EP0273182B1 - Procédé de nettoyage d'un réservoir - Google Patents

Procédé de nettoyage d'un réservoir Download PDF

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Publication number
EP0273182B1
EP0273182B1 EP87117112A EP87117112A EP0273182B1 EP 0273182 B1 EP0273182 B1 EP 0273182B1 EP 87117112 A EP87117112 A EP 87117112A EP 87117112 A EP87117112 A EP 87117112A EP 0273182 B1 EP0273182 B1 EP 0273182B1
Authority
EP
European Patent Office
Prior art keywords
container
hydrazine
cleaning
salt solution
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.)
Revoked
Application number
EP87117112A
Other languages
German (de)
English (en)
Other versions
EP0273182A1 (fr
Inventor
Klaus Kuhnke
Alexander Dr. Langner
Klaus Dipl.-Chem. Pflugbeil
Kurt Dipl.-Ing. Schindler
Dorothea Dipl.-Ing. Moldenhauer
Siegfried Dr. Köhler
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.)
Siemens AG
Original Assignee
Siemens AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=6314830&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0273182(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Siemens AG filed Critical Siemens AG
Publication of EP0273182A1 publication Critical patent/EP0273182A1/fr
Application granted granted Critical
Publication of EP0273182B1 publication Critical patent/EP0273182B1/fr
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

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Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—Iron or steel
    • 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

Definitions

  • the invention relates to a method for cleaning a container, in particular a steam generator in a nuclear power plant, iron oxide located in the container being dissolved by a complexing acid.
  • a cleaning method is known from DE-A 1 517 406 with which scale is removed from metal surfaces.
  • scale can contain iron oxide, it consists primarily of calcium compounds.
  • a saline solution containing, for example, a salt of nitrilotriacetic acid is used to remove scale.
  • Ammonia is also used to adjust the pH.
  • the known solution works passivating and decomposing. The main thing that decomposes is scale. The passivation is a protection of the cleaned surface by a layer to be applied. The surface is specifically oxidized. Otherwise, the dissolution temperature of the salt is not exceeded in the known. So there is not a fully dissolved salt.
  • the known method removes scale and not iron oxide.
  • the solution used has a passivating effect. This means that an iron oxide protective layer is built up.
  • a process for removing iron oxide is known from CA-A 1 062 590.
  • An acid is used, which may be mixed with hydrazine.
  • a multi-stage process the so-called Mark III process, is also known, which is carried out alternately in the acidic and in the neutral range. This complex cleaning process takes a lot of time and causes very high costs.
  • the invention was therefore based on the object of specifying a method for cleaning a container, in particular a steam generator, which, with very good effectiveness, minimizes attacks by the cleaning chemicals on the materials of the container and the lines, by not bringing any aggressive acids into contact with the surface. It is not intended to build up a protective layer of oxides, but rather to dissolve iron oxide. The chemicals used should always be completely dissolved in a solution for better effectiveness.
  • the object is achieved according to the invention in that a salt solution which is produced from an acid which is a complexing agent, from a volatile alkalizing agent and from a reducing agent and which has an alkaline reducing effect is introduced into the container in such a way that the saline solution for a predetermined period of time at a temperature between 150 ° C and 250 ° C and below the decomposition temperature of the anionic part of the salt solution for the purpose of forming an iron complex in the container, and that the dissolved iron complex is then removed by emptying the container.
  • the iron complexation and thus the cleaning of the container takes place with great effectiveness in the alkaline range.
  • the acid, or its anionic part causes the complex formation.
  • the volatile alkalizing agent raises the pH of the cleaning solution to the alkaline range.
  • the cleaning solution therefore has a reducing and not passivating effect. So no protective layer is built up, but iron oxide is removed.
  • the reducing conditions caused by the reducing agent are necessary, on the one hand, to reduce trivalent iron to divalent iron and, on the other hand, to reduce harmful effects of the cleaning solution on the metal surfaces of the container.
  • the desired iron complexation in the alkaline range is made possible.
  • a temperature below the dissolution temperature of a salt that is, a temperature at which the salt is not completely dissolved, is unsuitable for complex formation.
  • the pH value of the cleaning solution is of crucial importance for optimal cleaning efficiency. A pH value that is too low would lead to a high removal of base metal from unalloyed and low-alloyed materials in the container. If the pH is too high, the iron solubility is greatly reduced.
  • Optimal cleaning success with low base metal removal on unalloyed and low-alloy materials is achieved with the cleaning method according to the invention at a pH between 9.0 and 9.5 and at a temperature between 170 ° C and 220 ° C.
  • the advantage is achieved that in only one process step and with great effectiveness, the container is freed from iron oxide deposits without the surfaces of the container and the supply pipes being attacked or even damaged by acids. Containers and pipes are not attacked by the alkaline chemical solution.
  • the cleaning process according to the invention can be carried out 40 times faster and causes only a tenth of the costs incurred there.
  • nitrilotriacetic acid which is known per se, is used as the complex-forming acid.
  • Suitable volatile alkalizing agents are preferably ammonia, hydrazine, morpholine or a mixture of the substances mentioned. Hydrazine, for example, is used as the reducing agent. Hydrazine can thus act as a volatile alkalizing agent and as a reducing agent.
  • the dissolved salt is adjusted to a pH greater than 9.6 by a further addition of volatile alkalizing agent and then metered into the container.
  • the optimum pH value for cleaning which is between 9.0 and 9.5, is adjusted by partially evaporating the volatile alkalizing agent and water in the container. This pH value control advantageously prevents complex formation and thus removal in the mostly very long supply line to the container, which would result in reduced cleaning performance in the container itself.
  • the pH is to be controlled via the composition of the metered solution and the duration of the evaporation of the alkalizing agent.
  • the evaporation process advantageously results in homogeneous mixing of the solution in the container.
  • part of the solution in the container is evaporated for a limited time. This creates a flow within the container, which leads to even better contact between the cleaning solution and the surfaces to be cleaned.
  • alkalizing agents e.g. Hydrazine
  • the dissolved salt to be dosed is degassed, for example, before dosing and 0.1% to 5% hydrazine is added to it as a reducing agent. Hydrazine is also regularly metered into the container during cleaning, so that a hydrazine concentration of 10 to 500 milligrams per gram is set there.
  • the container is emptied.
  • the container is pressed empty, for example by an inert gas, in particular by nitrogen or water vapor. This prevents iron oxide from being formed again by penetrating atmospheric oxygen.
  • a possible proportion of copper in the deposits in the container does not interfere with the method according to the invention as long as it is less than 10%.
  • the copper can then be removed after the iron oxide has been removed in accordance with the invention.
  • the advantage of the invention is that containers, in particular steam generators of a nuclear power plant, can be reliably freed of iron oxide deposits in a short time and at low cost while protecting the metal surfaces. Particularly in the case of nuclear power plants, a particular advantage can be seen in the fact that only a downtime of approximately 12 hours is required for a complete cleaning of a steam generator.
  • impurities which are introduced and deposited in the form of salts in the container in continuous operation are effectively removed.
  • damage to the low and unalloyed base metals by etching is also excluded.
  • the chemicals required for the process according to the invention cause considerably lower costs than other cleaning processes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Food Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Detergent Compositions (AREA)

Claims (9)

  1. Procédé pour nettoyer un réservoir, notamment un générateur de vapeur dans une centrale nucléaire, selon lequel on dissout l'oxyde de fer situé dans le réservoir au moyen d'un acide complexant,
    caractérisé par le fait qu'on introduit dans le réservoir une solution salée, qui est formée à partir d'un acide, qui est un agent complexant, d'un agent volatil d'alcalisation et d'un agent réducteur, et a un effet réducteur alcalin, qu'on laisse reposer la solution dans le réservoir pendant un intervalle de temps prédéterminé à une température comprise entre 150°C et 250°C et inférieure à la température de décomposition de la partie anionique de la solution salée, pour obtenir la formation d'un complexe du fer, et qu'on retire ensuite le complexe de fer dissous en vidant le réservoir.
  2. Procédé suivant la revendication 1, caractérisé par le fait que l'acide est l'acide nitrolotriacétique.
  3. Procédé suivant la revendication 1, caractérisé par le fait que l'agent volatil d'alcalisation est l'ammoniac, l'hydrazine et/ou la morpholine.
  4. Procédé suivant la revendication 1, caractérisé par le fait que l'agent réducteur est l'hydrazine.
  5. Procédé suivant l'une des revendications 1 à 4, caractérisé par le fait qu'on règle la valeur du pH de la solution salée à une valeur supérieure à 9,6, avant de l'introduire dans le réservoir, au moyen d'une addition de l'agent volatil d'alcalisation et qu'on l'introduit ensuite seulement dans le réservoir, et qu'après ou pendant cette introduction, on règle une valeur du pH, optimale pour le nettoyage, entre 9,0 et 9,5 au moyen d'une évaporation partielle de l'agent volatil d'alcalisation dans le réservoir.
  6. Procédé suivant l'une des revendications 1 à 4, caractérisé par le fait qu'avant de retirer le contenu du réservoir, on l'évapore partiellement, ce qui fait apparaître un mélange homogène intime du contenu en raison du déplacement lié à l'ébullition.
  7. Procédé suivant l'une des revendications 1 à 4, caractérisé par le fait qu'avant d'introduire la solution salée dans le réservoir, on la dégaze et on mélange à cette solution 0,1 % à 5 % d'hydrazine et que, pendant l'intervalle de temps prédéterminé, on ajoute l'hydrazine d'une manière régulière et dosée et qu'on règle de ce fait une concentration d'hydrazine comprise entre 10 mg/kg et 500 mg/kg dans le réservoir.
  8. Procédé suivant l'une des revendications 1 à 4, caractérisé par le fait que lors du vidage du réservoir, on met ce dernier sous pression en utilisant un gaz inerte, notamment de l'azote ou de la vapeur d'eau.
  9. Procédé suivant l'une des revendications 1 à 4, caractérisé par le fait que, dans le cas de dépôts de cuivre dans le réservoir avec une concentration de cuivre supérieure à 10 % de tous les dépôts, on élimine le cuivre avant la complexation de l'oxyde de fer.
EP87117112A 1986-12-01 1987-11-19 Procédé de nettoyage d'un réservoir Revoked EP0273182B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3640428 1986-12-01
DE3640428 1986-12-01

Publications (2)

Publication Number Publication Date
EP0273182A1 EP0273182A1 (fr) 1988-07-06
EP0273182B1 true EP0273182B1 (fr) 1991-07-31

Family

ID=6314830

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87117112A Revoked EP0273182B1 (fr) 1986-12-01 1987-11-19 Procédé de nettoyage d'un réservoir

Country Status (7)

Country Link
US (1) US5164015A (fr)
EP (1) EP0273182B1 (fr)
JP (1) JPS63143276A (fr)
KR (1) KR950013495B1 (fr)
CA (1) CA1316799C (fr)
DE (1) DE3771859D1 (fr)
ES (1) ES2023397B3 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4131766A1 (de) * 1991-09-24 1993-03-25 Siemens Ag Verfahren zur dekontamination des primaerkreises eines kernkraftwerkes
DE4308209A1 (de) * 1993-03-15 1994-09-22 Siemens Ag Reinigungsverfahren

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5078894A (en) * 1990-04-30 1992-01-07 Arch Development Corporation Formulations for iron oxides dissolution
DE4117625C2 (de) * 1991-05-29 1997-09-04 Siemens Ag Reinigungsverfahren
DE4216383A1 (de) * 1992-05-18 1993-11-25 Siemens Ag Verfahren zum Reinigen eines geschlossenen Behälters
AU757069B2 (en) * 1998-05-22 2003-01-30 Siemens Aktiengesellschaft Method for cleaning a container
DE10238730A1 (de) * 2002-08-23 2004-03-04 Framatome Anp Gmbh Verfahren zur Reinigung des Dampferzeugers eines Druckwasserreaktors
DE102004054471B3 (de) * 2004-11-11 2006-04-27 Framatome Anp Gmbh Reinigungsverfahren zur Entfernung von Magnetit enthaltenden Ablagerungen aus einem Druckbehälter eines Kraftwerks
DE102007023247B3 (de) 2007-03-07 2008-08-07 Areva Np Gmbh Verfahren zur Entfernung von Magnetit und Kupfer enthaltenden Ablagerungen aus Behältern von Industrie- und Kraftwerksanlagen
DE102008005199B4 (de) 2008-01-18 2014-01-23 Areva Gmbh Verfahren zur Reinigung eines Wärmetauschers
KR101014751B1 (ko) * 2008-09-26 2011-02-15 한국전력공사 증기 발생기의 화학 세정 방법
EP2418023A1 (fr) * 2010-08-13 2012-02-15 Siemens Aktiengesellschaft Procédé pour terminer un nettoyage chimique d'une centrale thermique
JP6093551B2 (ja) 2012-11-06 2017-03-08 株式会社貝印刃物開発センター 剃刀

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE635216A (fr) * 1962-07-23
US3296027A (en) * 1964-11-19 1967-01-03 Nalco Chemical Co Removal and inhibition of scale formation in steam generation
US3627687A (en) * 1968-02-09 1971-12-14 Dow Chemical Co Cleaning of ferrous metal surfaces
US3627857A (en) * 1968-02-15 1971-12-14 Yawata Iron & Steel Co Heating controlling system in a multizone type continuously heating furnace
AT297442B (de) * 1970-04-01 1972-03-27 Unilever Nv Verfahren zum Reinigen, Entfetten, Entzundern und Beizen von Metallen
JPS503740A (fr) * 1973-05-16 1975-01-16
CA1062590A (fr) * 1976-01-22 1979-09-18 Her Majesty In Right Of Canada As Represented By Atomic Energy Of Canada Limited Methode de decontamination des reacteurs
DD237095A3 (de) * 1978-10-27 1986-07-02 Balaban Irmenin Jurij V Verfahren zur dekontamination von ausruestungen nuklearer dampferzeugungsanlagen
SE8204843L (sv) * 1982-01-18 1983-07-19 Dearborn Chemicals Co Reningsforfarande
FR2562710B1 (fr) * 1984-04-05 1989-02-17 Electricite De France Procede pour eliminer les depots formes dans un generateur de vapeur de reacteur nucleaire a eau pressurisee

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4131766A1 (de) * 1991-09-24 1993-03-25 Siemens Ag Verfahren zur dekontamination des primaerkreises eines kernkraftwerkes
DE4308209A1 (de) * 1993-03-15 1994-09-22 Siemens Ag Reinigungsverfahren

Also Published As

Publication number Publication date
KR950013495B1 (ko) 1995-11-08
DE3771859D1 (de) 1991-09-05
EP0273182A1 (fr) 1988-07-06
JPS63143276A (ja) 1988-06-15
KR880007138A (ko) 1988-08-26
ES2023397B3 (es) 1992-01-16
JPH0588317B2 (fr) 1993-12-21
US5164015A (en) 1992-11-17
CA1316799C (fr) 1993-04-27

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