EP0861925A1 - Matériau composite inhibiteur de la corrosion - Google Patents

Matériau composite inhibiteur de la corrosion Download PDF

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Publication number
EP0861925A1
EP0861925A1 EP98102552A EP98102552A EP0861925A1 EP 0861925 A1 EP0861925 A1 EP 0861925A1 EP 98102552 A EP98102552 A EP 98102552A EP 98102552 A EP98102552 A EP 98102552A EP 0861925 A1 EP0861925 A1 EP 0861925A1
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EP
European Patent Office
Prior art keywords
corrosion
metal oxide
composite material
material according
vpi
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.)
Granted
Application number
EP98102552A
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German (de)
English (en)
Other versions
EP0861925B1 (fr
Inventor
Horst Prof. Dr. Böttcher
Karl-Heinz Kallies
Georg Prof. Dr. Reinhard
Gerhard Hahn
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.)
Excor Korrosionsschutz- En Kallies Feinchemie Ag
Original Assignee
Excor Korrosionsschutz Technologien und Produkte GmbH
Feinchemie GmbH Sebnitz
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Filing date
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Application filed by Excor Korrosionsschutz Technologien und Produkte GmbH, Feinchemie GmbH Sebnitz filed Critical Excor Korrosionsschutz Technologien und Produkte GmbH
Publication of EP0861925A1 publication Critical patent/EP0861925A1/fr
Application granted granted Critical
Publication of EP0861925B1 publication Critical patent/EP0861925B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors

Definitions

  • the invention relates to a corrosion-inhibiting material, that contains one or more corrosion inhibitors.
  • VPI vapor phase inhibitors
  • VPI volatile corrosion inhibitors
  • Variants of this type are e.g. from H. H. Uhlig "Corrosion and Corrosion Protection”, Akademie-Verlag Berlin, 1970, p. 247 ff., or I.L. Rozenfeld “Corrosion Inhibitors” ( Russian), Izt-vo Chimija, Moskva 1977, pp. 316 ff. You own it Disadvantage that the release of the VPIs is undefined and a homogeneous distribution over the gas space is not guaranteed can be.
  • Other disadvantages are the risk that the CPI contained Bags are mechanically destroyed and become an undesirable one Contamination of the packaged goods as well the problems arising from the uneven distribution of the Bags in large storage rooms and large containers surrender.
  • the inert carrier material is said to be due to its structure-related porosity for continuous sublimation of the VPI components distributed in between and at the same time an agglomeration of the finely dispersed VPI components to larger mixed particles (e.g. formation of lumps counteract with encrusted surface due to water absorption).
  • desiccants has been common the opposite of the desired effect and leads after water absorption for preferred clumping.
  • the VPI's are in an organic solvent solved and soaked the packaging.
  • method of this type with various active ingredients and solvents are e.g. in JP 61-227188, JP 62-063686, JP 63-028888, JP 63-183182, JP 63-210285 and US 3 887 481.
  • the risk of these substances spreading and trickling out from or out of the packaging, so that not secured can be that the pretreated cardboard and paper for Time of their application for corrosion protection at all the required specific surface concentration of VPI have.
  • VPI's are components of the foamed polymer.
  • the crystalline VPI's in one of the Starting components are dispersed.
  • VPIs usually belong to other substance classes and the stability of the Dispergate is low.
  • Aggravating Added to this is the fact that the modern VPI's themselves consist of several substances with different chemical properties. Provided these are at all together with the components for foams
  • Such dispersions usually have dispersed a very wide range of grain sizes, low stability and problematic workability.
  • DD 295 668 describes a process for producing VPI containing polyurethane systems, in which the VPI's initially in a polyfunctional alcohol of molecular weight 500 to Dissolved 1000 g / mol and then introduced into the polyol be before adding polyisocyanate, catalyst, stabilizer and blowing agent the polyurethane is produced.
  • the procedure is only limited to VPIs in such Alcohols in the concentration required for corrosion protection are soluble and then as part of the polyol component do not interfere with the process of foaming. It is therefore not suitable to meet the complex requirements meet the temporary corrosion protection of today Ferrous and non-ferrous metals as well as multi-metal combinations be made, especially since it contains practically all inorganic active substances excludes from the application.
  • the object of the invention is to provide an improved material mechanically and chemically stable fixation of volatile Corrosion inhibitors on solid surfaces and a corrosion protective Specify packaging material.
  • the fixative Material should in particular be independent of the physicochemical Properties of the active ingredients and the type of surface be universal and technologically easy to use and eliminate the disadvantages of the methods described above. task the invention further is a method of manufacture of such material.
  • the task in particular can be solved in that known corrosion inhibitors in diffusion-inhibiting metal oxide gels (preferably in Layer form) are embedded, the inorganic matrix can be modified by organic polymers so that synergistic Effects regarding immobilization and layer quality result.
  • the composition of the metal oxide gel and the manufacturing technology allows the porosity of the composites formed so that a stable Release of the corrosion inhibitor into the gas phase via a long period of time.
  • the corrosion-inhibiting composite material is used in manufacturing of corrosion protective packaging materials, for coating of metallic and metallized objects as well as for corrosion protection in closed rooms.
  • the invention relates to a corrosion-inhibiting material, consisting of a composite containing a metal oxide gel, possibly modified by an organic polymer, and one or more Contains corrosion inhibitors, a process for its preparation, or the use of a corrosion-inhibiting Composite material for the production of anti-corrosion Packaging materials, for coating metallic and metallized objects and for corrosion protection in closed Clearing
  • Metal oxide gels such as Si0 2 , Al 2 0 3 , Ti0 2 , Zr0 2 or ZnO or mixtures thereof can be used as the matrix component, which can be obtained by a sol-gel process, for example by hydrolysis of the corresponding metal alkoxides to give the corresponding metal oxide sols and subsequent ones Gel formation by neutralization, heating or concentration, receives, cf. JCBrinker, GWScherer, "Sol-Gel Science", Academic Press, London 1990.
  • the metal oxide brine is formed by acid or base-catalyzed hydrolysis of the corresponding metal alkoxides in water or any water-miscible organic solvent (usually ethanol).
  • the active ingredient content in the metal oxide is around 1 to 15% by weight, preferably around 1 to 5% by weight, based on the weight of the Metal oxide in the sol (solids content) or in the gel.
  • the hydrolysis process (1) of the metal alkoxides can be carried out in the presence of mixed alkyl trialkoxysilanes R-Si (OR ') 3 , whereby modified metal oxide gels are formed which, based on 1 part by weight of metal oxide gel, contain 0 to 1 part by weight of R-Si0 n contain.
  • R is an organic alkyl radical, which may contain amino, hydroxy or alkoxy groups
  • R ' is an alkyl radical, primarily with 1-4 carbon atoms
  • n is ⁇ 2.
  • Metal oxide gel for Improvement of the layer quality is that 1 part by weight Metal oxide gel by 0 to 1 parts by weight of a dissolved or dispersed organic polymers such as cellulose derivatives, Starch derivatives, polyalkylene glycols or their derivatives, Homo- or copolymers based on acrylate and methacrylate, Polystyrene sulfone sulfonate or natural resins, or mixtures of the polymers mentioned, is modified.
  • a dissolved or dispersed organic polymers such as cellulose derivatives, Starch derivatives, polyalkylene glycols or their derivatives, Homo- or copolymers based on acrylate and methacrylate, Polystyrene sulfone sulfonate or natural resins, or mixtures of the polymers mentioned.
  • preferred Polymers as a composite component are polystyrene sulfonic acid, Hydroxypropyl, methyl and carboxymethyl cellulose or rosin.
  • the polymer additive has two functions: (a) supported by changing the composite structure by ionic groups as in the case of polystyrene sulfonate, you can delay the release of the corrosion inhibitor, (b) by the addition of polymer, especially soluble Cellulose derivatives, one can adjust the viscosity of the brine and thus the layer thickness under constant coating conditions increase sharply. So you are able to get the absolute amount of the released corrosion inhibitor Taxes.
  • the corrosion-inhibiting composite materials thus obtained are easy to manufacture and have good long-term stability due to the known chemical inertness of the Matrix component (in the simplest case, pure silicon dioxide), excellent layering properties and an effective Immobilization with a high corrosion-inhibiting effect.
  • the suitability for practically any inorganic is further advantage and organic substance classes, good adhesion to various Packaging materials and metallic objects as well as the possibility through the recipe and manufacturing technology the porosity of the composite material in wide Control borders.
  • the material according to the invention is therefore particularly suitable for Manufacture of anti-corrosive packaging materials, for coating metallic materials to be protected immediately and metallized objects as well as for corrosion protection in closed rooms by means of powdered corrosion inhibiting Composite materials.
  • Sol F viscosity 4.5 mPa, 20 ° C
  • Klucel H / Aqualon GmbH hydroxypropyl cellulose
  • the resulting Sol G has a viscosity of 48 mPa, 20 ° C.
  • a typical drawing speed of 30 cm / min with Sol F results in a dry layer thickness of 0.63 ⁇ m, with Sol G 2.82 ⁇ m.
  • the brine specified in Tab. 1 are mixed with the dissolved corrosion inhibitors and thus (a) different carriers are coated or (b) the mixture is gelled by neutralization with 2% ammonia solution and heating to 60 ° C. The solid gel is dried in air to remove the organic solvent and then in a vacuum desiccator to remove the residual moisture.
  • Manufacture of corrosion inhibiting composite materials No. Sol (100 ml) Inhibitor Coating 1 A 20 ml dicyclohexylammonium nitrite (5% in 90% EtOH) Diving paper 2nd D " Diving paper 3rd B 50 ml NaN0 2 + subst. phenol (2% in 60% EtOH) Diving paper 4th H 20 ml hydroquinone + subst.
  • the VPI-containing paper produced according to the invention was in the Comparison to a commercially available reference system Corrosion protection paper (R1) according to the usual in practice Method for "testing the corrosion-protective effect of VPI packaging materials" (see “Packaging Review” 5/1988, p. 37 ff.) tested.
  • R1 contained the after chemical analysis Active ingredients dicyclohexylamine, sodium nitrite, sodium salt of caprylic acid, Urea and benzotriazole, the former two Substances in approximately the same proportion as dicyclohexylammonium nitrite in paper no. 1.
  • Test specimens came from unalloyed Mass steel St-38 u2 for use. These were in accordance with regulations pretreated and alone or together with the testing VPI packaging in tightly sealed containers introduced and therein set conditions that a water condensation on the surface of the test specimen. The grinding surface of the test specimens was intended regularly visually for the existence of signs of corrosion examined.
  • the blank samples used without the use of VPI showed The first signs of corrosion in the Edge area; the test specimens exposed together with the R1 paper showed relatively even surface after approx. 11 d distributed rust spots.
  • the manufactured according to the invention Paper no. 1 also guaranteed according to regulations after 21 d Full corrosion protection effect, recognizable by the perfect appearance of the corresponding test specimens.
  • R2 commercial VPI paper
  • the VPI-containing solids were applied in a wide-area dish finely divided with 1 g / 100 cm 3 wet room volume. In the pure moist air, the first spotty signs of rust were already visible on the cast iron plates after about 7 hours. The corrosion protection was maintained in the chamber loaded with the commercially available VPI granules for about 62 hours. The samples which, together with the VPI-emitting powder produced according to the invention, were exposed to the damp room climate, did not show any rust formation even after the tests were stopped after 20 days. According to the invention, both the novel combination of corrosion inhibitors used and the constitution of the composite containing the VPI, which ensures continuous discharge into the gas phase, are responsible for this.
  • the one available according to the manufacturing method No. 4 according to the invention Paper has been designed to preserve the Gloss behavior of anodized Al plates examined.
  • the CLOSScomp / OPTRONIK measuring system was used to assess the gloss Berlin used. This takes from the respective reflection curve of the substrate the measured values maximum value P / dB (Peak height), maximum increase A / (dB / degree), full width at half maximum HW / Degree of the reflection curve and calculates the visual from it Degree of gloss Gt in%.
  • a loss of gloss caused by the first signs of corrosion is represented in lower values for P, A and Gt as well in an increase in HW.
  • the coated and the uncoated panels were stored in a climatic cabinet in accordance with IEC 68-2-30 cyclically loaded with moist air.
  • Polished copper and brass plates Ms63 were used between the invention coated, equally sized panels Layered PUR foam and in foils made of pure polyethylene (100 ⁇ m) welded in.
  • the samples packed in this way were the wet climate exposure described for No. 5 exposed according to IEC 68-2-30.
  • Copper lamellas the outside without electricity (chemical) with a are provided with a thin nickel layer Semiconductor industry even after long storage in a dry place Air remains bondable at room temperature.
  • With the reference system (R1) mentioned at no. 1 was not delayed this aging process.
  • the chemically nickel-plated Lamels could be stored in this VPI paper on average after 5 days of storage can no longer be bonded.
  • the slats were opposed immediately after the end of the nickel plating in a desiccator transferred, the bottom part with the manufactured according to the invention Powder No. 8 was filled, then the aging of the Ni primary oxide film remained inhibited and the lamellae could still d Storage can be bonded.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Paints Or Removers (AREA)
  • Anti-Oxidant Or Stabilizer Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Laminated Bodies (AREA)
EP98102552A 1997-02-28 1998-02-13 Matériau composite inhibiteur de la corrosion Expired - Lifetime EP0861925B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19708285 1997-02-28
DE19708285A DE19708285C2 (de) 1997-02-28 1997-02-28 Korrosionsinhibierendes Kompositmaterial, Verfahren zu dessen Herstellung und seine Verwendung

Publications (2)

Publication Number Publication Date
EP0861925A1 true EP0861925A1 (fr) 1998-09-02
EP0861925B1 EP0861925B1 (fr) 2002-01-23

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EP98102552A Expired - Lifetime EP0861925B1 (fr) 1997-02-28 1998-02-13 Matériau composite inhibiteur de la corrosion

Country Status (6)

Country Link
US (1) US5958115A (fr)
EP (1) EP0861925B1 (fr)
JP (1) JPH10324983A (fr)
AT (1) ATE212386T1 (fr)
CZ (1) CZ296315B6 (fr)
DE (2) DE19708285C2 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0976851A1 (fr) * 1998-07-29 2000-02-02 EXCOR Korrosionsforschung GmbH Inhibiteurs de la corrosion en phase vapeur, leur utilisation et méthode de leur fabrication
US8277911B2 (en) 2006-07-07 2012-10-02 Rengo Co., Ltd. Anticorrosion composition
CN104311971A (zh) * 2014-11-10 2015-01-28 青岛鑫盈鑫包装材料有限公司 多金属用防锈母粒及其制备方法和应用
EP3461931A1 (fr) * 2017-09-27 2019-04-03 EXCOR Korrosionsforschung GmbH Compositions des inhibiteurs de corrosion à phase vapeur et leur utilisation ainsi que leur procédé de production
CN113529089A (zh) * 2021-07-02 2021-10-22 北京首融汇科技发展有限公司 一种环保型气相缓蚀剂及气相防锈材料
CN115572976A (zh) * 2022-11-11 2023-01-06 山东韩师傅新材料有限公司 一种用于海洋建筑金属钢结构的复合缓蚀剂及其制备方法

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ES2238179B1 (es) * 2004-02-05 2006-11-01 Tolsa, S.A. Material inhidibor de corrosion de metales y su procedimiento de preparacion.
DE102004018624B4 (de) * 2004-04-17 2006-05-18 Daimlerchrysler Ag Verfahren zum Schutz von an ihrer Oberfläche nicht passivierbare Metalle aufweisenden Gegenständen und seine Verwendung
CN100343421C (zh) * 2004-10-18 2007-10-17 李振波 气相与干燥防锈方法
GB0608504D0 (en) * 2006-04-28 2006-06-07 Grid71 Ltd Corrosion-inhibiting composition
US20080099729A1 (en) * 2006-10-27 2008-05-01 Mcconnell Robin Corrosion inhibiting mixture
DE102010006099A1 (de) 2010-01-28 2011-08-18 EXCOR Korrosionsforschung GmbH, 01067 Zusammensetzungen von Dampfphasen-Korrosionsinhibitoren, Verfahren zu deren Herstellung und deren Verwendung für den temporären Korrosionsschutz
US11058161B2 (en) 2012-02-16 2021-07-13 Xefco Pty Ltd Heat reflecting composites with knitted insulation
CN102993878B (zh) * 2012-11-01 2016-03-09 安徽荣达阀门有限公司 一种含有二乙酰柠檬酸三乙酯的金属防锈剂
US10160184B2 (en) 2013-06-03 2018-12-25 Xefco Pty Ltd Insulated radiant barriers in apparel
CN104311975B (zh) * 2014-11-10 2016-08-24 青岛鑫盈鑫包装材料有限公司 月桂酸二乙醇酰胺硼酸酯气相防锈母粒及其制备方法和应用
US9656201B2 (en) 2014-12-24 2017-05-23 Northern Technologies International Corporation Smart, on-demand controlled release corrosion protection and/or prevention of metals in an enclosure
CN108359175A (zh) * 2018-02-11 2018-08-03 江阴通利光电科技有限公司 一种缓释型气相防锈拉伸聚丙烯薄膜的制备方法
DE102019100123B4 (de) 2019-01-04 2021-02-04 Excor Korrosionsforschung Gmbh Zusammensetzungen und Verfahren zur Vorbehandlung von Substraten für die nachfolgende Fixierung von Dampfphasen-Korrosionsinhibitoren
CN113292837B (zh) * 2021-06-07 2023-03-10 广东顾纳凯材料科技有限公司 仿金属外观母粒及其制备方法、聚烯烃复合材料

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0976851A1 (fr) * 1998-07-29 2000-02-02 EXCOR Korrosionsforschung GmbH Inhibiteurs de la corrosion en phase vapeur, leur utilisation et méthode de leur fabrication
US8277911B2 (en) 2006-07-07 2012-10-02 Rengo Co., Ltd. Anticorrosion composition
CN104311971A (zh) * 2014-11-10 2015-01-28 青岛鑫盈鑫包装材料有限公司 多金属用防锈母粒及其制备方法和应用
EP3461931A1 (fr) * 2017-09-27 2019-04-03 EXCOR Korrosionsforschung GmbH Compositions des inhibiteurs de corrosion à phase vapeur et leur utilisation ainsi que leur procédé de production
CN113529089A (zh) * 2021-07-02 2021-10-22 北京首融汇科技发展有限公司 一种环保型气相缓蚀剂及气相防锈材料
CN115572976A (zh) * 2022-11-11 2023-01-06 山东韩师傅新材料有限公司 一种用于海洋建筑金属钢结构的复合缓蚀剂及其制备方法
CN115572976B (zh) * 2022-11-11 2023-03-03 山东韩师傅新材料有限公司 一种用于海洋建筑金属钢结构的复合缓蚀剂及其制备方法

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DE19708285A1 (de) 1998-09-03
CZ296315B6 (cs) 2006-02-15
JPH10324983A (ja) 1998-12-08
EP0861925B1 (fr) 2002-01-23
US5958115A (en) 1999-09-28
ATE212386T1 (de) 2002-02-15
DE59802869D1 (de) 2002-03-14
DE19708285C2 (de) 2002-04-11
CZ51998A3 (cs) 1998-09-16

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