DE19533410B4 - Method for producing a protective layer on the inner surface of a copper pipe and use of drawing agents - Google Patents

Method for producing a protective layer on the inner surface of a copper pipe and use of drawing agents Download PDF

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Publication number
DE19533410B4
DE19533410B4 DE1995133410 DE19533410A DE19533410B4 DE 19533410 B4 DE19533410 B4 DE 19533410B4 DE 1995133410 DE1995133410 DE 1995133410 DE 19533410 A DE19533410 A DE 19533410A DE 19533410 B4 DE19533410 B4 DE 19533410B4
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Prior art keywords
copper pipe
organic
inorganic
water
protective layer
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Expired - Fee Related
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DE1995133410
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German (de)
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DE19533410A1 (en
Inventor
Ulrich Dr.-Ing. Reiter
Werner Dr.rer.nat. Harnischmacher
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KME Special Products GmbH and Co KG
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KM Europa Metal AG
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Priority to DE1995133410 priority Critical patent/DE19533410B4/en
Publication of DE19533410A1 publication Critical patent/DE19533410A1/en
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Publication of DE19533410B4 publication Critical patent/DE19533410B4/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B21C1/16—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes
    • B21C1/22—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B21C9/02—Selection of compositions therefor
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

Verfahren zur Erzeugung einer die Kupferlöslichkeit in Wasser begrenzenden Schutzschicht an der inneren Oberfläche eines Kupferrohrs, dadurch gekennzeichnet, dass beim Ziehen eines Kupferrohres ein mit CO2 und O2 bildenden Stoffen modifiziertes synthetisches auf Gruppen der Fettester oder Polyglykole basierendes Ziehmittel eingesetzt wird, dem organische oder anorganische halogenhaltige Verbindungen mit einem Anteil unter 5 Gewichtsprozent zugegeben werden.A process for producing a copper solubility in water delimiting protective layer on the inner surface of a copper pipe, characterized in that when pulling a copper pipe, a modified with CO 2 and O 2 forming substances synthetic based on groups of fatty esters or polyglycols is used, the organic or inorganic halogen-containing compounds are added in a proportion of less than 5 percent by weight.

Description

Die Erfindung betrifft ein Verfahren zur Erzeugung einer die Kupferlöslichkeit in Wasser begrenzenden Schutzschicht an der inneren Oberfläche eines Kupferrohrs sowie eine Verwendung von Ziehmitteln gemäß der Oberbegriffe der Ansprüche 1 beziehungsweise 4 und 5.The The invention relates to a process for producing a copper solubility in water-limiting protective layer on the inner surface of a Copper pipe and a use of drawing agents according to the preamble the claims 1 or 4 and 5.

Im Umfang der EP 0 647 723 A1 ist es bekannt, beim Nahtlosziehen von Installationsrohren aus Kupfer auf den Innenseiten der Kupferrohre dadurch eine dünne haftende Oxidschicht herzustellen, daß nach dem Vorziehen die Innenoberflächen der Kupferrohre aufgerauht, anschließend die aufgerauhten Zwischenrohre bei einer Temperatur von 350°C bis 650°C sowie bei in das Rohrinnere eingeleitetem, Sauerstoff enthaltenden Schutzgas geglüht werden und daß danach die Zwischenrohre einem halbharten/harten Härtezug unterworfen werden, an den sich eine thermische Behandlung mit einer Temperatur von 175°C bis 275°C unter Einleitung eines sauerstoffhaltigen Gasgemisches in das Rohrinnere anschließt.In the scope of EP 0 647 723 A1 It is known in the seamless drawing of installation pipes made of copper on the inner sides of the copper pipes thereby produce a thin adhesive oxide layer that roughened by preference, the inner surfaces of the copper pipes, then the roughened intermediate tubes at a temperature of 350 ° C to 650 ° C and at the tube interior initiated, oxygen-containing inert gas are annealed and that thereafter the intermediate tubes are subjected to a semi-hard / hard hardness train, followed by a thermal treatment at a temperature of 175 ° C to 275 ° C followed by introducing an oxygen-containing gas mixture into the tube interior.

Es wurde im bekannten Fall in mehrmonatigen Untersuchungsreihen festgestellt, daß die innerhalb von 24 Stunden an Trinkwasser abgegebene Kupfermenge bei einem pH-Wert des Trinkwassers von 7,6 etwa bei 1 mg/l lag. Mit diesen Meßwerten werden die Vorschriften der Europäischen Trinkwasserrichtlinie einwandfrei erfüllt.It was found in the known case in several-month series of tests, that the within 24 hours delivered to drinking water at copper a pH of drinking water of 7.6 was about 1 mg / l. With these measurements become the regulations of the European Drinking Water Directive perfectly fulfilled.

Der Erfindung liegt ausgehend vom Stand der Technik die Aufgabe zugrunde, ein Verfahren zur Erzeugung einer die Kupfer löslichkeit in Wasser begrenzenden Schutzschicht an der inneren Oberfläche eines Kupferrohrs und die Verwendung eines Zielmittels bei dem Verfahren aufzuzeigen, das im Vergleich zu dem bekannten Verfahren mit einfacheren Maßnahmen bei geringerem Aufwand den Aufbau einer derartigen Schutzschicht erheblich beschleunigt.Of the Invention is based on the prior art, the task, a method for producing a copper solubility in water limiting Protective layer on the inner surface of a copper pipe and the Use of a targeting agent in the process, which compared to the known method with simpler measures with less effort, the structure of such a protective layer considerably accelerated.

Die Lösung dieser Aufgabe besteht nach der Erfindung in den im Anspruch 1 sowie den Ansprüchen 4 und 5 aufgeführten Merkmalen.The solution This object is according to the invention in the claim 1 and to the claims 4 and 5 listed Features.

Danach wird jetzt beim Ziehen eines Kupferrohrs ein Ziehmittel eingesetzt, welches von seinen Charakteristika her so zusammengesetzt ist, daß es bereits während des Ziehvorgangs den Aufbau einer Schutzschicht, sei es nun Malachit (CuCO3Cu[OH]2) oder Atacamit (CuCl23Cu[OH]2), ermöglicht. Hierzu wird das eingesetzte Ziehmittel bewußt mit CO2 bzw. CO2 und O2 bildenden Stoffen modifiziert. Zu diesen Stoffen zählen beispielsweise Peroxide, wie Natriumperoxid, Bariumperoxid oder Kaliumperoxid. Daneben werden in geringen Mengen, das heißt in einer Größenordnung unter 5 Gew.%, halogenorganische oder auch andere chlor-/halogenhaltige Verbindungen zugesetzt. Hierbei handelt es sich insbesondere um Trichlorethylen. Der pH-Wert des Ziehmittels wird entsprechend der jeweils zu erzeugenden Schicht eingestellt, das heißt, ob man nun eine Malachit- oder eine Atacamitschicht erzeugen will. Die Ziehmittelrezeptur ist so modifiziert, daß grundsätzlich auf größere Mineralölanteile verzichtet wird, um Rückstände zu vermeiden, die zu Restkohlenstoffgehalten > 0,2 mg/dm2 führen.Thereafter, a drawing agent is now used in drawing a copper pipe, which is composed of its characteristics forth so that it already during the drawing process, the construction of a protective layer, whether malachite (CuCO 3 Cu [OH] 2 ) or atacamite (CuCl 2 3Cu [OH] 2 ). For this purpose, the drawing agent used is deliberately modified with CO 2 or CO 2 and O 2- forming substances. These substances include, for example, peroxides, such as sodium peroxide, barium peroxide or potassium peroxide. In addition, in small amounts, that is in the order of less than 5 wt.%, Are added halogen-organic or other chlorine / halogen compounds. These are in particular trichlorethylene. The pH of the drawing agent is adjusted according to the particular layer to be produced, that is, whether you want to create a malachite or an atacamite layer. The drawing agent formulation is modified in such a way that generally larger mineral oil components are dispensed with in order to avoid residues which lead to residual carbon contents> 0.2 mg / dm 2 .

Der große Vorteil der Erfindung liegt darin, daß nunmehr Schutzschichten auf einfachem Wege in extrem kurzer Zeit erzeugt werden können, die Kupferrohre auch für den Einsatz bei sauren Wässern und anderen Medien geeignet machen, wo Kupfer sonst nur eingeschränkt oder überhaupt nicht eingesetzt werden kann. Die Schutzschichten begrenzen die Cu-Löslichkeit auf ein sehr niedriges vollkommen unbedenkliches Niveau von ca. 1 mg/l nach zwölf Stunden Stagnation.Of the size Advantage of the invention is that now protective layers easy way can be generated in an extremely short time, the Copper pipes also for the use in acidic waters and other media suitable, where copper otherwise limited or at all can not be used. The protective layers limit the Cu-solubility to a very low, completely harmless level of approx. 1 mg / l after twelve Hours of stagnation.

Je nach den Erfordernissen kann es entsprechend den Merkmalen des Anspruchs 2 vorteilhaft sein, daß das fertig gezogene Kupferrohr unter hinsichtlich der Luftfeuchtigkeit sowie der Temperatur definierten Randbedingungen eine bestimmte Zeit gelagert wird, um die erforderlichen Reaktionen ablaufen zu lassen.ever according to the requirements it may according to the features of the claim 2 be advantageous that the finished copper pipe under in terms of humidity as well as the temperature defined boundary conditions a certain Time is stored to drain the required reactions to let.

Insbesondere werden diese Randbedingungen gemäß Anspruch 3 dadurch definiert, daß das fertig gezogene Kupferrohr bei einer Luftfeuchtigkeit > 70 % und einer Temperatur > 25°C < 60°C über 6 bis 120 Stunden gelagert wird.Especially These boundary conditions according to claim 3 defined by the fact that finished copper pipe with an air humidity> 70% and a temperature> 25 ° C <60 ° C over 6 to Stored for 120 hours.

Ein Ziehmittel zum Einsatz bei dem Verfahren zur Erzeugung einer die Kupferlöslichkeit in Wasser begrenzenden Schutzschicht an der inneren Oberfläche eines Kupferrohrs kennzeichnet sich bei der Ausführungsform gemäß Anspruch 4 durch folgende Zusammensetzung in Gewichtsprozenten: Fettester bestimmter Länge 40-95% Emulgatoren 3-15% Korrosionsinhibitoren 2-30% halogenhaltige Lösemittel 1-15% Wasser 0-10% Tenside 0-5% CO2 bis zur Sättigung alternativ anorganische Halogenverbindungen oder anorganische Carbonate O2 bis zur Sättigung alternativ organische oder anorganische Peroxide A pulling agent for use in the process of forming a copper solubility in water-limiting protective layer on the inner surface of a copper pipe is featured in the embodiment Form according to claim 4 by the following composition in weight percent: Fat ester of certain length 40-95% emulsifiers 3-15% corrosion inhibitors 2-30% halogen-containing solvents 1-15% water 0-10% surfactants 0-5% CO 2 to saturation alternatively inorganic halogen compounds or inorganic carbonates O 2 to saturation alternatively organic or inorganic peroxides

Ein Ziehmittel zum Einsatz bei dem vorstehend beschriebenen Verfahren kennzeichnet sich gemäß einer weiteren Ausführungsform durch folgende Zusammensetzung in Gewichtsprozenten: Polyglykole 40-95% Emulgatoren 0-8% Korrosionsinhibitoren 5-30% halogenhaltige Lösemittel 1-15% Wasser 0-30% Tenside 0-5% CO2 bis zur Sättigung alternativ anorganische Halogenverbindungen oder anorganische Carbonate O2 bis zur Sättigung alternativ organische oder anorganische Peroxide A drawing agent for use in the method described above is characterized according to a further embodiment by the following composition in weight percent: polyglycols 40-95% emulsifiers 0-8% corrosion inhibitors 5-30% halogen-containing solvents 1-15% water 0-30% surfactants 0-5% CO 2 to saturation alternatively inorganic halogen compounds or inorganic carbonates O 2 to saturation alternatively organic or inorganic peroxides

Claims (5)

Verfahren zur Erzeugung einer die Kupferlöslichkeit in Wasser begrenzenden Schutzschicht an der inneren Oberfläche eines Kupferrohrs, dadurch gekennzeichnet, dass beim Ziehen eines Kupferrohres ein mit CO2 und O2 bildenden Stoffen modifiziertes synthetisches auf Gruppen der Fettester oder Polyglykole basierendes Ziehmittel eingesetzt wird, dem organische oder anorganische halogenhaltige Verbindungen mit einem Anteil unter 5 Gewichtsprozent zugegeben werden.A process for producing a copper solubility in water delimiting protective layer on the inner surface of a copper pipe, characterized in that when pulling a copper pipe, a modified with CO 2 and O 2 forming substances synthetic based on groups of fatty esters or polyglycols is used, the organic or inorganic halogen-containing compounds are added in a proportion of less than 5 percent by weight. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das fertig gezogene Kupferrohr unter hinsichtlich der Luftfeuchtigkeit sowie der Raumtemperatur definierten Randbedingungen eine bestimmte Zeit gelagert wird.Method according to claim 1, characterized in that that the finished copper pipe is under in terms of humidity as well as the room temperature defined boundary conditions a certain Time is stored. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das fertig gezogene Kupferrohr bei einer Luftfeuchtigkeit > 70 % und einer Temperatur > 25°C < 60°C über sechs bis einhundertzwanzig Stunden gelagert wird.Method according to claim 1 or 2, characterized that the finished copper pipe at an air humidity> 70% and a temperature> 25 ° C <60 ° C over six stored for one hundred and twenty hours. Verwendung eines Ziehmittels zum Einsatz bei einem Verfahren nach einem der Ansprüche 1 bis 3, gekennzeichnet durch folgende Zusammensetzung in Gewichtsprozenten: Fettester bestimmter Länge 40-95% Emulgatoren 3-15% Korrosionsinhibitoren 2-30% organische halogenhaltige Lösemittel 1-15% Wasser 0-10% Tenside 0-5% CO2 bis zur Sättigung alternativ anorganische Halogenverbindungen oder anorganische Carbonate O2 bis zur Sättigung alternativ organische oder anorganische Peroxide
Use of a drawing agent for use in a method according to one of claims 1 to 3, characterized by the following composition in weight percent: Fat ester of certain length 40-95% emulsifiers 3-15% corrosion inhibitors 2-30% organic halogenated solvents 1-15% water 0-10% surfactants 0-5% CO 2 to saturation alternatively inorganic halogen compounds or inorganic carbonates O 2 to saturation alternatively organic or inorganic peroxides
Verwendung eines Ziehmittels zum Einsatz bei einem Verfahren nach einem der Ansprüche 1 bis 3, gekennzeichnet durch folgende Zusammensetzung in Gewichtsprozenten: Polyglykole 40-95% Emulgatoren 0-8% Korrosionsinhibitoren 5-30% organische halogenhaltige Lösungsmittel 1-15% Wasser 0-30% Tenside 0-5% CO2 bis zur Sättiung alternativ anorganische Halogenverbindungen oder Carbonate O2 bis zur Sättigung alternativ organische oder anorganische Peroxide
Use of a drawing agent for use in a method according to one of claims 1 to 3, characterized by the following composition in weight percent: polyglycols 40-95% emulsifiers 0-8% corrosion inhibitors 5-30% organic halogenated solvents 1-15% water 0-30% surfactants 0-5% CO 2 to saturation alternatively inorganic halogen compounds or carbonates O 2 to saturation alternatively organic or inorganic peroxides
DE1995133410 1995-09-09 1995-09-09 Method for producing a protective layer on the inner surface of a copper pipe and use of drawing agents Expired - Fee Related DE19533410B4 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007055446A1 (en) * 2007-11-12 2009-05-14 Hansgrohe Ag Provision of water-bearing components from brass alloys with reduced metal ion release

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19819925A1 (en) * 1998-05-05 1999-11-11 Km Europa Metal Ag Process for creating a protective layer on the inner surface of a copper pipe
CN111036882A (en) * 2019-12-17 2020-04-21 江西云泰铜业有限公司 Method for processing special-shaped copper bar

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3932865C2 (en) * 1989-10-02 1991-08-14 Okan Dr. Maastricht Nl Akin
EP0647723A1 (en) * 1993-10-09 1995-04-12 KM Europa Metal Aktiengesellschaft Process for manufacturing of seamless drawn medium hard/hard copper fitting tubes
EP0493280B1 (en) * 1990-12-26 1995-12-06 Trefimetaux Copper tube with improved corrosion resistance and process for manufacturing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3932865C2 (en) * 1989-10-02 1991-08-14 Okan Dr. Maastricht Nl Akin
DE4110584C2 (en) * 1989-10-02 1994-06-16 Akin Okan Process for the production of a metal pipe protected against corrosion
EP0493280B1 (en) * 1990-12-26 1995-12-06 Trefimetaux Copper tube with improved corrosion resistance and process for manufacturing the same
EP0647723A1 (en) * 1993-10-09 1995-04-12 KM Europa Metal Aktiengesellschaft Process for manufacturing of seamless drawn medium hard/hard copper fitting tubes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007055446A1 (en) * 2007-11-12 2009-05-14 Hansgrohe Ag Provision of water-bearing components from brass alloys with reduced metal ion release

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