WO2000008235A1 - Use of di-tert-butylsulphide (tbds) and/or tert-butylmercaptan (tbm) as corrosion inhibitors in microbial corrosion of metals - Google Patents

Use of di-tert-butylsulphide (tbds) and/or tert-butylmercaptan (tbm) as corrosion inhibitors in microbial corrosion of metals Download PDF

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Publication number
WO2000008235A1
WO2000008235A1 PCT/EP1999/005644 EP9905644W WO0008235A1 WO 2000008235 A1 WO2000008235 A1 WO 2000008235A1 EP 9905644 W EP9905644 W EP 9905644W WO 0008235 A1 WO0008235 A1 WO 0008235A1
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tert
tbds
tbm
corrosion
metals
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PCT/EP1999/005644
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German (de)
French (fr)
Inventor
José ROJAS-CHAPANA
Helmut Tributsch
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Hahn-Meitner-Institut Berlin Gmbh
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Priority to AU55101/99A priority Critical patent/AU5510199A/en
Publication of WO2000008235A1 publication Critical patent/WO2000008235A1/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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/16—Sulfur-containing compounds
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/16—Sulfur-containing compounds
    • C23F11/161—Mercaptans

Definitions

  • TBDS di-tert-butyl sulfide
  • TBM tert-butyl mercaptan
  • the invention relates to the use of di-tert-butyl sulfide (TBDS) and / or tert-butyl mercaptan (TBM) for inhibiting the microbial corrosion of metals and their alloys, in particular steel.
  • TBDS di-tert-butyl sulfide
  • TBM tert-butyl mercaptan
  • the object of the invention can be achieved by using di-tert-butyl disulfide (TBDS), tert-butyl mercaptan (TBM) or a mixture of both compounds.
  • TBDS and TBM have proven to be inhibitors of microbial corrosion in that they prevent the attack of the microorganisms of the genus Thiobacillus on the sulfide layers.
  • FeS 2 pyrite layers
  • TBM is the actual active ingredient which prevents bacterial corrosion by forming disulfide bonds with the metal sulfides.
  • the compounds according to the invention are preferably applied as a protective film to the metal surface to be protected. This can be done, for example Painting the compounds dissolved in water and / or an organic solvent. In the event that TBDS is applied as a layer, this must be activated so that TBDS is split into TBM.
  • the cover layer is activated by UV treatment, heating, microwave treatment or plasma treatment.
  • a solution of TBDS and TBM is used, e.g. an aqueous alcoholic solution.
  • the TBDS is split into the TBM in this solution by adding alkali lye.
  • the solution must be applied to the metal surface relatively quickly, so that not too much TBM is converted back into TBDS by air oxidation.
  • This variant is quite suitable for the treatment of small metal surfaces, for the treatment of larger surfaces it is recommended to use TBDS due to the better handling.
  • the compounds according to the invention are suitable for inhibiting corrosion for all metals or alloys on which sulfide layers can be formed, such as iron, copper, zinc, lead, nickel, cobalt or molbdenum.
  • sulfide layers such as iron, copper, zinc, lead, nickel, cobalt or molbdenum.
  • the use of the corrosion inhibitors according to the invention on steel has proven to be extremely effective.
  • Organometallic chemical vapor deposition is a process for the preparation of thin polycrystals and epitaxial layers. The layers are deposited from the gas phase. Organometallic compounds mostly serve as starting materials (precursors). The separation process is as follows: A carrier gas is passed through so-called bubblers. The organometallic compounds are in liquid or solid form in the bubbler. The raw materials are thereby taken up in the carrier gas. The carrier gas transports the starting compounds past a heated substrate. The starting compounds contain the elements with which the layer is to be formed. In a reaction, the compounds decompose above the substrate surface. This releases the elements that contribute to layer formation. These accumulate on the substrate surface and thus form the layer. The excess decay products are fed into the exhaust air with the carrier gas.
  • a carrier gas is passed through so-called bubblers.
  • the organometallic compounds are in liquid or solid form in the bubbler.
  • the raw materials are thereby taken up in the carrier gas.
  • the carrier gas transports the starting compounds past a heated substrate.
  • the pyrite layers were prepared with the MOCVD system as described in "Solar Energy Materials and Solar Cells" 1993, 29, 289-370.
  • A) elemental sulfur and b) TBDS were used as the suitable sulfur precursor.
  • Iron pentacarbonyl [Fe (CO) 5 ] was used as the iron precursor for the preparation of pyrite.
  • Example la The pyrite layers produced in Example la) using elemental sulfur as a precursor were treated with a thin film of TBM in an isolation chamber.
  • the layer was rinsed with plenty of water to remove the excess TBM.
  • the layer was flotated and cultivated as in Example 2 with Tuovine medium and bacteria. It was surprisingly found that there was no bacterial corrosion, although it was to be expected that the reaction of TBM with sulfuric acid (Tuovine buffer) would result in H 2 S having a positive effect on the corrosion activity of the bacteria.

Abstract

The invention relates to the use of di-tert-butylsulphide (TBDS) and/or tert-butylmercaptan (TBM) in order to inhibit microbial corrosion of metals and the alloys thereof, especially steel.

Description

Verwendung von Di - tert -Butylsulfid (TBDS) und/oder tert -Butylmercaptan (TBM) als Korrosionsinhibi toren der mikrobiellen Korrosion von Metallen Use of di-tert-butyl sulfide (TBDS) and / or tert-butyl mercaptan (TBM) as corrosion inhibitors for microbial corrosion of metals
Beschreibungdescription
Die Erfindung betrifft die Verwendung von Di-tert- Butylsulfid (TBDS) und/oder tert-Butylmercaptan (TBM) zur Inhibierung der mikrobiellen Korrosion von Metallen und deren Legierungen, insbesondere von Stahl.The invention relates to the use of di-tert-butyl sulfide (TBDS) and / or tert-butyl mercaptan (TBM) for inhibiting the microbial corrosion of metals and their alloys, in particular steel.
Es ist bekannt, daß Metalle und Metallegierungen, insbesondere Stahl, einer mikrobiellen Korrosion unter- liegen. So wird in den USA ein großer Teil der Korrosionsverluste (bis zu 200 Milliarden US-Dollar/Jahr) der Biokorrosion zugeschrieben (W.K. Choi, A.E. Torma, Effects of Biofilm of Thiobacillus ferrooxidans on Stainless Steel in Aerobic Environment, 1993 EPD Cong., paper no. 27 (Denver, CO: The Minerals, Metals, and Materials Society, 1993) .It is known that metals and metal alloys, especially steel, are subject to microbial corrosion. In the USA, a large part of the corrosion losses (up to $ 200 billion / year) is attributed to biocorrosion (WK Choi, AE Torma, Effects of Biofilm of Thiobacillus ferrooxidans on Stainless Steel in Aerobic Environment, 1993 EPD Cong., Paper no. 27 (Denver, CO: The Minerals, Metals, and Materials Society, 1993).
Mechanistische Untersuchungen am Beispiel des Stahls haben gezeigt, daß die mikrobielle Korrosion von Metallen über die Bildung von Sulfidschichten an der Metalloberfläche abläuft, die dann von Sulfid- oxidierenden Bakterien ( Thiobacilli) zu Sulfaten und Schwefelsäure abgebaut werden (H. Tributsch et al . , CORROSION, Vol. 54, No . 3, S. 216-227, 1998). Die Schwefelsäure wird als ein wichtiger Faktor in der Biokorrosion von Stahl beschrieben. Zur Verhinderung oder zumindest Inhibierung der unter Beteiligung der ThioJacilli-Bakterien ablaufenden mikrobiellen Korrosion von Metallen sind bisher keine wirksamen Mittel bekannt geworden.Mechanistic studies using the example of steel have shown that the microbial corrosion of metals takes place via the formation of sulfide layers on the metal surface, which are then broken down by sulfide-oxidizing bacteria (Thiobacilli) to sulfates and sulfuric acid (H. Tributsch et al., CORROSION , Vol. 54, No. 3, pp. 216-227, 1998). Sulfuric acid is described as an important factor in the biocorrosion of steel. No effective means have hitherto been known for preventing or at least inhibiting the microbial corrosion of metals which takes place with the participation of the ThioJacilli bacteria.
Es war deshalb die Aufgabe der Erfindung, Mittel aufzufinden, die die mikrobielle Korrosion von Metallen und deren Legierungen verhindern oder zumindest inhibieren. Insbesondere sollen biokorrosionsinhibierende Mittel für Stahl bereitgestellt werden.It was therefore the object of the invention to find agents which prevent or at least inhibit the microbial corrosion of metals and their alloys. In particular, biocorrosion inhibitors for steel are to be provided.
Es wurde überraschenderweise gefunden, daß die Aufgabe der Erfindung durch den Einsatz von Di-tert- Butyldisulfid (TBDS) , tert-Butylmercaptan (TBM) oder einem Gemisch beider Verbindungen gelöst werden kann. TBDS und TBM haben sich insofern als Inhibitoren der mikrobiellen Korrosion erwiesen, als sie den Angriff der Mikroorganismen der Gattung Thiobacillus auf die Sulfidschichten verhindern. So haben Langzeitversuche von mit TBDS sulfurisierten Pyritschichten (FeS2) gezeigt, daß Thiobacillen, die auf diesen Schichten angesiedelt wurden, abgetötet wurden, während die Pyritoberfläche erhalten blieb.It has surprisingly been found that the object of the invention can be achieved by using di-tert-butyl disulfide (TBDS), tert-butyl mercaptan (TBM) or a mixture of both compounds. TBDS and TBM have proven to be inhibitors of microbial corrosion in that they prevent the attack of the microorganisms of the genus Thiobacillus on the sulfide layers. Long-term tests of pyrite layers (FeS 2 ) sulfurized with TBDS have shown that thiobacilli, which were deposited on these layers, were killed while the pyrite surface was preserved.
Erfindungsgemäß ist es bevorzugt, TBDS oder ein Gemisch aus TBDS und TBM als Korrosionsinhibitor zu verwenden, da TBM selbst eine gering in Wasser lösliche und vor allem übelriechende Flüssigkeit ist . Prinzipiell wurde jedoch festgestellt, daß TBM der eigentliche Wirkstoff ist, der die bakterielle Korrosion verhindert, indem er mit den Metallsulfiden Disulfidbindungen ausbildet.According to the invention, it is preferred to use TBDS or a mixture of TBDS and TBM as a corrosion inhibitor, since TBM itself is a slightly water-soluble and, above all, malodorous liquid. In principle, however, it was found that TBM is the actual active ingredient which prevents bacterial corrosion by forming disulfide bonds with the metal sulfides.
Vorzugsweise werden die erfindungsgemäßen Verbindungen als Schutzfilm auf die zu schützende Metalloberfläche aufgebracht. Dies kann beispielsweise durch Aufstreichen der in Wasser und/oder einem organischen Lösungsmittel gelösten Verbindungen erfolgen. Für den Fall, daß TBDS als Schicht aufgebracht wird, muß diese aktiviert werden, damit TBDS zu TBM gespalten wird. Die Aktivierung der Deckschicht wird mittels UV-Behandlung, durch Erwärmung, Mikrowellenbehandlung oder Plasmabehandlung vorgenommen.The compounds according to the invention are preferably applied as a protective film to the metal surface to be protected. This can be done, for example Painting the compounds dissolved in water and / or an organic solvent. In the event that TBDS is applied as a layer, this must be activated so that TBDS is split into TBM. The cover layer is activated by UV treatment, heating, microwave treatment or plasma treatment.
In einer anderen bevorzugten Ausführungsform wird eine Lösung aus TBDS und TBM eingesetzt, z.B. eine wäßrigalkoholische Lösung. Durch Zusatz von Alkalilauge wird das TBDS in dieser Lösung zum TBM gespalten. Hier muß das Aufbringen der Lösung auf die Metalloberfläche allerdings relativ schnell erfolgen, damit nicht all zuviel TBM durch Luftoxidation in TBDS zurückverwandelt wird. Diese Variante ist zur Behandlung kleiner Metalloberflächen durchaus geeignet, zur Behandlung größerer Oberflächen empfiehlt es sich, aufgrund der besseren Handhabbarkeit TBDS zu verwenden.In another preferred embodiment, a solution of TBDS and TBM is used, e.g. an aqueous alcoholic solution. The TBDS is split into the TBM in this solution by adding alkali lye. Here, however, the solution must be applied to the metal surface relatively quickly, so that not too much TBM is converted back into TBDS by air oxidation. This variant is quite suitable for the treatment of small metal surfaces, for the treatment of larger surfaces it is recommended to use TBDS due to the better handling.
Die erfindungsgemäßen Verbindungen eignen sich zur Korrosionsinhibierung für alle Metalle bzw. Legierungen, auf denen Sulfidschichten ausgebildet werden können, wie beispielsweise Eisen, Kupfer, Zink, Blei, Nickel, Cobalt oder Molbdän. Insbesondere hat sich der Einsatz der erfindungsgemäßen Korrosionsinhibitoren auf Stahl als äußerst wirksam herausgestellt.The compounds according to the invention are suitable for inhibiting corrosion for all metals or alloys on which sulfide layers can be formed, such as iron, copper, zinc, lead, nickel, cobalt or molbdenum. In particular, the use of the corrosion inhibitors according to the invention on steel has proven to be extremely effective.
Nachfolgend soll die Erfindung anhand von Ausfüh- rungsbeispielen näher erläutert werden. AusführungsbeispieleThe invention is to be explained in more detail below with the aid of exemplary embodiments. Embodiments
Beispiel 1 :Example 1 :
Präparation von Pγri t schichten mittels Niederdruck- MOCVD-Anlacre (Metal Organic Chemical Vapor Deposition)Preparation of Pγri layers using low-pressure MOCVD-Anlacre (Metal Organic Chemical Vapor Deposition)
Bei der metallorganischen chemischen Gasphasenab- scheidung (MOCVD) handelt es sich um ein Verfahren zur Präparation von dünnen Polykristallen und epitaktischen Schichten. Dabei werden die Schichten aus der Gasphase abgeschieden. Als Ausgangsstoffe (Precursoren) dienen meist metallorganische Verbindungen. Der Abscheidevorgang läuft wie folgt ab: Ein Trägergas wird durch sogenannte Bubbler geleitet. Im Bubbler befinden sich die metallorganischen Verbindungen in flüssiger oder fester Form. Die Ausgangsstoffe werden dadurch in das Trägergas aufgenommen. Das Trägergas transportiert die Ausgangsverbindungen an einem geheizten Substrat vorbei. Die Ausgangsverbindungen enthalten die Ele- mente, mit denen die Schicht gebildet werden soll. In einer Reaktion zersetzen sich die Verbindungen über der Substratoberfläche. Dadurch werden die zur Schichtbildung beitragenden Elemente freigesetzt . Diese lagern sich an der Substratoberfläche an und bilden somit die Schicht. Die überschüssigen Zerfallsprodukte werden mit dem Trägergas der Abluft zugeführt. Für das vorliegende Beispiel wurden die Pyritschichten mit der MOCVD-Anlage präpariert wie sie in „Solar Energy Materials and Solar Cells" 1993, 29, 289-370 beschrieben ist. Als geeig- neter Schwefelprecursor wurde a) elementarer Schwefel und b) TBDS verwendet. Als Eisenprecursor wurde zur Präparation von Pyrit Eisenpentacarbonyl [Fe(CO)5] verwendet . Beispiel 2 :Organometallic chemical vapor deposition (MOCVD) is a process for the preparation of thin polycrystals and epitaxial layers. The layers are deposited from the gas phase. Organometallic compounds mostly serve as starting materials (precursors). The separation process is as follows: A carrier gas is passed through so-called bubblers. The organometallic compounds are in liquid or solid form in the bubbler. The raw materials are thereby taken up in the carrier gas. The carrier gas transports the starting compounds past a heated substrate. The starting compounds contain the elements with which the layer is to be formed. In a reaction, the compounds decompose above the substrate surface. This releases the elements that contribute to layer formation. These accumulate on the substrate surface and thus form the layer. The excess decay products are fed into the exhaust air with the carrier gas. For the present example, the pyrite layers were prepared with the MOCVD system as described in "Solar Energy Materials and Solar Cells" 1993, 29, 289-370. A) elemental sulfur and b) TBDS were used as the suitable sulfur precursor. Iron pentacarbonyl [Fe (CO) 5 ] was used as the iron precursor for the preparation of pyrite. Example 2:
TBDS als Inhibi tor der mikrobiellen Korrosion von EisenTBDS as an inhibitor of microbial corrosion of iron
Jeweils 1 cm2 der gemäß Beispiel lb) unter Verwendung von TBDS als Schwefelprecursor präparierten Pyritschichten von 100 nm Dicke werden in einer in-situ Pyrit-Kulturkammer mit einer wäßrigen ThioJa- cillus ferrooxidans-Suspension (» 50.000 Bakterien/μl) in Tuovinen-Nährmedium [vgl . Tuovinen und Kelly in „Arch. Mikrobiol. 88, 285-298 (1973)"] beimpft.In each case 1 cm 2 of the pyrite layers of 100 nm thickness prepared according to Example 1b) using TBDS as sulfur precursor are in an in-situ pyrite culture chamber with an aqueous ThioJacillus ferrooxidans suspension (»50,000 bacteria / μl) in Tuovine nutrient medium [see . Tuovinen and Kelly in “Arch. Microbiol. 88, 285-298 (1973) "].
Zum Vergleich wurden die gemäß Beispiel la) unter Verwendung von elementarem Schwefel als Precursor erzeugten Pyritschichten auf die gleiche Weise untersucht.For comparison, the pyrite layers produced according to Example la) using elemental sulfur as a precursor were examined in the same way.
Es zeigte sich, daß die TBDS-Pyritschichten von den Bakterien nicht angegriffen wurden. Die Untersuchungen wurden mittels optischer und elektronischer Mikroskopie durchgeführt und in allen Fällen waren die Bakterien unfähig, Pyrit als Energiequelle zu verwerten. Die Langzeitversuche wurden bis zu 3 Monaten verfolgt. Nach dieser Zeit wurde festgestellt, daß die Bakterien abgetötet worden waren, während die Pyritoberfläche erhalten blieb.It was found that the TBDS pyrite layers were not attacked by the bacteria. The investigations were carried out using optical and electronic microscopy and in all cases the bacteria were unable to use pyrite as an energy source. The long-term trials were followed up to 3 months. After this time it was found that the bacteria had been killed while the pyrite surface was preserved.
Im Gegensatz dazu zeigten die unter Verwendung von elementarem Schwefel erzeugten Pyritschichten die bekannten Auflösungserscheinungen.In contrast, the pyrite layers produced using elemental sulfur showed the known dissolution phenomena.
Beispiel 3 :Example 3:
Erfindungsgemäße Behandlung von Pyrit schichten mi t TBMTreatment of pyrite layers according to the invention with TBM
Die in Beispiel la) unter Verwendung von elementarem Schwefel als Precursor erzeugten Pyritschichten wurden mit einem dünnen Film TBM in einer Isolationskammer behandelt .The pyrite layers produced in Example la) using elemental sulfur as a precursor were treated with a thin film of TBM in an isolation chamber.
Nach ca. 8 Stunden wurde die Schicht mit reichlich Wasser gespült, um das Übermaß an TBM zu beseitigen. Die Schicht wurde abflotiert und wie in Beispiel 2 mit Tuovinen-Medium und Bakterien kultiviert. Es wurde überraschend festgestellt, daß keine bakterielle Korrosion stattfand, obwohl zu erwarten war, daß durch die Reaktion von TBM mit Schwefelsäure (Tuovinen-Puffer) das entstandene H2S eine positive Wirkung auf die Korrosionsaktivität der Bakterien haben würde. After about 8 hours, the layer was rinsed with plenty of water to remove the excess TBM. The layer was flotated and cultivated as in Example 2 with Tuovine medium and bacteria. It was surprisingly found that there was no bacterial corrosion, although it was to be expected that the reaction of TBM with sulfuric acid (Tuovine buffer) would result in H 2 S having a positive effect on the corrosion activity of the bacteria.

Claims

Patentansprüche claims
1. Verwendung von Di-tert-Butylsulfid (TBDS) und/oder tert-Butylmercaptan (TBM) zur Inhibierung der mikrobiellen Korrosion von Metallen und deren Legierungen.1. Use of di-tert-butyl sulfide (TBDS) and / or tert-butyl mercaptan (TBM) to inhibit the microbial corrosion of metals and their alloys.
Verwendung nach Anspruch 1 zur Inhibierung der mikrobiellen Korrosion von Stahl . Use according to claim 1 for inhibiting the microbial corrosion of steel.
PCT/EP1999/005644 1998-08-07 1999-08-04 Use of di-tert-butylsulphide (tbds) and/or tert-butylmercaptan (tbm) as corrosion inhibitors in microbial corrosion of metals WO2000008235A1 (en)

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DE1998136544 DE19836544C2 (en) 1998-08-07 1998-08-07 Use of di-tert-butyl disulfide (TBDS) and / or tert-butyl mercaptan (TBM) as corrosion inhibitors of the microbial corrosion of metals
DE19836544.6 1998-08-07

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