500 g of ozone per m 3 , in the ozonizer 25, and is injected towards the line 27 at the bottom of the contactor 2.
  • the ratio of ceric sulfate (Ce 4+ ) to cerous sulphate (Ce 3+ ) is between 20 and 0.1 and preferably between 3 and 0.5.
  • the ratio Ce 4+ / Ce 3+ must be maintained at a value greater than or equal to 1 to ensure sufficient attack speed.
  • the ozone flow rate is adjusted according to the particular application and is essentially a function of the treated surface, the etching rate of the material of the parts to be decontaminated and the regeneration efficiency.
  • This flow rate is normally between 0.1 and 1 kg O 3 / h for 20 m 2 of treated surface.
  • the oxygen charged with residual ozone leaving the exhaust pipe 11 is first cooled in the condenser 13 to condense the acid vapors that are evacuated via the tank 16 to the buffer tank 4 via the ducts 17 and 9.
  • the gases leaving the condenser 13 are removed from the liquid aerosols in the stripper 14 after which the residual ozone is destroyed in the unit 15.
  • the flow rate of the solution pumped by the pump 20 depends on the particular application but is generally between 10 and 100 renewals of the contents of the decontamination tank 1.
  • the solution is filtered after decontamination.
  • the valves 32, 34 and 35 are open and the pump 30 is turned on.
  • the solution is pumped from the buffer tank 4 and discharged through the filter 33 to this buffer tank 4.
  • the filtration rate is normally from 1 to 10 renewals of the contents of the tank 4 per hour.
  • the ultrasound probes 7 plunging into the bath of the tank 1 can emit ultrasound. These ultrasounds accelerate the kinetics of the process and can achieve either lower residual contamination levels, or achieve identical efficiencies in shorter times.
  • the residence time of the parts to be decontaminated in the decontamination tank 1 can be reduced to 1 to 8 hours, depending on the particular application.
  • the solution in the decontamination tank 1 is transferred to the buffer tank 4 after opening the valve 23 and the basket 18 is removed from the tank 1, drained and transferred to a rinsing tank.
  • the cleaning of the parts in the rinsing tank is achieved by preferably using an ultrasonic cleaning combined with a closed circuit filtration of the rinsing solution.
  • the basket 18 is removed from the rinsing tank and drained and the pieces are removed from the basket 18 and checked.
  • these parts are either discharged as non-radioactive waste, recycled for a second pass through the decontamination device, disposed of as radioactive waste or discharged to a metal waste melting facility.
  • the solution is transferred from the buffer tank 4 via line 38 in the liquid effluent storage tank 40 by opening valve 39.
  • the device described above can be used to decontaminate the equipment on site. It is sufficient to connect the circulation loop 5 via a pump and temporary conduits to this equipment.
  • the solution circulating in the loop 5, the oxidation and the regeneration take place at the same time and continuously, at the same rather high temperature.
  • the regeneration efficiency that is the ratio between the amount of ozone used and the amount of ozone produced, is high. The rate of destruction of the ozone and the activation energy of the oxidation reaction are therefore sufficiently low.
  • the contactor 2 allows optimal extraction of ozone from the gas phase, that is to say oxygen or air, and a sufficient contact time between the gas loaded with ozone and the solution.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Claims (14)

  1. Verfahren zur Dekontaminierung von metallischen Oberflächen, bei dem diese mit Hilfe einer Säurelösung aus 4-wertigem Cer behandelt werden, wobei das Cer-Ion in einem Gas-Flüssigkeits-Kontaktapparat (2), der im Wesentlichen die gleiche Temperatur wie die Lösung aufweist, kontinuierlich mit Ozon regeneriert wird,
    dadurch gekennzeichnet, dass die metallische Oberfläche bei einer Temperatur zwischen 60°C und 90°C durch die das 4-wertige Cer enthaltene Säurelösung behandelt wird, wobei das 4-wertige Cer durch Einspritzung von Ozon in die Dekontaminierungslösung in einem Gas-Flüssigkeitskontaktapparat (2) vom Typ statischer Mischer regeneriert wird, in den das Ozon und die Säurelösung auf Cer-Basis in Fließrichtung befördert werden.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet, dass die Cer-haltige Säurelösung als Säuremedium Schwefelsäure enthält, die vorzugsweise eine Konzentration zwischen 10-1 und 2 M aufweist.
  3. Verfahren nach Anspruch 1 oder 2,
    dadurch gekennzeichnet, dass das 4-wertige Cer aus Cersulfat stammt, das vorzugsweise eine Konzentration zwischen 0,1 und 50 g pro 1 Lösung aufweist.
  4. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet, dass die in der Lösung zu dekontaminierenden Werkstücke Ultraschallwellen ausgesetzt sind.
  5. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet, dass die Lösung während der Dekontaminierung in einem geschlossenen Kreislauf (5) umläuft, der aus einem Dekontaminierungsbehälter (1), in dem die Dekontaminierung stattfindet, einem Pufferbehälter (4) und einem Gas-Flüssigkeits-Kontaktapparat (2) gebildet ist, in den das Ozon für die Regenerierung eingespritzt wird, die über Rohrleitungen (9, 19, 21) verbunden sind.
  6. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet , dass die Lösung nach der Dekontaminierung gefiltert wird.
  7. Anlage zur Dekontaminierung von metallischen Oberflächen, umfassend einen Dekontaminierungsbehälter (1) und einen Gas-Flüssigkeits-Kontaktapparat, der an ein Ozonerzeugungssystem (3) angeschlossen ist, wobei der Behälter (1) und der Kontaktapparat (2) in einem Kreislauf (5) für den Umlauf der Dekontaminierungslösung angeordnet sind,
    dadurch gekennzeichnet, dass der Gas-Flüssigkeits-Kontaktapparat (2) für die Regenerierung ein Gas-Flüssigkeits-Kontaktapparat vom Typ statischer Mischer ist.
  8. Anlage nach Anspruch 7,
    dadurch gekennzeichnet, dass sie einen Pufferbehälter (4) aufweist, der mit einem Überlaufrohr (8) des Dekontaminierungsbehälters (1) verbunden ist, wobei der Zulauf des Kontaktapparats (2) über eine Rohrleitung (19) mit dem Pufferbehälter (4) und der Ablauf des Kontaktapparats (2) über eine Rohrleitung (21) mit dem Dekontaminierungsbehälter (1) verbunden ist, wobei eine Pumpe (20) in der ersten Rohrleitung (19) angeordnet ist und das Ozonerzeugungssystem (3) zwischen dieser Pumpe (20) und dem Kontaktapparat (2) auch mit dieser Rohrleitung (19) verbunden ist, wobei die Rohrleitungen (19 und 21) Bestandteil des Umlaufkreislaufs sind (5).
  9. Anlage nach Anspruch 8,
    dadurch gekennzeichnet, dass in dem Pufferbehälter (4) Heizmittel (10) angeordnet sind.
  10. Anlage nach Anspruch 8,
    dadurch gekennzeichnet, dass in dem Dekontaminierungsbehälter (1) Heizmittel (10) angeordnet sind.
  11. Anlage nach einem der vorhergehenden Ansprüche 7 bis 10,
    dadurch gekennzeichnet, dass an dem Dekontaminierungsbehälter (1) mindestens eine Ultraschallsonde (7) angeordnet ist.
  12. Anlage nach einem der vorhergehenden Ansprüche 7 bis 10,
    dadurch gekennzeichnet, dass der Kontaktapparat (2) ein statischer Mischer ist, der eine mit Füllelementen gefüllte Kolonne aufweist.
  13. Anlage nach Anspruch 8 oder 9,
    dadurch gekennzeichnet, dass sie einen Filterkreislauf mit einem Filter (33) aufweist, der mit dem Pufferbehälter (4) verbunden ist.
  14. Anlage nach einem der vorhergehenden Ansprüche 7 bis 13,
    dadurch gekennzeichnet, dass der Dekontaminierungsbehälter (1) aus Zirkonium ist.
EP99903548A 1998-02-20 1999-02-16 Verfahren und anlage zur dekontamination metallischer oberflächen Expired - Lifetime EP1060476B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
BE9800132 1998-02-20
BE9800132A BE1011754A3 (fr) 1998-02-20 1998-02-20 Procede et installation de decontamination de surfaces metalliques.
PCT/BE1999/000019 WO1999043006A1 (fr) 1998-02-20 1999-02-16 Procede et installation de decontamination de surfaces metalliques

Publications (2)

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EP1060476A1 EP1060476A1 (de) 2000-12-20
EP1060476B1 true EP1060476B1 (de) 2006-11-15

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EP (1) EP1060476B1 (de)
AT (1) ATE345571T1 (de)
BE (1) BE1011754A3 (de)
DE (1) DE69933997T2 (de)
ES (1) ES2277425T3 (de)
WO (1) WO1999043006A1 (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2792763B1 (fr) * 1999-04-26 2004-05-28 Commissariat Energie Atomique Procede de decontamination radioactive d'une paroi en acier et dispositif de decontamination radioactive
JP2003098294A (ja) * 2001-09-27 2003-04-03 Hitachi Ltd オゾンを用いた除染方法及びその装置
KR101086600B1 (ko) * 2006-02-09 2011-11-23 가부시끼가이샤 도시바 화학 제염 장치 및 그 제염 방법

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH619807A5 (de) * 1976-04-07 1980-10-15 Foerderung Forschung Gmbh
CA1229480A (en) * 1983-07-12 1987-11-24 Alexander P. Murray Ozone oxidation of deposits in cooling systems of nuclear reactors
SE451915B (sv) * 1984-03-09 1987-11-02 Studsvik Energiteknik Ab Forfarande for dekontaminering av tryckvattenreaktorer
FR2565021B1 (fr) * 1984-05-25 1992-03-06 Toshiba Kk Appareil de decontamination de dechets metalliques radioactifs
CA1230806A (en) * 1984-05-29 1987-12-29 Clifton G. Slater Ceric acid decontamination of nuclear reactors
EP0180826B1 (de) * 1984-10-31 1990-07-11 Siemens Aktiengesellschaft Verfahren zur chemischen Dekontamination von Grosskomponenten und Systemen aus metallischen Werkstoffen von Kernreaktoren
FR2590716B1 (fr) * 1985-11-26 1992-05-15 Electricite De France Procede de decontamination de parois de reacteurs nucleaires, en particulier des parois du circuit primaire des reacteurs nucleaires a circuit d'eau pressurisee
SE465142B (sv) * 1988-08-11 1991-07-29 Studsvik Ab Foerfarande foer dekontaminering av korrosionsprodukter i kaernkraftsreaktorer
JPH0727073B2 (ja) * 1990-03-20 1995-03-29 森川産業株式会社 放射能に汚染された物体の除染方法及び除染装置、並びに同除染に用いられた材料の除染方法及び除染装置
FR2687005B1 (fr) * 1992-02-03 1994-10-21 Framatome Sa Procede et installation de decontamination de la partie primaire d'un generateur de vapeur usage d'un reacteur nucleaire a eau ordinaire sous pression.
FR2701155B1 (fr) * 1993-02-02 1995-04-21 Framatome Sa Procédé et installation de décontamination de couvercles usagés de cuves de réacteurs nucléaires à eau légère.
FR2706217A1 (fr) * 1993-06-08 1994-12-16 Framatome Sa Procédé de remise en état d'un échangeur de chaleur de centrale nucléaire, notamment d'un échangeur de chaleur de circuit auxiliaire de refroidissement d'un réacteur nucléaire à l'arrêt.

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Publication number Publication date
ATE345571T1 (de) 2006-12-15
ES2277425T3 (es) 2007-07-01
DE69933997T2 (de) 2007-05-10
WO1999043006A1 (fr) 1999-08-26
DE69933997D1 (de) 2006-12-28
BE1011754A3 (fr) 1999-12-07
EP1060476A1 (de) 2000-12-20

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