EP0602347B1 - Procédé pour le balayage et le reconditionnement de systèmes de transfert - Google Patents

Procédé pour le balayage et le reconditionnement de systèmes de transfert Download PDF

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Publication number
EP0602347B1
EP0602347B1 EP93116941A EP93116941A EP0602347B1 EP 0602347 B1 EP0602347 B1 EP 0602347B1 EP 93116941 A EP93116941 A EP 93116941A EP 93116941 A EP93116941 A EP 93116941A EP 0602347 B1 EP0602347 B1 EP 0602347B1
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EP
European Patent Office
Prior art keywords
flushing
flushing gas
transfer systems
media
process according
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.)
Expired - Lifetime
Application number
EP93116941A
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German (de)
English (en)
Other versions
EP0602347A1 (fr
Inventor
Manfred Dr. Eschwey
Ulrich Klebe
Jürgen Dr. Schram
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.)
Messer Griesheim GmbH
Original Assignee
Messer Griesheim GmbH
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Filing date
Publication date
Application filed by Messer Griesheim GmbH filed Critical Messer Griesheim GmbH
Publication of EP0602347A1 publication Critical patent/EP0602347A1/fr
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising

Definitions

  • the invention relates to a method for rinsing passivated transfer systems for corrosive gaseous process media according to the preamble of claim 1.
  • these are steels with an austenitic structure such as austenitic stainless steels or austenitic structure components, such as austenite ferrites or CrNi alloys, CuNi alloys or the like, whose limited resistance to corrosive media is solely due to the formation of dense, homogeneous passive layers of approx 10 ⁇ m based.
  • this layer is at least covered with a monomolecular water layer (Fig. 2/1). If this layer comes into contact with dry gaseous hydrogen chloride, this water layer is first removed. The driving force behind this reaction is the enormous hydration tendency of HCl. The original, pure oxide passive layer is then converted into a mixture of metal chlorides and oxides. The iron and chromium oxides are only kinetically but not thermodynamically stable with respect to the corrosive medium HCl, especially with a large excess of HCl. This process, which takes place in the absence of oxygen, is called acid corrosion (Fig. 2 / II). The resulting metal halide layer prevents further dissolution of the metal.
  • the invention is therefore based on the object of providing a method for rinsing and reconditioning transfer systems for corrosive media from passivatable materials, which makes it possible to increase the service life of the transfer systems and to reduce the contamination of the media.
  • the metal halide is converted into the corresponding hydroxide by means of the water vapor.
  • the halogen hydrogen formed is removed by hydrate formation.
  • the hydroxide is then converted into a stable passive oxide layer using dry oxygen or ozone.
  • the preferred ranges for the admixtures O 2 according to the invention extend from 0.1% to 100% and / or from O 3 from 0.1 to 100 g / m 3 and / or from water vapor from 10 ppm to 100%.
  • the metal halide surfaces can be reconditioned using a one- or two-stage procedure:
  • a perfectly passivated and dried surface of an austenitic material consists of a dense, very thin, homogeneous metal oxide layer that approx. 200 ° C is covered with a monomolecular water layer (Fig.1 / I).
  • this water layer is first removed.
  • the driving force behind this reaction is the tendency towards hydration of halide-containing corrosive media.
  • the original, pure oxide passive layer is converted into a mixture of metal halides and oxides (Fig.1 / II).
  • the resulting metal halide layer prevents further dissolution of the metal.
  • the metal halides are converted into the corresponding hydroxides.
  • the hydrogen halide formed is removed by hydrate formation (Fig. 1 / III).
  • a shiny metallic surface is formed.
  • Repassivation is carried out by flushing with a gas mixture which, in addition to an inert carrier gas, contains a gaseous oxidizing agent such as oxygen or ozone.
  • the hydroxides are largely converted into the more stable oxides of the respective metal (Fig. 2 / IV).
  • the metal halide surface of a passivatable material is reconditioned at a temperature between room temperature and 400 ° C. of a purge gas containing oxygen and water vapor (for example 20% O 2 ; 100 ppm H 2 O).
  • a purge gas containing oxygen and water vapor for example 20% O 2 ; 100 ppm H 2 O.
  • the metal halides are converted into the corresponding hydroxides, at the same time the hydrogen halide formed is removed by hydrate formation and the hydroxides are converted into oxides of the respective metal. Due to the simultaneous surface reaction, the two-step process described in embodiment 1 is advantageously replaced by a one-step process.
  • the purge gas contains a gaseous oxidizing agent, such as oxygen or ozone, which is also able to oxidize the metal halides directly.
  • a gaseous oxidizing agent such as oxygen or ozone

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Claims (6)

  1. Procédé de balayage de systèmes de transfert passivés pour des milieux de procédé, gazeux, corrosifs, qui activent la surface superficielle passivée des matières comme par exemple en austénite ou en austénite-ferrite,
    caractérisé en ce qu'
    on transforme de nouveau la surface superficielle activée à l'état passif en excluant les milieux de procédé pendant le balayage du système de transfert avec un gaz de balayage contenant de l'ozone, de l'oxygène et/ou de la vapeur d'eau.
  2. Procédé selon la revendication 1,
    caractérisé en ce que
    le gaz de balayage est de l'air.
  3. Procédé selon la revendication 1 ou 2,
    caractérisé en ce que la température du gaz de balayage est comprise entre la température ambiante et 400°C.
  4. Procédé selon la revendication 1, pour des surfaces superficielles contenant des halogénures métalliques,
    caractérisé par
    un procédé en deux étapes consistant tout d'abord à transformer l'halogénure métallique en un hydroxyde correspondant à l'aide d'un gaz de balayage contenant de l'humidité, puis on transforme l'hydroxyde à l'aide d'un gaz de balayage sec contenant de l'oxygène ou de l'ozone en une couche d'oxyde passivée, stable.
  5. Procédé selon l'une des revendications 1 à 4,
    caractérisé en ce que
    le milieu gazeux corrosif est formé d'un élément choisi dans le groupe HCl, Cl2, HF, HBr, NH3.
  6. Procédé selon l'une des revendications 1 à 5,
    caractérisé en ce que
    le gaz de rinçage contient entre 0,1 et 100 % en volume de O2, entre 0,1 et 100 g/m3 d'ozone O3 et/ou entre 10 ppm et 100 % de vapeur d'eau.
EP93116941A 1992-12-18 1993-10-20 Procédé pour le balayage et le reconditionnement de systèmes de transfert Expired - Lifetime EP0602347B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4242967A DE4242967A1 (de) 1992-12-18 1992-12-18 Verfahren zum Spülen und Rekonditionieren von Transfersystemen
DE4242967 1992-12-18

Publications (2)

Publication Number Publication Date
EP0602347A1 EP0602347A1 (fr) 1994-06-22
EP0602347B1 true EP0602347B1 (fr) 1997-05-14

Family

ID=6475770

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93116941A Expired - Lifetime EP0602347B1 (fr) 1992-12-18 1993-10-20 Procédé pour le balayage et le reconditionnement de systèmes de transfert

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EP (1) EP0602347B1 (fr)
AT (1) ATE153081T1 (fr)
DE (2) DE4242967A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6648988B2 (en) 2001-08-17 2003-11-18 Exxonmobil Research And Engineering Company Furnace run length extension by fouling control

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3145236C2 (de) * 1981-11-13 1984-11-22 M.A.N. Maschinenfabrik Augsburg-Nürnberg AG, 8000 München Verfahren zur Herstellung von verformungsbeständigen oxydischen Schutzschichten
US4519851A (en) * 1984-06-15 1985-05-28 International Business Machines Corporation Method for providing pinhole free dielectric layers
JPH02179867A (ja) * 1988-12-29 1990-07-12 Tadahiro Omi プロセスガス供給システム
IT1251524B (it) * 1991-03-18 1995-05-16 Vincenzo Lagana Metodo per la passivazione delle superfici metalliche interessate da condizioni e agenti promotori di corrosione
US5188714A (en) * 1991-05-03 1993-02-23 The Boc Group, Inc. Stainless steel surface passivation treatment

Also Published As

Publication number Publication date
DE59306445D1 (de) 1997-06-19
DE4242967A1 (de) 1994-06-23
ATE153081T1 (de) 1997-05-15
EP0602347A1 (fr) 1994-06-22

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