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WO2004085557A1 - Procede d'elevation de la resistance a la corrosion de tubes, et tubes produits selon ce procede - Google Patents

Procede d'elevation de la resistance a la corrosion de tubes, et tubes produits selon ce procede Download PDF

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Publication number
WO2004085557A1
WO2004085557A1 PCT/EP2004/000865 EP2004000865W WO2004085557A1 WO 2004085557 A1 WO2004085557 A1 WO 2004085557A1 EP 2004000865 W EP2004000865 W EP 2004000865W WO 2004085557 A1 WO2004085557 A1 WO 2004085557A1
Authority
WO
WIPO (PCT)
Prior art keywords
tubes
fluoropolymer
coated
wall
fluoφolymer
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.)
Ceased
Application number
PCT/EP2004/000865
Other languages
German (de)
English (en)
Inventor
Peter Kurze
Dora Banerjee
Marco Kohler
Ulrike KRÜGER
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.)
Aalberts Surface Technologies GmbH Kerpen
Original Assignee
AHC Oberflaechenechnik GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE10313966A external-priority patent/DE10313966A1/de
Application filed by AHC Oberflaechenechnik GmbH filed Critical AHC Oberflaechenechnik GmbH
Publication of WO2004085557A1 publication Critical patent/WO2004085557A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D35/00—Pliable tubular containers adapted to be permanently or temporarily deformed to expel contents, e.g. collapsible tubes for toothpaste or other plastic or semi-liquid material; Holders therefor
    • B65D35/14—Pliable tubular containers adapted to be permanently or temporarily deformed to expel contents, e.g. collapsible tubes for toothpaste or other plastic or semi-liquid material; Holders therefor with linings or inserts
    • B65D35/16—Pliable tubular containers adapted to be permanently or temporarily deformed to expel contents, e.g. collapsible tubes for toothpaste or other plastic or semi-liquid material; Holders therefor with linings or inserts for minimising or preventing corrosion of body
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2400/00—Characterised by the use of unspecified polymers
    • C08J2400/14—Water soluble or water swellable polymers, e.g. aqueous gels

Definitions

  • the present invention relates to a method for increasing the corrosion resistance of tubes, in particular tubes made of aluminum or aluminum alloys. Likewise, the present invention relates to the tubes manufactured or corrosion-treated in this way. Furthermore, the present invention relates to the use of fluoropolymers to increase the corrosion resistance or service life of tubes.
  • tube denotes in particular in the packaging technology used, elongated, for. B. cylindrical, flexible, elastically or plastically deformable containers made of metal (z. B. aluminum or tin) or plastic (z. B. polyethylene
  • metal tubes predominantly tubes 35 made of aluminum or aluminum alloys, are often used, which are produced, for example, by cold forming or deep drawing. Since this Tu ben or tube body often do not have the corrosion resistance required for the respective application, they are often coated on the inner walls with an anti-corrosion varnish (e.g. an epoxy resin or a polyurethane resin). This then results in tubes with a longer service life or increased corrosion resistance, which, however, are still not sufficient for certain applications.
  • an anti-corrosion varnish e.g. an epoxy resin or a polyurethane resin
  • plastic tubes e.g. made of PE or PP
  • plastic tubes cannot always be used optimally in terms of their haptic properties and the problem of residual emptying.
  • the problem underlying the present invention is therefore to improve or increase the service life or the corrosion resistance of tubes.
  • the object of the present invention in accordance with a first aspect is thus a method for increasing the corrosion resistance (corrosion resistance) or service life of tubes, wherein the inner wall (s) of the tubes are coated with at least one fluoropolymer.
  • the coating of the inner wall (s) of the tubes with at least one fluoropolymer surprisingly leads not only to a significant increase in the corrosion resistance, but also to an improvement in the (residual) drainability and dust / dirt repellency.
  • the method according to the invention can be applied not only to tubes, but also equally with regard to any containers used to hold flowable, in particular liquid or pasty media, such as tubes or cans (e.g. canned goods) - or beverage cans) is suitable.
  • the method according to the invention is particularly suitable for tubes, and the method according to the invention has proven particularly useful for this.
  • a particularly effective protection against corrosion of the treated tubes is obtained if the inner wall (s) of the tubes are (at least substantially) completely, preferably completely, coated with the fluoropolymer.
  • the fluoropolymer coating is applied at least essentially homogeneously, in particular with a uniform layer thickness.
  • the layer thickness with which the fluoropolymer can be applied can vary within a wide range; In practice, layer thicknesses of 0.1 lim to 10,000 nm, in particular 1 nm to 5,000 nm, preferably 1 nm to 1,000 nm, preferably 5 nm to 500 nm, very particularly preferably 10 nm to 250 nm, have proven successful.
  • the fluoropolymer coating can be applied in a manner known per se and by any method.
  • the fluoropolymer coating is applied by bringing the inner wall to be coated or the inner walls of the tubes to be coated into contact with a solution or dispersion of the fluoropolymer (s) in question, in particular at least essentially completely therewith wetted, and then the solvent or dispersant removed. After removal of the solvent or dispersion medium, a thin, homogeneous polymer film results which adheres to the inner walls of the tubes.
  • the contacting can be carried out, for example, by immersion, spraying, misting, spraying, filling, etc. with the solution or dispersion of the fluoropolymer.
  • the fluoropolymer in particular in the form of a preferably organically based solution or dispersion, of 0.1 to 100% by weight o, preferably 1 to 10% by weight o, in particular approximately 1% by weight o, of the fluoropolymer, based on the total weight of the solution or dispersion;
  • All known, arbitrary organic solvents are suitable as solvents or dispersants, in particular those with low volatility, such as, for example, ethers, and also mixtures of such solvents.
  • Such solutions or dispersions are commercially available.
  • a 1% strength by weight solution or dispersion of a fluoropolymer in a mixture of methyl perfluoroisobutyl ether / methyl nonafluorobutyl ether has proven particularly useful 3M Kunststoff GmbH, Neuss, under the trade name "3M Easy Clean Coating ECC-1000".
  • the solvent or dispersant used can then be removed by evaporation, stripping, etc. This can be done under atmospheric pressure or under reduced pressure, either at ambient temperature or at elevated temperatures.
  • the solvent or dispersant can then optionally be recovered or recovered by condensation.
  • FIG. 1A, 1B and IC schematically illustrate the sequence of a method according to the invention in accordance with the previously described embodiment:
  • FIG. 1A shows the untreated tube body 1.
  • FIG. 1B schematically shows an embodiment of the method according to the invention, the inner walls of the tube body 1 being wetted with the solution or dispersion of a fluoropolymer 2 suitable according to the invention via a spray nozzle 3. After removal of the solvent or dispersion medium, a tube body 1 is formed, as shown in FIG. IC, which is completely and homogeneously coated with the coating of a fluoropolymer 2 on its inner walls.
  • the process according to the invention has the decisive advantage that the inner walls to be coated with the fluoropolymer do not have any surface treatment beforehand (ie before the fluoropolymer is applied), in particular no surface structuring, for example by mechanical treatment (e.g. roughening, polishing, grinding, roughening or the like) ) or by chemical treatment (e.g. by etching or the like). Nevertheless, it may be necessary in individual cases to clean, in particular degrease, the surface or inner wall to be coated before applying the fluoropolymer; this is particularly the case if - e.g. B. due to the manufacturing process of the tube - remnants of fats adhere to the surface to be coated or the inner wall.
  • the surface or inner wall to be coated with the fluoropolymer can be coated with a lacquer, resin or wax, in particular with an anti-corrosion lacquer, resin or wax, preferably an epoxy resin or a polyurethane resin, before applying the fluoropolymer. are coated, the fluoropolymer coating then finally being applied to this lacquer, resin or wax layer.
  • the thickness of the paint, resin or Wax layer can vary within wide limits and is generally in the range from 0.1 ⁇ m to 500 ⁇ m, in particular 1 ⁇ m to 100 ⁇ m. Suitable corrosion protection lacquers, resins or waxes are known to the person skilled in the art for these purposes. Examples of this are the epoxy resins of the type "ET 02/111", marketed by Hober, Bodelshausen, and of the type “R 676", marketed by Valsba, Switzerland.
  • the outer walls of the tubes can also be coated with the fluoropolymer.
  • the fluoropolymer coating applied in the manner according to the invention may be advantageous to finally subject to a heat treatment, in particular by annealing.
  • a heat treatment in particular by annealing.
  • the fluoropolymer layer being solidified and possibly hardened (if fluoroprepolymers are used, the heat treatment step can in particular also lead to further polymerisation or hardening of the prepolymers).
  • This also increases the resistance of the fluoropolymer coating and thus the corrosion resistance of the tubes.
  • the bond between the fluoropolymer layer and the underlying substrate or the underlying inner wall is improved.
  • the temperatures of the heat treatment are selected and adapted by the person skilled in the art, depending on the application, in particular with regard to the type of fluoropolymer and the tube material.
  • Heat treatment temperatures in the range from 25 ° C. to 225 ° C., in particular 50 ° C. to 200 ° C., are generally used.
  • the treatment time depends on the type of fluoropolymer and the tube material and can vary widely; in general, the treatment time is 0.01 hours to 10 hours, in particular 0.01 hours to 1 hour.
  • fluoropolymer is widely understood according to the invention and includes both fluoropolymers and fluoropolymers; Likewise, the term “fluoropolymer” as it is understood according to the invention also means the corresponding prepolymers. Any fluoropolymers and fluoropolymers and fluoropolymers can thus be used in the process according to the invention, provided that they are suitable for use in the process according to the invention. The person skilled in the art will select the suitable fluoropolymer based on his specialist knowledge, depending on the application.
  • fluoropolymers in general, reference can be made, for example, to Römpp chemistry lexicon, 10th edition, vol. 2, 1997, pp. 1393/1394, keyword: “fluoropolymers” with the literature cited therein.
  • fluoropolymers are generally referred to both fluorine-containing polymers with only carbon atoms and also those with heteroatoms in the main chain.
  • Representatives of the first groups are homopolymers and copolymers of olefinically unsaturated fluorinated monomers, of which - in alphabetical order - chlorotrifluoroethylene, fluorovinylsulfonic acid, hexafluoroisobutylene, hexafluoropropylene, perfluorovinylmethyl ether, tetrafluoroethylene, vinyl fluoride and vinylidene fluoride have become of technical importance.
  • the fluoropolymers resulting from these monomers are classified into the categories polytetrafluoroethylene, fluorothermoplastics and fluoroelastomers or fluororubbers.
  • Representatives of the fluoropolymers with heteroatoms in the main chain are the polyfluorosilicones and polyfluoroalkoxyphosphazenes as well as the fluorinated polyepoxides and polyurethanes.
  • Fluoropolymers suitable according to the invention have good adhesive properties with respect to the surfaces or inner walls to be coated of the tubes so that they adhere to them, preferably through physical or chemical interactions or bonds (e.g. covalent bonds). Furthermore, fluoropolymers suitable according to the invention have, in particular, film-forming properties. According to the invention, preference is given to using nonionic fluoropolymers.
  • Fluoropolymers suitable according to the invention are hydrophobic and oleophobic and in particular have liquid-repellent properties.
  • the method according to the invention thus results in tubes whose inner walls are coated with a hydrophobic and / or oleophobic, in particular liquid-repellent, fluoropolymer film.
  • the fluoropolymer is selected such that, based on the pure substance (ie based on the pure fluoropolymer itself), it has a surface tension (interfacial tension) ⁇ of the order of magnitude ⁇ 30 mN / m, in particular ⁇ 25 mN / m having; According to the invention, it is particularly preferred if this surface or interfacial tension of the fluoropolymer (based on the pure fluoropolymer) is in particular ⁇ 20 mN / m, particularly preferably ⁇ 18 mN / m, very particularly preferably approximately 14 mN / m to approximately 16 mN / damn.
  • PTFE polytetrafluoroethylene
  • the surface tension of the fluoropolymer coating applied according to the invention shows changed values in comparison to the pure fluoropolymer; This is due to the fact that the underlying substrate or tube metal influences the surface tension, in particular due to the small layer thickness of the fluoropolymer coating. This phenomenon, ie the change or influence of the surface tension of thin layers in contact with an underlying substrate, compared to the surface tension of the pure substance as such is known per se to the person skilled in the art.
  • the fluoropolymer coating applied directly or directly to the inner tube wall (s), in particular made of aluminum or aluminum alloys has a surface or interfacial tension of the order of magnitude ⁇ 30 mN / m, in particular ⁇ 27 mN / m, preferably ⁇ 25 mN / m, very particularly preferably ⁇ 23 mN / m.
  • a layer of a lacquer, resin and / or wax, in particular an anti-corrosion lacquer, resin and / or wax, preferably an epoxy resin, between the fluoropolymer coating and the inner tube wall (s) or a polyurethane resin is provided, d. H. If the fluoropolymer coating is not applied directly or directly to the inner wall (s) of the tube, but rather to the lacquer, resin or wax layer on top of it, this lacquer, resin or wax layer also influences the surface or interfacial tension of the fluoropolymer coating. coating.
  • the fluoropolymer coating applied to the lacquer, resin or wax layer has a surface or interfacial tension of the order of magnitude ⁇ 50 mN / m, in particular ⁇ 45 mN / m, preferably ⁇ 42 mN / m.
  • Fluoropolymers suitable according to the invention have a boiling point / range from 250 ° C. to 350 ° C., in particular 290 ° C. to 320 ° C., preferably 295 ° C. to 315 ° C., particularly preferably 300 ° C. to 310 ° C.
  • the fluoropolymers used according to the invention are preferably liquid at 20 ° C. and normal pressure (atmospheric pressure).
  • the vapor pressure of fluoropolymers suitable according to the invention is in the temperature range from 20 ° C. to 50 ° C. below 50 torr, in particular below 30 torr, preferably below 25 torr.
  • Fluoropolymers suitable according to the invention have a density at 20 ° C.
  • fluoropolymers suitable according to the invention have a water solubility at 20 ° C. of less than 10 ppm, preferably less than 5 ppm, particularly preferably less than 3 ppm. Furthermore, fluoropolymers suitable according to the invention have a dynamic viscosity at 20 ° C.
  • a fluoropolymer according to the invention which is particularly preferred according to the invention from 3M Kunststoff GmbH, Neuss, under the trade name "3M Easy Clean Coating ECC-1000" as an approximately 1% by weight solution or dispersion in methyl perfluoroisobutyl ether / Methyl nonafluorobutyl ether expelled.
  • fluoropolymers suitable according to the invention are described, for example, in EP-A-0 690 880 or in the corresponding German equivalent DE 694 05 859 T2, the respective disclosures of which are hereby fully incorporated by reference.
  • fluorine-containing polymers which have at least one mono-, di- or trivalent fluoroaliphate unit derived from a fluoroaliphatic sulfamic acid salt and which can be obtained by radical polymerization of an aqueous solution or dispersion of a polymerizable mixture of a sulfinate with a fluoroaliphatic radical and an oxidizing agent that can oxidize the sulfinate to a sulfonyl radical, such as. B.
  • the method according to the invention can be applied to all types of tubes.
  • tubes made of plastic or metal these can consist, for example, of pure metals or of alloys or of mixtures of different metals.
  • Tube metals are aluminum, iron and / or tin.
  • the method according to the invention can be applied to tubes which consist of aluminum or an aluminum alloy.
  • Such tubes can for example by cold forming, for. B. by drawing processes, in particular deep drawing, made of the metal or metals mentioned.
  • the present invention further relates to tubes which can be produced or coated using the method according to the invention.
  • FIG. 2A and 2B schematically show sections of tube bodies, the inner walls of which have been coated by the method according to the invention.
  • the inner walls of the tube body 1 are completely provided with a fluoropolymer layer 2.
  • a layer of an anti-corrosion lacquer, resin or wax 4 is additionally provided between the inner walls of the tube body 1 and the fluoropolymer coating 2.
  • the tubes which can be produced or coated according to the invention can be used to hold flowable, in particular liquid or pasty or dough-like media of all kinds, for. B. in the form of ointments or creams can be used.
  • Pharmaceuticals and pharmaceuticals, food and beverages, adhesives, chemicals, cleaning, care, washing and body care products can be mentioned here by way of example.
  • Another object of the present invention is the use of at least one fluoropolymer to increase the service life or corrosion resistance (corrosion resistance) of tubes, the inner wall (s) of the tubes being coated with the fluoropolymer.
  • corrosion resistance corrosion resistance
  • the emptiness and dust / dirt repellency of the tubes are also improved in this way.
  • the tubes were then treated as follows: o A first series of 5 tubes was not further treated. These tubes served as a reference. (“Reference tubes”) ⁇ In a second series of 5 tubes, the inner walls of the tubes were coated in a customary manner with an epoxy resin lacquer which is customary for this purpose.
  • the untreated reference tubes of the first series were completely corroded after 30 days.
  • the external appearance showed that the iodine-containing healing ointment had changed color due to reaction with the metal of the tube and had thus become unusable.
  • the iodine-containing healing ointment already changed color after 30 days, although in comparison to the first series of tubes there was no "erosion” or "corrosion". However, after 60 days, the tubes of the second series had an appearance comparable to that of the first series ("through corrosion").
  • the third series of tubes and the fourth series of tubes still showed no signs of corrosion even after 120 days.
  • the iodine wound healing ointment remained unstained.
  • An analysis of the iodine-containing healing ointment showed that there were no traces of tube material (aluminum) in the healing ointment.
  • Only after 240 days did the third series of tubes show very slight signs of corrosion (but this only limited to the inner walls, ie no "through corrosion" of the tubes), while the fourth series of tubes even after 240 days of storage at 40 ° C still remained unchanged and showed no signs of corrosion.
  • the tubes of the third and fourth series treated according to the invention thus had significantly improved service lives or corrosion resistance both compared to the reference tubes (first series) and compared to the tubes of the prior art (second series).
  • a comparison of the tubes of the third and fourth series according to the invention shows that by combining a corrosion protection lacquer (here specifically: epoxy resin lacquer) with the fluoropolymer coating provided according to the invention, an even longer service life or corrosion resistance than the fluoropolymer coating alone is achieved, ie a synergistic one Effect occurs. Furthermore, measurements of the surface or interfacial tension with respect to the inner walls of the tubes were carried out on the tubes of the first to fourth series described above.
  • a corrosion protection lacquer here specifically: epoxy resin lacquer
  • a comparison of the third and fourth series of tubes with each other also shows the influence of the substrate lying under the fluoropolymer coating (aluminum metal or epoxy resin) on the surface tension of the fluoropolymer coating.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

L'invention concerne un procédé d'élévation de la résistance à la corrosion de tubes, procédé selon lequel la paroi intérieure des tubes est recouverte d'au moins un polymère fluoré. L'invention concerne également des tubes produits selon ce procédé.
PCT/EP2004/000865 2003-03-25 2004-01-31 Procede d'elevation de la resistance a la corrosion de tubes, et tubes produits selon ce procede Ceased WO2004085557A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10313398 2003-03-25
DE10313398.4 2003-03-25
DE10313966A DE10313966A1 (de) 2003-03-25 2003-03-27 Verfahren zur Erhöhung der Korrosionsbeständigkeit von Tuben sowie auf diese Weise hergestellte Tuben
DE10313966.4 2003-03-27

Publications (1)

Publication Number Publication Date
WO2004085557A1 true WO2004085557A1 (fr) 2004-10-07

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Application Number Title Priority Date Filing Date
PCT/EP2004/000865 Ceased WO2004085557A1 (fr) 2003-03-25 2004-01-31 Procede d'elevation de la resistance a la corrosion de tubes, et tubes produits selon ce procede

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Country Link
WO (1) WO2004085557A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8790760B2 (en) 2005-07-26 2014-07-29 Basf Se Container made from plastics materials with a polymeric organofluorine interior coating for active-compound formulations for crop protection or protection of materials

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4693396A (en) * 1984-12-28 1987-09-15 Colgate-Palmolive Company Laminate substrate and article therefrom incorporating fluorinated polyethylene

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4693396A (en) * 1984-12-28 1987-09-15 Colgate-Palmolive Company Laminate substrate and article therefrom incorporating fluorinated polyethylene

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8790760B2 (en) 2005-07-26 2014-07-29 Basf Se Container made from plastics materials with a polymeric organofluorine interior coating for active-compound formulations for crop protection or protection of materials

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