EP1630251B1 - Process for coating apparatus and parts of apparatus used to make chemical plants - Google Patents

Process for coating apparatus and parts of apparatus used to make chemical plants Download PDF

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EP1630251B1
EP1630251B1 EP04022161A EP04022161A EP1630251B1 EP 1630251 B1 EP1630251 B1 EP 1630251B1 EP 04022161 A EP04022161 A EP 04022161A EP 04022161 A EP04022161 A EP 04022161A EP 1630251 B1 EP1630251 B1 EP 1630251B1
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coated
coating
activator
layer
parts
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EP1630251A2 (en
EP1630251A3 (en
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Bernd Terstegen
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Priority to ES04022161T priority patent/ES2291792T3/en
Priority to EP04022161A priority patent/EP1630251B1/en
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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
    • 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
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/088—Iron or steel solutions containing organic acids

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  • the invention relates to a method for coating of apparatuses and apparatus parts for chemical plant construction consisting of metals, in particular stainless steels, in which the surfaces to be coated are pretreated and subsequently coated with at least one layer of a Ni-P alloy by electroless plating with the aid of a plating bath become.
  • Such a procedure is over DE-A 100 16 215 known.
  • On the surfaces to be protected first elevations are formed. This is done by adding inorganic particles of oxides, silicates, carbonates, carbides or nitrides to the plating bath or by structuring the surfaces by etching, embossing or blasting.
  • the coating is applied by chemical or autocatalytic deposition by filling the apparatus with metal electrolyte solution or by immersing pieces of equipment in dip baths containing the metal electrolyte solution.
  • a nickel-phosphorus alloy is preferably used. This may contain a halogenated polymer, especially for a coating consisting of two layers.
  • a metal layer is first deposited on the surfaces and then applied to this a metal-polymer dispersion layer.
  • the invention is based on a method for electroless chemical deposition of metal-polymer dispersion layers, which is known per se (US Pat. W. Riedel: Functional Vemickelung, Verlag Eugen Leize, Saulgau, 1989, pp. 231-236, ISBN 3-750480-044-x ).
  • the deposition of the metal layer or the metal-polymer dispersion phases serves to coat the apparatuses and apparatus parts of chemical plant construction known per se. Since the layers adhere well only on a clean surface, all materials must be subjected to a pre-treatment before electroplating.
  • chemical nickel systems which are phosphorus-containing nickel alloys having a phosphorus content of about 0.5 to about 15 wt .-%.
  • the layers are applied by chemical or autocatalytic deposition on the surfaces to be protected, the necessary electrons are not provided by an external power source, but are generated by chemical reaction in the electrolyte itself.
  • Such solutions are marketed, for example, by Riedel, Galvan- und Filtertechnik GmbH, Halle, Westphalia and Atotech GmbH, Berlin.
  • a layer of a Nl-P alloy containing particles of a halogenated polymer is applied to the pretreated surfaces of the apparatus or apparatus parts.
  • the optional polymer to be used is preferably fluorinated.
  • suitable fluorinated polymers are polytetrafluoroethylene, perfluoroalkoxy polymers (PFA, for example with C 1 -C 8 -alkoxy units), copolymers of tetrafluoroethylene and perfluoroalkylvinylether, for example perfluorovinylpryl ether.
  • Particularly preferred are polytetrafluoroethylene (PTFE) and perfluoroalkoxy polymers (PFA, according to DIN 7728, Part 1, Jan. 1988).
  • the polymer content of the coating is mainly influenced by the amount of polymer dispersion added and the choice of detergents.
  • the concentration of the polymer plays the major role here; high polymer concentrations of the immersion baths lead to a disproportionately high polymer content in the nickel-phosphorus-polymer dispersion layer.
  • the parts to be coated are immersed in immersion baths containing the nickel electrolyte solution.
  • Another embodiment of the method according to the invention consists in that the containers to be coated are filled with nickel electrolyte solution.
  • Another suitable method is to pump the electrolyte solution through the part to be coated. This variant is shown schematically in FIG. 1, which shows the coating of a heat exchanger.
  • the heat exchanger is designated by (1). It has connections (2) and (3) for the inlet and outlet of a heating medium.
  • the means necessary for the pretreatment and coating of the surfaces of the heat exchanger are contained in the reservoirs (4), (5), (6) and (7), wherein, for example, in (4) a mordant, in (5) a surfactant cleaner, in (6) the activator according to the invention and in (7) the nickel electrolyte solution can be stored.
  • These agents are successively conveyed by means of a pump (8) through the heat exchanger and returned via the return (9) back into the reservoir.
  • the activator is removed from the heat exchanger by means of nitrogen.
  • a connection (10) is provided for this purpose.
  • the annealing time is generally 5 minutes to 3 hours, preferably 35 to 60 minutes.
  • the treated surfaces of the invention allow good heat transfer, although the coatings have a significant thickness of 1 to 100 microns.
  • the polymer content of the dispersion coating is 5 to 30% by volume.
  • the surfaces also have excellent durability.
  • the nickel-polymer dispersion layer contains an additional polymer to further enhance the non-stick properties of the coating.
  • This polymer may be halogenated or non-halogenated. Particularly preferred is the use of polytetrafluoroethylene or ethylene polymers and ethylene copolymers.
  • This optionally used polymer is also added as a dispersion or slurry in an aqueous surfactant solution, the order of addition of the dispersions being not critical. It is important that the particles of the further, halogenated or non-halogenated polymer are coarser than those of the halogenated polymer. Thus, mean particle diameters of 5 to 50 microns have been found to be advantageous.
  • a further cover layer of a perfluoroalkoxy polymer (PFA) can be applied to this layer structure by dipping, spraying or electrostatic powder coating. Such a coating is shown in FIG. 2.
  • the method according to the invention can be applied to all surfaces of apparatuses and apparatus parts which are threatened by deposits for chemical plant construction, in particular apparatuses and apparatus parts made of metals, particularly preferably of stainless steels.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Chemically Coating (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Pretreatment Of Seeds And Plants (AREA)
  • Fertilizers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

Coating of stainless steel chemical unit equipment and parts where the surface to be coated is pretreated and coated with at least one layer of Ni-P alloy by current-free (sic) deposition from a galvanizing bath. The surface to be coated is pickled with an activator solution at 40-85 [deg] C containing HF or HF salt (10-300 ml), sulfuric acid 1-5 ml), sublimed Fe(III) chloride (1-2 g), Ni chloride (6-12 g), citric acid (10-20 ml) and water.

Description

Die Erfindung betrifft ein Verfahren zur Beschichtung von aus Metallen, insbesondere Edelstählen bestehenden Apparaten und Apparateteilen für den chemischen Anlagenbau, bei dem die zu beschichtenden Oberflächen vorbehandelt und anschließend mit wenigstens einer Schicht aus einer Ni-P-Legierung durch stromloses Abscheiden mit Hilfe eines Galvanisierbades überzogen werden.The invention relates to a method for coating of apparatuses and apparatus parts for chemical plant construction consisting of metals, in particular stainless steels, in which the surfaces to be coated are pretreated and subsequently coated with at least one layer of a Ni-P alloy by electroless plating with the aid of a plating bath become.

Ein solches Verfahren ist aus DE-A 100 16 215 bekannt. Auf den zu schützenden Oberflächen werden dabei zunächst Erhebungen ausgebildet. Dies erfolgt dadurch, dass dem Galvanisierbad anorganische Partikel aus Oxiden, Silikaten, Carbonaten, Carbiden oder Nitriden zugesetzt oder die Oberflächen durch Anätzen, Prägen oder Strahlen strukturiert werden. Die Beschichtung wird durch chemische oder autokatalytische Abscheidung aufgebracht, indem die Apparate mit Metall-Elektrolytlösung befüllt oder Apparateteile in Tauchbäder getaucht werden, die die Metall-Elektrolytlösung enthalten. Als Metall-Elektrolytlösung wird vorzugsweise eine Nickel-Phosphor-Legierung verwendet. Diese kann, insbesondere für eine aus zwei Schichten bestehenden Überzug ein halogeniertes Polymer enthalten. Zur Haftverbesserung wird dabei auf den Oberflächen zunächst eine Metall-Schicht abgeschieden und anschließend auf diese eine Metall-Polymer-Dispersionsschicht aufgebracht.Such a procedure is over DE-A 100 16 215 known. On the surfaces to be protected first elevations are formed. This is done by adding inorganic particles of oxides, silicates, carbonates, carbides or nitrides to the plating bath or by structuring the surfaces by etching, embossing or blasting. The coating is applied by chemical or autocatalytic deposition by filling the apparatus with metal electrolyte solution or by immersing pieces of equipment in dip baths containing the metal electrolyte solution. As the metal electrolytic solution, a nickel-phosphorus alloy is preferably used. This may contain a halogenated polymer, especially for a coating consisting of two layers. To improve adhesion, a metal layer is first deposited on the surfaces and then applied to this a metal-polymer dispersion layer.

Die Oberflächen derart beschichteter Apparate und Apparateteile zeichnen sich durch hohe mechanische Stabilität und Widerstandsfähigkeit gegen Korrosion aus. Es hat sich indes gezeigt, dass bei galvanischen Überzügen auf Apparaten und Apparateteilen aus Edelstählen, wie sie häufig im chemischen Anlagenbau eingesetzt werden, Haftungsprobleme auftreten, die dann zu einem Ablösen der Beschichtung führen können. Ursächlich hierfür ist die Entstehung von Oxyd- und Anlaufschichten vor der eigentlichen Beschichtung, die besonders bei atmosphärisch offenen Systemen praktisch nicht zu vermeiden ist.The surfaces of such coated apparatus and apparatus parts are characterized by high mechanical stability and resistance to corrosion. However, it has been shown that in galvanic coatings on apparatus and apparatus parts made of stainless steels, as they are often used in chemical plant construction, adhesion problems occur, which can then lead to a detachment of the coating. The reason for this is the formation of oxide and tarnish layers before the actual coating, which is practically unavoidable especially in atmospherically open systems.

Mit der Erfindung soll ein Verfahren zur Beschichtung von Apparaten und Apparateteilen aus Metallen, insbesondere Edelstählen, geschaffen werden, welches auch auf solchen Werkstoffen die Ausbildung eines stabilen und dauerhaften Oberflächenschutzes gewährleistet. Als Besonderheit ist zusätzlich gefordert, dass komplexe Innengeometrien von Apparaten aus Edelstählen mit einem korrosionsvermindernden Überzug versehen werden können.With the invention, a process for the coating of apparatus and apparatus parts of metals, especially stainless steels, to be created, which ensures the formation of a stable and durable surface protection on such materials. As a special feature, it is additionally required that complex internal geometries of stainless steel apparatus can be provided with a corrosion-reducing coating.

Zur Lösung dieser Aufgabe werden die Maßnahmen nach dem Kennzeichnen des Anspruchs 1 vorgeschlagen.To solve this problem, the measures are proposed according to the characterizing of claim 1.

Zweckmäßige Weiterbildungen des erfindungsgemäßen Verfahrens sind Gegenstand der Unteransprüche 2 bis 5.Advantageous developments of the method according to the invention are the subject of the dependent claims 2 to 5.

Der Erfindung liegt ein Verfahren zur stromlosen chemischen Abscheidung von Metall-Polymer-Dispersionsschichten zugrunde, das an sich bekannt ist ( W. Riedel: Funktionelle Vemickelung, Verlag Eugen Leize, Saulgau, 1989, S. 231 bis 236, ISBN 3-750480-044-x ). Die Abscheidung der Metallschicht oder der Metall-Polymer-Dispersionsphasen dient zur Beschichtung der an sich bekannten Apparate und Apparateteile des chemischen Anlagenbaus. Da die Schichten nur auf einer sauberen Oberfläche gut haften, müssen alle Werkstoffe vor dem Galvanisieren einer Vorbehandlung unterworfen werden.The invention is based on a method for electroless chemical deposition of metal-polymer dispersion layers, which is known per se (US Pat. W. Riedel: Functional Vemickelung, Verlag Eugen Leize, Saulgau, 1989, pp. 231-236, ISBN 3-750480-044-x ). The deposition of the metal layer or the metal-polymer dispersion phases serves to coat the apparatuses and apparatus parts of chemical plant construction known per se. Since the layers adhere well only on a clean surface, all materials must be subjected to a pre-treatment before electroplating.

Es wurde nun gefunden, dass für einen verbesserten Haftungserfolg die Vorbehandlung der Oberflächen von Apparaten und Apparateteilen aus Edelstählen mit Hilfe eines Aktivators aus einem Gemisch aus

  • 10 bis 300 ml Salz- oder Flusssäure,
  • 1 bis 5 ml Schwefelsäure,
  • 1 bis 2 gr Eisen(III)chrlorid (sublimiert),
  • 6 bis 12 gr Nickelchlorid,
  • 10 bis 20 ml Zitronensäure und
  • Wasser,
jeweils bezogen auf 1 Liter des Aktivators, besonders wirksam ist. Insbesondere wenn der Aktivator auf eine Temperatur von 40°C bis 85°C erwärmt ist, lassen sich die Edelstahloberflächen sehr rasch und gründlich dekapieren. Der Aktivator wird anschließend mittels eines inerten Mediums, vorzugsweise mittels Stickstoff oder einer Metall-Elektrolytlösung entfernt. Die zu schützenden Oberflächen können dann unmittelbar beschichtet werden.It has now been found that for an improved adhesion success, the pretreatment of the surfaces of apparatus and apparatus parts made of stainless steels with the aid of an activator of a mixture of
  • 10 to 300 ml of hydrochloric or hydrofluoric acid,
  • 1 to 5 ml of sulfuric acid,
  • 1 to 2 gr of iron (III) chrloride (sublimed),
  • 6 to 12 gr nickel chloride,
  • 10 to 20 ml of citric acid and
  • Water,
in each case based on 1 liter of the activator, is particularly effective. In particular, when the activator is heated to a temperature of 40 ° C to 85 ° C, the stainless steel surfaces can be very quickly and thoroughly decapitated. The activator is subsequently removed by means of an inert medium, preferably by means of nitrogen or a metal electrolyte solution. The surfaces to be protected can then be coated directly.

Für die Beschichtung werden sogenannte Chemisch-Nickel-Systeme verwendet, das sind phosphorhaltige Nickellegierungen mit einem Phosphorgehalt von etwa 0,5 bis etwa 15 Gew.-%. Die Schichten werden durch chemische oder autokatalytische Abscheidung auf die zu schützenden Oberflächen aufgebracht, wobei die dazu nötigen Elektronen nicht durch eine äußere Stromquelle zur Verfügung gestellt, sondern durch chemische Umsetzung im Elektrolyten selbst erzeugt werden.For the coating so-called chemical nickel systems are used, which are phosphorus-containing nickel alloys having a phosphorus content of about 0.5 to about 15 wt .-%. The layers are applied by chemical or autocatalytic deposition on the surfaces to be protected, the necessary electrons are not provided by an external power source, but are generated by chemical reaction in the electrolyte itself.

Es werden zweckmäßig handelsübliche Nickelelektrolytlösungen eingesetzt, die Ni2+, Natriumhypophosphit, Carbonsäuren und Fluorid und ggf. Abscheidungsmodertoren wie Pb2+ enthalten. Solche Lösungen werden zum Beispiel von der Riedel, Galvan- und Filtertechnik GmbH, Halle, Westfalen und der Atotech Deutschland GmbH, Berlin, vertrieben. Besonders bevorzugt sind Lösungen, die einen pH-Wert um 5 aufweisen und etwa 27 g/l NiSo4 ·6 H2O und etwa 21 g/l NaH2PO2 ·H2O bei einem PFA-Gehalt von 1 bis 25 g/l enthalten.Commercially available nickel electrolyte solutions are expediently used which contain Ni 2 +, sodium hypophosphite, carboxylic acids and fluoride and optionally deposition moderators such as Pb 2+ . Such solutions are marketed, for example, by Riedel, Galvan- und Filtertechnik GmbH, Halle, Westphalia and Atotech Deutschland GmbH, Berlin. Especially preferred are solutions having a pH of about 5 and about 27 g / l NiSO 4 · 6 H 2 O and about 21 g / l NaH 2 PO 2 · H 2 O in a PFA content of 1 to 25 g / l included.

Nach einem weiteren Merkmal der Erfindung wird auf die vorbehandelten Oberflächen der Apparate oder Apparateteile eine Schicht aus einer Nl-P-Legierung, die Partikel eines halogenierten Polymers enthält, aufgebracht.According to a further feature of the invention, a layer of a Nl-P alloy containing particles of a halogenated polymer is applied to the pretreated surfaces of the apparatus or apparatus parts.

Das optional zu verwendende Polymer ist bevorzugt fluoriert. Beispiele für geeignete fluorierte Polymere sind Polytetrafluorethylen, Perfluor-Alkoxy-Polymere (PFA, z.B. mit C1-C8-Alkoxyeinheiten), Copolymerisate von Tetrafluorethylen und Perfluoralkylvinylether z.B. Perfluorvinylprpylether. Besonders bevorzugt sind Polytetrafluorethylen (PTFE) und Perfluor-Alkoxy-Polymere (PFA, nach DIN 7728, Teil 1, Jan. 1988).The optional polymer to be used is preferably fluorinated. Examples of suitable fluorinated polymers are polytetrafluoroethylene, perfluoroalkoxy polymers (PFA, for example with C 1 -C 8 -alkoxy units), copolymers of tetrafluoroethylene and perfluoroalkylvinylether, for example perfluorovinylpryl ether. Particularly preferred are polytetrafluoroethylene (PTFE) and perfluoroalkoxy polymers (PFA, according to DIN 7728, Part 1, Jan. 1988).

Der Polymeranteil der Beschichtung wird hauptsächlich durch die Menge der zugesetzten Polymerdispersion und die Wahl der Detergentien beeinflusst. Dabei spielt die Konzentration des Polymers die größere Rolle; hohe Polymerkonzentrationen der Tauchbäder führen zu einem überproportional hohen Polymeranteil in der Nickel-Phosphor-Polymer-Dispersionsschicht.The polymer content of the coating is mainly influenced by the amount of polymer dispersion added and the choice of detergents. The concentration of the polymer plays the major role here; high polymer concentrations of the immersion baths lead to a disproportionately high polymer content in the nickel-phosphorus-polymer dispersion layer.

Zur Kontaktierung werden die zu beschichtenden Teile in Tauchbäder getaucht, die die Nickel-Elektrolytlösung enthalten. Eine andere Ausführungsform des erfindungsgemäßen Verfahren besteht darin, dass die zu beschichtenden Behälter mit Nickel-Elektrolytlösung befüllt werden. Ein weiteres geeignetes Verfahren besteht darin, die Elektrolyt-Lösung durch das zu beschichtende Teil zu pumpen. Diese Variante ist in der Figur 1, die das Beschichten eines Wärmetauschers zeigt, schematisch dargestellt.For contacting, the parts to be coated are immersed in immersion baths containing the nickel electrolyte solution. Another embodiment of the method according to the invention consists in that the containers to be coated are filled with nickel electrolyte solution. Another suitable method is to pump the electrolyte solution through the part to be coated. This variant is shown schematically in FIG. 1, which shows the coating of a heat exchanger.

Der Wärmetauscher ist mit (1) bezeichnet. Er besitzt Anschlüsse (2) und (3) für den Zu- und Ablauf eines Heizmediums. Die für die Vorbehandlung und Beschichtung der Oberflächen des Wärmetauschers erforderlichen Mittel sind in den Vorratsbehältern (4), (5), (6) und (7) enthalten, wobei beispielsweise in (4) ein Beizmittel, in (5) ein Tensidreiniger, in (6) der erfindungsgemäße Aktivator und in (7) die Nickel-Elektrolytlösung bevorratet sein kann. Diese Mittel werden nacheinander mit Hilfe einer Pumpe (8) durch den Wärmetauscher gefördert und über den Rücklauf (9) wieder in die Vorratsbehälter zurückgeführt. Nach Abschluss der Vorbehandlung wird der Aktivator mittels Stickstoff aus dem Wärmetauscher entfernt. Hierzu ist ein Anschluss (10) vorgesehen.The heat exchanger is designated by (1). It has connections (2) and (3) for the inlet and outlet of a heating medium. The means necessary for the pretreatment and coating of the surfaces of the heat exchanger are contained in the reservoirs (4), (5), (6) and (7), wherein, for example, in (4) a mordant, in (5) a surfactant cleaner, in (6) the activator according to the invention and in (7) the nickel electrolyte solution can be stored. These agents are successively conveyed by means of a pump (8) through the heat exchanger and returned via the return (9) back into the reservoir. After completion of the pretreatment, the activator is removed from the heat exchanger by means of nitrogen. For this purpose, a connection (10) is provided.

Vorzugsweise tempert man im Anschluss an den Beschichtungsvorgang bei Temperaturen von 200 bis 400°C, vor allem bei 315 bis 380°C. Die Temperungsdauer beträgt im allgemeinen 5 Minuten bis 3 Stunden, bevorzugt 35 bis 60 Minuten.Preference is given to tempering at temperatures of 200 to 400 ° C, especially at 315 to 380 ° C following the coating process. The annealing time is generally 5 minutes to 3 hours, preferably 35 to 60 minutes.

Es wurde gefunden, dass die erfindungsgemäße behandelten Oberflächen einen guten Wärmedurchgang ermöglichen, obwohl die Beschichtungen eine nicht unerhebliche Dicke von 1 bis 100 µm. Der Polymeranteil der Dispersionsbeschichtung beträgt 5 bis 30 Vol.-%. Die Oberflächen weisen ferner eine exzellente Haltbarkeit auf.It has been found that the treated surfaces of the invention allow good heat transfer, although the coatings have a significant thickness of 1 to 100 microns. The polymer content of the dispersion coating is 5 to 30% by volume. The surfaces also have excellent durability.

In einer weiteren Ausführungsform enthält die Nickel-Polymer-Dispersionsschicht ein zusätzliches Polymer, um die antihaftenden Eigenschaften der Beschichtung weiter zu verstärken. Dieses Polymer kann halogeniert oder nicht-halogeniert sein. Besonders bevorzugt ist die Verwendung von Polytetrafluorethylen oder Ethylenpolymerisaten und Ethylencopolymerisaten. Dieses optional verwendete Polymer gibt man ebenfalls als Dispersion oder Aufschlämmung in einer wässrigen Tensidlösung zu, wobei die Reihenfolge der Zugabe der Dispersionen unkritisch ist. Wichtig ist, dass die Partikel des weiteren, halogenierten oder nicht-halogenierten Polymers gröber sind als die des halogenierten Polymers. So haben sich mittlere Partikeldurchmesser von 5 bis 50 µm als vorteilhaft herausgestellt. Schließlich kann auf diesen Schichtaufbau eine weitere Deckschicht aus einem Perfluor-Alkoxy -Polymeren (PFA) durch Tauchen, Spritzen oder elektrostatisches Pulverbeschichten aufgebracht werden. Eine solche Beschichtung zeigt Figur 2.In another embodiment, the nickel-polymer dispersion layer contains an additional polymer to further enhance the non-stick properties of the coating. This polymer may be halogenated or non-halogenated. Particularly preferred is the use of polytetrafluoroethylene or ethylene polymers and ethylene copolymers. This optionally used polymer is also added as a dispersion or slurry in an aqueous surfactant solution, the order of addition of the dispersions being not critical. It is important that the particles of the further, halogenated or non-halogenated polymer are coarser than those of the halogenated polymer. Thus, mean particle diameters of 5 to 50 microns have been found to be advantageous. Finally, a further cover layer of a perfluoroalkoxy polymer (PFA) can be applied to this layer structure by dipping, spraying or electrostatic powder coating. Such a coating is shown in FIG. 2.

Das erfindungsgemäße Verfahren lässt sich aufgrund seiner einfachen Handhabung an allen von Ablagerungen bedrohten Oberflächen von Apparaten und Apparateteilen für den chemischen Anlagenbau, insbesondere Apparaten und Apparateteilen aus Metallen, besonders bevorzugt aus Edelstählen anwenden.Due to its simple handling, the method according to the invention can be applied to all surfaces of apparatuses and apparatus parts which are threatened by deposits for chemical plant construction, in particular apparatuses and apparatus parts made of metals, particularly preferably of stainless steels.

Claims (5)

  1. A process for coating of chemical apparatuses and apparatus parts for chemical plant construction, made of steel, particularly stainless steel, where the surfaces to be coated are pre-treated and subsequently coated with at least one layer of Ni-P alloy by electroless deposition from a galvanizing bath, wherein the surfaces are pickled with the help of an activator, which is heated to 40 °C to 85 °C and which is composed of a mixture of (related to 1 litre of activator substance)
    10 to 300 ml salt or hydrofluoric acid,
    1 to 5 ml sulphuric acid,
    1 to 2 gr iron (III) chloride (sublimated),
    6 to 12 gr nickel chloride,
    10 to 20 ml citric acid and water,
    and wherein the activator is removed by means of an inert medium and the surfaces are then directly coated.
  2. A process as claimed in claim 1, wherein the activator is removed by means of nitrogen or a metal electrolytic solution.
  3. A process as claimed in claim 1, wherein the pre-treated surfaces are coated with a layer of Ni-P alloy, which contains particles of a halogenated polymer.
  4. A process as claimed in claim 3, wherein a further layer of perfluor-alkoxy-polymers (PFA) is applied.
  5. A process as claimed in claim 3, wherein a top layer is produced by dipping, spraying or electrostatic powder coating.
EP04022161A 2004-09-17 2004-09-17 Process for coating apparatus and parts of apparatus used to make chemical plants Active EP1630251B1 (en)

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Application Number Priority Date Filing Date Title
AT04022161T ATE368137T1 (en) 2004-09-17 2004-09-17 METHOD FOR COATING APPARATUS AND APPARATUS PARTS FOR CHEMICAL PLANT ENGINEERING
DE502004004444T DE502004004444D1 (en) 2004-09-17 2004-09-17 Process for coating apparatus and apparatus parts for chemical plant construction
ES04022161T ES2291792T3 (en) 2004-09-17 2004-09-17 PROCEDURE FOR THE COVERING OF APPLIANCES AND APPLIANCE PARTS FOR THE CONSTRUCTION OF CHEMICAL PLANTS.
EP04022161A EP1630251B1 (en) 2004-09-17 2004-09-17 Process for coating apparatus and parts of apparatus used to make chemical plants

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EP1630251A2 EP1630251A2 (en) 2006-03-01
EP1630251A3 EP1630251A3 (en) 2006-03-08
EP1630251B1 true EP1630251B1 (en) 2007-07-25

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DE102008014272A1 (en) * 2008-03-04 2009-09-10 Deutsches Zentrum für Luft- und Raumfahrt e.V. Coating for a heat transfer element of a heat transfer device at a side that is turned to a media space with vapor-liquid-phase change, comprises a matrix made of a metallic material, and hydrophobic polymer islands arranged at the matrix
DE102008020037A1 (en) 2008-04-21 2009-10-29 Snt Schauenburg Nanotec Gmbh Coating method comprises treating surface with activator, followed by electroless plating with nickel-phosphorus alloy, activator containing hydrochloric acid, nickel chloride, acetic acid, citric acid, lactic acid, succinic acid and water

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102234810A (en) * 2010-04-20 2011-11-09 深圳富泰宏精密工业有限公司 Cleaning agent for etched stainless steel and using method thereof
DE202014102805U1 (en) 2014-06-18 2014-07-17 CSB Chemische Spezialbeschichtungen GmbH Pickling solution for pickling metals
DE102014108588B3 (en) * 2014-06-18 2015-09-03 CSB Chemische Spezialbeschichtungen GmbH Pickling solution and process for pickling metals
DE102014113543A1 (en) * 2014-09-19 2016-03-24 Endress + Hauser Gmbh + Co. Kg Media-resistant multi-layer coating for a measuring device for process technology

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3029158A (en) * 1960-12-06 1962-04-10 Gen Am Transport Processes of chemical nickel plating of amphoteric and like materials
JPS61246373A (en) * 1985-04-23 1986-11-01 Yamato Denki Kogyo Kk Pretreating agent and pretreatment of free-cutting steel prior to electroless plating
DE19860526A1 (en) * 1998-12-30 2000-07-06 Basf Ag Heat exchangers with reduced tendency to form deposits and processes for their production
DE10016215A1 (en) * 2000-03-31 2001-10-04 Basf Ag Process for coating apparatus and apparatus parts for chemical plant construction

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102008014272A1 (en) * 2008-03-04 2009-09-10 Deutsches Zentrum für Luft- und Raumfahrt e.V. Coating for a heat transfer element of a heat transfer device at a side that is turned to a media space with vapor-liquid-phase change, comprises a matrix made of a metallic material, and hydrophobic polymer islands arranged at the matrix
DE102008020037A1 (en) 2008-04-21 2009-10-29 Snt Schauenburg Nanotec Gmbh Coating method comprises treating surface with activator, followed by electroless plating with nickel-phosphorus alloy, activator containing hydrochloric acid, nickel chloride, acetic acid, citric acid, lactic acid, succinic acid and water

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DE502004004444D1 (en) 2007-09-06
ES2291792T3 (en) 2008-03-01

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